JP2017029953A - Powder particle heat treatment apparatus and powder particle manufacturing method - Google Patents
Powder particle heat treatment apparatus and powder particle manufacturing method Download PDFInfo
- Publication number
- JP2017029953A JP2017029953A JP2015155154A JP2015155154A JP2017029953A JP 2017029953 A JP2017029953 A JP 2017029953A JP 2015155154 A JP2015155154 A JP 2015155154A JP 2015155154 A JP2015155154 A JP 2015155154A JP 2017029953 A JP2017029953 A JP 2017029953A
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- Prior art keywords
- toner
- powder particles
- straight line
- hot air
- heat treatment
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Abstract
Description
本発明は、電子写真法、静電記録法、静電印刷法、またはトナージェット方式記録法の如き画像形成方法に用いられるトナーの熱処理装置及びトナーの製造方法に関する。 The present invention relates to a toner heat treatment apparatus and a toner manufacturing method used in an image forming method such as an electrophotographic method, an electrostatic recording method, an electrostatic printing method, or a toner jet recording method.
電子写真の画像形成方法においては、静電荷像を現像するためのトナーが使用される。トナーの製造法としては粉砕法及び重合法に大別され、簡便な製法としては粉砕法が挙げられる。
その一般的な製法として、まず転写材に定着させるための結着樹脂、トナーとしての色味を出させる着色剤、定着部材とトナーとの剥離性を向上させるワックス等の原料を混合する。次にこれらの混合物を溶融混練、冷却固化し、混練物を得る。更に得られた混練物を粉砕手段により微細化し必要に応じて所望の粒度分布に分級した後、流動化剤等を添加することで画像形成に供するトナーとしている。
In an electrophotographic image forming method, a toner for developing an electrostatic image is used. The toner production method is roughly classified into a pulverization method and a polymerization method, and a simple production method includes a pulverization method.
As a general manufacturing method, first, a binder resin for fixing on a transfer material, a colorant for producing a color as a toner, and a wax for improving the releasability between the fixing member and the toner are mixed. Next, these mixtures are melt-kneaded and cooled and solidified to obtain a kneaded product. Further, the obtained kneaded material is refined by a pulverizing means, classified to a desired particle size distribution as necessary, and then a fluidizing agent or the like is added to obtain a toner for image formation.
近年、複写機やプリンターの高画質化及び高精細化に伴ってトナーに要求される性能も一段と厳しくなり、トナーの粒子径は小さくかつ直径１０μｍ以上の粗大粒子が含有されないシャープな粒度分布のものが要求されるようになってきている。
また高画質化として要求されることの一つとして、画像面内のグロス均一性がある。画像の面内グロスの均一性は定着部材とトナーとの剥離性に相関があることから、トナーにはグロス均一性向上のためにワックスが添加されている。
In recent years, the performance required of toner has become more severe with the increase in image quality and definition of copying machines and printers, and the particle size of the toner is small and has a sharp particle size distribution that does not contain coarse particles of 10 μm or more in diameter. Is becoming required.
Further, as one of the demands for higher image quality, there is gloss uniformity within the image plane. Since the uniformity of the in-plane gloss of the image has a correlation with the peelability between the fixing member and the toner, wax is added to the toner to improve the gloss uniformity.
更に、複写機やプリンター用の転写材として通常の紙以外にも様々なマテリアルに対応することが必要となってきており、トナーの転写性の向上も要求される。このためワックスを含有するトナー用粉体粒子を球形化することが必要とされるようになってきている。
このような要求に対し、熱処理によりトナー用粉体粒子を溶融し球形化する製法が挙げられる。しかしワックスを含有するトナー用粉体粒子を熱処理すると粉体粒子内部のワックスが溶融し、トナー用粉体粒子の表面に染み出すことによって付着力が増加する。そのため熱処理装置内に融着が発生する場合や、溶融したトナーが互いに合一することで粗大粒子が増加する場合もある。このためトナーを安定的に製造することが困難なことがあった。
Furthermore, it is necessary to deal with various materials other than ordinary paper as a transfer material for copying machines and printers, and improvement in toner transferability is also required. For this reason, it has become necessary to spheroidize powder particles for toner containing wax.
In response to such a requirement, there is a manufacturing method in which the powder particles for toner are melted and spheroidized by heat treatment. However, when the powder particles for toner containing the wax are heat-treated, the wax inside the powder particles melts and oozes out on the surface of the powder particles for toner, thereby increasing the adhesion. For this reason, fusion may occur in the heat treatment apparatus, or coarse particles may increase due to the fusion of the melted toner. For this reason, it may be difficult to stably produce the toner.
従来の熱処理によりトナー用粉体を溶融し球形化する技術としては、原料である粉体粒子を分散させるための旋回機構と、分散された粉体原料をその内側から加熱する加熱機構を持つ熱処理装置が提案されている（特許文献１参照）。
しかしこの装置構成でトナー用粉体粒子を熱処理する場合、原料の分散気流と加熱気流がお互いに逆の旋回方向となる。このため粉体粒子の処理量を増加させると、粉体粒子が互いに衝突し合一し粗大粒子になる場合や、装置内で生じる気流の乱れによって装置の天面や壁面に粉体粒子が付着し融着物が生じる場合があった。
これに対し熱処理装置の熱処理室の側壁上部からの冷却風をスリット状に吹き込むことにより粉体粒子の付着及び乱流を抑え、生産性を向上させるという提案がなされている（特許文献２参照）。
しかしこの装置構成でトナー用粉体粒子を熱処理する場合、原料の分散気流と加熱気流は旋回流であるのに対し導入される冷却風は垂直となる。このためやはり装置内で乱気流が発生してしまい、ワックスを含有するトナー用粉体粒子の処理量を増加させて熱処理を行うと、粉体粒子が互いに衝突し合一し粗大粒子になる場合や、粉体粒子が装置内に融着する場合があった。更にこの装置構成では原料の分散気流によって加熱気流が冷却されてしまうため粉体粒子の球形化に必要以上の熱量をかけなくてはならず、熱効率が悪いと言う問題があった。
これに対し、熱風を旋回して供給するための旋回部材を装置内に具備した熱処理装置が提案されている（特許文献３参照）。処理室は、円筒状の外壁と外壁内部の体積を規制するよう配置された円柱状内部部材から形成される二重円筒状となっており、旋回部材は処理室の上部に配置されている。旋回部材は複数のブレードを有しており、熱風の旋回を制御し、効率よく旋回流を生み出すため熱効率は上昇する。
しかしこの装置構成でトナー用粉体粒子を熱処理する場合、特許文献３のブレードの形状は、熱風の流れる方向をブレードの入口付近で急激に変えるものとなっている。よってブレード間を通る熱風がスムーズに流れず、熱風の一部はトナーの熱処理に使用されず無駄になるため熱効率にいまだ課題があった。また、処理室上部の円柱状内部部材近傍では流れの淀みが生じており、旋回部材方向へ向かう巻き上がり流が発生する。その巻き上がり流は高温であり、溶融状態の粉体粒子同士が合一し粗大粒子の割合が増加する問題があった。同時に溶融状態の粉体粒子が円柱状内部部材の上部の壁面に融着しやすいという問題があった。
このように熱処理によってワックスを含有するトナーを球形化するトナーの熱処理装置及び製造方法において、これまでの方法では粗大粒子と装置内融着の抑制かつ熱効率の良化に関して改良の余地があった。
As a technology for melting and spheroidizing toner powder by conventional heat treatment, there is a swivel mechanism for dispersing powder particles as raw materials, and a heat treatment having a heating mechanism for heating the dispersed powder raw materials from the inside. An apparatus has been proposed (see Patent Document 1).
However, when the powder particles for toner are heat-treated with this apparatus configuration, the raw material dispersed air flow and the heated air flow are in opposite swirl directions. For this reason, if the processing amount of the powder particles is increased, the powder particles may collide with each other to become coarse particles, or the powder particles may adhere to the top surface or wall surface of the device due to the turbulence of the airflow generated in the device. In some cases, a melted product was produced.
On the other hand, it has been proposed that the cooling air from the upper part of the side wall of the heat treatment chamber of the heat treatment apparatus is blown into a slit shape to suppress the adhesion and turbulence of the powder particles and improve the productivity (see Patent Document 2). .
However, when the powder particles for toner are heat-treated with this apparatus configuration, the dispersed air flow and heating air flow of the raw material are swirl flows, whereas the cooling air introduced is vertical. For this reason, turbulent air flow is also generated in the apparatus, and if the heat treatment is performed by increasing the processing amount of the powder particles for toner containing wax, the powder particles may collide with each other and become coarse particles. In some cases, the powder particles are fused in the apparatus. Furthermore, in this apparatus configuration, since the heated air stream is cooled by the dispersed air stream of the raw material, it is necessary to apply an amount of heat more than necessary to spheroidize the powder particles, and there is a problem that the thermal efficiency is poor.
On the other hand, the heat processing apparatus which equipped the inside with the turning member for turning and supplying a hot air is proposed (refer patent document 3). The processing chamber has a double cylindrical shape formed of a cylindrical outer wall and a columnar inner member arranged to regulate the volume inside the outer wall, and the swivel member is arranged at the upper part of the processing chamber. The swirl member has a plurality of blades, and the swirl of hot air is controlled to generate swirl flow efficiently, so that the thermal efficiency is increased.
However, when the powder particles for toner are heat-treated with this apparatus configuration, the shape of the blade of Patent Document 3 changes the direction in which hot air flows in the vicinity of the blade entrance. Therefore, the hot air passing between the blades does not flow smoothly, and a part of the hot air is not used for the heat treatment of the toner and is wasted. Further, stagnation of the flow is generated in the vicinity of the cylindrical internal member at the upper part of the processing chamber, and a winding flow toward the revolving member is generated. The winding flow is high temperature, and there is a problem that the powder particles in the molten state are united to increase the proportion of coarse particles. At the same time, there is a problem that the powder particles in a molten state are easily fused to the upper wall surface of the cylindrical inner member.
As described above, in the toner heat treatment apparatus and manufacturing method for spheroidizing the toner containing wax by heat treatment, there has been room for improvement in the conventional methods in terms of suppressing the fusion of coarse particles and the apparatus and improving the thermal efficiency.
本発明の目的は、熱処理によってワックスを含有するトナー用粉体粒子を球形化する際に、原料の処理量を増加させても粗大粒子と装置内融着を低減し、かつ投入熱量を抑制するトナーの熱処理装置及びトナーの製造方法を提供することにある。 It is an object of the present invention to reduce coarse particles and in-device fusion and suppress the amount of input heat even when the amount of raw material is increased when the powder particles for toner containing wax are spheroidized by heat treatment. It is an object of the present invention to provide a toner heat treatment apparatus and a toner manufacturing method.
本発明では上述した従来技術の課題を解決すべく鋭意検討の結果、ワックスの粉体粒子表面への染み出しと、熱処理装置の熱風、冷風の供給方法に関連があることを知見してトナーの製造方法を発明するに至った。
すなわち本発明は、ワックスを含有する粉体粒子の熱処理装置であって、該熱処理装置は、
（１）円筒状の外壁の内周面と、該外壁の内部に該外壁の中心軸と同軸上に配置された円柱状の内部部材の外周面とで形成され、該粉体粒子の熱処理が行われる同軸二重円筒状の処理室と、
（２）該処理室に該粉体粒子を供給するための粉体粒子供給手段と、
（３）供給された該粉体粒子を熱処理するための熱風を供給する熱風供給手段と、
（４）供給された該粉体粒子を冷却するための冷風を該処理室内に供給する冷風供給手段と、
（５）熱処理された該粉体粒子を該処理室の外に排出する排出手段と、
（６）該熱風を該処理室において螺旋状に旋回させるための旋回部材とを具備し、
該旋回部材は、
該内部部材の天面上に、該内部部材の中心軸から等距離に、該中心軸の周囲に配列された同形状の複数のブレードを有し、
該ブレードを含みかつ該中心軸と直交する断面において、該中心軸から近い方の該ブレードの端部と該中心軸とを結ぶ直線と、該端部に接する直線とのなす角度で規定されるブレードの入口角度ａが、下記式（１）を満たすことを特徴とする粉体粒子の熱処理装置である。
−１０°≦ａ≦１０° 式（１）
In the present invention, as a result of intensive studies to solve the above-mentioned problems of the prior art, it has been found that there is a relationship between the exudation of the wax to the powder particle surface and the method of supplying hot air and cold air of the heat treatment apparatus. It came to invent the manufacturing method.
That is, the present invention is a heat treatment apparatus for powder particles containing wax, the heat treatment apparatus comprising:
(1) An inner peripheral surface of a cylindrical outer wall and an outer peripheral surface of a cylindrical inner member arranged coaxially with the central axis of the outer wall inside the outer wall, and heat treatment of the powder particles A coaxial double cylindrical processing chamber,
(2) powder particle supply means for supplying the powder particles to the processing chamber;
(3) hot air supply means for supplying hot air for heat-treating the supplied powder particles;
(4) cold air supply means for supplying cold air for cooling the supplied powder particles into the processing chamber;
(5) discharging means for discharging the heat-treated powder particles out of the processing chamber;
(6) a swirling member for swirling the hot air in the processing chamber in a spiral shape;
The swivel member is
On the top surface of the internal member, there are a plurality of blades of the same shape arranged around the central axis at an equal distance from the central axis of the internal member,
In a cross section including the blade and perpendicular to the central axis, the cross section is defined by an angle formed by a straight line connecting the end of the blade closer to the central axis and the central axis and a straight line in contact with the end. The powder particle heat treatment apparatus is characterized in that the inlet angle a of the blade satisfies the following formula (1).
−10 ° ≦ a ≦ 10 ° Formula (1)
本発明のトナーの製造方法によれば、熱処理によってワックスを含有するトナー用粉体粒子を球形化する際に、ワックスの粉体粒子表面への染み出しと合一粒子の発生及び装置内融着を抑制し、小粒径でシャープなトナーを大量に製造することができる。 According to the toner manufacturing method of the present invention, when powder particles for toner containing wax are spheroidized by heat treatment, exudation of wax to the surface of powder particles, generation of coalesced particles, and fusion in the apparatus. And a sharp toner with a small particle diameter can be produced in large quantities.
以下、好ましい実施の形態を挙げて本発明を更に詳細に説明する。
まず、本発明に用いる熱処理装置の概略を、図１〜図１４を用いて説明する。
Hereinafter, the present invention will be described in more detail with reference to preferred embodiments.
First, an outline of a heat treatment apparatus used in the present invention will be described with reference to FIGS.
図１は、本発明による熱処理装置の一例を示した概略的斜視図である。
図２は、図１における、Ａ−Ａ´面での概略的断面図である。
図１、図２に示したように、本発明の熱処理装置は、円筒状の外壁１と、外壁１の内部の体積を規制するよう外壁１の中心軸と同軸上に配置された円柱状の内部部材２とで形成される、粉体粒子の熱処理が行われる同軸二重円筒状の処理室３を持つ。本発明の熱処理装置は、更に処理室に熱風を供給する熱風供給手段４と、粉体粒子を供給する粉体粒子供給手段５と、冷風を供給する第一冷風供給手段６及び第二冷風供給手段７と、処理室から粉体を排出する排出手段８を持つ。
FIG. 1 is a schematic perspective view showing an example of a heat treatment apparatus according to the present invention.
FIG. 2 is a schematic cross-sectional view taken along the plane AA ′ in FIG. 1.
As shown in FIGS. 1 and 2, the heat treatment apparatus of the present invention has a cylindrical outer wall 1 and a columnar shape arranged coaxially with the central axis of the outer wall 1 so as to regulate the volume inside the outer wall 1. It has a coaxial double cylindrical processing chamber 3 formed by the internal member 2 and in which heat treatment of the powder particles is performed. The heat treatment apparatus of the present invention further includes hot air supply means 4 for supplying hot air to the processing chamber, powder particle supply means 5 for supplying powder particles, first cold air supply means 6 for supplying cold air, and second cold air supply. Means 7 and discharge means 8 for discharging powder from the processing chamber.
外壁１は、処理量が３０ｋｇ／ｈｒ程度のときは内周面径Ｔ（ｍｍ）が１００ｍｍ≦Ｔ≦３００ｍｍであることが好ましく、１００ｍｍ≦Ｔ≦２００ｍｍであることがより好ましい。外壁１の内周面径が上記の範囲内であれば粉体粒子を効率良く熱処理することができる。外壁１の内周面径Ｔが１００ｍｍ以上であれば処理室３内での粉体粒子濃度が大きくなり過ぎず、処理量を増加させることができる。また内周面径Ｔが３００ｍｍ以下であれば処理室の体積に対する壁面からの冷却が強くなり過ぎず、熱効率が低下することもない。 When the processing amount is about 30 kg / hr, the outer wall 1 preferably has an inner peripheral surface diameter T (mm) of 100 mm ≦ T ≦ 300 mm, and more preferably 100 mm ≦ T ≦ 200 mm. If the inner peripheral surface diameter of the outer wall 1 is within the above range, the powder particles can be efficiently heat-treated. If the inner peripheral surface diameter T of the outer wall 1 is 100 mm or more, the powder particle concentration in the processing chamber 3 does not become too high, and the processing amount can be increased. Moreover, if the inner peripheral surface diameter T is 300 mm or less, cooling from the wall surface with respect to the volume of the processing chamber does not become excessively strong, and thermal efficiency does not decrease.
処理量が２５０ｋｇ／ｈｒ程度のときは内周面径Ｔ（ｍｍ）が３５０ｍｍ≦Ｔ≦９００ｍｍであることが好ましく、３５０ｍｍ≦Ｔ≦５５０ｍｍであることがより好ましい。外壁１の内周面径が上記の範囲内であれば粉体粒子を効率良く熱処理することができる。外壁１の内周面径Ｔが３５０ｍｍ以上であれば処理室３内での粉体粒子濃度が大きくなり過ぎず、処理量を増加させることができる。また外壁１の内周面径Ｔが５５０ｍｍ以下であれば処理室の体積に対する壁面からの冷却が強くなり過ぎず、熱効率が低下することもない。更に外壁１の内周面径Ｔが９００ｍｍ以下であればブロワーやヒーター、冷風発生装置などの熱処理装置の付帯設備を大型化する必要がなく、トナーの製造エネルギー上好ましい。 When the processing amount is about 250 kg / hr, the inner peripheral surface diameter T (mm) is preferably 350 mm ≦ T ≦ 900 mm, and more preferably 350 mm ≦ T ≦ 550 mm. If the inner peripheral surface diameter of the outer wall 1 is within the above range, the powder particles can be efficiently heat-treated. If the inner peripheral surface diameter T of the outer wall 1 is 350 mm or more, the powder particle concentration in the processing chamber 3 does not become too high, and the processing amount can be increased. Moreover, if the inner peripheral surface diameter T of the outer wall 1 is 550 mm or less, the cooling from the wall surface with respect to the volume of the processing chamber does not become too strong, and the thermal efficiency does not decrease. Further, if the inner peripheral surface diameter T of the outer wall 1 is 900 mm or less, it is not necessary to enlarge the incidental equipment of a heat treatment device such as a blower, a heater, or a cold air generator, which is preferable in terms of toner production energy.
処理室３は、外壁１及び内部部材２によって構成される。外壁１及び内部部材２は、粉体粒子の融着を防止するため冷却ジャケットによって冷却されていることが好ましい。冷却ジャケットには冷却水（好ましくはエチレングリコール等の不凍液）を導入し、処理室内面の表面温度が４０℃以下であることが好ましい。処理室内面の表面温度が４０℃以下であることにより、ワックスを含有するトナー用粉体粒子を熱処理した際に熱処理装置内の融着を軽減することができる。 The processing chamber 3 includes an outer wall 1 and an inner member 2. It is preferable that the outer wall 1 and the inner member 2 are cooled by a cooling jacket in order to prevent fusion of the powder particles. Cooling water (preferably an antifreeze such as ethylene glycol) is introduced into the cooling jacket, and the surface temperature of the processing chamber inner surface is preferably 40 ° C. or lower. When the surface temperature of the inner surface of the processing chamber is 40 ° C. or lower, fusion in the heat treatment apparatus can be reduced when the toner powder particles containing wax are heat treated.
熱風供給手段４は、処理室３の上流に設けられ、粉体粒子を熱処理するための熱風を供給する。近年要求されるトナーの転写性の向上に対応するためには熱処理された粉体粒子の平均円形度は０．９６０以上であることが好ましく、０．９６５以上であることがより好ましい。このため処理室内に供給される熱風は、熱風供給手段４の出口部での温度Ｎ（℃）が１００℃≦Ｎ≦３００℃であることが好ましい。Ｎが１００℃以上であれば粉体粒子の球形化が十分にでき、また３００℃以下であれば粉体粒子が高温になり過ぎて粒子同士の合一や装置内で融着を引き起こすこともない。 The hot air supply means 4 is provided upstream of the processing chamber 3 and supplies hot air for heat-treating the powder particles. In order to cope with the improvement in toner transfer properties required in recent years, the average circularity of the heat-treated powder particles is preferably 0.960 or more, and more preferably 0.965 or more. For this reason, it is preferable that the hot air supplied into the processing chamber has a temperature N (° C.) at the outlet of the hot air supply means 4 of 100 ° C. ≦ N ≦ 300 ° C. If N is 100 ° C. or higher, the powder particles can be sufficiently spheroidized, and if it is 300 ° C. or lower, the powder particles are too hot and may cause coalescence of particles or fusion within the apparatus. Absent.
また本発明の熱処理装置は、熱風を螺旋状に旋回させるための旋回部材９を具備している。
図３は、旋回部材９を説明する概略的断面図である。
旋回部材９は、図３に示すように、内部部材２の天面上に、内部部材の中心軸１０から等距離に、該中心軸の周囲に配列された同形状の複数のブレード１１から成る。
ブレードを含む中心軸１０と直交する断面において、
中心軸１０から近い方のブレードの端部と中心軸１０とを結ぶ直線を直線１２とし、
該端部に接する直線を直線１３とした場合に、
直線１２と直線１３とのなす角度で規定されるブレードの入口角度ａが、下記式（１）を満たすことを特徴とする。
−１０°≦ａ≦１０° 式（１）
外壁１の内周面径は１５０ｍｍ、内部部材２の外周面径は１１０ｍｍとして、熱処理装置の気流シミュレーションを実施した結果を図４、図５に示す。
Moreover, the heat processing apparatus of this invention is equipped with the turning member 9 for turning a hot air helically.
FIG. 3 is a schematic cross-sectional view illustrating the turning member 9.
As shown in FIG. 3, the swivel member 9 is composed of a plurality of blades 11 having the same shape arranged on the top surface of the internal member 2 at an equal distance from the central axis 10 of the internal member and arranged around the central axis. .
In a cross section perpendicular to the central axis 10 including the blade,
A straight line connecting the end of the blade closer to the central axis 10 and the central axis 10 is a straight line 12.
When the straight line in contact with the end is a straight line 13,
The blade entrance angle a defined by the angle formed by the straight line 12 and the straight line 13 satisfies the following formula (1).
−10 ° ≦ a ≦ 10 ° Formula (1)
FIG. 4 and FIG. 5 show the results of airflow simulation of the heat treatment apparatus with the inner peripheral surface diameter of the outer wall 1 being 150 mm and the outer peripheral surface diameter of the inner member 2 being 110 mm.
図４、図５は、旋回部材９の高さ中央における処理室の中心軸と直交する断面における、熱風の流れの向きを矢印の向きで示し、熱風の速度の大きさを矢印の色の濃淡（レンジ）で示している。
図４は、ブレードの入口角度ａが７１°のときの流れの向きを示す断面図である。
図５は、ブレードの入口角度ａが０°のときの流れの向きを示す断面図である。
熱風流量はともに３．０ｍ３／分である。図４から分かるように、入口角度ａが大きいとき、ブレード１１の入口付近で熱風の流れる方向が急激に変わるため、ブレード間を通る熱風がスムーズに流れず、ブレード内で渦が生じている。これは熱効率の低下につながる。一方、図５から分かるように、ブレードの入口角度ａが０°のとき、ブレードの入口付近で熱風はスムーズに流れる。よってブレード間を通る熱風を無駄なくトナーの熱処理に使用できる。
4 and 5 show the direction of hot air flow in the direction perpendicular to the central axis of the processing chamber at the center of the height of the swivel member 9 in the direction of the arrow, and the magnitude of the speed of the hot air in the shade of the color of the arrow. (Range).
FIG. 4 is a cross-sectional view showing the flow direction when the inlet angle a of the blade is 71 °.
FIG. 5 is a cross-sectional view showing the flow direction when the inlet angle a of the blade is 0 °.
Both hot air flow rates are 3.0 m 3 / min. As can be seen from FIG. 4, when the inlet angle a is large, the direction of hot air flowing abruptly changes near the inlet of the blade 11, so the hot air passing between the blades does not flow smoothly, and vortices are generated in the blade. This leads to a decrease in thermal efficiency. On the other hand, as can be seen from FIG. 5, when the blade inlet angle a is 0 °, the hot air flows smoothly in the vicinity of the blade inlet. Therefore, the hot air passing between the blades can be used for heat treatment of the toner without waste.
また実機で確認したところ、−１０°≦ａ≦１０°の範囲であれば熱風温度を大きく上昇させることなくトナーを熱処理できることが分かった。つまりこの範囲内であればトナーの熱処理時に目立った熱効率の低下は見られないことが分かった。
入口角度ａがこの範囲外になると、熱効率低下を補うため熱風温度を上昇する必要があり、熱風温度の上昇による粉体粒子の合一が発生しやすい。
Further, as a result of confirmation with an actual machine, it has been found that the toner can be heat-treated without significantly increasing the hot air temperature within a range of −10 ° ≦ a ≦ 10 °. In other words, within this range, it was found that there was no noticeable decrease in thermal efficiency during the heat treatment of the toner.
If the inlet angle a is outside this range, it is necessary to increase the hot air temperature to compensate for the decrease in thermal efficiency, and coalescence of powder particles due to the increase in hot air temperature is likely to occur.
図６は、本発明の熱処理装置に用いられるブレードの出口角度と垂直出口角度を説明する概略的断面図である。
図６に示すように、ブレード１１を含みかつ中心軸１０と直交する断面において、
中心軸１０から遠い方のブレードの端部と中心軸１０とを結ぶ直線を直線１４とし、
該端部に接する直線を接線１５とした場合に、
直線１４と接線１５とのなす角度で規定されるブレードの出口角度をｂとする。
また、第１のブレードの中心軸１０から遠い方の端部と中心軸１０とを結ぶ直線を直線１６とし、
第１のブレードと旋回方向側に隣り合う第２のブレードの法線のうち、第１のブレードの中心軸１０から遠い方の端部を通る直線を直線１７とし、
第１のブレードの中心軸１０から遠い方の端部を通り、かつ直線１７に対して直交する直線を直線１８とした場合に、
直線１６と直線１８とのなす角度で規定されるブレードの垂直出口角度をｃとする。
このとき、本発明による旋回部材９においては、下記式（２）を満たすことが好ましい。
０°≦ｂ−ｃ≦１０° 式（２）
外壁１の内周面径は１５０ｍｍ、内部部材２の外周面径は１１０ｍｍとして、熱処理装置の気流シミュレーションを実施した結果を図７、図８に示す。
FIG. 6 is a schematic cross-sectional view for explaining the exit angle and vertical exit angle of the blade used in the heat treatment apparatus of the present invention.
As shown in FIG. 6, in a cross section including the blade 11 and orthogonal to the central axis 10,
A straight line connecting the end of the blade farther from the central axis 10 and the central axis 10 is a straight line 14;
When the straight line in contact with the end is tangent 15,
Let b be the exit angle of the blade defined by the angle formed by the straight line 14 and the tangent 15.
Further, a straight line connecting the end far from the central axis 10 of the first blade and the central axis 10 is a straight line 16,
Of the normal lines of the second blade adjacent to the first blade in the swirl direction side, a straight line passing through the end far from the central axis 10 of the first blade is defined as a straight line 17.
When a straight line that passes through the end portion far from the central axis 10 of the first blade and is orthogonal to the straight line 17 is a straight line 18,
Let c be the vertical exit angle of the blade defined by the angle formed by the straight line 16 and the straight line 18.
At this time, in the turning member 9 according to the present invention, it is preferable to satisfy the following formula (2).
0 ° ≦ b−c ≦ 10 ° Formula (2)
FIG. 7 and FIG. 8 show the results of air flow simulation of the heat treatment apparatus with the outer peripheral surface diameter of the outer wall 1 being 150 mm and the outer peripheral surface diameter of the inner member 2 being 110 mm.
図７、図８は、旋回部材９の高さ中央における処理室の中心軸と直交する断面における、熱風の流れの向きを矢印の向きで示し、熱風の速度の大きさを矢印の色の濃淡（レンジ）で示している。
図７は、出口角度ｂが９０°、垂直出口角度ｃが６５°のときの結果であり、ｂ−ｃ＝２５°である。
図８は、出口角度ｂが８０°、垂直出口角度ｃが７７°のときの結果であり、ｂ−ｃ＝３°である。熱風流量はともに３．０ｍ３／分である。
7 and 8 show the direction of hot air flow in the direction perpendicular to the central axis of the processing chamber at the center of the height of the swivel member 9 in the direction of the arrow, and the magnitude of the speed of the hot air in the shade of the color of the arrow. (Range).
FIG. 7 shows the results when the exit angle b is 90 ° and the vertical exit angle c is 65 °, and bc = 25 °.
FIG. 8 shows the results when the exit angle b is 80 ° and the vertical exit angle c is 77 °, and bc = 3 °. Both hot air flow rates are 3.0 m 3 / min.
シミュレーション結果を用いて、ブレード１１間の熱風出口の一つを３等分したときの周方向速度の平均値を算出した。算出した位置を図７にａ１、ａ２、ａ３、図８にｂ１、ｂ２、ｂ３として示している。それぞれの算出値は、ａ１＝３７．０ｍ／秒、ａ２＝３４．１ｍ／秒、ａ３＝２５．６ｍ／秒、ｂ１＝４５．８ｍ／秒、ｂ２＝４３．２ｍ／秒、ｂ３＝３７．４ｍ／秒となった。 Using the simulation results, the average value of the circumferential speed when one of the hot air outlets between the blades 11 was divided into three equal parts was calculated. The calculated positions are shown as a1, a2, a3 in FIG. 7 and b1, b2, b3 in FIG. The calculated values are as follows: a1 = 37.0 m / sec, a2 = 34.1 m / sec, a3 = 25.6 m / sec, b1 = 45.8 m / sec, b2 = 43.2 m / sec, b3 = 37. It became 4 m / sec.
ここで、熱風出口での周方向速度のばらつきを、この算出値を用いて、（ブレード間の両端部の周方向速度差／ブレード外側の周方向速度）によって算出する。図７は、（ａ１−ａ３）／ａ１＝（３７．０−２５．６）／（３７．０）＝０．３１となる。一方、図８は、（ｂ１−ｂ３）／ｂ１＝（４５．８−３７．４）／（４５．８）＝０．１８となる。これより、図８のブレード形状の方が、図７のブレード形状よりも熱風出口での周方向速度のばらつきが小さいことが分かる。 Here, the variation in the circumferential speed at the hot air outlet is calculated by (the difference in the circumferential speed at both ends between the blades / the circumferential speed outside the blade) using this calculated value. In FIG. 7, (a1−a3) / a1 = (37.0−25.6) / (37.0) = 0.31. On the other hand, in FIG. 8, (b1-b3) / b1 = (45.8-37.4) / (45.8) = 0.18. From this, it can be seen that the blade shape of FIG. 8 has less variation in the circumferential speed at the hot air outlet than the blade shape of FIG.
つまり、ブレード１１の出口角度ｂと垂直出口角度ｃの差が小さいとき、ブレードから流出する熱風の周方向速度のばらつきが小さくなることが分かった。また、更なる検討の結果、ｂ−ｃ＝０°のときばらつきが最も小さくなることが分かった。
ブレードから流出する熱風の周方向速度のばらつきが小さくなると、粉体粒子に偏りなく十分な遠心力を与えることができ、粉体粒子の合一を抑制することができる。また実機検討との比較により、粉体粒子の合一を許容値以内に抑えるためには、周方向速度のばらつきを０．２０以下にすればよいことが分かった。その時、ばらつきが０．２０となるのはｂ−ｃ＝１０°のときであることから、０°≦ｂ−ｃ≦１０°ならば、粉体粒子に十分な遠心力を与えることができ、粉体粒子の合一を許容値以内に抑制できる。
That is, it was found that when the difference between the outlet angle b of the blade 11 and the vertical outlet angle c is small, the variation in the circumferential speed of the hot air flowing out from the blade is small. Further, as a result of further investigation, it was found that the variation is the smallest when bc = 0 °.
When the variation in the circumferential speed of the hot air flowing out from the blade is reduced, a sufficient centrifugal force can be applied to the powder particles without deviation, and coalescence of the powder particles can be suppressed. In addition, it was found by comparison with actual machine studies that the variation in the circumferential speed should be 0.20 or less in order to keep the coalescence of the powder particles within an allowable value. At that time, since the variation becomes 0.20 when bc = 10 °, if 0 ° ≦ b−c ≦ 10 °, a sufficient centrifugal force can be applied to the powder particles, The coalescence of the powder particles can be suppressed within an allowable value.
熱風供給手段４は、略円錐状の分配部材１９をさらに持つことが好ましい。熱風供給手段が略円錐状の分配部材を持つことにより処理室３に供給された熱風の偏りを無くすことができ、粉体粒子を熱処理する際に過剰な温度をかける必要が無くなる。 The hot air supply means 4 preferably further has a substantially conical distribution member 19. Since the hot air supply means has a substantially conical distribution member, the bias of the hot air supplied to the processing chamber 3 can be eliminated, and it is not necessary to apply an excessive temperature when the powder particles are heat-treated.
粉体粒子供給手段５は、熱風供給手段４の下流に外壁１の内周面に供給されるように設けられ、粉体粒子は高圧エア供給ノズル（図示せず）からの搬送気体によって搬送され処理室３に供給される。 The powder particle supply means 5 is provided downstream of the hot air supply means 4 so as to be supplied to the inner peripheral surface of the outer wall 1, and the powder particles are conveyed by a carrier gas from a high pressure air supply nozzle (not shown). It is supplied to the processing chamber 3.
図９は、本発明の熱処理装置に用いられる粉体粒子供給手段の位置を示す概略的断面図である。
粉体粒子供給手段５は、図９に示すように搬送気体が外壁の内周面の接線に沿いかつ装置内の熱風螺旋流の方向と一致して供給されるように配置される。これにより粉体粒子を含む搬送気流が処理室３に入った瞬間の乱気流が防止できるため、粗大粒子の発生を抑制することができる。
FIG. 9 is a schematic sectional view showing the position of the powder particle supply means used in the heat treatment apparatus of the present invention.
As shown in FIG. 9, the powder particle supply means 5 is arranged so that the carrier gas is supplied along the tangent line of the inner peripheral surface of the outer wall and in accordance with the direction of the hot air spiral flow in the apparatus. Thereby, since the turbulent air flow at the moment when the carrier air flow containing the powder particles enters the processing chamber 3 can be prevented, the generation of coarse particles can be suppressed.
粉体粒子供給手段５は、円筒状の処理室３の中心軸と直交する同一断面上に存在するように処理室の外周部に複数設けられている。粉体粒子供給手段の分割数が多いほど、一口当たりの粉体粒子濃度を低下することができる。そのため分割数に応じて熱処理に必要な熱風温度を低下させることが可能となる。また同様の理由で粉体粒子の処理量が増加した場合、合一粒子の発生を防止することが可能となる。 A plurality of powder particle supply means 5 are provided on the outer periphery of the processing chamber so as to exist on the same cross section orthogonal to the central axis of the cylindrical processing chamber 3. The greater the number of divided powder particle supply means, the lower the powder particle concentration per mouth. Therefore, the hot air temperature required for the heat treatment can be lowered according to the number of divisions. Moreover, when the processing amount of powder particles increases for the same reason, it is possible to prevent the generation of coalesced particles.
なお、本発明の熱処理装置の粉体供給手段の分割数は例えば外壁１の内周面径が１５０ｍｍの場合は、４分割から８分割の間が好ましく、より好ましくは４分割導入である。粉体供給手段が４分割の場合、熱風温度の低減と合一粒子の発生の抑制に対し最大の効果がある。４分割以上であれば上述の粉体粒子供給手段一口当たりの粉体濃度の低減効果および処理量の増加が期待できる。また８分割以下であれば粉体粒子供給手段の出口同士が近すぎず、分割導入された粉体粒子が処理室内で再度合流したりしない。 For example, when the inner peripheral surface diameter of the outer wall 1 is 150 mm, the number of divisions of the powder supply means of the heat treatment apparatus of the present invention is preferably between 4 and 8 divisions, more preferably 4 divisions. When the powder supply means is divided into four parts, the maximum effect is obtained for reducing the hot air temperature and suppressing the generation of coalesced particles. If it is four or more, it is expected that the powder concentration per unit of the powder particle supply means is reduced and the processing amount is increased. In addition, if the number of divisions is eight or less, the outlets of the powder particle supply means are not too close to each other, and the divided and introduced powder particles do not merge again in the processing chamber.
第一冷風供給手段６及び第二冷風供給手段７は、粉体粒子供給手段５の下流に設置され、粉体粒子を冷却するための冷風を供給する。 The first cold air supply means 6 and the second cold air supply means 7 are installed downstream of the powder particle supply means 5 and supply cold air for cooling the powder particles.
図１０は、第一冷風供給手段の位置を示す概略的断面図である。
第一冷風供給手段６は、図１０に示すように供給された冷風が外壁１の内周面に沿って供給されるように、かつ装置内螺旋流の方向と一致するように、かつ円筒状の外壁の中心軸と直交する同一断面上に存在するように複数設けられている。これにより装置内に冷風が導入された瞬間の乱気流を防止でき、合一粒子の発生を抑制することができる。
FIG. 10 is a schematic cross-sectional view showing the position of the first cold air supply means.
The first cold air supply means 6 has a cylindrical shape so that the supplied cold air is supplied along the inner peripheral surface of the outer wall 1 and coincides with the direction of the spiral flow in the apparatus as shown in FIG. A plurality of the outer walls are provided on the same cross section perpendicular to the central axis of the outer wall. Thereby, the turbulent airflow at the moment when cold air is introduced into the apparatus can be prevented, and the generation of coalesced particles can be suppressed.
なお、粉体粒子供給手段５より下側かつ第一冷風供給手段６より上側の、粉体粒子供給手段５と第一冷風供給手段６に囲まれた領域は粉体粒子の熱処理ゾーンとなる。このため第一冷風供給手段６は粉体粒子の熱変形が十分に完了した位置に配置すればよい。
第一冷風供給手段６は、分割数が多いほど熱処理された粉体粒子を冷却する効率が高まる。これによって粉体粒子の冷却ムラが抑制され、円形度のそろった粉体粒子を製造することが可能となる。なお、図１０に示す例では、第一冷風供給手段６の分割数は、粉体粒子供給手段５と同じである４分割とした。
An area surrounded by the powder particle supply means 5 and the first cold air supply means 6 below the powder particle supply means 5 and above the first cold air supply means 6 is a heat treatment zone for the powder particles. For this reason, the 1st cold wind supply means 6 should just be arrange | positioned in the position where the thermal deformation of the powder particle was fully completed.
The first cold air supply means 6 increases the efficiency of cooling the heat-treated powder particles as the number of divisions increases. As a result, uneven cooling of the powder particles is suppressed, and powder particles with uniform circularity can be produced. In the example shown in FIG. 10, the number of divisions of the first cold air supply unit 6 is the same as that of the powder particle supply unit 5.
図１１は、第二冷風供給手段及び排出手段の位置を示す概略的断面図である。
第二冷風供給手段７は、図１１に示すように３分割し、供給された冷風が外壁１の内周面に沿って供給されるようかつ装置内旋回流を維持するように外壁の内周面の下端部に配置する。これによって底面に滞留融着する粉体粒子を抑制することができる。
FIG. 11 is a schematic cross-sectional view showing the positions of the second cold air supply means and the discharge means.
The second cold air supply means 7 is divided into three parts as shown in FIG. 11 so that the supplied cold air is supplied along the inner peripheral surface of the outer wall 1 and maintains the swirl flow in the apparatus. Place at the bottom of the surface. As a result, powder particles staying and fusing on the bottom surface can be suppressed.
排出手段８は、図１１に示すように外壁の内周面の下端部に配置され、熱処理された粉体粒子を処理室外に排出する。また、図１、２に示すように、排出手段８は旋回する粉体粒子の旋回方向を維持するように設けている。
これによって粉体粒子にかかる遠心力を利用して、粉体粒子の乱れを防止しつつ速やかに装置外へ排出することが可能となり、外壁１及び内部部材２への付着、融着が軽減される。なお排出手段８の先にはブロワー（不図示）が設けられ、ブロワーにより吸引搬送される構成となる。
As shown in FIG. 11, the discharge means 8 is disposed at the lower end portion of the inner peripheral surface of the outer wall, and discharges the heat-treated powder particles out of the processing chamber. As shown in FIGS. 1 and 2, the discharging means 8 is provided so as to maintain the swirling direction of the swirling powder particles.
As a result, the centrifugal force applied to the powder particles can be used to quickly discharge out of the apparatus while preventing disturbance of the powder particles, and adhesion and fusion to the outer wall 1 and the inner member 2 can be reduced. The A blower (not shown) is provided at the tip of the discharge means 8 and is sucked and conveyed by the blower.
熱処理装置内に供給される圧縮エア、熱風及び冷風の流量の総量ＱＩＮとブロワーにより吸引される風量ＱＯＵＴの関係は、ＱＩＮ≦ＱＯＵＴの関係となるように調整されるのが好ましい。ＱＩＮ≦ＱＯＵＴであれば装置内の圧力が負圧となるため、処理室内のトナー粒子が装置外に排出されやすくなり粉体粒子が過剰に熱を受けることを防止できる。その結果、合一粒子の増加や装置内の融着を低減することができるため長期のトナー製造が可能となる。 The relationship between the total amount QIN of the flow rates of compressed air, hot air, and cold air supplied into the heat treatment apparatus and the air amount QOUT sucked by the blower is preferably adjusted so as to satisfy the relationship of QIN ≦ QOUT. If QIN ≦ QOUT, the pressure inside the apparatus becomes negative, so that the toner particles in the processing chamber are easily discharged out of the apparatus, and the powder particles can be prevented from receiving excessive heat. As a result, the increase in coalesced particles and the fusion in the apparatus can be reduced, so that long-term toner production is possible.
内部部材２は、外壁１と該外壁内部の体積を規制するよう外壁中心軸と同軸上に配置される。
これによって処理室３は同軸二重円筒状となり、トナー流速が速くなり、粉体粒子の排出性を向上させることができるとともに、排出手段８近傍における付着や融着、粉体粒子の合一を防止することができる。
The inner member 2 is arranged coaxially with the outer wall central axis so as to regulate the outer wall 1 and the volume inside the outer wall.
As a result, the processing chamber 3 has a coaxial double cylindrical shape, the toner flow rate is increased, the powder particle dischargeability can be improved, and adhesion and fusion in the vicinity of the discharge means 8 and the coalescence of the powder particles can be performed. Can be prevented.
図１２は、本発明の熱処理装置に用いられる処理室上部の概略的断面図である。
図１２に示すように、内部部材２の上端部の曲率半径をＲとし、外壁１の内周面の半径（内周面径）と内部部材２の外周面の半径（外周面径）との差（内外円筒半径差）をｄとした場合に、式（３）を満たすことが好ましい。
Ｒ≧０．１×ｄ 式（３）
外壁１の内周面径を１５０ｍｍとし、内部部材２の外周面径を１１０ｍｍとして、熱処理装置の気流シミュレーションを実施した結果を図１３、図１４に示す。
FIG. 12 is a schematic cross-sectional view of the upper part of the processing chamber used in the heat treatment apparatus of the present invention.
As shown in FIG. 12, the radius of curvature of the upper end portion of the inner member 2 is R, and the radius of the inner peripheral surface (inner peripheral surface diameter) of the outer wall 1 and the radius of the outer peripheral surface of the inner member 2 (outer peripheral surface diameter). When the difference (inner and outer cylinder radius difference) is d, it is preferable to satisfy the expression (3).
R ≧ 0.1 × d Formula (3)
FIG. 13 and FIG. 14 show the results of airflow simulation of the heat treatment apparatus with the inner wall surface diameter of the outer wall 1 being 150 mm and the outer surface diameter of the inner member 2 being 110 mm.
図１３は、前記曲率半径Ｒが０ｍｍのときの流れの向きを示す断面図である。
図１４は、前記曲率半径Ｒが７ｍｍのときの流れの向きを示す断面図である。
図１３、図１４は、処理室３の中心軸を含み、中心軸と平行な断面における熱風の流れの向きを矢印の向きで示し、熱風の速度の大きさを矢印の色の濃淡（レンジ）で示している。
図１３は、内外円筒半径差ｄ＝２０ｍｍに対し曲率半径Ｒ＝０ｍｍのとき、つまりＲ／ｄ＝０のときの結果である。図１４は、内外円筒半径差ｄ＝２０ｍｍに対し曲率半径Ｒ＝７ｍｍのとき、つまりＲ／ｄ＝０．３５のときの結果である。熱風流量はともに３．０ｍ３／分である。
FIG. 13 is a cross-sectional view showing the flow direction when the radius of curvature R is 0 mm.
FIG. 14 is a cross-sectional view showing the flow direction when the radius of curvature R is 7 mm.
FIGS. 13 and 14 include the central axis of the processing chamber 3 and indicate the direction of hot air flow in the direction parallel to the cross section parallel to the central axis in the direction of the arrow. The magnitude of the hot air velocity is shaded by the color of the arrow (range). Is shown.
FIG. 13 shows the results when the radius of curvature R = 0 mm with respect to the inner / outer cylindrical radius difference d = 20 mm, that is, when R / d = 0. FIG. 14 shows the results when the radius of curvature R = 7 mm with respect to the inner / outer cylindrical radius difference d = 20 mm, that is, when R / d = 0.35. Both hot air flow rates are 3.0 m 3 / min.
図１３から分かるように、曲率半径Ｒが０ｍｍのとき、旋回部材９から処理室３へと流れる熱風は急激に曲がる流れとなり、処理室の上部かつ内部部材２の近傍に旋回部材の方向へ向かう巻き上がり流が発生する。
一方、図１４から分かるように、円柱状内部部材の上端部に曲率を持たせることで、熱風は円柱状内部部材の上端部の丸みに沿って流れることになり、処理室の上部かつ円柱状内部部材の近傍に発生する巻き上がり流が抑制される。
巻き上がり流が抑制されると円柱状内部部材上部の壁面への融着を低減することができる。ちなみに図１３、図１４の左上にも巻き上がり流が発生しているが、この部分にはトナーは入り込まないため融着は生じない。
As can be seen from FIG. 13, when the radius of curvature R is 0 mm, the hot air flowing from the swiveling member 9 to the processing chamber 3 becomes a sharply bending flow, and moves toward the swiveling member in the upper part of the processing chamber and in the vicinity of the internal member 2. A roll-up flow is generated.
On the other hand, as can be seen from FIG. 14, by giving a curvature to the upper end portion of the cylindrical inner member, the hot air flows along the roundness of the upper end portion of the cylindrical inner member. Winding flow generated in the vicinity of the internal member is suppressed.
When the rolling-up flow is suppressed, the fusion of the upper part of the cylindrical inner member to the wall surface can be reduced. Incidentally, a roll-up flow is also generated in the upper left of FIGS. 13 and 14, but since no toner enters this portion, no fusing occurs.
実機で曲率半径を変更し検討を重ねた結果、曲率半径Ｒ≧０．１×ｄとなるとき、円柱状内部部材上部の壁面への融着をほとんど見られない状態に低減できることが分かった。また、曲率半径Ｒ≧０．５×ｄとなるとき、融着を全く見られない状態に低減できることが分かった。
ただし、曲率半径を大きくすると旋回部材９の熱風出口が上下に伸び、熱風出口の面積が大きくなり、そのため熱風速度が遅くなり熱効率が低下する可能性がある。
よって曲率半径Ｒは融着の低減と熱効率の両立を考え、以下の範囲で制御することが好ましい。
（０．１×ｄ）≦Ｒ＜（１．０×ｄ）
As a result of changing the radius of curvature with the actual machine and repeatedly examining it, it was found that when the radius of curvature R ≧ 0.1 × d, it was possible to reduce the fusion to the wall surface of the upper part of the cylindrical inner member to be hardly seen. Further, it has been found that when the radius of curvature R ≧ 0.5 × d, the fusion can be reduced to a state where no fusion is seen.
However, when the radius of curvature is increased, the hot air outlet of the swiveling member 9 extends vertically, and the area of the hot air outlet increases, so that the hot air speed becomes slow and the thermal efficiency may decrease.
Therefore, the curvature radius R is preferably controlled within the following range in consideration of both fusion reduction and thermal efficiency.
(0.1 × d) ≦ R <(1.0 × d)
次に、本発明のトナー粒子製造装置を用いて、トナーを製造する手順について説明する。
［トナー製造手順］
＜原料混合工程＞
まず、原料混合工程では、トナー原料として、少なくとも樹脂、着色剤を所定量秤量して配合し、混合する。混合装置の一例としては、ヘンシェルミキサー（日本コークス工業（株）製）；スーパーミキサー（（株）カワタ製）；リボコーン（（株）大川原製作所製）；ナウターミキサー、タービュライザー、サイクロミックス（ホソカワミクロン（株）製）；スパイラルピンミキサー（太平洋機工（株）製）；レーディゲミキサー（（株）マツボー製）等がある。
Next, a procedure for producing toner using the toner particle production apparatus of the present invention will be described.
[Toner manufacturing procedure]
<Raw material mixing process>
First, in the raw material mixing step, at least a resin and a colorant are weighed and mixed as a toner raw material, and mixed. As an example of the mixing device, Henschel mixer (manufactured by Nippon Coke Industries Co., Ltd.); Super mixer (manufactured by Kawata Co., Ltd.); Ribocorn (manufactured by Okawara Seisakusho Co., Ltd.); Hosokawa Micron Co., Ltd.); Spiral Pin Mixer (manufactured by Taiheiyo Kiko Co., Ltd.); and Ladige Mixer (manufactured by Matsubo Co., Ltd.).
＜溶融混練工程＞
更に、混合したトナー原料を溶融混練工程にて、溶融混練して、樹脂類を溶融し、その中の着色剤等を分散させる。混練装置の一例としては、ＴＥＭ型押し出し機（東芝機械（株）製）；ＴＥＸ二軸混練機（（株）日本製鋼所製）；ＰＣＭ混練機（（株）池貝製）；ニーデックス（日本コークス工業（株）製）等が挙げられる。連続生産できる等の優位性から、バッチ式練り機よりも、１軸または２軸押出機といった連続式の練り機が好ましい。
＜冷却工程＞
更に、トナー原料を溶融混練することによって得られる着色樹脂組成物は、溶融混練後、２本ロール等で圧延され、水冷等で冷却する冷却工程を経て冷却される。
<Melting and kneading process>
Further, the mixed toner material is melt-kneaded in a melt-kneading step to melt the resins and disperse the colorant and the like therein. As an example of the kneading apparatus, a TEM type extruder (manufactured by Toshiba Machine Co., Ltd.); a TEX twin-screw kneader (manufactured by Nippon Steel Works, Ltd.); a PCM kneader (manufactured by Ikekai Co., Ltd.); Coke Kogyo Co., Ltd.). A continuous kneader such as a single-screw or twin-screw extruder is preferable to a batch kneader because of the advantage of being capable of continuous production.
<Cooling process>
Furthermore, the colored resin composition obtained by melt-kneading the toner raw material is rolled by a two-roll roll after melt-kneading, and then cooled through a cooling step of cooling by water cooling or the like.
＜粉砕工程＞
上記で得られた着色樹脂組成物の冷却物は、次いで、粉砕工程で所望の粒径にまで粉砕される。粉砕工程では、まず、クラッシャー、ハンマーミル、フェザーミル等で粗粉砕され、更に、クリプトロンシステム（川崎重工業（株）製）、スーパーローター（日清エンジニアリング（株）製）等で微粉砕され、トナー微粒子を得る。
<Crushing process>
The cooled product of the colored resin composition obtained above is then pulverized to a desired particle size in a pulverization step. In the pulverization process, first, coarsely pulverized with a crusher, hammer mill, feather mill, etc., and further finely pulverized with a kryptron system (manufactured by Kawasaki Heavy Industries, Ltd.), a super rotor (manufactured by Nissin Engineering Co., Ltd.), etc. Toner fine particles are obtained.
＜分級工程＞
得られたトナー微粒子は、分級工程にて、所望の粒径を有するトナー用粉体粒子に分級される。分級機としては、ターボプレックス、ファカルティ 、ＴＳＰセパレータ、ＴＴＳＰセパレータ（ホソカワミクロン（株）製）；エルボージェット（日鉄鉱業（株）製）等がある。
<Classification process>
The obtained toner fine particles are classified into toner powder particles having a desired particle diameter in a classification step. Examples of the classifier include turboplex, faculty, TSP separator, TTSP separator (manufactured by Hosokawa Micron Corporation); elbow jet (manufactured by Nippon Steel Mining Co., Ltd.) and the like.
＜熱処理工程＞
続いて、得られたトナー用粉体粒子を熱処理工程で本発明の熱処理装置を用いて球形化処理を行う。
本発明のトナーの製造方法においては、熱処理工程の前に、得られたトナー用粉体粒子に必要に応じて無機微粒子等を添加しても構わない。トナー用粉体粒子に無機微粒子等を添加する方法としては、トナー用粉体粒子と公知の各種外添剤を所定量配合し、粉体にせん断力を与える高速撹拌機を外添機として用いて、撹拌・混合する。
粉体にせん断力を与える高速撹拌機としては以下の高速撹拌機が挙げられる。
ヘンシェルミキサー、メカノハイブリッド（日本コークス工業（株）製）
スーパーミキサー、ノビルタ（ホソカワミクロン（株）製）等
<Heat treatment process>
Subsequently, the obtained powder particles for toner are subjected to a spheronization treatment in the heat treatment step using the heat treatment apparatus of the present invention.
In the toner production method of the present invention, inorganic fine particles or the like may be added to the obtained toner powder particles as necessary before the heat treatment step. As a method of adding inorganic fine particles or the like to toner powder particles, a high-speed stirrer that mixes a predetermined amount of toner powder particles and various known external additives and gives a shearing force to the powder is used as an external additive. Stir and mix.
Examples of the high-speed stirrer that gives a shearing force to the powder include the following high-speed stirrers.
Henschel mixer, mechano hybrid (Nippon Coke Kogyo Co., Ltd.)
Super mixer, Nobilta (manufactured by Hosokawa Micron Corporation), etc.
本発明のトナーの製造方法では、熱処理工程の前に、トナー用粉体粒子に無機微粉体が添加されていることで、トナー用粉体粒子に流動性が付与され、処理室に導入されたトナー用粉体粒子がより均一に分散して熱風と接触することが可能となる。その結果、均一性に優れたトナーを得ることができる。 In the toner manufacturing method of the present invention, the inorganic powder is added to the toner powder particles before the heat treatment step, so that fluidity is imparted to the toner powder particles and introduced into the processing chamber. The toner powder particles can be more uniformly dispersed and contacted with hot air. As a result, a toner having excellent uniformity can be obtained.
本発明のトナーの製造方法では、熱処理後に粗大な粒子が存在する場合、必要に応じて、分級によって粗大粒子を除去する工程を有していても構わない。粗大粒子を除去する分級機としては、ターボプレックス、ＴＳＰセパレータ、ＴＴＳＰセパレータ（ホソカワミクロン（株）製）；エルボージェット（日鉄鉱業（株）製）等が挙げられる。
更に、熱処理後、必要に応じて、粗粒等を篩い分けるために、例えば、ウルトラソニック（晃栄産業（株）製）；レゾナシーブ、ジャイロシフター（（株）徳寿工作所）；ターボスクリーナー（フロイント・ターボ（株）製）；ハイボルター（東洋ハイテック（株）製）等の篩分機を用いても良い。
なお、本発明の熱処理工程は上記微粉砕後であっても良いし、分級後でもよい。
In the toner manufacturing method of the present invention, when coarse particles are present after the heat treatment, a step of removing the coarse particles by classification may be included as necessary. Examples of the classifier for removing coarse particles include turboplex, TSP separator, TTSP separator (manufactured by Hosokawa Micron Corporation); elbow jet (manufactured by Nippon Steel Mining Co., Ltd.) and the like.
Further, after the heat treatment, if necessary, for example, Ultrasonic (manufactured by Koei Sangyo Co., Ltd.); Resona Sheave, Gyroshifter (Tokuju Kogyo Co., Ltd.); Turbo Screener ( A sieving machine such as Freund Turbo (made by Toyo Hitec Co., Ltd.) may be used.
The heat treatment step of the present invention may be after the fine pulverization or after classification.
［トナー構成材料］
次に本発明のトナーの製造方法に用いるトナー構成材料について説明する。
本発明で用いられる結着樹脂としては、公知の樹脂が用いられるが、例えば、ポリスチレン、ポリビニルトルエンの如きスチレン誘導体の単重合体；スチレン−プロピレン共重合体、スチレン−ビニルトルエン共重合体、スチレン−ビニルナフタリン共重合体、スチレン−アクリル酸メチル共重合体、スチレン−アクリル酸エチル共重合体、スチレン−アクリル酸ブチル共重合体、スチレン−アクリル酸オクチル共重合体、スチレン−アクリル酸ジメチルアミノエチル共重合体、スチレン−メタクリル酸メチル共重合体、スチレン−メタクリル酸エチル共重合体、スチレン−メタクリル酸ブチル共重合体、スチレン−メタクリル酸オクチル共重合体、スチレン−メタクリル酸ジメチルアミノエチル共重合体、スチレン−ビニルメチルエーテル共重合体、スチレン−ビニルエチルエーテル共重合体、スチレン−ビニルメチルケトン共重合体、スチレン−ブタジエン共重合体、スチレン−イソプレン共重合体、スチレン−マレイン酸共重合体、スチレン−マレイン酸エステル共重合体の如きスチレン系共重合体；ポリメチルメタクリレート、ポリブチルメタクリレート、ポリ酢酸ビニル、ポリエチレン、ポリプロピレン、ポリビニルブチラール、シリコーン樹脂、ポリエステル樹脂、ポリアミド樹脂、エポキシ樹脂、ポリアクリル樹脂、ロジン、変性ロジン、テルペン樹脂、フェノール樹脂、脂肪族又は脂環族炭化水素樹脂、芳香族石油樹脂が挙げられ、これらの樹脂は単独もしくは混合して用いても良い。
これらの中で、本発明の結着樹脂として好ましく用いられる重合体としては、スチレン系共重合体とポリエステルユニットを有する樹脂である。
[Toner component]
Next, the toner constituent materials used in the toner manufacturing method of the present invention will be described.
As the binder resin used in the present invention, known resins can be used. For example, homopolymers of styrene derivatives such as polystyrene and polyvinyltoluene; styrene-propylene copolymers, styrene-vinyltoluene copolymers, styrene -Vinylnaphthalene copolymer, styrene-methyl acrylate copolymer, styrene-ethyl acrylate copolymer, styrene-butyl acrylate copolymer, styrene-octyl acrylate copolymer, styrene-dimethylaminoethyl acrylate Copolymer, styrene-methyl methacrylate copolymer, styrene-ethyl methacrylate copolymer, styrene-butyl methacrylate copolymer, styrene-octyl methacrylate copolymer, styrene-dimethylaminoethyl methacrylate copolymer , Styrene-vinyl methyl ether Polymer, styrene-vinyl ethyl ether copolymer, styrene-vinyl methyl ketone copolymer, styrene-butadiene copolymer, styrene-isoprene copolymer, styrene-maleic acid copolymer, styrene-maleic acid ester copolymer Styrene copolymer such as coalesced; polymethyl methacrylate, polybutyl methacrylate, polyvinyl acetate, polyethylene, polypropylene, polyvinyl butyral, silicone resin, polyester resin, polyamide resin, epoxy resin, polyacrylic resin, rosin, modified rosin, terpene Examples thereof include resins, phenol resins, aliphatic or alicyclic hydrocarbon resins, and aromatic petroleum resins, and these resins may be used alone or in combination.
Among these, the polymer preferably used as the binder resin of the present invention is a resin having a styrene copolymer and a polyester unit.
スチレン系共重合体に用いる重合性モノマーとしては、次のようなものが挙げられる。例えば、スチレン；ｏ−メチルスチレン、ｍ−メチルスチレン、ｐ−メチルスチレン、α−メチルスチレン、ｐ−フェニルスチレン、ｐ−エチルスチレン、２，４−ジメチルスチレン、ｐ−ｎ−ブチルスチレン、ｐ−ｔｅｒｔ−ブチルスチレン、ｐ−ｎ−ヘキシルスチレン、ｐ−ｎ−オクチルスチレン、ｐ−ｎ−ノニルスチレン、ｐ−ｎ−デシルスチレン、ｐ−ｎ−ドデシルスチレン、ｐ−メトキシスチレン、ｐ−クロルスチレン、３，４−ジクロルスチレン、ｍ−ニトロスチレン、ｏ−ニトロスチレン、ｐ−ニトロスチレンの如きスチレン及びその誘導体；エチレン、プロピレン、ブチレン、イソブチレンの如き不飽和モノオレフィン類；ブタジエン、イソプレンの如き不飽和ポリエン類；塩化ビニル、塩化ビニリデン、臭化ビニル、フッ化ビニルの如きハロゲン化ビニル類；酢酸ビニル、プロピオン酸ビニル、ベンゾエ酸ビニルの如きビニルエステル類；メタクリル酸メチル、メタクリル酸エチル、メタクリル酸プロピル、メタクリル酸ｎ−ブチル、メタクリル酸イソブチル、メタクリル酸ｎ−オクチル、メタクリル酸ドデシル、メタクリル酸２−エチルヘキシル、メタクリル酸ステアリル、メタクリル酸フェニル、メタクリル酸ジメチルアミノエチル、メタクリル酸ジエチルアミノエチルの如きα−メチレン脂肪族モノカルボン酸エステル類；アクリル酸メチル、アクリル酸エチル、アクリル酸プロピル、アクリル酸ｎ−ブチル、アクリル酸イソブチル、アクリル酸ｎ−オクチル、アクリル酸ドデシル、アクリル酸２−エチルヘキシル、アクリル酸ステアリル、アクリル酸２−クロルエチル、アクリル酸フェニルの如きアクリル酸エステル類；ビニルメチルエーテル、ビニルエチルエーテル、ビニルイソブチルエーテルの如きビニルエーテル類；ビニルメチルケトン、ビニルヘキシルケトン、メチルイソプロペニルケトンの如きビニルケトン類；Ｎ−ビニルピロール、Ｎ−ビニルカルバゾール、Ｎ−ビニルインドール、Ｎ−ビニルピロリドンの如きＮ−ビニル化合物；ビニルナフタリン類；アクリロニトリル、メタクリロニトリル、アクリルアミドの如きアクリル酸もしくはメタクリル酸誘導体。 The following are mentioned as a polymerizable monomer used for a styrene-type copolymer. For example, styrene; o-methylstyrene, m-methylstyrene, p-methylstyrene, α-methylstyrene, p-phenylstyrene, p-ethylstyrene, 2,4-dimethylstyrene, pn-butylstyrene, p- tert-butyl styrene, pn-hexyl styrene, pn-octyl styrene, pn-nonyl styrene, pn-decyl styrene, pn-dodecyl styrene, p-methoxy styrene, p-chloro styrene, Styrene and its derivatives such as 3,4-dichlorostyrene, m-nitrostyrene, o-nitrostyrene, p-nitrostyrene; unsaturated monoolefins such as ethylene, propylene, butylene and isobutylene; and styrene and derivatives thereof such as butadiene and isoprene. Saturated polyenes; vinyl chloride, vinylidene chloride, vinyl bromide, fluorine Vinyl halides such as vinyl; vinyl esters such as vinyl acetate, vinyl propionate, vinyl benzoate; methyl methacrylate, ethyl methacrylate, propyl methacrylate, n-butyl methacrylate, isobutyl methacrylate, n-methacrylate Α-methylene aliphatic monocarboxylic acid esters such as octyl, dodecyl methacrylate, 2-ethylhexyl methacrylate, stearyl methacrylate, phenyl methacrylate, dimethylaminoethyl methacrylate, diethylaminoethyl methacrylate; methyl acrylate, ethyl acrylate Propyl acrylate, n-butyl acrylate, isobutyl acrylate, n-octyl acrylate, dodecyl acrylate, 2-ethylhexyl acrylate, stearyl acrylate, 2-acrylate Acrylic esters such as lorethyl and phenyl acrylate; vinyl ethers such as vinyl methyl ether, vinyl ethyl ether and vinyl isobutyl ether; vinyl ketones such as vinyl methyl ketone, vinyl hexyl ketone and methyl isopropenyl ketone; N-vinyl pyrrole; N-vinyl compounds such as N-vinyl carbazole, N-vinyl indole and N-vinyl pyrrolidone; vinyl naphthalenes; acrylic acid or methacrylic acid derivatives such as acrylonitrile, methacrylonitrile and acrylamide.
更に、マレイン酸、シトラコン酸、イタコン酸、アルケニルコハク酸、フマル酸、メサコン酸の如き不飽和二塩基酸；マレイン酸無水物、シトラコン酸無水物、イタコン酸無水物、アルケニルコハク酸無水物の如き不飽和二塩基酸無水物；マレイン酸メチルハーフエステル、マレイン酸エチルハーフエステル、マレイン酸ブチルハーフエステル、シトラコン酸メチルハーフエステル、シトラコン酸エチルハーフエステル、シトラコン酸ブチルハーフエステル、イタコン酸メチルハーフエステル、アルケニルコハク酸メチルハーフエステル、フマル酸メチルハーフエステル、メサコン酸メチルハーフエステルの如き不飽和二塩基酸のハーフエステル；ジメチルマレイン酸、ジメチルフマル酸の如き不飽和二塩基酸エステル；アクリル酸、メタクリル酸、クロトン酸、ケイヒ酸の如きα，β−不飽和酸；クロトン酸無水物、ケイヒ酸無水物の如きα，β−不飽和酸無水物、前記α，β−不飽和酸と低級脂肪酸との無水物；アルケニルマロン酸、アルケニルグルタル酸、アルケニルアジピン酸、これらの酸無水物及びこれらのモノエステルの如きカルボキシル基を有するモノマーが挙げられる。 In addition, unsaturated dibasic acids such as maleic acid, citraconic acid, itaconic acid, alkenyl succinic acid, fumaric acid, mesaconic acid; maleic anhydride, citraconic anhydride, itaconic anhydride, alkenyl succinic anhydride, etc. Unsaturated dibasic acid anhydride; maleic acid methyl half ester, maleic acid ethyl half ester, maleic acid butyl half ester, citraconic acid methyl half ester, citraconic acid ethyl half ester, citraconic acid butyl half ester, itaconic acid methyl half ester, Unsaturated dibasic acid half esters such as alkenyl succinic acid methyl half ester, fumaric acid methyl half ester, mesaconic acid methyl half ester; dimethyl maleic acid, unsaturated dibasic acid ester such as dimethyl fumaric acid; acrylic acid, Α, β-unsaturated acids such as phosphoric acid, crotonic acid and cinnamic acid; α, β-unsaturated acid anhydrides such as crotonic acid anhydride and cinnamic acid anhydride, the α, β-unsaturated acids and lower fatty acids And monomers having a carboxyl group such as alkenylmalonic acid, alkenylglutaric acid, alkenyladipic acid, acid anhydrides and monoesters thereof.
更に、２−ヒドロキシエチルアクリレート、２−ヒドロキシエチルメタクリレート、２−ヒドロキシプロピルメタクリレートなどのアクリル酸またはメタクリル酸エステル類；４−（１−ヒドロキシ−１−メチルブチル）スチレン、４−（１−ヒドロキシ−１−メチルヘキシル）スチレンの如きヒドロキシ基を有するモノマーが挙げられる。
本発明ではポリエステルユニットを有する樹脂が特に好ましく用いられる。前記「ポリエステルユニット」とは、ポリエステルに由来する部分を意味し、ポリエステルユニットを構成する成分としては、具体的には、２価以上のアルコールモノマー成分と２価以上のカルボン酸、２価以上のカルボン酸無水物及び２価以上のカルボン酸エステル等の酸モノマー成分が挙げられる。
Furthermore, acrylic acid or methacrylic acid esters such as 2-hydroxyethyl acrylate, 2-hydroxyethyl methacrylate, 2-hydroxypropyl methacrylate; 4- (1-hydroxy-1-methylbutyl) styrene, 4- (1-hydroxy-1) -Methylhexyl) Monomers having a hydroxy group such as styrene.
In the present invention, a resin having a polyester unit is particularly preferably used. The “polyester unit” means a part derived from polyester. Specifically, as a component constituting the polyester unit, a divalent or higher alcohol monomer component and a divalent or higher carboxylic acid, a divalent or higher valent acid, and the like. Examples include acid monomer components such as carboxylic acid anhydrides and divalent or higher carboxylic acid esters.
本発明に用いられるトナーは、これらのポリエステルユニットを構成する成分を原料の一部とし、縮重合された部分を有する樹脂を用いることができる。
例えば、２価以上のアルコールモノマー成分として、具体的には、２価アルコールモノマー成分としては、ポリオキシプロピレン（２．２）−２，２−ビス（４−ヒドロキシフェニル）プロパン、ポリオキシプロピレン（３．３）−２，２−ビス（４−ヒドロキシフェニル）プロパン、ポリオキシエチレン（２．０）−２，２−ビス（４−ヒドロキシフェニル）プロパン、ポリオキシプロピレン（２．０）−ポリオキシエチレン（２．０）−２，２−ビス（４−ヒドロキシフェニル）プロパン、ポリオキシプロピレン（６）−２，２−ビス（４−ヒドロキシフェニル）プロパン等のビスフェノールＡのアルキレンオキシド付加物、エチレングリコール、ジエチレングリコール、トリエチレングリコール、１，２−プロピレングリコール、１，３−プロピレングリコール、１，４−ブタンジオール、ネオペンチルグリコール、１，４−ブテンジオール、１，５−ペンタンジオール、１，６−ヘキサンジオール、１，４−シクロヘキサンジメタノール、ジプロピレングリコール、ポリエチレングリコール、ポリプロピレングリコール、ポリテトラメチレングリコール、ビスフェノールＡ、水素添加ビスフェノールＡ等が挙げられる。
For the toner used in the present invention, a resin having a polycondensation portion using a component constituting these polyester units as a part of a raw material can be used.
For example, as a dihydric or higher alcohol monomer component, specifically, as a dihydric alcohol monomer component, polyoxypropylene (2.2) -2,2-bis (4-hydroxyphenyl) propane, polyoxypropylene ( 3.3) -2,2-bis (4-hydroxyphenyl) propane, polyoxyethylene (2.0) -2,2-bis (4-hydroxyphenyl) propane, polyoxypropylene (2.0) -poly Alkylene oxide adducts of bisphenol A such as oxyethylene (2.0) -2,2-bis (4-hydroxyphenyl) propane, polyoxypropylene (6) -2,2-bis (4-hydroxyphenyl) propane, Ethylene glycol, diethylene glycol, triethylene glycol, 1,2-propylene glycol, 1, -Propylene glycol, 1,4-butanediol, neopentyl glycol, 1,4-butenediol, 1,5-pentanediol, 1,6-hexanediol, 1,4-cyclohexanedimethanol, dipropylene glycol, polyethylene glycol , Polypropylene glycol, polytetramethylene glycol, bisphenol A, hydrogenated bisphenol A, and the like.
３価以上のアルコールモノマー成分としては、例えばソルビット、１，２，３，６−ヘキサンテトロール、１，４−ソルビタン、ペンタエリスリトール、ジペンタエリスリトール、トリペンタエリスリトール、１，２，４−ブタントリオール、１，２，５−ペンタントリオール、グリセリン、２−メチルプロパントリオール、２−メチル−１，２，４−ブタントリオール、トリメチロールエタン、トリメチロールプロパン、１，３，５−トリヒドロキシメチルベンゼン等が挙げられる。 Examples of the trivalent or higher alcohol monomer component include sorbit, 1,2,3,6-hexanetetrol, 1,4-sorbitan, pentaerythritol, dipentaerythritol, tripentaerythritol, 1,2,4-butanetriol. 1,2,5-pentanetriol, glycerin, 2-methylpropanetriol, 2-methyl-1,2,4-butanetriol, trimethylolethane, trimethylolpropane, 1,3,5-trihydroxymethylbenzene, etc. Is mentioned.
２価のカルボン酸モノマー成分としては、フタル酸、イソフタル酸及びテレフタル酸の如き芳香族ジカルボン酸類又はその無水物；コハク酸、アジピン酸、セバシン酸及びアゼライン酸の如きアルキルジカルボン酸類又はその無水物；炭素数６乃至１８のアルキル基又はアルケニル基で置換されたコハク酸もしくはその無水物；フマル酸、マレイン酸及びシトラコン酸の如き不飽和ジカルボン酸類又はその無水物；が挙げられる。
３価以上のカルボン酸モノマー成分としては、トリメリット酸、ピロメリット酸、ベンゾフェノンテトラカルボン酸やその無水物等の多価カルボン酸等が挙げられる。
また、その他のモノマーとしては、ノボラック型フェノール樹脂のオキシアルキレンエーテル等の多価アルコール類等が挙げられる。
Examples of the divalent carboxylic acid monomer component include aromatic dicarboxylic acids such as phthalic acid, isophthalic acid and terephthalic acid or anhydrides thereof; alkyldicarboxylic acids such as succinic acid, adipic acid, sebacic acid and azelaic acid or anhydrides thereof; And succinic acid substituted with an alkyl group or alkenyl group having 6 to 18 carbon atoms or an anhydride thereof; unsaturated dicarboxylic acids such as fumaric acid, maleic acid and citraconic acid, or anhydrides thereof.
Examples of the trivalent or higher carboxylic acid monomer component include trimellitic acid, pyromellitic acid, polyvalent carboxylic acid such as benzophenone tetracarboxylic acid and its anhydride, and the like.
Examples of other monomers include polyhydric alcohols such as oxyalkylene ethers of novolak type phenol resins.
本発明で使用される着色剤としては、以下のものが挙げられる。
黒色着色剤としては、カーボンブラック；磁性体；イエロー着色剤、マゼンタ着色剤及びシアン着色剤とを用いて黒色に調整したものが挙げられる。
The following are mentioned as a coloring agent used by this invention.
Examples of the black colorant include carbon black; a magnetic material; a black colorant prepared using a yellow colorant, a magenta colorant, and a cyan colorant.
マゼンタトナー用着色顔料しては、以下のものが挙げられる。縮合アゾ化合物、ジケトピロロピロール化合物、アンスラキノン、キナクリドン化合物、塩基染料レーキ化合物、ナフトール化合物、ベンズイミダゾロン化合物、チオインジゴ化合物、ペリレン化合物が挙げられる。具体的には、Ｃ．Ｉ．ピグメントレッド１、２、３、４、５、６、７、８、９、１０、１１、１２、１３、１４、１５、１６、１７、１８、１９、２１、２２、２３、３０、３１、３２、３７、３８、３９、４０、４１、４８：２、４８：３，４８：４、４９、５０、５１、５２、５３、５４、５５、５７：１、５８、６０、６３、６４、６８、８１：１、８３、８７、８８、８９、９０、１１２、１１４、１２２、１２３、１４４、１４６、１５０、１６３、１６６、１６９、１７７、１８４、１８５、２０２、２０６、２０７、２０９、２２０、２２１、２３８、２５４、２６９；Ｃ．Ｉ．ピグメントバイオレット１９、Ｃ．Ｉ．バットレッド１、２、１０、１３、１５、２３、２９、３５が挙げられる。
着色剤には、顔料単独で使用してもかまわないが、染料と顔料とを併用してその鮮明度を向上させた方がフルカラー画像の画質の点から好ましい。
Examples of the color pigment for magenta toner include the following. Examples include condensed azo compounds, diketopyrrolopyrrole compounds, anthraquinones, quinacridone compounds, basic dye lake compounds, naphthol compounds, benzimidazolone compounds, thioindigo compounds, and perylene compounds. Specifically, C.I. I. Pigment Red 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 21, 22, 23, 30, 31, 32, 37, 38, 39, 40, 41, 48: 2, 48: 3, 48: 4, 49, 50, 51, 52, 53, 54, 55, 57: 1, 58, 60, 63, 64, 68, 81: 1, 83, 87, 88, 89, 90, 112, 114, 122, 123, 144, 146, 150, 163, 166, 169, 177, 184, 185, 202, 206, 207, 209, 220, 221, 238, 254, 269; I. Pigment violet 19, C.I. I. Bat red 1, 2, 10, 13, 15, 23, 29, 35 are mentioned.
The colorant may be used alone as a pigment, but it is preferable from the viewpoint of the image quality of a full-color image to improve the sharpness by using a dye and a pigment together.
マゼンタトナー用染料としては、以下のものが挙げられる。Ｃ．Ｉソルベントレッド１、３、８、２３、２４、２５、２７、３０、４９、８１、８２、８３、８４、１００、１０９、１２１、Ｃ．Ｉ．ディスパースレッド９、Ｃ．Ｉ．ソルベントバイオレット８、１３、１４、２１、２７、Ｃ．Ｉ．ディスパーバイオレット１の如き油溶染料、Ｃ．Ｉ．ベーシックレッド１、２、９、１２、１３、１４、１５、１７、１８、２２、２３、２４、２７、２９、３２、３４、３５、３６、３７、３８、３９、４０、Ｃ．Ｉ．ベーシックバイオレット１、３、７、１０、１４、１５、２１、２５、２６、２７、２８などの如きの塩基性染料。 Examples of the magenta toner dye include the following. C. I solvent red 1, 3, 8, 23, 24, 25, 27, 30, 49, 81, 82, 83, 84, 100, 109, 121, C.I. I. Disper thread 9, C.I. I. Solvent Violet 8, 13, 14, 21, 27, C.I. I. Oil-soluble dyes such as Disper Violet 1, C.I. I. Basic Red 1, 2, 9, 12, 13, 14, 15, 17, 18, 22, 23, 24, 27, 29, 32, 34, 35, 36, 37, 38, 39, 40, C.I. I. Basic dyes such as basic violet 1, 3, 7, 10, 14, 15, 21, 25, 26, 27, 28.
シアントナー用着色顔料としては、以下のものが挙げられる。Ｃ．Ｉ．ピグメントブルー１、２、３、７、１５：２、１５：３、１５：４、１６、１７、６０、６２、６６；Ｃ．Ｉ．バットブルー６、Ｃ．Ｉ．アシッドブルー４５、フタロシアニン骨格にフタルイミドメチルを１乃至５個置換した銅フタロシアニン顔料。 Examples of the color pigment for cyan toner include the following. C. I. Pigment Blue 1, 2, 3, 7, 15: 2, 15: 3, 15: 4, 16, 17, 60, 62, 66; I. Bat Blue 6, C.I. I. Acid Blue 45, a copper phthalocyanine pigment in which 1 to 5 phthalimidomethyls are substituted on the phthalocyanine skeleton.
イエロー用着色顔料としては、以下のものが挙げられる。縮合アゾ化合物、イソインドリノン化合物、アンスラキノン化合物、アゾ金属化合物、メチン化合物、アリルアミド化合物。具体的には、Ｃ．Ｉ．ピグメントイエロー１、２、３、４、５、６、７、１０、１１、１２、１３、１４、１５、１６、１７、２３、６２、６５、７３、７４，８３、９３、９５、９７，１０９、１１０、１１１、１２０、１２７、１２８、１２９、１４７、１５５、１６８、１７４、１８０、１８１、１８５、１９１；Ｃ．Ｉ．バットイエロー１、３、２０が挙げられる。また、Ｃ．Ｉ．ダイレクトグリーン６、Ｃ．Ｉ．ベーシックグリーン４、Ｃ．Ｉ．ベーシックグリーン６、ソルベントイエロー１６２などの染料も使用することができる。 Examples of the color pigment for yellow include the following. Condensed azo compounds, isoindolinone compounds, anthraquinone compounds, azo metal compounds, methine compounds, allylamide compounds. Specifically, C.I. I. Pigment Yellow 1, 2, 3, 4, 5, 6, 7, 10, 11, 12, 13, 14, 15, 16, 17, 23, 62, 65, 73, 74, 83, 93, 95, 97, 109, 110, 111, 120, 127, 128, 129, 147, 155, 168, 174, 180, 181, 185, 191; I. Bat yellow 1, 3, and 20 are mentioned. In addition, C.I. I. Direct Green 6, C.I. I. Basic Green 4, C.I. I. Dyes such as Basic Green 6 and Solvent Yellow 162 can also be used.
また、上記トナーにおいて、結着樹脂に予め、着色剤を混合し、マスターバッチ化させたものを用いることが好ましい。そして、この着色剤マスターバッチとその他の原材料（結着樹脂及びワックス等）を溶融混練させることにより、トナー中に着色剤を良好に分散させることができる。
結着樹脂に着色剤を混合し、マスターバッチ化させる場合は、多量の着色剤を用いても着色剤の分散性を悪化させず、また、トナー粒子中における着色剤の分散性を良化し、混色性や透明性等の色再現性が優れる。また、転写材上でのカバーリングパワーが大きいトナーを得ることができる。また、着色剤の分散性が良化することにより、トナー帯電性の耐久安定性が優れ、高画質を維持した画像を得ることが可能となる。
Further, in the toner, it is preferable to use a toner obtained by mixing a colorant with a binder resin in advance to form a master batch. Then, the colorant can be favorably dispersed in the toner by melt-kneading this colorant master batch and other raw materials (binder resin, wax, etc.).
When a colorant is mixed with the binder resin to make a master batch, even if a large amount of colorant is used, the dispersibility of the colorant is not deteriorated, and the dispersibility of the colorant in the toner particles is improved. Excellent color reproducibility such as color mixing and transparency. Further, a toner having a large covering power on the transfer material can be obtained. Further, since the dispersibility of the colorant is improved, it is possible to obtain an image having excellent durability stability of toner chargeability and maintaining high image quality.
本発明においては、熱処理工程の前に、トナー用粉体粒子に、流動化剤、転写助剤、帯電安定化剤などをヘンシェルミキサーの如き混合機で混合して用いることができる。
また、流動化剤としては、流動性が添加前後を比較すると増加し得るものであれば、どのようなものでも使用可能である。例えば、フッ化ビニリデン微粉末、ポリテトラフルオロエチレン微粉末の如きフッ素系樹脂粉末；酸化チタン微粉末、アルミナ微粉末、湿式製法シリカ、乾式製法シリカの如き微粉末シリカ；それらをシラン化合物、及び有機ケイ素化合物、チタンカップリング剤、シリコーンオイルにより表面処理を施した処理シリカを使用することが可能である。
In the present invention, before the heat treatment step, the powder particles for toner can be mixed with a fluidizing agent, a transfer aid, a charge stabilizer and the like using a mixer such as a Henschel mixer.
As the fluidizing agent, any fluidizing agent can be used as long as it can increase the fluidity before and after the addition. For example, fluorine resin powders such as vinylidene fluoride fine powder and polytetrafluoroethylene fine powder; fine powder silica such as titanium oxide fine powder, alumina fine powder, wet process silica, and dry process silica; and silane compounds and organic It is possible to use treated silica that has been surface treated with a silicon compound, a titanium coupling agent, or silicone oil.
また酸化チタン微粉末であれば、硫酸法、塩素法、揮発性チタン化合物例えばチタンアルコキシド，チタンハライド，チタンアセチルアセトネートの低温酸化（熱分解，加水分解）により得られる酸化チタン微粒子が用いられる。結晶系としてはアナターゼ型，ルチル型，これらの混晶型，アモルファスのいずれのものも用いることができる。 In the case of titanium oxide fine powder, fine particles of titanium oxide obtained by low-temperature oxidation (thermal decomposition, hydrolysis) of sulfuric acid method, chlorine method, volatile titanium compounds such as titanium alkoxide, titanium halide and titanium acetylacetonate are used. As the crystal system, any of anatase type, rutile type, mixed crystal type thereof, and amorphous type can be used.
そしてアルミナ微粉末であれば、バイヤー法、改良バイヤー法、エチレンクロルヒドリン法、水中火花放電法、有機アルミニウム加水分解法、アルミニウムミョウバン熱分解法、アンモニウムアルミニウム炭酸塩熱分解法、塩化アルミニウムの火焔分解法により得られるアルミナ微粉体が用いられる。結晶系としてはα，β，γ，δ，ξ，η，θ，κ，χ，ρ型、これらの混晶型、アモルファスのいずれのものも用いられ、α，δ，γ，θ，混晶型，アモルファスのものが好ましく用いられる。 And if it is alumina fine powder, buyer method, improved buyer method, ethylene chlorohydrin method, underwater spark discharge method, organoaluminum hydrolysis method, aluminum alum pyrolysis method, ammonium aluminum carbonate pyrolysis method, aluminum chloride flame Alumina fine powder obtained by a decomposition method is used. As the crystal system, α, β, γ, δ, ξ, η, θ, κ, χ, ρ type, mixed crystal type, amorphous type, α, δ, γ, θ, mixed crystal can be used. A mold or an amorphous material is preferably used.
前記微粉体は、その表面がカップリング剤やシリコーンオイルによって疎水化処理をされていることがより好ましい。
微粉体の表面の疎水化処理方法は、微粉体と反応あるいは物理吸着する有機ケイ素化合物等で化学的、または物理的に処理する方法である。
More preferably, the surface of the fine powder is subjected to a hydrophobic treatment with a coupling agent or silicone oil.
The method of hydrophobizing the surface of the fine powder is a method of chemically or physically treating with an organosilicon compound that reacts or physically adsorbs with the fine powder.
上記疎水化処理方法として好ましい方法は、ケイ素ハロゲン化合物の蒸気相酸化により生成されたシリカ微粒子を有機ケイ素化合物で処理する方法である。そのような方法に使用される有機ケイ素化合物の例は、以下のものが挙げられる。ヘキサメチルジシラザン、トリメチルシラン、トリメチルクロルシラン、トリメチルエトキシシラン、ジメチルジクロルシラン、メチルトリクロルシラン、アリルジメチルクロルシラン、アリルフェニルジクロルシラン、ベンジルジメチルクロルシラン、ブロムメチルジメチルクロルシラン、α−クロルエチルトリクロルシラン、β−クロルエチルトリクロルシラン、クロルメチルジメチルクロルシラン、トリオルガノシリルメルカプタン、トリメチルシリルメルカプタン、トリオルガノシリルアクリレート、ビニルジメチルアセトキシシラン、ジメチルエトキシシラン、ジメチルジメトキシシラン、ジフェニルジエトキシシラン、ヘキサメチルジシロキサン、１，３−ジビニルテトラメチルジシロキサン、１，３−ジフェニルテトラメチルジシロキサンおよび１分子当り２から１２個のシロキサン単位を有し末端に位置する単位にそれぞれ１個宛のＳｉに結合した水酸基を含有するジメチルポリシロキサン。
上記流動化剤は単独で用いても、複数種を組合せて用いても良い。
A preferable method for the hydrophobic treatment is a method in which silica fine particles produced by vapor phase oxidation of a silicon halogen compound are treated with an organosilicon compound. Examples of the organosilicon compound used in such a method include the following. Hexamethyldisilazane, trimethylsilane, trimethylchlorosilane, trimethylethoxysilane, dimethyldichlorosilane, methyltrichlorosilane, allyldimethylchlorosilane, allylphenyldichlorosilane, benzyldimethylchlorosilane, bromomethyldimethylchlorosilane, α-chloro Ethyltrichlorosilane, β-chloroethyltrichlorosilane, chloromethyldimethylchlorosilane, triorganosilyl mercaptan, trimethylsilyl mercaptan, triorganosilyl acrylate, vinyldimethylacetoxysilane, dimethylethoxysilane, dimethyldimethoxysilane, diphenyldiethoxysilane, hexamethyl Disiloxane, 1,3-divinyltetramethyldisiloxane, 1,3-diphenyltetramethyldisiloxane Siloxane and dimethylpolysiloxane containing 2 to 12 siloxane units per molecule and containing hydroxyl groups bonded to one Si at each terminal unit.
The above fluidizing agents may be used alone or in combination of two or more.
また、上記流動化剤は、トナー用粉体粒子１００質量部に対して流動化剤０．１乃至８．０質量部、好ましくは０．１乃至４．０質量部使用するのが良い。添加量が０．１質量部未満ではトナー用粉体粒子に流動性を付与することができなく、好ましくない。また、４．０質量部を超える場合ではトナー用粉体粒子と無機微粉体の混合が困難になり、トナー用粉体粒子の熱処理の生産上好ましくない。
なお、上記の添加剤は、外添工程で外添剤として用いても良い。
上記トナーの各種物性の測定方法及び、以下の実施例中で測定した各種物性の測定方法に関して以下に説明する。
The fluidizing agent is used in an amount of 0.1 to 8.0 parts by weight, preferably 0.1 to 4.0 parts by weight, based on 100 parts by weight of toner powder particles. If the addition amount is less than 0.1 parts by mass, it is not preferable because the fluidity cannot be imparted to the toner powder particles. On the other hand, when the amount exceeds 4.0 parts by mass, it becomes difficult to mix the toner powder particles and the inorganic fine powder, which is not preferable for the heat treatment production of the toner powder particles.
In addition, you may use said additive as an external additive in an external addition process.
A method for measuring various physical properties of the toner and a method for measuring various physical properties measured in the following examples will be described below.
＜重量平均粒径（Ｄ４）の測定方法＞
トナーの重量平均粒径（Ｄ４）は、以下のようにして算出する。測定装置としては、１００μｍのアパーチャーチューブを備えた細孔電気抵抗法による精密粒度分布測定装置「コールター・カウンター Ｍｕｌｔｉｓｉｚｅｒ ３」（登録商標、ベックマン・コールター（株）製）を用いる。測定条件の設定及び測定データの解析は、付属の専用ソフト「ベックマン・コールター Ｍｕｌｔｉｓｉｚｅｒ ３ Ｖｅｒｓｉｏｎ３．５１」（ベックマン・コールター（株）製）を用いる。なお、測定は実効測定チャンネル数２万５千チャンネルで行う。
測定に使用する電解水溶液は、特級塩化ナトリウムをイオン交換水に溶解して濃度が約１質量％となるようにしたもの、例えば、「ＩＳＯＴＯＮ ＩＩ」（ベックマン・コールター（株）製）が使用できる。
<Measurement method of weight average particle diameter (D4)>
The weight average particle diameter (D4) of the toner is calculated as follows. As a measuring device, a precise particle size distribution measuring device “Coulter Counter Multisizer 3” (registered trademark, manufactured by Beckman Coulter, Inc.) using a pore electrical resistance method provided with a 100 μm aperture tube is used. For setting of measurement conditions and analysis of measurement data, attached dedicated software “Beckman Coulter Multisizer 3 Version 3.51” (manufactured by Beckman Coulter, Inc.) is used. The measurement is performed with 25,000 effective measurement channels.
As the electrolytic aqueous solution used for the measurement, a special grade sodium chloride is dissolved in ion-exchanged water so as to have a concentration of about 1% by mass, for example, “ISOTON II” (manufactured by Beckman Coulter, Inc.) can be used. .
測定、解析を行う前に、以下のように専用ソフトの設定を行なった。
専用ソフトの「標準測定方法（ＳＯＭ）を変更」画面において、コントロールモードの総カウント数を５００００粒子に設定し、測定回数を１回、Ｋｄ値は「標準粒子１０．０μｍ」（ベックマン・コールター（株）製）を用いて得られた値を設定する。「閾値／ノイズレベルの測定ボタン」を押すことで、閾値とノイズレベルを自動設定する。また、カレントを１６００μＡに、ゲインを２に、電解液をＩＳＯＴＯＮ ＩＩに設定し、「測定後のアパーチャーチューブのフラッシュ」にチェックを入れる。
専用ソフトの「パルスから粒径への変換設定」画面において、ビン間隔を対数粒径に、粒径ビンを２５６粒径ビンに、粒径範囲を２μｍから６０μｍまでに設定する。
Prior to measurement and analysis, the dedicated software was set up as follows.
On the “Change Standard Measurement Method (SOM)” screen of the dedicated software, set the total count in the control mode to 50000 particles, set the number of measurements once, and set the Kd value to “standard particles 10.0 μm” (Beckman Coulter ( The value obtained by using the product) is set. By pressing the “Threshold / Noise Level Measurement Button”, the threshold and noise level are automatically set. In addition, the current is set to 1600 μA, the gain is set to 2, the electrolyte is set to ISOTON II, and the “aperture tube flush after measurement” is checked.
In the “Pulse to particle size conversion setting” screen of the dedicated software, the bin interval is set to logarithmic particle size, the particle size bin is set to 256 particle size bin, and the particle size range is set to 2 μm to 60 μm.
具体的な測定法は以下の通りである。
（１）Ｍｕｌｔｉｓｉｚｅｒ ３専用のガラス製２５０ｍＬ丸底ビーカーに前記電解水溶液約２００ｍＬを入れ、サンプルスタンドにセットし、スターラーロッドの撹拌を反時計回りで２４回転／秒にて行なう。そして、専用ソフトの「アパーチャーのフラッシュ」機能により、アパーチャーチューブ内の汚れと気泡を除去しておく。
The specific measurement method is as follows.
(1) About 200 mL of the electrolytic solution is placed in a glass 250 mL round-bottom beaker dedicated to Multisizer 3 and set on a sample stand, and the stirrer rod is stirred counterclockwise at 24 rpm. Then, the dirt and bubbles in the aperture tube are removed by the “aperture flush” function of the dedicated software.
（２）ガラス製の１００ｍＬ平底ビーカーに前記電解水溶液約３０ｍＬを入れる。この中に分散剤として「コンタミノンＮ」（非イオン界面活性剤、陰イオン界面活性剤、有機ビルダーからなるｐＨ７の精密測定器洗浄用中性洗剤の１０質量％水溶液、和光純薬工業（株）製）をイオン交換水で約３質量倍に希釈した希釈液を約０．３ｍＬ加える。 (2) About 30 mL of the electrolytic solution is placed in a glass 100 mL flat bottom beaker. As a dispersant, “Contaminone N” (a nonionic surfactant, an anionic surfactant, a 10% by weight aqueous solution of a neutral detergent for washing a pH 7 precision measuring instrument comprising an organic builder, Wako Pure Chemical Industries, Ltd. About 0.3 mL of a diluted solution obtained by diluting (made in ()) with ion-exchanged water about 3 times by mass.
（３）発振周波数５０ｋＨｚの発振器２個を位相を１８０度ずらした状態で内蔵し、電気的出力１２０Ｗの超音波分散器「Ｕｌｔｒａｓｏｎｉｃ Ｄｉｓｐｅｎｓｉｏｎ Ｓｙｓｔｅｍ Ｔｅｔｏｒａ１５０」（日科機バイオス（株）製）を準備する。超音波分散器の水槽内に約３．３ｌのイオン交換水を入れ、この水槽中にコンタミノンＮを約２ｍＬ添加する。 (3) Two oscillators with an oscillation frequency of 50 kHz are incorporated with the phase shifted by 180 degrees, and an ultrasonic disperser “Ultrasonic Dissipation System Tetora150” (manufactured by Nikki Bios Co., Ltd.) with an electrical output of 120 W is prepared. . About 3.3 liters of ion-exchanged water is placed in the water tank of the ultrasonic disperser, and about 2 mL of Contaminone N is added to the water tank.
（４）前記（２）のビーカーを前記超音波分散器のビーカー固定穴にセットし、超音波分散器を作動させる。そして、ビーカー内の電解水溶液の液面の共振状態が最大となるようにビーカーの高さ位置を調整する。 (4) The beaker of (2) is set in the beaker fixing hole of the ultrasonic disperser, and the ultrasonic disperser is operated. And the height position of a beaker is adjusted so that the resonance state of the liquid level of the electrolyte solution in a beaker may become the maximum.
（５）前記（４）のビーカー内の電解水溶液に超音波を照射した状態で、トナー約１０ｍｇを少量ずつ前記電解水溶液に添加し、分散させる。そして、更に６０秒間超音波分散処理を継続する。なお、超音波分散にあたっては、水槽の水温が１０℃以上４０℃以下となる様に適宜調節する。 (5) In a state where the electrolytic aqueous solution in the beaker of (4) is irradiated with ultrasonic waves, about 10 mg of toner is added to the electrolytic aqueous solution little by little and dispersed. Then, the ultrasonic dispersion process is continued for another 60 seconds. In ultrasonic dispersion, the temperature of the water tank is appropriately adjusted so as to be 10 ° C. or higher and 40 ° C. or lower.
（６）サンプルスタンド内に設置した前記（１）の丸底ビーカーに、ピペットを用いてトナーを分散した前記（５）の電解質水溶液を滴下し、測定濃度が約５％となるように調整する。そして、測定粒子数が５００００個になるまで測定を行う。 (6) To the round bottom beaker of (1) installed in the sample stand, the electrolyte solution of (5) in which the toner is dispersed is dropped using a pipette, and the measurement concentration is adjusted to about 5%. . Measurement is performed until the number of measured particles reaches 50,000.
（７）測定データを装置付属の前記専用ソフトにて解析を行い、重量平均粒径（Ｄ４）を算出する。なお、専用ソフトでグラフ／体積％と設定したときの、「分析／体積統計値（算術平均）」画面の「平均径」が重量平均粒径（Ｄ４）である。 (7) The measurement data is analyzed with the dedicated software attached to the apparatus, and the weight average particle diameter (D4) is calculated. The “average diameter” on the “analysis / volume statistic (arithmetic average)” screen when the graph / volume% is set with the dedicated software is the weight average particle diameter (D4).
＜微粉量の算出方法＞
トナー中の個数基準の微粉量（個数％）は、前記のＭｕｌｔｉｓｉｚｅｒ ３の測定を行った後、データを解析することにより算出する。
例えば、トナー中の４．０μｍ以下の粒子の個数％は、以下の手順で算出する。まず、専用ソフトでグラフ／個数％に設定して測定結果のチャートを個数％表示とする。そして、「書式／粒径／粒径統計」画面における粒径設定部分の「＜」にチェックし、その下の粒径入力部に「４」を入力する。「分析／個数統計値（算術平均）」画面を表示したときの「＜４μｍ」表示部の数値が、トナー中の４．０μｍ以下の粒子の個数％である。
<Calculation method of fine powder amount>
The number-based fine powder amount (number%) in the toner is calculated by analyzing the data after measuring the Multisizer 3 described above.
For example, the number% of particles of 4.0 μm or less in the toner is calculated by the following procedure. First, the graph / number% is set with the dedicated software, and the measurement result chart is displayed in number%. Then, check “<” in the particle size setting portion on the “format / particle size / particle size statistics” screen, and enter “4” in the particle size input section below. The numerical value of the “<4 μm” display portion when the “analysis / number statistics (arithmetic mean)” screen is displayed is the number% of particles of 4.0 μm or less in the toner.
＜粗粉量の算出方法＞
トナー中の体積基準の粗粉量（体積％）は、前記のＭｕｌｔｉｓｉｚｅｒ ３の測定を行った後、データを解析することにより算出する。
例えば、トナー中の１０．０μｍ以上の粒子の体積％は、以下の手順で算出する。まず、専用ソフトでグラフ／体積％に設定して測定結果のチャートを体積％表示とする。そして、「書式／粒径／粒径統計」画面における粒径設定部分の「＞」にチェックし、その下の粒径入力部に「１０」を入力する。「分析／体積統計値（算術平均）」画面を表示したときの「＞１０μｍ」表示部の数値が、トナー中の１０．０μｍ以上の粒子の体積％である。
<Calculation method of coarse powder amount>
The volume-based coarse powder amount (volume%) in the toner is calculated by analyzing the data after measuring the Multisizer 3 described above.
For example, the volume percentage of particles of 10.0 μm or more in the toner is calculated by the following procedure. First, graph / volume% is set with dedicated software, and the measurement result chart is displayed as volume%. Then, check “>” in the particle size setting portion on the “format / particle size / particle size statistics” screen, and enter “10” in the particle size input section below. When the “analysis / volume statistic (arithmetic average)” screen is displayed, the numerical value of the “> 10 μm” display portion is the volume% of particles of 10.0 μm or more in the toner.
＜平均円形度の測定方法＞
トナー粒子の平均円形度は、フロー式粒子像分析装置「ＦＰＩＡ−３０００」（シスメックス（株）製）によって、校正作業時の測定及び解析条件で測定する。
具体的な測定方法は、以下の通りである。まず、ガラス製の容器中に予め不純固形物などを除去したイオン交換水約２０ｍＬを入れる。この中に分散剤として「コンタミノンＮ」（非イオン界面活性剤、陰イオン界面活性剤、有機ビルダーからなるｐＨ７の精密測定器洗浄用中性洗剤の１０質量％水溶液、和光純薬工業（株）製）をイオン交換水で約３質量倍に希釈した希釈液を約０．２ｍＬ加える。更に測定試料を約０．０２ｇ加え、超音波分散器を用いて２分間分散処理を行い、測定用の分散液とする。その際、分散液の温度が１０℃以上４０℃以下となる様に適宜冷却する。超音波分散器としては、発振周波数５０ｋＨｚ、電気的出力１５０Ｗの卓上型の超音波洗浄器分散器（「ＶＳ−１５０」（（株）ヴェルヴォクリーア社製））を用い、水槽内には所定量のイオン交換水を入れ、この水槽中に前記コンタミノンＮを約２ｍＬ添加する。
<Measuring method of average circularity>
The average circularity of the toner particles is measured by a flow type particle image analyzer “FPIA-3000” (manufactured by Sysmex Corporation) under the measurement and analysis conditions during the calibration operation.
A specific measurement method is as follows. First, about 20 mL of ion-exchanged water from which impure solids and the like are previously removed is placed in a glass container. As a dispersant, “Contaminone N” (a nonionic surfactant, an anionic surfactant, a 10% by weight aqueous solution of a neutral detergent for washing a pH 7 precision measuring instrument comprising an organic builder, Wako Pure Chemical Industries, Ltd. About 0.2 mL of a diluted solution obtained by diluting (made in ()) with ion-exchanged water about 3 times by mass is added. Further, about 0.02 g of a measurement sample is added, and dispersion treatment is performed for 2 minutes using an ultrasonic disperser to obtain a dispersion for measurement. In that case, it cools suitably so that the temperature of a dispersion liquid may become 10 to 40 degreeC. As the ultrasonic disperser, a desktop ultrasonic cleaner disperser (“VS-150” (manufactured by Vervo Creer)) with an oscillation frequency of 50 kHz and an electric output of 150 W is used. A fixed amount of ion-exchanged water is added, and about 2 mL of the contamination N is added to the water tank.
測定には、標準対物レンズ（１０倍）を搭載した前記フロー式粒子像分析装置を用い、シース液にはパーティクルシース「ＰＳＥ−９００Ａ」（シスメックス（株）製）を使用した。前記手順に従い調整した分散液を前記フロー式粒子像分析装置に導入し、ＨＰＦ測定モードで、トータルカウントモードにて３０００個のトナー粒子を計測する。そして、粒子解析時の２値化閾値を８５％とし、解析粒子径を円相当径１．９８５μｍ以上３９．６９μｍ未満に限定し、トナー粒子の平均円形度を求める。 The flow type particle image analyzer equipped with a standard objective lens (10 ×) was used for the measurement, and a particle sheath “PSE-900A” (manufactured by Sysmex Corporation) was used as the sheath liquid. The dispersion prepared in accordance with the above procedure is introduced into the flow type particle image analyzer, and 3000 toner particles are measured in the HPF measurement mode and in the total count mode. Then, the binarization threshold at the time of particle analysis is set to 85%, the analysis particle diameter is limited to the circle equivalent diameter of 1.985 μm or more and less than 39.69 μm, and the average circularity of the toner particles is obtained.
測定にあたっては、測定開始前に標準ラテックス粒子（Ｄｕｋｅ Ｓｃｉｅｎｔｉｆｉｃ社製の「ＲＥＳＥＡＲＣＨ ＡＮＤ ＴＥＳＴ ＰＡＲＴＩＣＬＥＳ Ｌａｔｅｘ Ｍｉｃｒｏｓｐｈｅｒｅ Ｓｕｓｐｅｎｓｉｏｎｓ ５２００Ａ」をイオン交換水で希釈）を用いて自動焦点調整を行う。その後、測定開始から２時間毎に焦点調整を実施することが好ましい。
なお、本願実施例では、シスメックス（株）による校正作業が行われた、シスメックス（株）が発行する校正証明書の発行を受けたフロー式粒子像分析装置を使用した。解析粒子径を円相当径１．９８５μｍ以上３９．６９μｍ未満に限定した以外は、校正証明を受けた時の測定及び解析条件で測定を行った。
In the measurement, automatic focus adjustment is performed using standard latex particles ("DISE Scientific AND RESPARTIC AND TEST PARTILES Latex Microsphere Suspensions 5200A" diluted with ion-exchanged water) before starting the measurement. Thereafter, it is preferable to perform focus adjustment every two hours from the start of measurement.
In the examples of the present application, a flow-type particle image analyzer that has been issued a calibration certificate issued by Sysmex Corporation, which has been calibrated by Sysmex Corporation, was used. Measurement was performed under the measurement and analysis conditions when the calibration certificate was received, except that the analysis particle diameter was limited to a circle equivalent diameter of 1.985 μm or more and less than 39.69 μm.
＜円形度が０．９９０以上の粒子の割合の算出方法＞
本発明において、円形度が０．９９０以上の粒子の割合は、円形度の分布を示す指標として用いており、頻度（％）で表わされる。具体的には、ＦＰＩＡ−３０００によって測定したトナーの平均円形度における、頻度テーブルの範囲１．００の頻度（％）の値と、０．９９０−＞１．０００の頻度（％）の値を足した値を用いた。
<Calculation method of the proportion of particles having a circularity of 0.990 or more>
In the present invention, the proportion of particles having a circularity of 0.990 or more is used as an index indicating the distribution of circularity, and is represented by frequency (%). Specifically, in the average circularity of the toner measured by FPIA-3000, the frequency (%) value in the frequency table range 1.00 and the frequency (%) value in 0.990-> 1.000 are set. The added value was used.
以下、本発明の実施例および比較例を挙げて本発明を更に具体的に説明するが、本発明はこれらの実施例に限定されるものではない。
（トナー用粉体粒子Ａの製造例）
ポリエステルユニットを有する樹脂：１００質量部
（重量平均分子量（Ｍｗ）：８２４５０、数平均分子量（Ｍｎ）：３６５０、ピーク分子量：（Ｍｐ）８５５０）
パラフィンワックス：４質量部
（最大吸熱ピーク温度７８℃）
３，５−ジ−ｔ−ブチルサリチル酸アルミニウム化合物：１．０質量部
Ｃ．Ｉ．ピグメントブルー１５：３．５質量部
EXAMPLES Hereinafter, the present invention will be described more specifically with reference to examples and comparative examples of the present invention, but the present invention is not limited to these examples.
(Production example of powder particle A for toner)
Resin having a polyester unit: 100 parts by mass (weight average molecular weight (Mw): 82450, number average molecular weight (Mn): 3650, peak molecular weight: (Mp) 8550)
Paraffin wax: 4 parts by mass (maximum endothermic peak temperature 78 ° C.)
3,5-di-t-butylsalicylic acid aluminum compound: 1.0 part by mass C.I. I. Pigment Blue 15: 3.5 parts by mass
上記の処方の材料をヘンシェルミキサーＦＭ−７５型（日本コークス工業（株）製）で混合した後、温度を１２０℃に設定した二軸混練機ＰＣＭ−３０型（（株）池貝製）にて混練した。得られた混練物を冷却し、ハンマーミルにて１ｍｍ以下に粗粉砕し、粗砕物とし、得られた粗砕物を、機械式粉砕機Ｔ−２５０（フロイント・ターボ（株）製）にて粉砕し、粉体微粒子を得た。続いて、得られた粉体微粒子を、ファカルティＦ−３００（ホソカワミクロン（株）製）により分級し、粉体粒子とした。 After mixing the materials of the above prescription with a Henschel mixer FM-75 type (manufactured by Nihon Coke Kogyo Co., Ltd.), a biaxial kneader PCM-30 type (manufactured by Ikekai Co., Ltd.) with the temperature set at 120 ° C. Kneaded. The obtained kneaded product is cooled, coarsely pulverized to 1 mm or less with a hammer mill to obtain a coarsely pulverized product, and the obtained crushed product is pulverized with a mechanical pulverizer T-250 (manufactured by Freund Turbo). As a result, fine powder particles were obtained. Subsequently, the obtained powder fine particles were classified by Faculty F-300 (manufactured by Hosokawa Micron Corporation) to obtain powder particles.
更に、下記材料をヘンシェルミキサーＦＭ−７５型（日本コークス工業（株）製）に投入し、回転羽根の周速を５０．０ｍ／秒とし、混合時間３分で混合することにより、粉体粒子Ａの表面に、シリカと酸化チタンを付着させたトナー用粉体粒子を得た。
粉体粒子：１００質量部
シリカ：３．５質量部
（ゾルゲル法で作成したシリカ微粒子にヘキサメチルジシラザン処理１．５質量％で表面処理した後、分級によって所望の粒度分布に調整したもの。）
酸化チタン：０．５質量部
（アナターゼ形の結晶性を有するメタチタン酸を表面処理したもの。）
Furthermore, the following materials were put into a Henschel mixer FM-75 type (manufactured by Nihon Coke Kogyo Co., Ltd.), the peripheral speed of the rotary blade was 50.0 m / sec, and the mixing was performed for 3 minutes to obtain powder particles. Toner powder particles having silica and titanium oxide adhered to the surface of A were obtained.
Powder particles: 100 parts by mass Silica: 3.5 parts by mass (Silica fine particles prepared by the sol-gel method are surface-treated with 1.5% by mass of hexamethyldisilazane treatment and then adjusted to a desired particle size distribution by classification. )
Titanium oxide: 0.5 part by mass (surface-treated metatitanic acid having anatase crystallinity)
このとき得られたトナー用粉体粒子は、重量平均粒径（Ｄ４）が６．７μｍ、粒径４．０μｍ以下の粒子が２５．０個数％であり、粒径１０．０μｍ以上の粒子が２．７体積％であった。
更に、ＦＰＩＡ３０００にて平均円形度を測定した結果、平均円形度が０．９４６であった。
以下、これをトナー用粉体粒子Ａとする。
これらの結果を表１にまとめた。
The obtained powder particles for toner have a weight average particle diameter (D4) of 6.7 μm, 25.0% by number of particles having a particle diameter of 4.0 μm or less, and particles having a particle diameter of 10.0 μm or more. It was 2.7% by volume.
Furthermore, as a result of measuring the average circularity with FPIA3000, the average circularity was 0.946.
Hereinafter, this is referred to as toner powder particles A.
These results are summarized in Table 1.
（トナー用粉体粒子Ｂの製造例）
本製造例では、パラフィンワックスの添加量を６質量部にした以外は、トナー用粉体粒子Ａと同様の製造方法にて、トナー用粉体粒子Ｂを得た。
このとき得られたトナー用粉体粒子Ｂの重量平均粒径（Ｄ４）、粒径４．０μｍ以下の粒子の割合、粒径１０．０μｍ以上の粒子の割合、平均円形度を測定した結果を表１にまとめた。
(Production example of powder particle B for toner)
In this production example, toner powder particles B were obtained by the same production method as that for toner powder particles A, except that the amount of paraffin wax added was 6 parts by mass.
The weight average particle diameter (D4), the ratio of particles having a particle diameter of 4.0 μm or less, the ratio of particles having a particle diameter of 10.0 μm or more, and the average circularity were measured. The results are summarized in Table 1.
（トナー用粉体粒子Ｃの製造例）
本製造例では、パラフィンワックスの添加量を８質量部にした以外は、トナー用粉体粒子Ａと同様の製造方法にて、トナー用粉体粒子Ｃを得た。
このとき得られたトナー用粉体粒子Ｂの重量平均粒径（Ｄ４）、粒径４．０μｍ以下の粒子の割合、粒径１０．０μｍ以上の粒子の割合、平均円形度を測定した結果を表１にまとめた。
(Production example of powder particle C for toner)
In this production example, toner powder particles C were obtained by the same production method as that for toner powder particles A, except that the amount of paraffin wax added was 8 parts by mass.
The weight average particle diameter (D4), the ratio of particles having a particle diameter of 4.0 μm or less, the ratio of particles having a particle diameter of 10.0 μm or more, and the average circularity were measured. The results are summarized in Table 1.
〔実施例１〕
本実施例では図１、図２に示した熱処理装置を用い、トナー用粉体粒子Ａを熱処理した。本実施例において装置の円筒状の外壁の内周面径は１５０ｍｍ、円柱状の内部部材の外周面径は１１０ｍｍとした。
熱処理装置は熱風を旋回させるための旋回部材を具備し、旋回部材は複数のブレードを有している。ブレードの鉛直方向の高さは、１５ｍｍとした。ブレードの形状は、図６に示すように２つの円弧を連結した形状とした。
図３に示す入口角度ａを０°とし、図６に示す出口角度ｂを８０°とし、垂直出口角度ｃを８０°とした。よってｂ−ｃ＝０°となる。また、ブレードの枚数は１０枚とした。
[Example 1]
In this example, the powder particles A for toner were heat-treated using the heat treatment apparatus shown in FIGS. In this example, the inner peripheral surface diameter of the cylindrical outer wall of the apparatus was 150 mm, and the outer peripheral surface diameter of the columnar inner member was 110 mm.
The heat treatment apparatus includes a turning member for turning hot air, and the turning member has a plurality of blades. The vertical height of the blade was 15 mm. The shape of the blade was such that two arcs were connected as shown in FIG.
The inlet angle a shown in FIG. 3 was 0 °, the outlet angle b shown in FIG. 6 was 80 °, and the vertical outlet angle c was 80 °. Therefore, bc = 0 °. The number of blades was 10.
粉体粒子供給手段は図９に示すように４分割とし、処理室の中心軸と直交する同一断面上に９０°間隔に、本体内螺旋流の角度と一致するように処理室中心軸直交断面に対し本体下端方向に２７°の角度を付けて配置した。粉体供給手段各出口の縦の長さは６０ｍｍ、横の長さは４ｍｍとし、各出口断面積を２４０ｍｍ２、総断面積は９６０ｍｍ２とした。また高圧エア供給ノズルから供給される搬送気体の流量は、各口０．０２ｍ３／分とした。 The powder particle supply means is divided into four as shown in FIG. 9, and the processing chamber central axis orthogonal cross section so as to coincide with the angle of the spiral flow in the main body at intervals of 90 ° on the same cross section orthogonal to the central axis of the processing chamber. With respect to the main body, it was arranged at an angle of 27 ° in the lower end direction of the body. The vertical length of each outlet of the powder supply means was 60 mm, the horizontal length was 4 mm, the sectional area of each outlet was 240 mm 2 , and the total sectional area was 960 mm 2 . The flow rate of the carrier gas supplied from the high pressure air supply nozzle was 0.02 m 3 / min for each port.
冷風供給手段は図１に示した様に第一、第二の二段階とする。
第一冷風供給手段は図１０に示すように４分割とし、粉体供給手段出口下端から第一冷風供給手段上端までの距離を１００ｍｍとした。また処理室の中心軸と直交する同一断面上に各口を４５°等間隔に、かつ本体内螺旋流の角度と一致するように処理室中心軸直交断面に対し本体下端方向に２７°の角度を付けて配置した。第一冷風供給手段各出口の縦の長さは８０ｍｍ、横の長さは４ｍｍとし、各出口断面積は３２０ｍｍ２、総断面積は１２８０ｍｍ２とした。
As shown in FIG. 1, the cold air supply means has first and second stages.
The first cold air supply means was divided into four as shown in FIG. 10, and the distance from the lower end of the powder supply means outlet to the upper end of the first cold air supply means was 100 mm. In addition, each port on the same cross section orthogonal to the central axis of the processing chamber is equally spaced at 45 °, and an angle of 27 ° toward the lower end of the main body with respect to the cross section orthogonal to the central axis of the processing chamber so as to coincide with the angle of the spiral flow in the main body. Was placed. The vertical length of each outlet of the first cold air supply means was 80 mm, the horizontal length was 4 mm, the sectional area of each outlet was 320 mm 2 , and the total sectional area was 1280 mm 2 .
第二冷風供給手段は図１１に示すように４分割とし、第二冷風供給手段下端が底面と一致するように９０°間隔に計１８０°に、かつ底面と平行に配置した。第二冷風供給手段各出口の縦の長さは８０ｍｍ、横の長さは４ｍｍとし、各出口断面積は３２０ｍｍ２、総断面積は１２８０ｍｍ２とした。
排出手段は図１１に示すように、第二冷風供給手段中央口の対向位置に排出手段下端が底面と一致するようにかつ底面と平行に配置した。また排出手段入口は、縦の長さ７５ｍｍ、横の長さ３０ｍｍ、断面積は２２５０ｍｍ２とした。
The second cold air supply means was divided into four as shown in FIG. 11, and was arranged at a total interval of 180 ° and parallel to the bottom surface so that the lower end of the second cold air supply means coincided with the bottom surface. The vertical length of each outlet of the second cold air supply means was 80 mm, the horizontal length was 4 mm, the sectional area of each outlet was 320 mm 2 , and the total sectional area was 1280 mm 2 .
As shown in FIG. 11, the discharge means was disposed at a position opposite to the central outlet of the second cold air supply means so that the lower end of the discharge means coincided with the bottom face and parallel to the bottom face. The discharge means inlet had a vertical length of 75 mm, a horizontal length of 30 mm, and a cross-sectional area of 2250 mm 2 .
円柱状内部部材は図１２に示すように、円柱状外壁と外壁内部の体積を規制するよう外壁中心軸と同軸上に配置した。円柱状内部部材の上端部は、処理室の内外円筒半径差ｄ＝２０ｍｍに対し、曲率半径Ｒ＝１０ｍｍの丸みを持つとした。このとき、Ｒ／ｄ＝０．５となる。
上記装置構成を装置構成１とする。
As shown in FIG. 12, the cylindrical inner member was arranged coaxially with the outer wall central axis so as to regulate the volume of the cylindrical outer wall and the outer wall. The upper end of the columnar inner member is rounded with a radius of curvature R = 10 mm with respect to the inner / outer cylinder radius difference d = 20 mm of the processing chamber. At this time, R / d = 0.5.
The apparatus configuration is referred to as apparatus configuration 1.
装置構成１を用いてトナー用粉体粒子Ａの処理量（ｋｇ／ｈｒ）を２０ｋｇ／ｈｒとしてトナー用粉体粒子Ａを熱処理し、平均円形度０．９６５のトナー用熱処理粒子を得た。
＜運転条件１＞
この時の運転条件（以下、運転条件１とも記載する。）は、以下のとおりであった。
熱風温度１７０℃、熱風風量７．０ｍ３／分であった。
第一冷風温度は−５℃、総流量は０．２ｍ３／分とし、各口それぞれ０．０５ｍ３／分の冷風を処理室内に供給した。
第二冷風温度は−５℃、総流量は０．１５ｍ３／分とし、各口それぞれ０．０５ｍ３／分の冷風を処理室内に供給した。
運転時間は１時間とした。
この時の条件を運転条件１とする。
Using the apparatus configuration 1, the toner powder particles A were heat-treated at a treatment amount (kg / hr) of the toner powder particles A of 20 kg / hr to obtain heat-treated particles for toner having an average circularity of 0.965.
<Operating condition 1>
The operating conditions at this time (hereinafter also referred to as operating conditions 1) were as follows.
The hot air temperature was 170 ° C., and the hot air flow rate was 7.0 m 3 / min.
The first cold air temperature was −5 ° C., the total flow rate was 0.2 m 3 / min, and 0.05 m 3 / min of cold air was supplied into each processing chamber.
The second cold air temperature is -5 ° C., total flow to 0.15 m 3 / min was fed cold air respectively the mouth 0.05 m 3 / min into the processing chamber.
The operation time was 1 hour.
The condition at this time is referred to as operation condition 1.
この時得られた熱処理後のトナー用粉体粒子は、以下のとおりであった。
重量平均粒径（Ｄ４）が６．８μｍ、
粒径４．０μｍ以下の粒子が２４．４個数％、
粒径１０．０μｍ以上の粒子が３．６体積％、
粗大粒子は非常に少なかった。
また運転後に本体内の融着状況を目視によって確認したが、融着物は全く認められなかった。
The powder particles for toner after heat treatment obtained at this time were as follows.
The weight average particle size (D4) is 6.8 μm,
24.4% by number of particles having a particle size of 4.0 μm or less,
3.6% by volume of particles having a particle size of 10.0 μm or more,
There were very few coarse particles.
In addition, the fusion situation in the main body was visually confirmed after the operation, but no fusion product was observed.
次に同じく装置構成１を用いてトナー用粉体粒子Ａの処理量を３０ｋｇ／ｈｒとしてトナー用粉体粒子Ａを熱処理し、平均円形度０．９６５のトナー用熱処理粒子を得た。
この時の条件は熱風温度２００℃、熱風風量１０．０ｍ３／分であった。第一冷風温度は−５℃、総流量は０．２ｍ３／分とし、各口それぞれ０．０５ｍ３／分の冷風を処理室内に供給した。同様に第二冷風温度は−５℃、総流量は０．１５ｍ３／分とし、各口それぞれ０．０５ｍ３／分の冷風を処理室内に供給した。
Next, using the same apparatus configuration 1, the toner powder particles A were heat-treated at a processing amount of the toner powder particles A of 30 kg / hr to obtain heat-treated particles for toner having an average circularity of 0.965.
The conditions at this time were a hot air temperature of 200 ° C. and a hot air flow rate of 10.0 m 3 / min. The first cold air temperature was −5 ° C., the total flow rate was 0.2 m 3 / min, and 0.05 m 3 / min of cold air was supplied into each processing chamber. Similarly the second cold air temperature is -5 ° C., total flow to 0.15 m 3 / min was fed cold air respectively the mouth 0.05 m 3 / min into the processing chamber.
この時得られた熱処理後のトナー用粉体粒子は、以下のとおりであった。
重量平均粒径（Ｄ４）が６．９μｍ、
粒径４．０μｍ以下の粒子が２４．１個数％、
粒径１０．０μｍ以上の粒子が３．９体積％。
また２０ｋｇ／ｈｒ処理時と比較して３０ｋｇ／ｈｒ処理時での粒径１０．０μｍ以上の粒子の体積％での増加は０．３％であり、処理量を増加しても粗粉は非常に少なかった。また運転後に本体内の融着状況を確認したが、融着物は全く認められなかった。
以上得られたトナーの熱処理結果の評価を下記の基準で行った。
The powder particles for toner after heat treatment obtained at this time were as follows.
The weight average particle size (D4) is 6.9 μm,
24.1% by number of particles having a particle size of 4.0 μm or less,
3.9% by volume of particles having a particle size of 10.0 μm or more.
In addition, the increase in volume% of particles having a particle size of 10.0 μm or more at 30 kg / hr treatment is 0.3% compared to 20 kg / hr treatment, and the coarse powder is very There were few. Further, the fusion situation inside the main body was confirmed after the operation, but no fusion product was observed.
Evaluation of the heat treatment results of the toner obtained above was performed according to the following criteria.
＜粗粉量に対する評価＞
得られた熱処理後のトナー用粉体粒子に含有される１０．０μｍ以上の粒子の割合ｓ（体積％）を粗粉量の評価の基準とし、下記の基準で判断した。
Ａ： ｓ＜５．０
Ｂ： ５．０≦ｓ＜１０．０
Ｃ：１０．０≦ｓ＜１５．０
Ｄ：１５．０≦ｓ＜２０．０
Ｅ：２０．０≦ｓ
<Evaluation for the amount of coarse powder>
The ratio s (volume%) of particles of 10.0 μm or more contained in the obtained powder particles for heat-treated toner was used as a criterion for evaluation of the amount of coarse powder, and was judged according to the following criteria.
A: s <5.0
B: 5.0 ≦ s <10.0
C: 10.0 ≦ s <15.0
D: 15.0 ≦ s <20.0
E: 20.0 ≦ s
＜処理量を増加した時の粗粉量の増加に関する評価＞
３０ｋｇ／ｈｒ処理時の粗粉割合（体積％）と、２０ｋｇ／ｈｒ処理時の粗粉割合（体積％）との差Δｓを、本発明の熱処理装置における処理量の増加させやすさの指標とし、下記の基準で判断した。
Ａ： Δｓ＜２．０
Ｂ：２．０≦Δｓ＜４．０
Ｃ：４．０≦Δｓ＜６．０
Ｄ：６．０≦Δｓ＜８．０
Ｅ：８．０≦Δｓ
<Evaluation on increase of coarse powder amount when processing amount is increased>
The difference Δs between the coarse powder ratio (volume%) at the time of 30 kg / hr treatment and the coarse powder ratio (volume%) at the time of 20 kg / hr treatment is used as an index of the ease of increasing the treatment amount in the heat treatment apparatus of the present invention. Judgment was made based on the following criteria.
A: Δs <2.0
B: 2.0 ≦ Δs <4.0
C: 4.0 ≦ Δs <6.0
D: 6.0 ≦ Δs <8.0
E: 8.0 ≦ Δs
＜熱処理装置の融着に対する評価＞
各実施例の条件で１時間運転後、トナー用粉体粒子の供給を止めた。そして、工業用ビデオスコープ「ＩＰＬＥＸ ＳＡ ＩＩ Ｒ」（オリンパス（株）製）のスコープ部を熱処理装置側面や粉体粒子輸送経路配管の点検口（不図示）から挿入し、融着状況を確認し、下記の基準で判断した。
Ａ：融着物が全く認められないレベル
Ｂ：融着物が僅かに認められるが、運転上支障のないレベル
Ｃ：融着が認められるが、運転上支障のないレベル
Ｄ：融着が認められ、運転ができなくなるレベル
Ｅ：大きな融着物が認められ、運転ができなくレベル
これらの結果を表２にまとめた。
<Evaluation of heat treatment equipment for fusion>
After operating for 1 hour under the conditions of each example, the supply of toner powder particles was stopped. And insert the scope part of the industrial videoscope “IPLEX SA II R” (Olympus Co., Ltd.) from the side of the heat treatment device and the inspection port (not shown) of the powder particle transport route piping, and confirm the fusion situation. Judgment was made based on the following criteria.
A: No fusion material is observed at all level B: Fused material is slightly recognized, but there is no operational trouble level C: Fusion is observed, but there is no operational trouble level D: Fusion is recognized, Level E at which operation becomes impossible: Large melted material was observed, and operation was impossible at level. These results are summarized in Table 2.
〔実施例２〕
本実施例では、装置構成１を用いて、トナー用粉体粒子Ｂを処理した。
運転条件は、熱風の温度を１８０℃とした以外は、運転条件１と同じとした。
その結果トナー処理量は、２０ｋｇ／ｈｒで平均円形度０．９６５のトナー用熱処理粒子を得た。トナー用粉体粒子Ｂはワックス添加量が６質量部とトナー用粉体粒子Ａより増えたため、平均円形度０．９６５を得るための熱風温度が高くなった。
[Example 2]
In this example, the apparatus powder 1 was used to process the toner powder particles B.
The operating conditions were the same as the operating conditions 1 except that the temperature of the hot air was 180 ° C.
As a result, toner heat treatment particles having an average circularity of 0.965 and a toner processing amount of 20 kg / hr were obtained. In the toner powder particle B, the amount of wax added was 6 parts by mass and increased from the toner powder particle A, so that the hot air temperature for obtaining an average circularity of 0.965 was increased.
次に同じく装置構成１を用いて、トナー用粉体粒子Ｂの処理量を３０ｋｇ／ｈｒとしてトナー用粉体粒子Ｂを熱処理し、平均円形度０．９６５のトナー用熱処理粒子を得た。
この時の運転条件は、熱風の温度を２１０℃とした以外は、運転条件１と同じとした。
熱風温度は実施例１よりも高くなったが、粗粉量ｓは非常に少なく評価Ａであった。また処理量を２０ｋｇ／ｈｒから３０ｋｇ／ｈｒに増加させても粗粉量の差Δｓは非常に少なく評価Ａであった。また装置内部に熱処理されたトナー用熱処理粒子の融着は全くなく評価Ａであった。
これらの結果を表２にまとめた。
Next, using the same apparatus configuration 1, the toner powder particles B were heat-treated at a treatment amount of the toner powder particles B of 30 kg / hr to obtain heat-treated particles for toner having an average circularity of 0.965.
The operating conditions at this time were the same as the operating conditions 1 except that the temperature of the hot air was 210 ° C.
Although the hot air temperature was higher than that in Example 1, the amount of coarse powder s was very small and was evaluated as A. Further, even when the processing amount was increased from 20 kg / hr to 30 kg / hr, the difference Δs in the amount of coarse powder was very small, and the evaluation was A. The heat-treated particles for toner heat-treated inside the apparatus were not fused at all and were evaluated as A.
These results are summarized in Table 2.
〔実施例３〕
本実施例では、装置構成１を用いて、トナー用粉体粒子Ｃを熱処理した。
運転条件は、熱風の温度を１９０℃とした以外は、運転条件１と同じとした。
その結果トナー処理量は、２０ｋｇ／ｈｒで、平均円形度０．９６５のトナー用熱処理粒子を得た。トナー用粉体粒子Ｂはワックス添加量が８質量部とトナー用粉体粒子Ｂより増えたため、平均円形度０．９６５を得るための熱風温度が実施例１、実施例２と比較して高くなった。
Example 3
In this example, the toner powder particles C were heat-treated using the apparatus configuration 1.
The operating conditions were the same as the operating conditions 1 except that the temperature of the hot air was 190 ° C.
As a result, the heat treatment particles for toner having a toner throughput of 20 kg / hr and an average circularity of 0.965 were obtained. Since the toner powder particle B has an added amount of wax of 8 parts by mass and increased from the toner powder particle B, the hot air temperature for obtaining an average circularity of 0.965 is higher than those in the first and second embodiments. became.
次に同じく装置構成１を用いて、トナー用粉体粒子Ｃの処理量を３０ｋｇ／ｈｒとしてトナー用粉体粒子Ｂを熱処理し、平均円形度０．９６５のトナー用熱処理粒子を得た。
この時の運転条件は、熱風温度を２２０℃とした以外は、運転条件１と同じとした。
熱風温度は実施例１よりも高くなったが、粗粉量ｓは非常に少なく評価Ａであった。また処理量を２０ｋｇ／ｈｒから３０ｋｇ／ｈｒに増加させても粗粉量の差Δｓは非常に少なく評価Ａであった。また装置内部に熱処理されたトナー用熱処理粒子の融着は全くなく、評価Ａであった。
これらの結果を表２にまとめた。
Next, using the same apparatus configuration 1, the toner powder particles B were heat-treated at a treatment amount of the toner powder particles C of 30 kg / hr to obtain heat-treated particles for toner having an average circularity of 0.965.
The operating conditions at this time were the same as the operating conditions 1 except that the hot air temperature was 220 ° C.
Although the hot air temperature was higher than that in Example 1, the amount of coarse powder s was very small and was evaluated as A. Further, even when the processing amount was increased from 20 kg / hr to 30 kg / hr, the difference Δs in the amount of coarse powder was very small, and the evaluation was A. Further, there was no fusion of heat-treated toner particles heat-treated inside the apparatus, and the evaluation was A.
These results are summarized in Table 2.
〔実施例４〕
本実施例では、装置構成１を基に円柱状の内部部材の上端部は、処理室の内外円筒半径差ｄ＝２０ｍｍに対し、曲率半径Ｒ＝２ｍｍの丸みを持つとした。このとき、Ｒ／ｄ＝０．１となる。この装置構成を装置構成２としてトナー用粉体粒子Ｃを熱処理した。
運転条件は、熱風の温度を、トナー処理量が２０ｋｇ／ｈｒのときは１９０℃とし、トナー処理量が３０ｋｇ／ｈｒのときは２２０℃とした以外は、運転条件１と同じとした。実施例３と比較すると、熱風温度は同一であった。
Example 4
In the present embodiment, the upper end portion of the columnar inner member based on the apparatus configuration 1 is rounded with a curvature radius R = 2 mm with respect to the inner / outer cylindrical radius difference d = 20 mm of the processing chamber. At this time, R / d = 0.1. With this apparatus configuration as apparatus configuration 2, the toner powder particles C were heat-treated.
The operating conditions were the same as operating conditions 1 except that the temperature of the hot air was 190 ° C. when the toner throughput was 20 kg / hr and 220 ° C. when the toner throughput was 30 kg / hr. Compared with Example 3, the hot air temperature was the same.
また粗粉量ｓは２０ｋｇ／ｈｒ処理時に４．５体積％となり、３０ｋｇ／ｈｒ処理時に４．９体積％となり、評価Ａであった。このため処理量を２０ｋｇ／ｈｒから３０ｋｇ／ｈｒに増加させても粗粉量の差Δｓは０．４体積％となり、評価Ａであった。また融着はほとんど見られず、評価Ｂであった。
これらの結果から、曲率半径Ｒと内外円筒半径差ｄの比がＲ／ｄ＝０．１のとき、実施例３には劣るものの融着を抑えられることが分かった。
これらの結果を表２にまとめた。
The coarse powder amount s was 4.5% by volume during the 20 kg / hr treatment, and 4.9% by volume during the 30 kg / hr treatment, which was evaluated as A. For this reason, even when the processing amount was increased from 20 kg / hr to 30 kg / hr, the difference Δs in the amount of coarse powder was 0.4% by volume, which was an evaluation A. Further, almost no fusion was observed, and the evaluation was B.
From these results, it was found that when the ratio of the radius of curvature R and the inner / outer cylinder radius difference d is R / d = 0.1, fusion can be suppressed although it is inferior to Example 3.
These results are summarized in Table 2.
〔実施例５〕
本実施例では、装置構成１を基に円柱状の内部部材の上端部は、処理室の内外円筒半径差ｄ＝２０ｍｍに対し、曲率半径Ｒ＝２０ｍｍの丸みを持つとした。このとき、Ｒ／ｄ＝１となる。この装置構成を装置構成３としてトナー用粉体粒子Ｃを熱処理した。
運転条件は、熱風の温度を、トナー処理量が２０ｋｇ／ｈｒのときは２００℃とし、トナー処理量が３０ｋｇ／ｈｒのときは２３０℃とした以外は、運転条件１と同じとした。実施例３と比較すると、１０℃高い熱風が必要であった。これは曲率半径が大きくなったことで旋回部材の熱風出口面積が大きくなり、そのため熱風速度が遅くなり熱効率が低下したことが原因と考えられる。
Example 5
In this embodiment, the upper end portion of the columnar inner member based on the apparatus configuration 1 is rounded with a curvature radius R = 20 mm with respect to the inner / outer cylindrical radius difference d = 20 mm of the processing chamber. At this time, R / d = 1. With this apparatus configuration as apparatus configuration 3, the toner powder particles C were heat-treated.
The operating conditions were the same as operating conditions 1 except that the temperature of the hot air was 200 ° C. when the toner throughput was 20 kg / hr and 230 ° C. when the toner throughput was 30 kg / hr. Compared with Example 3, hot air 10 ° C. higher was required. This is considered to be because the hot air outlet area of the swivel member is increased due to the increase in the radius of curvature, so that the hot air speed is reduced and the thermal efficiency is lowered.
また粗粉量ｓは２０ｋｇ／ｈｒ処理時に４．５体積％となり、３０ｋｇ／ｈｒ処理時に６．０体積％となり、評価Ｂであった。このため処理量を２０ｋｇ／ｈｒから３０ｋｇ／ｈｒに増加した場合の粗粉量の差Δｓは１．５体積％となり、評価Ａであった。融着は全くなく、評価Ａであった。
これらの結果から、曲率半径Ｒと内外円筒半径差ｄの比がＲ／ｄ＝１のとき、実施例３に比べ熱効率の低下があるものの融着を抑えられることが分かった。
これらの結果を表２にまとめた。
The coarse powder amount s was 4.5% by volume when treated with 20 kg / hr, and 6.0% by volume when treated with 30 kg / hr. Therefore, the difference Δs in the amount of coarse powder when the processing amount was increased from 20 kg / hr to 30 kg / hr was 1.5 vol%, which was an evaluation A. There was no fusion, and the evaluation was A.
From these results, it was found that when the ratio of the curvature radius R and the inner / outer cylindrical radius difference d is R / d = 1, the fusion can be suppressed although the thermal efficiency is reduced as compared with Example 3.
These results are summarized in Table 2.
〔実施例６〕
本実施例では、装置構成１を基に円柱状の内部部材の外周面径を９０ｍｍとした。また、円柱状の内部部材の上端部は、処理室の内外円筒半径差ｄ＝３０ｍｍに対し、曲率半径Ｒ＝３ｍｍの丸みを持つとした。このとき、Ｒ／ｄ＝０．１となる。この装置構成を装置構成４としてトナー用粉体粒子Ｃを熱処理した。
運転条件は、熱風の温度を、トナー処理量が２０ｋｇ／ｈｒのときは２００℃とし、トナー処理量が３０ｋｇ／ｈｒのときは２３０℃とした以外は、運転条件１と同じとした。実施例３と比較すると、１０℃高い熱風が必要であった。これは内外円筒半径差が大きくなり、そのため処理室を通る熱風速度が遅くなり熱効率が低下したことが原因と考えられる。
Example 6
In the present example, the outer peripheral surface diameter of the cylindrical inner member was set to 90 mm based on the device configuration 1. Further, the upper end portion of the columnar inner member is rounded with a curvature radius R = 3 mm with respect to the inner / outer cylinder radius difference d = 30 mm of the processing chamber. At this time, R / d = 0.1. With this apparatus configuration as apparatus configuration 4, the toner powder particles C were heat-treated.
The operating conditions were the same as operating conditions 1 except that the temperature of the hot air was 200 ° C. when the toner throughput was 20 kg / hr and 230 ° C. when the toner throughput was 30 kg / hr. Compared with Example 3, hot air 10 ° C. higher was required. This is considered to be because the difference between the inner and outer cylindrical radii is increased, and therefore the hot air velocity passing through the processing chamber is reduced and the thermal efficiency is lowered.
また粗粉量ｓは２０ｋｇ／ｈｒ処理時に４．５体積％となり、３０ｋｇ／ｈｒ処理時に５．５体積％となり、評価Ｂであった。このため処理量を２０ｋｇ／ｈｒから３０ｋｇ／ｈｒに増加した場合の粗粉量の差Δｓは１．０体積％となり、評価Ａであった。また融着はほとんど見られず、評価Ｂであった。
これらの結果から、Ｒ／ｄ＝０．１であれば内外円筒半径差ｄを大きくしても、実施例４と同様、融着を抑えられることが分かった。
これらの結果を表２にまとめた。
The coarse powder amount s was 4.5% by volume at the time of 20 kg / hr treatment, and 5.5% by volume at the time of 30 kg / hr treatment. For this reason, the difference Δs in the amount of coarse powder when the treatment amount was increased from 20 kg / hr to 30 kg / hr was 1.0 vol%, which was an evaluation A. Further, almost no fusion was observed, and the evaluation was B.
From these results, it was found that if R / d = 0.1, the fusion could be suppressed as in Example 4 even if the inner and outer cylindrical radius difference d was increased.
These results are summarized in Table 2.
〔実施例７〕
本実施例では、装置構成１を基に円柱状の内部部材の外周面径を１３０ｍｍとした。また、円柱状の内部部材の上端部は、処理室の内外円筒半径差ｄ＝１０ｍｍに対し、曲率半径Ｒ＝１０ｍｍの丸みを持つとした。このとき、Ｒ／ｄ＝１となる。この装置構成を装置構成５としてトナー用粉体粒子Ｃを熱処理した。
運転条件は、熱風の温度を、トナー処理量が２０ｋｇ／ｈｒのときは２００℃とし、トナー処理量が３０ｋｇ／ｈｒのときは２３０℃とした以外は、運転条件１と同じとした。実施例３と比較すると、１０℃高い熱風が必要であった。これは曲率半径が大きくなったことで旋回部材の熱風出口面積が大きくなり、そのため熱風速度が遅くなり熱効率が低下したことが原因と考えられる。
Example 7
In this example, the outer peripheral surface diameter of the cylindrical inner member was set to 130 mm based on the device configuration 1. Further, the upper end portion of the columnar inner member is rounded with a radius of curvature R = 10 mm with respect to the inner / outer cylindrical radius difference d = 10 mm of the processing chamber. At this time, R / d = 1. Using this apparatus configuration as apparatus configuration 5, the toner powder particles C were heat-treated.
The operating conditions were the same as operating conditions 1 except that the temperature of the hot air was 200 ° C. when the toner throughput was 20 kg / hr and 230 ° C. when the toner throughput was 30 kg / hr. Compared with Example 3, hot air 10 ° C. higher was required. This is considered to be because the hot air outlet area of the swivel member is increased due to the increase in the radius of curvature, so that the hot air speed is reduced and the thermal efficiency is lowered.
また粗粉量ｓは２０ｋｇ／ｈｒ処理時に４．７体積％となり、３０ｋｇ／ｈｒ処理時に６．５体積％となり、評価Ｂであった。このため処理量を２０ｋｇ／ｈｒから３０ｋｇ／ｈｒに増加した場合の粗粉量の差Δｓは１．８体積％となり、評価Ａであった。また融着は全くなく、評価Ａであった。
これらの結果から、Ｒ／ｄ＝１であれば内外円筒半径差ｄを小さくしても、実施例５と同様、融着を抑えられることが分かった。
これらの結果を表２にまとめた。
The coarse powder amount s was 4.7% by volume at 20 kg / hr, and 6.5% by volume at 30 kg / hr, which was evaluated as B. For this reason, the difference Δs in the amount of coarse powder when the treatment amount was increased from 20 kg / hr to 30 kg / hr was 1.8% by volume, which was an evaluation A. Moreover, there was no fusion | melting and it was evaluation A.
From these results, it was found that if R / d = 1, the fusion could be suppressed as in Example 5 even if the inner / outer cylindrical radius difference d was reduced.
These results are summarized in Table 2.
〔実施例８〕
本実施例では、装置構成１を基に円柱状の内部部材の上端部は、処理室の内外円筒半径差ｄ＝２０ｍｍに対し、曲率半径Ｒ＝０ｍｍとした。このとき、Ｒ／ｄ＝０となる。この装置構成を装置構成６としてトナー用粉体粒子Ｃを熱処理した。
運転条件は、熱風の温度を、トナー処理量が２０ｋｇ／ｈｒのときは１９０℃とし、トナー処理量が３０ｋｇ／ｈｒのときは２２０℃とした以外は、運転条件１と同じとした。実施例３と比較すると、熱風の温度は同一であった。
Example 8
In the present embodiment, the upper end portion of the columnar inner member based on the apparatus configuration 1 has a radius of curvature R = 0 mm with respect to the inner / outer cylindrical radius difference d = 20 mm of the processing chamber. At this time, R / d = 0. With this apparatus configuration as apparatus configuration 6, the toner powder particles C were heat-treated.
The operating conditions were the same as operating conditions 1 except that the temperature of the hot air was 190 ° C. when the toner throughput was 20 kg / hr and 220 ° C. when the toner throughput was 30 kg / hr. Compared with Example 3, the temperature of the hot air was the same.
また粗粉量ｓは２０ｋｇ／ｈｒ処理時に４．７体積％となり、３０ｋｇ／ｈｒ処理時に６．６体積％となり、評価Ｂであった。このため処理量を２０ｋｇ／ｈｒから３０ｋｇ／ｈｒに増加した場合の粗粉量の差Δｓは１．９体積％となり、評価Ａであった。また、融着については内部部材の上部の壁面に軽微な融着が認められ、評価Ｃであった。
これはＲ／ｄ＝０としたことによって、処理室の上部かつ円柱状の内部部材の近傍に巻き上がり流が発生したことによる。
これらの結果を表２にまとめた。
The coarse powder amount s was 4.7% by volume at 20 kg / hr, and 6.6% by volume at 30 kg / hr, which was evaluated as B. Therefore, the difference Δs in the amount of coarse powder when the treatment amount was increased from 20 kg / hr to 30 kg / hr was 1.9% by volume, which was an evaluation A. As for fusion, slight fusion was observed on the upper wall surface of the internal member, and the evaluation was C.
This is because by setting R / d = 0, a winding flow is generated in the upper part of the processing chamber and in the vicinity of the cylindrical internal member.
These results are summarized in Table 2.
〔実施例９〕
本実施例では、装置構成６を基に旋回部材のブレードの出口角度ｂを９０°とし、垂直出口角度ｃを８０°とした。よってｂ−ｃ＝１０°となる。この装置構成を装置構成７としてトナー用粉体粒子Ｃを熱処理した。
運転条件は、熱風の温度を、トナー処理量が２０ｋｇ／ｈｒのときは１９０℃とし、トナー処理量が３０ｋｇ／ｈｒのときは２２０℃とした以外は、運転条件１と同じとした。実施例８と比較すると、熱風の温度は同一であった。
Example 9
In this example, the exit angle b of the blade of the swivel member was 90 ° and the vertical exit angle c was 80 ° based on the device configuration 6. Therefore, bc = 10 °. Using this apparatus configuration as apparatus configuration 7, the toner powder particles C were heat-treated.
The operating conditions were the same as operating conditions 1 except that the temperature of the hot air was 190 ° C. when the toner throughput was 20 kg / hr and 220 ° C. when the toner throughput was 30 kg / hr. Compared with Example 8, the temperature of the hot air was the same.
また粗粉量ｓは２０ｋｇ／ｈｒ処理時に４．９体積％となり、３０ｋｇ／ｈｒ処理時に６．８体積％となり、評価Ｂであった。このため処理量を２０ｋｇ／ｈｒから３０ｋｇ／ｈｒに増加した場合の粗粉量の差Δｓは１．９体積％となり、評価Ａであった。また、融着については内部部材の上部の壁面に軽微な融着が認められ、評価Ｃであった。
これらの結果から、ｂ−ｃ＝１０°のとき熱処理時の粉体粒子の合一が僅かに増加することが分かった。
これらの結果を表２にまとめた。
The coarse powder amount s was 4.9% by volume when treated with 20 kg / hr, and 6.8% by volume when treated with 30 kg / hr. Therefore, the difference Δs in the amount of coarse powder when the treatment amount was increased from 20 kg / hr to 30 kg / hr was 1.9% by volume, which was an evaluation A. As for fusion, slight fusion was observed on the upper wall surface of the internal member, and the evaluation was C.
From these results, it was found that when bc = 10 °, coalescence of the powder particles during the heat treatment slightly increases.
These results are summarized in Table 2.
〔実施例１０〕
本実施例では、装置構成７を基に旋回部材のブレードの出口角度ｂを９０°とし、垂直出口角度ｃを７９°とした。よってｂ−ｃ＝１１°となる。この装置構成を装置構成８としてトナー用粉体粒子Ｃを熱処理した。
運転条件は、熱風の温度を、トナー処理量が２０ｋｇ／ｈｒのときは１９０℃とし、トナー処理量が３０ｋｇ／ｈｒのときは２２０℃とした以外は、運転条件１と同じとした。実施例９と比較すると、熱風温度は同一であった。
Example 10
In the present embodiment, the outlet angle b of the blade of the swivel member is 90 ° and the vertical outlet angle c is 79 ° based on the device configuration 7. Therefore, bc = 11 °. With this apparatus configuration as apparatus configuration 8, the toner powder particles C were heat-treated.
The operating conditions were the same as operating conditions 1 except that the temperature of the hot air was 190 ° C. when the toner throughput was 20 kg / hr and 220 ° C. when the toner throughput was 30 kg / hr. Compared with Example 9, the hot air temperature was the same.
また粗粉量ｓは２０ｋｇ／ｈｒ処理時に５．０体積％となり、３０ｋｇ／ｈｒ処理時に７．１体積％となり、評価Ｂであった。このため処理量を２０ｋｇ／ｈｒから３０ｋｇ／ｈｒに増加した場合の粗粉量の差Δｓは２．１体積％となり、評価Ｂであった。また、融着については内部部材の上部の壁面に軽微な融着が認められ、評価Ｃであった。
シミュレーションにおいて、ｂ−ｃ＞１０°となるとブレードから流出する熱風の周方向速度のばらつきが許容値を超えることを確認した。このため、熱処理時の粉体粒子の合一が増加し、粗粉量の差Δｓの評価が悪化したと考えられる。
これらの結果を表２にまとめた。
The coarse powder amount s was 5.0% by volume at 20 kg / hr, and 7.1% by volume at 30 kg / hr, which was evaluated as B. For this reason, the difference Δs in the amount of coarse powder when the processing amount was increased from 20 kg / hr to 30 kg / hr was 2.1% by volume, which was an evaluation B. As for fusion, slight fusion was observed on the upper wall surface of the internal member, and the evaluation was C.
In the simulation, it was confirmed that the variation in the circumferential speed of the hot air flowing out from the blade exceeded the allowable value when bc> 10 °. For this reason, it is considered that the coalescence of the powder particles during the heat treatment increased and the evaluation of the difference Δs in the amount of coarse powder deteriorated.
These results are summarized in Table 2.
〔実施例１１〕
本実施例では、装置構成８を基に旋回部材のブレードの入口角度ａを１０°とした。この装置構成を装置構成９としてトナー用粉体粒子Ｃを熱処理した。
運転条件は、熱風の温度を、トナー処理量が２０ｋｇ／ｈｒのときは２１０℃とし、トナー処理量が３０ｋｇ／ｈｒのときは２３０℃とした以外は、運転条件１と同じとした。実施例１０と比較すると、２０ｋｇ／ｈｒ処理時は２０℃高い熱風が必要で、３０ｋｇ／ｈｒ処理時は１０℃高い熱風が必要であった。これは熱風の流れる方向がブレードの入口付近で変わり、ブレード間を通る熱風がスムーズに流れないため、熱効率が僅かに低下したことが原因と考えられる。
Example 11
In the present example, the inlet angle a of the blade of the swivel member was set to 10 ° based on the device configuration 8. With this apparatus configuration as apparatus configuration 9, the toner powder particles C were heat-treated.
The operating conditions were the same as the operating conditions 1 except that the temperature of the hot air was 210 ° C. when the toner throughput was 20 kg / hr and 230 ° C. when the toner throughput was 30 kg / hr. Compared with Example 10, hot air 20 ° C. higher was required during the 20 kg / hr treatment, and hot air higher 10 ° C. was required during the 30 kg / hr treatment. This is probably because the hot air flow direction changes near the entrance of the blade, and the hot air passing between the blades does not flow smoothly, so the thermal efficiency is slightly reduced.
また粗粉量ｓは２０ｋｇ／ｈｒ処理時に５．２体積％となり、３０ｋｇ／ｈｒ処理時に９．５体積％となり、評価Ｂであった。このため処理量を２０ｋｇ／ｈｒから３０ｋｇ／ｈｒに増加した場合の粗粉量の差Δｓは４．３体積％となり、評価Ｃであった。また、融着については内部部材の上部の壁面に軽微な融着が認められ、評価Ｃであった。
これらの結果から、ａ＝１０°のとき熱風温度が高くなるために熱処理時の粉体粒子の合一が僅かに増加することが分かった。
これらの結果を表２にまとめた。
The coarse powder amount s was 5.2% by volume when treated with 20 kg / hr, and 9.5% by volume when treated with 30 kg / hr. For this reason, the difference Δs in the amount of coarse powder when the processing amount was increased from 20 kg / hr to 30 kg / hr was 4.3 vol%, which was an evaluation C. As for fusion, slight fusion was observed on the upper wall surface of the internal member, and the evaluation was C.
From these results, it was found that, when a = 10 °, the hot air temperature is high, and the coalescence of the powder particles during the heat treatment is slightly increased.
These results are summarized in Table 2.
〔実施例１２〕
本実施例では、装置構成８を基に旋回部材のブレードの入口角度ａを−１０°とした。この装置構成を装置構成１０としてトナー用粉体粒子Ｃを熱処理した。
運転条件は、熱風の温度を、トナー処理量が２０ｋｇ／ｈｒのときは２１０℃とし、トナー処理量が３０ｋｇ／ｈｒのときは２３０℃とした以外は、運転条件１と同じとした。実施例１０と比較すると、２０ｋｇ／ｈｒ処理時は２０℃高い熱風が必要で、３０ｋｇ／ｈｒ処理時は１０℃高い熱風が必要であった。これは熱風の流れる方向がブレードの入口付近で変わり、ブレード間を通る熱風がスムーズに流れないため、熱効率が僅かに低下したことが原因と考えられる。
Example 12
In the present embodiment, the inlet angle a of the blade of the swivel member is set to −10 ° based on the device configuration 8. Using this apparatus configuration as apparatus configuration 10, powder particles C for toner were heat-treated.
The operating conditions were the same as the operating conditions 1 except that the temperature of the hot air was 210 ° C. when the toner throughput was 20 kg / hr and 230 ° C. when the toner throughput was 30 kg / hr. Compared with Example 10, hot air 20 ° C. higher was required during the 20 kg / hr treatment, and hot air higher 10 ° C. was required during the 30 kg / hr treatment. This is probably because the hot air flow direction changes near the entrance of the blade, and the hot air passing between the blades does not flow smoothly, so the thermal efficiency is slightly reduced.
また粗粉量ｓは２０ｋｇ／ｈｒ処理時に５．４体積％となり、３０ｋｇ／ｈｒ処理時に９．８体積％となり、評価Ｂであった。このため処理量を２０ｋｇ／ｈｒから３０ｋｇ／ｈｒに増加した場合の粗粉量の差Δｓは４．４体積％となり、評価Ｃであった。また、融着については円柱状内部部材上部の壁面に軽微な融着が認められ、評価Ｃであった。
これらの結果から、ａ＝−１０°のとき熱風温度が高くなるために熱処理時の粉体粒子の合一が僅かに増加することが分かった。
これらの結果を表２にまとめた。
以上の本実施例は、装置の円筒状の外壁の内周面径を１５０ｍｍとしているが、本発明はこの条件に限定されるものではない。内周面径を大きくすることでより多くのトナー用粉体粒子を熱処理することが可能である。
The coarse powder amount s was 5.4% by volume at 20 kg / hr, and 9.8% by volume at 30 kg / hr. Therefore, the difference Δs in the amount of coarse powder when the processing amount was increased from 20 kg / hr to 30 kg / hr was 4.4% by volume, which was an evaluation C. Regarding the fusion, slight fusion was observed on the wall surface of the upper part of the cylindrical inner member, and the evaluation was C.
From these results, it was found that, when a = −10 °, the hot air temperature becomes high, and the coalescence of the powder particles during the heat treatment slightly increases.
These results are summarized in Table 2.
In the above embodiment, the inner peripheral surface diameter of the cylindrical outer wall of the apparatus is 150 mm, but the present invention is not limited to this condition. It is possible to heat-treat more toner powder particles by increasing the inner peripheral surface diameter.
〔比較例１〕
本比較例では、装置構成９を基に旋回部材のブレードの入口角度ａを１１°とした。この装置構成を装置構成１１としてトナー用粉体粒子Ｃを熱処理した。
運転条件は、熱風の温度を、トナー処理量が２０ｋｇ／ｈｒのときは２２０℃とし、トナー処理量が３０ｋｇ／ｈｒのときは２４０℃とした以外は、運転条件１と同じとした。実施例１１と比較すると、１０℃高い熱風が必要であった。これは熱風の流れる方向がブレードの入口付近で変わり、ブレード間を通る熱風がスムーズに流れないため、熱効率が僅かに低下したことが原因と考えられる。
[Comparative Example 1]
In this comparative example, the inlet angle “a” of the blade of the swivel member was set to 11 ° based on the device configuration 9. With this apparatus configuration as apparatus configuration 11, the toner powder particles C were heat-treated.
The operating conditions were the same as operating conditions 1 except that the temperature of the hot air was 220 ° C. when the toner throughput was 20 kg / hr and 240 ° C. when the toner throughput was 30 kg / hr. Compared with Example 11, hot air 10 ° C. higher was required. This is probably because the hot air flow direction changes near the entrance of the blade, and the hot air passing between the blades does not flow smoothly, so the thermal efficiency is slightly reduced.
また粗粉量ｓは２０ｋｇ／ｈｒ処理時に５．４体積％となり、３０ｋｇ／ｈｒ処理時に１０．０体積％となり、評価Ｃであった。このため処理量を２０ｋｇ／ｈｒから３０ｋｇ／ｈｒに増加した場合の粗粉量の差Δｓは４．６体積％となり、評価Ｃであった。また、融着については円柱状内部部材上部の壁面に軽微な融着が認められ、評価Ｃであった。
これらの結果から、ａ＞１０°となると熱風温度が高くなるために熱処理時の粉体粒子の合一が増加し、粗粉量ｓの評価が悪化したことが分かった。
これらの結果を表２にまとめた。
The coarse powder amount s was 5.4% by volume when treated with 20 kg / hr, and 10.0% by volume when treated with 30 kg / hr. Therefore, the difference Δs in the amount of coarse powder when the treatment amount was increased from 20 kg / hr to 30 kg / hr was 4.6% by volume, which was an evaluation C. Regarding the fusion, slight fusion was observed on the wall surface of the upper part of the cylindrical inner member, and the evaluation was C.
From these results, it was found that when a> 10 °, the hot air temperature increased, so that the coalescence of the powder particles during the heat treatment increased and the evaluation of the coarse powder amount s deteriorated.
These results are summarized in Table 2.
〔比較例２〕
本比較例では、装置構成１０を基に旋回部材のブレードの入口角度ａを−１１°とした。この装置構成を装置構成１２としてトナー用粉体粒子Ｃを熱処理した。
運転条件は、熱風の温度を、トナー処理量が２０ｋｇ／ｈｒのときは２２０℃とし、トナー処理量が３０ｋｇ／ｈｒのときは２４０℃とした以外は、運転条件１と同じとした。実施例１２と比較すると、１０℃高い熱風が必要であった。これは熱風の流れる方向がブレードの入口付近で変わり、ブレード間を通る熱風がスムーズに流れないため、熱効率が僅かに低下したことが原因と考えられる。
[Comparative Example 2]
In this comparative example, the inlet angle a of the blade of the swivel member was set to -11 ° based on the device configuration 10. Using this apparatus configuration as apparatus configuration 12, the powder particles C for toner were heat-treated.
The operating conditions were the same as operating conditions 1 except that the temperature of the hot air was 220 ° C. when the toner throughput was 20 kg / hr and 240 ° C. when the toner throughput was 30 kg / hr. Compared with Example 12, hot air 10 ° C. higher was required. This is probably because the hot air flow direction changes near the entrance of the blade, and the hot air passing between the blades does not flow smoothly, so the thermal efficiency is slightly reduced.
また粗粉量ｓは２０ｋｇ／ｈｒ処理時に５．６体積％となり、３０ｋｇ／ｈｒ処理時に１０．２体積％となり、評価Ｃであった。このため処理量を２０ｋｇ／ｈｒから３０ｋｇ／ｈｒに増加した場合の粗粉量の差Δｓは４．６体積％となり、評価Ｃであった。また、融着については円柱状内部部材上部の壁面に軽微な融着が認められ、評価Ｃであった。
これらの結果から、ａ＜−１０°となると熱風温度が高くなるために熱処理時の粉体粒子の合一が増加し、粗粉量ｓの評価が悪化したことが分かった。
これらの結果を表２にまとめた。
The coarse powder amount s was 5.6% by volume at the time of 20 kg / hr treatment, and 10.2% by volume at the time of 30 kg / hr treatment. Therefore, the difference Δs in the amount of coarse powder when the treatment amount was increased from 20 kg / hr to 30 kg / hr was 4.6% by volume, which was an evaluation C. Regarding the fusion, slight fusion was observed on the wall surface of the upper part of the cylindrical inner member, and the evaluation was C.
From these results, it was found that when a <−10 °, the hot air temperature increased, so that the coalescence of the powder particles during the heat treatment increased, and the evaluation of the coarse powder amount s deteriorated.
These results are summarized in Table 2.
〔比較例３〕
図１５に本比較例で使用した装置の構成を示した。かかる装置の構成を装置構成１３としてトナー用粉体粒子Ｃを熱処理し、平均円形度０．９６５のトナー用熱処理粒子を得た。本装置は排出手段１５８が一口のストレート排気、粉体供給手段１５５が一口、熱風供給手段１５４から熱風がストレートに供給される構成となっている。またこの時の排出手段１５８の排気口の総断面積と粉体供給手段１５５の出口（供給口）の総断面積との関係は、排気口の総断面積＞供給口の総断面積となっている。粉体供給手段１５５から供給されたトナー用紛体粒子は分散板１５１に衝突し、左右に分散される。
[Comparative Example 3]
FIG. 15 shows the configuration of the apparatus used in this comparative example. The toner powder particles C were heat-treated with the device configuration as device configuration 13 to obtain toner heat-treated particles having an average circularity of 0.965. In this apparatus, the discharge means 158 is a single straight exhaust, the powder supply means 155 is a single discharge, and hot air is supplied straight from the hot air supply means 154. At this time, the relationship between the total cross-sectional area of the exhaust port of the discharge means 158 and the total cross-sectional area of the outlet (supply port) of the powder supply means 155 is such that the total cross-sectional area of the exhaust port> the total cross-sectional area of the supply port. ing. The toner powder particles supplied from the powder supply means 155 collide with the dispersion plate 151 and are dispersed left and right.
運転条件は、熱風の温度を、トナー処理量が２０ｋｇ／ｈｒのときは２５０℃とし、トナー処理量が３０ｋｇ／ｈｒのときは３４０℃とした以外は、運転条件１と同じとした。また本装置構成ではメッシュ１５２から外気を取り込むことによって装置内を冷却する構成をとっているため、冷風は導入しなかった。よって実施例３と比較して熱風温度は上昇した。 The operating conditions were the same as operating conditions 1 except that the temperature of the hot air was 250 ° C. when the toner throughput was 20 kg / hr and 340 ° C. when the toner throughput was 30 kg / hr. Further, in this apparatus configuration, the inside of the apparatus is cooled by taking in outside air from the mesh 152, and thus cold air was not introduced. Therefore, compared with Example 3, the hot air temperature rose.
粗粉量ｓは、２０ｋｇ／ｈｒ処理時には１８．３体積％、３０ｋｇ／ｈｒ処理時には２７．５体積％となり、評価Ｅであった。このため処理量を２０ｋｇ／ｈｒから３０ｋｇ／ｈｒに増加した場合の粗粉量の差Δｓは９．２体積％となり、評価Ｅであった。また、融着については装置内部に運転に支障が出るレベルの大きな融着が認められ、評価Ｅであった。
これらの結果を表２にまとめた。
The coarse powder amount s was 18.3% by volume during the 20 kg / hr treatment and 27.5 vol.% During the 30 kg / hr treatment, which was an evaluation E. Therefore, the difference Δs in the amount of coarse powder when the treatment amount was increased from 20 kg / hr to 30 kg / hr was 9.2% by volume, which was an evaluation E. As for the fusion, a large degree of fusion that would hinder the operation inside the apparatus was recognized, and the evaluation was E.
These results are summarized in Table 2.
〔比較例４〕
図１６に本比較例で使用した装置の構成を示した。（ａ）は熱風供給手段１６４および粉体供給手段１６５を上から見た図である。（ｂ）は装置全体の概略構成を示す断面図である。かかる装置の構成を装置構成１４としてトナー用粉体粒子Ｃを熱処理し、平均円形度０．９６５のトナー用熱処理粒子を得た。本装置は排出手段１６８が一口のストレート排気、粉体供給手段１６５が一口で、粉体供給手段１６５から供給されるトナー用粉体粒子と熱風供給手段１６４から供給される熱風とが逆方向に旋回して装置内に供給される構成となっている。また冷風供給手段はスリット１６１を設けることによって装置の壁面からストレートに導入される第一冷風供給手段１６６と、排出手段１６８を冷却するために接線方向から導入される第二冷風供給手段１６７が設けられている。
[Comparative Example 4]
FIG. 16 shows the configuration of the apparatus used in this comparative example. (A) is the figure which looked at the hot air supply means 164 and the powder supply means 165 from the top. (B) is sectional drawing which shows schematic structure of the whole apparatus. The toner powder particles C were heat-treated with the apparatus structure as the apparatus structure 14 to obtain heat-treated particles for toner having an average circularity of 0.965. In this apparatus, the discharge means 168 is a single straight exhaust, the powder supply means 165 is a single discharge, and the toner powder particles supplied from the powder supply means 165 and the hot air supplied from the hot air supply means 164 are in opposite directions. It is the structure which turns and is supplied in an apparatus. The cold air supply means is provided with a first cold air supply means 166 introduced straight from the wall surface of the apparatus by providing the slit 161, and a second cold air supply means 167 introduced from the tangential direction to cool the discharge means 168. It has been.
本比較例における運転条件と運転条件１との相違点は以下のとおりである。
熱風温度 トナー処理量が２０ｋｇ／ｈｒのとき ３００℃、
トナー処理量が３０ｋｇ／ｈｒのとき ４００℃。
第一冷風供給手段から供給される冷風の流量 ０．２ｍ３／分、
第二冷風供給手段から供給される冷風の流量 ０．１５ｍ３／分。
実施例３と比較して熱風温度は上昇した。
The difference between the operating condition and the operating condition 1 in this comparative example is as follows.
Hot air temperature When the toner processing amount is 20 kg / hr, 300 ° C.,
400 ° C. when the toner processing amount is 30 kg / hr.
The flow rate of cold air supplied from the first cold air supply means is 0.2 m 3 / min,
The flow rate of cold air supplied from the second cold air supply means is 0.15 m 3 / min.
Compared with Example 3, the hot air temperature rose.
粗粉量ｓは、２０ｋｇ／ｈｒ処理時に２０．０体積％となり、３０ｋｇ／ｈｒ処理時に３０．０体積％となり、評価Ｅであった。このため処理量を２０ｋｇ／ｈｒから３０ｋｇ／ｈｒに増加した場合の粗粉量の差Δｓは１０．０体積％となり、評価Ｅであった。また、融着については装置内部に運転に支障が出るレベルの大きな融着が認められ、評価Ｅであった。
これらの結果を表２にまとめた。
The coarse powder amount s was 20.0% by volume during the 20 kg / hr treatment, and 30.0% by volume during the 30 kg / hr treatment, which was an evaluation E. For this reason, the difference Δs in the amount of coarse powder when the processing amount was increased from 20 kg / hr to 30 kg / hr was 10.0% by volume, which was an evaluation E. As for the fusion, a large degree of fusion that would hinder the operation inside the apparatus was recognized, and the evaluation was E.
These results are summarized in Table 2.
〔比較例５〕
図１７に本比較例で使用した装置の構成を示した。（ａ）は熱風供給手段１７４および粉体供給手段１７５を上から見た図である。（ｂ）は装置全体の概略構成を示す断面図である。かかる装置の構成を装置構成１５としてトナー用粉体粒子Ｃを熱処理し、平均円形度０．９６５のトナー用熱処理粒子を得た。本比較例の装置構成は比較例４で示した装置構成１４の熱風供給手段と粉体供給手段を改造し、トナー用粉体粒子１７１と熱風が同方向に旋回して装置内に供給される構成となっている。また熱風供給手段１７４と粉体供給手段１７５の関係は、図１７の様に粉体供給手段１７５の外側から熱風が供給される構成となっている。また、図１６に示した装置と同様に、図１７に示した装置もスリット１６１を備える。
[Comparative Example 5]
FIG. 17 shows the configuration of the apparatus used in this comparative example. (A) is the figure which looked at the hot air supply means 174 and the powder supply means 175 from the top. (B) is sectional drawing which shows schematic structure of the whole apparatus. The toner powder particles C were heat-treated with the apparatus structure as apparatus structure 15 to obtain heat-treated particles for toner having an average circularity of 0.965. The apparatus configuration of this comparative example is a modification of the hot air supply means and the powder supply means of the apparatus configuration 14 shown in Comparative Example 4, and the toner powder particles 171 and the hot air are swung in the same direction and supplied into the apparatus. It has a configuration. Further, the relationship between the hot air supply means 174 and the powder supply means 175 is such that hot air is supplied from the outside of the powder supply means 175 as shown in FIG. Similarly to the apparatus shown in FIG. 16, the apparatus shown in FIG. 17 includes a slit 161.
本比較例における運転条件と運転条件１との相違点は以下のとおりである。
熱風温度 トナー処理量が２０ｋｇ／ｈｒのとき ３５０℃。
第一冷風供給手段から供給される冷風の流量 ０．２ｍ３／分、
第二冷風供給手段から供給される冷風の流量 ０．１５ｍ３／分。
実施例３と比較して２０ｋｇ／ｈｒ処理時の熱風温度は上昇した。
The difference between the operating condition and the operating condition 1 in this comparative example is as follows.
Hot air temperature 350 ° C. when toner throughput is 20 kg / hr.
The flow rate of cold air supplied from the first cold air supply means is 0.2 m 3 / min,
The flow rate of cold air supplied from the second cold air supply means is 0.15 m 3 / min.
Compared to Example 3, the hot air temperature during the 20 kg / hr treatment increased.
粗粉量ｓは２０ｋｇ／ｈｒ処理時に２０．０体積％、３０ｋｇ／ｈｒ処理時は熱風温度を４５０℃まで上げても平均円形度０．９６５を得ることができなかった。このため粗粉量ｓ、粗粉量の差Δｓ及び融着の評価を行うことができなかった。
これらの結果を表２にまとめた。
The coarse powder amount s was 20.0% by volume during the 20 kg / hr treatment, and an average circularity of 0.965 could not be obtained even when the hot air temperature was increased to 450 ° C. during the 30 kg / hr treatment. Therefore, the coarse powder amount s, the coarse powder amount difference Δs, and the fusion cannot be evaluated.
These results are summarized in Table 2.
〔参考例１〕
本参考例で用いる装置構成は、装置構成１を基にブレードの形状において入口角度ａが−１０°≦ａ≦１０°の範囲から大きく外れ、７１°とした構成となっている。更に、円柱状内部部材の上端部は、処理室の内外円筒半径差ｄ＝２０ｍｍに対し、曲率半径Ｒ＝０ｍｍとした。このとき、Ｒ／ｄ＝０となる。一方、旋回部材のブレードの出口角度ｂを７１°とし、垂直出口角度ｃを６９°とした。よってｂ−ｃ＝２°となっている。この装置構成を装置構成１６としてトナー用粉体粒子Ａを熱処理し、平均円形度０．９６５のトナー用熱処理粒子を得た。
運転条件は、熱風の温度を、トナー処理量が２０ｋｇ／ｈｒのときは２００℃とし、トナー処理量が３０ｋｇ／ｈｒのときは２２０℃とした以外は、運転条件１と同じとした。実施例１と比較すると、２０ｋｇ／ｈｒ処理時は３０℃高い熱風が必要であった。また３０ｋｇ／ｈｒ処理時は２０℃高い熱風が必要であった。
[Reference Example 1]
The apparatus configuration used in this reference example is configured such that the inlet angle a greatly deviates from the range of −10 ° ≦ a ≦ 10 ° in the blade shape based on the device configuration 1 and is 71 °. Further, the upper end portion of the columnar inner member has a radius of curvature R = 0 mm with respect to the inner / outer cylinder radius difference d = 20 mm of the processing chamber. At this time, R / d = 0. On the other hand, the exit angle b of the blade of the swivel member was 71 °, and the vertical exit angle c was 69 °. Therefore, bc = 2 °. Using this apparatus configuration as apparatus configuration 16, the toner powder particles A were heat-treated to obtain toner heat-treated particles having an average circularity of 0.965.
The operating conditions were the same as operating conditions 1 except that the temperature of the hot air was 200 ° C. when the toner throughput was 20 kg / hr and 220 ° C. when the toner throughput was 30 kg / hr. Compared to Example 1, hot air of 30 ° C. higher was required during the 20 kg / hr treatment. Further, hot air of 20 ° C. was required during the 30 kg / hr treatment.
粗粉量ｓは、２０ｋｇ／ｈｒ処理時に５．０体積％、３０ｋｇ／ｈｒ処理時に１３．０体積％となり、評価Ｃであった。このため処理量を２０ｋｇ／ｈｒから３０ｋｇ／ｈｒに増加した場合の粗粉量の差Δｓは８．０体積％となり、評価Ｅであった。また、融着については円柱状内部部材上部の壁面に融着が認められ、評価Ｄであった。
これらの結果から、ａ＞１０°のため熱風温度が高くなり熱処理時の粉体粒子の合一が増加し、粗粉量ｓ及び粗粉量の差Δｓの評価が悪化したと考えられる。またＲ／ｄ＝０としたことによって、処理室の上部かつ円柱状内部部材の近傍に巻き上がり流が発生し、融着の評価が悪化したと考えられる。
これらの結果を表２にまとめた。
The amount of coarse powder s was 5.0 vol% at the time of 20 kg / hr treatment and 13.0 vol% at the time of 30 kg / hr treatment, which was an evaluation C. Therefore, the difference Δs in the amount of coarse powder when the treatment amount was increased from 20 kg / hr to 30 kg / hr was 8.0% by volume, which was an evaluation E. Further, the fusion was observed on the wall surface of the upper part of the cylindrical inner member, and the evaluation was D.
From these results, since a> 10 °, the hot air temperature is increased, the coalescence of the powder particles during the heat treatment is increased, and the evaluation of the coarse powder amount s and the coarse powder amount difference Δs is considered to be deteriorated. Further, by setting R / d = 0, it is considered that a roll-up flow is generated in the upper part of the processing chamber and in the vicinity of the cylindrical inner member, and the evaluation of fusion is deteriorated.
These results are summarized in Table 2.
〔参考例２〕
本参考例では装置構成１６を用いてトナー用粉体粒子Ｃを熱処理し、平均円形度０．９６５のトナー用熱処理粒子を得た。
運転条件は、熱風の温度を、トナー処理量が２０ｋｇ／ｈｒのときは２３０℃とし、トナー処理量が３０ｋｇ／ｈｒのときは２５０℃とした以外は、運転条件１と同じとした。実施例３と比較すると、２０ｋｇ／ｈｒ処理時は４０℃高い熱風が必要であった。また３０ｋｇ／ｈｒ処理時は３０℃高い熱風が必要であった。
[Reference Example 2]
In this reference example, the toner powder particles C were heat-treated using the apparatus configuration 16 to obtain toner heat-treated particles having an average circularity of 0.965.
The operating conditions were the same as operating conditions 1 except that the temperature of the hot air was 230 ° C. when the toner throughput was 20 kg / hr and 250 ° C. when the toner throughput was 30 kg / hr. Compared to Example 3, hot air higher by 40 ° C. was required during the 20 kg / hr treatment. Further, hot air of 30 ° C. was required during the 30 kg / hr treatment.
粗粉量ｓは、２０ｋｇ／ｈｒ処理時に６．０体積％、３０ｋｇ／ｈｒ処理時に１５．０体積％となり、評価Ｄであった。このため処理量を２０ｋｇ／ｈｒから３０ｋｇ／ｈｒに増加した場合の粗粉量の差Δｓは９．０体積％となり、評価Ｅであった。また、融着については円柱状内部部材上部の壁面に融着が認められ、評価Ｄであった。
これらの結果から参考例１と同様の理由により、粗粉量ｓ、粗粉量の差Δｓ、融着の評価が悪化したと考えられる。
これらの結果を表２にまとめた。
Coarse powder amount s was 6.0 vol% at the time of 20 kg / hr treatment, and 15.0 vol% at the time of 30 kg / hr treatment, which was evaluated D. Therefore, the difference Δs in the amount of coarse powder when the treatment amount was increased from 20 kg / hr to 30 kg / hr was 9.0% by volume, which was an evaluation E. Further, the fusion was observed on the wall surface of the upper part of the cylindrical inner member, and the evaluation was D.
From these results, it is considered that the coarse powder amount s, the coarse powder amount difference Δs, and the evaluation of fusion deteriorated for the same reason as in Reference Example 1.
These results are summarized in Table 2.
１：外壁
２：内部部材
３：処理室
４、１５４、１６４、１７４：熱風供給手段
５、１５５、１６５、１７５：粉体粒子供給手段
６、１６６：第一冷風供給手段
７、１６７：第二冷風供給手段
８、１５８、１６８：排出手段
９：熱風旋回部材
１０：円柱状内部部材の中心軸
１１：熱風旋回部材のブレード
１２：中心軸から近い方のブレードの端部と中心軸とを結ぶ直線
１３：中心軸から近い方のブレードの端部に接する直線
１４：中心軸から遠い方のブレードの端部と中心軸とを結ぶ直線
１５：中心軸から遠い方のブレードの端部に接する直線
１６：中心軸から遠い方のブレードの端部と中心軸とを結ぶ直線
１７：第１のブレードと旋回方向側に隣り合う第２のブレードの法線のうち、第１のブレードの中心軸１０から遠い方の端部を通る直線
１８：第１のブレードの中心軸１０から遠い方の端部を通り、かつ直線１７に対して直交する直線
１９：略円錐状の熱風分配部材
１５１：分散板
１５２：メッシュ
１６１：スリット
１７１：トナー用粉体粒子
1: outer wall 2: inner member 3: processing chambers 4, 154, 164, 174: hot air supply means 5, 155, 165, 175: powder particle supply means 6, 166: first cold air supply means 7, 167: second Cold air supply means 8, 158, 168: Discharge means 9: Hot air swirling member 10: Center axis of the cylindrical inner member 11: Blade 12 of the hot air swirling member: Connect the end of the blade closer to the central axis and the central axis Straight line 13: A straight line contacting the end of the blade closer to the central axis 14: A straight line connecting the end of the blade farther from the central axis and the central axis 15: A straight line contacting the end of the blade farther from the central axis 16: A straight line connecting the end of the blade farther from the central axis and the central axis 17: Among the normal lines of the first blade and the second blade adjacent to the turning direction, the central axis 10 of the first blade A straight line passing through the end far from 8: A straight line 19 passing through an end of the first blade far from the central axis 10 and orthogonal to the straight line 17: a substantially conical hot air distribution member 151: a dispersion plate 152: a mesh 161: a slit 171: toner Powder particles
Claims (5)
（１）円筒状の外壁の内周面と、該外壁の内部に該外壁の中心軸と同軸上に配置された円柱状の内部部材の外周面とで形成され、該粉体粒子の熱処理が行われる同軸二重円筒状の処理室と、
（２）該処理室に該粉体粒子を供給するための粉体粒子供給手段と、
（３）供給された該粉体粒子を熱処理するための熱風を供給する熱風供給手段と、
（４）供給された該粉体粒子を冷却するための冷風を該処理室内に供給する冷風供給手段と、
（５）熱処理された該粉体粒子を該処理室の外に排出する排出手段と、
（６）該熱風を該処理室において螺旋状に旋回させるための旋回部材とを具備し、
該旋回部材は、
該内部部材の天面上に、該内部部材の中心軸から等距離に、該中心軸の周囲に配列された同形状の複数のブレードを有し、
該ブレードを含みかつ該中心軸と直交する断面において、該中心軸から近い方の該ブレードの端部と該中心軸とを結ぶ直線と、該端部に接する直線とのなす角度で規定されるブレードの入口角度ａが、下記式（１）を満たすことを特徴とする粉体粒子の熱処理装置。
−１０°≦ａ≦１０° 式（１） A heat treatment apparatus for powder particles containing wax, the heat treatment apparatus,
(1) An inner peripheral surface of a cylindrical outer wall and an outer peripheral surface of a cylindrical inner member arranged coaxially with the central axis of the outer wall inside the outer wall, and heat treatment of the powder particles A coaxial double cylindrical processing chamber,
(2) powder particle supply means for supplying the powder particles to the processing chamber;
(3) hot air supply means for supplying hot air for heat-treating the supplied powder particles;
(4) cold air supply means for supplying cold air for cooling the supplied powder particles into the processing chamber;
(5) discharging means for discharging the heat-treated powder particles out of the processing chamber;
(6) a swirling member for swirling the hot air in the processing chamber in a spiral shape;
The swivel member is
On the top surface of the internal member, there are a plurality of blades of the same shape arranged around the central axis at an equal distance from the central axis of the internal member,
In a cross section including the blade and perpendicular to the central axis, the cross section is defined by an angle formed by a straight line connecting the end of the blade closer to the central axis and the central axis and a straight line in contact with the end. An apparatus for heat-treating powder particles, wherein an inlet angle a of the blade satisfies the following formula (1):
−10 ° ≦ a ≦ 10 ° Formula (1)
該中心軸から遠い方のブレードの端部と該中心軸を結ぶ直線を第１−１の直線とし、
該端部に接する直線を第１−２の直線とした場合に、
第１−１の直線と第１−２の直線とのなす角度で規定されるブレードの出口角度をｂとし、
第１のブレードの該中心軸から遠い方の端部と該中心軸とを結ぶ直線を第２−１の直線とし、
第１のブレードと旋回方向側に隣り合う第２のブレードの法線のうち、第１のブレードの該中心軸から遠い方の該端部を通る直線を第２−２の直線とし、
第１のブレードの中心軸１０から遠い方の端部を通り、かつ第２−２の直線に対して直交する直線を第２−３の直線とした場合に、
第２−１の直線と第２−３の直線とのなす角度で規定されるブレードの垂直出口角度をｃとするとき、下記式（２）を満たす請求項１に記載の熱処理装置。
０°≦ｂ−ｃ≦１０° 式（２） In a cross section including the blade and perpendicular to the central axis,
A straight line connecting the end of the blade farther from the central axis and the central axis is a 1-1 straight line,
When the straight line in contact with the end is a first-second straight line,
The exit angle of the blade defined by the angle formed by the 1-1 straight line and the 1-2 straight line is b,
A straight line connecting the end of the first blade far from the central axis and the central axis is a 2-1 straight line,
Of the normal lines of the second blade adjacent to the first blade in the turning direction side, a straight line passing through the end portion far from the central axis of the first blade is defined as a 2-2 straight line,
When a straight line that passes through the end far from the central axis 10 of the first blade and is orthogonal to the 2-2 straight line is a 2-3 straight line,
2. The heat treatment apparatus according to claim 1, wherein a vertical exit angle of the blade defined by an angle formed by the 2-1 straight line and the 2-3 straight line is c, and the following formula (2) is satisfied.
0 ° ≦ b−c ≦ 10 ° Formula (2)
前記外壁の内周面の半径（内周面径）と前記内部部材の外周面の半径（外周面径）との差（内外円筒半径差）をｄとした場合に、下記式（３）を満たす請求項１又は２に記載の熱処理装置。
Ｒ≧０．１×ｄ 式（３） The radius of curvature of the upper end of the internal member is R,
When the difference (inner and outer cylinder radius difference) between the radius of the inner peripheral surface of the outer wall (inner peripheral surface diameter) and the radius of the outer peripheral surface of the inner member (outer peripheral surface diameter) is d, The heat treatment apparatus according to claim 1 or 2, which is satisfied.
R ≧ 0.1 × d Formula (3)
該熱処理装置が、請求項１乃至４の何れか一項に記載の粉体粒子の熱処理装置であることを特徴とするトナーの製造方法。
A toner manufacturing method for obtaining a toner through a heat treatment step of heat-treating powder particles containing a binder resin and a colorant using a heat treatment apparatus,
5. A toner manufacturing method, wherein the heat treatment apparatus is the powder particle heat treatment apparatus according to any one of claims 1 to 4.
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