JP2011053289A - Semiconductive endless belt - Google Patents
Semiconductive endless belt Download PDFInfo
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- JP2011053289A JP2011053289A JP2009199825A JP2009199825A JP2011053289A JP 2011053289 A JP2011053289 A JP 2011053289A JP 2009199825 A JP2009199825 A JP 2009199825A JP 2009199825 A JP2009199825 A JP 2009199825A JP 2011053289 A JP2011053289 A JP 2011053289A
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- endless belt
- semiconductive endless
- conductive material
- ion conductive
- porous silica
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Landscapes
- Electrostatic Charge, Transfer And Separation In Electrography (AREA)
Abstract
Description
本発明は、電子写真方式の画像形成装置に用いられる半導電性エンドレスベルトに関するものであり、特に、イオン伝導性材料を添加することにより半導電性を付与した半導電性エンドレスベルトに関する。 The present invention relates to a semiconductive endless belt used in an electrophotographic image forming apparatus, and more particularly to a semiconductive endless belt provided with semiconductivity by adding an ion conductive material.
電子写真方式の画像形成装置は、高速化、高画質化、カラー化が進んでおり、これらの画像形成装置には転写搬送ベルトや中間転写ベルトとして半導電性エンドレスベルトが多用されている。転写搬送ベルトは記録媒体を搬送すると同時に感光体上のトナー像を記録媒体へ直接転写するため、画像形成時には感光体と転写搬送ベルトとの間に記録媒体が介在し、両者は直接接触することはない。しかしながら、非画像形成時には、記録媒体が介在しないため、感光体と転写搬送ベルトとを直接接触させた状態で停止させる画像形成装置もある。一方、中間転写ベルトは感光体と直接接触して感光体上のトナー像を受け取るため、感光体と直接接触する頻度が高い。 Electrophotographic image forming apparatuses are increasing in speed, image quality, and color. In these image forming apparatuses, semiconductive endless belts are frequently used as transfer conveyance belts and intermediate transfer belts. Since the transfer and conveyance belt conveys the recording medium and simultaneously transfers the toner image on the photosensitive member directly to the recording medium, the recording medium is interposed between the photosensitive member and the transfer and conveyance belt during image formation. There is no. However, there is also an image forming apparatus that stops in a state where the photosensitive member and the transfer conveyance belt are in direct contact with each other because no recording medium is interposed during non-image formation. On the other hand, since the intermediate transfer belt receives the toner image on the photosensitive member directly in contact with the photosensitive member, the intermediate transfer belt is frequently in direct contact with the photosensitive member.
これらの画像形成装置に用いられるエンドレスベルトには、体積抵抗率が1×105〜1×1013Ω・cmの半導電性領域の電気抵抗とその均一性が求められている。エンドレスベルトへ半導電性領域の電気抵抗を付与するには、熱可塑性樹脂へカーボンブラックや導電性フィラーのような電子伝導性材料、もしくはイオン伝導性材料を配合する方法が知られており、そのコンパウンドを成形することにより半導電性エンドレスベルトが得られる。 Endless belts used in these image forming apparatuses are required to have electrical resistance and uniformity in a semiconductive region having a volume resistivity of 1 × 10 5 to 1 × 10 13 Ω · cm. In order to give the endless belt electrical resistance in the semiconductive region, a method of blending an electron conductive material such as carbon black or a conductive filler or an ion conductive material into a thermoplastic resin is known. A semiconductive endless belt can be obtained by molding the compound.
イオン伝導性材料を用いた半導電性エンドレスベルトは、エンドレスベルト面内の電気抵抗のバラツキやロット間のバラツキが小さい、電気抵抗の制御が容易であるという特徴がある。しかしながら、イオン伝導性材料を配合した半導電性エンドレスベルトを装着した画像形成装置は、半導電性エンドレスベルトと感光体とを接触させた状態で高温高湿条件下へ長期間放置した後に印刷を行うと、感光体と接触していた部分に転写不良に起因する白抜けが発生するという問題があった。この現象は、感光体表面に形成されたトナーの顕像が中間転写ベルト、あるいは転写搬送ベルト上の記録媒体へ転写しないことによるものであり、感光体表面が汚染されていることによるものであることが判明している。 A semiconductive endless belt using an ion conductive material is characterized in that variation in electric resistance in the endless belt surface and variation between lots are small, and that electric resistance can be easily controlled. However, an image forming apparatus equipped with a semiconductive endless belt containing an ion conductive material can be printed after being left in a high temperature and high humidity condition for a long time with the semiconductive endless belt in contact with the photoreceptor. When this is done, there is a problem in that white spots due to transfer defects occur in the portions that are in contact with the photoreceptor. This phenomenon is due to the fact that the toner image formed on the surface of the photosensitive member is not transferred to the recording medium on the intermediate transfer belt or the transfer conveying belt, and the photosensitive member surface is contaminated. It has been found.
感光体汚染による光応答特性の低下を防止する方法として、特許文献1に、イオン導電剤を含むと共に表層に研磨材を分散させた構造を有する中間転写媒体を搭載した画像形成装置が提案されている。この提案は、中間転写媒体の表層に分散させた研磨材がイオン導電剤により汚染された感光体表面を研磨し、感光体表面の汚染物質を除去するというものである。しかしながら、この方法では、感光体表面は常時研磨され続け、感光体の耐久性が低下するという問題があった。 As a method for preventing a decrease in light response characteristics due to photoconductor contamination, Patent Document 1 proposes an image forming apparatus equipped with an intermediate transfer medium having a structure containing an ionic conductive agent and having an abrasive dispersed in a surface layer. Yes. In this proposal, the surface of the photosensitive member contaminated with the ionic conductive agent is polished by the abrasive dispersed in the surface layer of the intermediate transfer medium, and the contaminant on the surface of the photosensitive member is removed. However, this method has a problem that the surface of the photoconductor is always polished and the durability of the photoconductor is reduced.
また、特許文献2には、遠心成型で得た内周面部より外周面部の硬質粒子濃度を高くした中間転写ベルトを用いた画像形成装置は、高温高湿条件下でプリントを行っても感光体上に形成されたトナー像を記録媒体へ高転写率で転写でき、べた画像の白抜け、文字画像の中抜け及び文字部のトナー散りを発生させずに記録媒体上へトナー画像を形成することができることが記載されている。これは、硬質粒子を中間転写ベルトの表面近傍に高濃度に存在させ表面硬度をアップさせることにより、中間転写ベルト表面はトナーによる変形がなくなり、小粒径トナーで形成されたトナー像でも、記録媒体へ高転写率で転写できるものと推察している。従って、この中間転写ベルトは感光体汚染を防止する効果を目的としたものではない。 Further, Patent Document 2 discloses that an image forming apparatus using an intermediate transfer belt in which the hard particle concentration in the outer peripheral surface portion is higher than that in the inner peripheral surface portion obtained by centrifugal molding is a photoconductor even when printing is performed under high temperature and high humidity conditions. The toner image formed on the recording medium can be transferred to the recording medium at a high transfer rate, and the toner image can be formed on the recording medium without causing white spots in the solid image, voids in the character image, and toner scattering in the character portion. It is described that can be. This is because hard particles are present in a high concentration near the surface of the intermediate transfer belt to increase the surface hardness, so that the surface of the intermediate transfer belt is not deformed by toner, and even a toner image formed with a small particle size toner can be recorded. It is assumed that it can be transferred to a medium at a high transfer rate. Therefore, the intermediate transfer belt is not intended to prevent the photoreceptor contamination.
一方、特許文献3には、繊維材料より形成された基布と、ポリ塩化ビニル系樹脂層と、可塑剤移行防止層と、光触媒防汚層とを有し、前記可塑剤移行防止層が特定の合成シリカを含有する可撓性重合体樹脂層と、合成シリカを含有しない追加可撓性重合体樹脂層とからなる防汚性シートが提案されている。この防汚性シートは、特定の合成シリカが、ポリ塩化ビニル系樹脂層から移行してきた可塑剤を可塑剤移行防止層内に保持し、可塑剤が防汚シート表面へ移行するのを防止することによる防汚性、及び耐光性の低下を抑制するという効果を有している。しかしながら、当該発明は、中・大型テント、テント倉庫、トラック用の幌、看板用バックリットなどの産業用資材用途として有用な防汚性シートに関するものであり、電子写真用の半導電性エンドレスベルトとは利用分野、技術分野共に全く異なっている。 On the other hand, Patent Document 3 has a base fabric formed from a fiber material, a polyvinyl chloride resin layer, a plasticizer migration prevention layer, and a photocatalyst antifouling layer, and the plasticizer migration prevention layer is specified. An antifouling sheet comprising a flexible polymer resin layer containing synthetic silica and an additional flexible polymer resin layer not containing synthetic silica has been proposed. In this antifouling sheet, the specific synthetic silica holds the plasticizer that has migrated from the polyvinyl chloride resin layer in the plasticizer migration preventing layer, and prevents the plasticizer from migrating to the surface of the antifouling sheet. It has the effect of suppressing the deterioration of antifouling property and light resistance. However, the present invention relates to an antifouling sheet useful for industrial materials such as medium and large tents, tent warehouses, truck hoods, signboard backlits, etc., and is a semiconductive endless belt for electrophotography. Is completely different in both the application field and the technical field.
従来、イオン伝導性材料を含有する半導電性エンドレスベルトを搭載した画像形成装置は感光体表面の汚染によると考えられる画像不良が発生するという問題があった。その原因を究明するために、感光体表面を分析した結果、半導電性エンドレスベルトへ添加されているイオン伝導性材料の成分が感光体表面へ付着していることが明らかとなった。さらに詳細に検討を進めた結果、半導電性エンドレスベルトの製造過程において高温で成形加工する工程、即ち、コンパウンド化工程、押出し成形工程、周長規制工程において、イオン伝導性材料が熱分解反応により微量の低分子量成分を生成し、それが半導電性エンドレスベルト表面へブリードアウトし、感光体表面を汚染しているものと推定した。
本発明者等はこの推定に基づき、半導電性エンドレスベルトの製造工程で低分子量成分が生成した場合でも感光体を汚染させない半導電性エンドレスベルトについて鋭意検討を重ね本発明に到達したものである。
すなわち、本発明は、上記課題を解決するものであって、イオン伝導性材料を含む半導電性エンドレスベルトにおいて、特に高温高湿中へ長時間放置された場合にも、半導電性エンドレスベルト加工時に生成した低分子量成分が半導電性エンドレスベルトからブリードアウトするのを抑制し感光体を汚染させない半導電性エンドレスベルトを提供することを課題とする。
Conventionally, an image forming apparatus equipped with a semiconductive endless belt containing an ion conductive material has a problem that an image defect considered to be caused by contamination of the surface of the photoreceptor occurs. As a result of analyzing the surface of the photoreceptor in order to investigate the cause, it was found that the components of the ion conductive material added to the semiconductive endless belt adhered to the surface of the photoreceptor. As a result of further detailed investigation, in the process of forming the semiconductive endless belt at a high temperature, that is, in the compounding process, the extrusion molding process, and the circumferential length regulating process, the ion conductive material is subjected to a thermal decomposition reaction. It was estimated that a small amount of a low molecular weight component was produced, which bleeded out to the surface of the semiconductive endless belt and contaminated the surface of the photoreceptor.
Based on this estimation, the present inventors have earnestly studied a semiconductive endless belt that does not contaminate the photoreceptor even when a low molecular weight component is produced in the production process of the semiconductive endless belt, and reached the present invention. .
That is, the present invention solves the above-described problem, and in a semiconductive endless belt containing an ion conductive material, particularly when left in high temperature and high humidity for a long time, the semiconductive endless belt processing It is an object of the present invention to provide a semiconductive endless belt that suppresses bleeding out of a low molecular weight component sometimes generated from the semiconductive endless belt and does not contaminate the photoreceptor.
本発明によれば、
(1)熱可塑性樹脂にイオン伝導性材料が配合された半導電性エンドレスベルトにおいて、半導電性エンドレスベルトが熱可塑性樹脂、イオン伝導性材料、およびJIS K5101−13に準じて測定された吸油量が50〜350ml/100gである多孔質シリカよりなることを特徴とする半導電性エンドレスベルト;
(2)熱可塑性樹脂が融点190℃以下のフッ素系樹脂である(1)記載の半導電性エンドレスベルト:
(3)イオン伝導性材料が高分子型帯電防止剤であることを特徴とする(1)乃至(2)記載の半導電性エンドレスベルト;
(4)多孔質シリカの平均粒子径が0.5〜15μmである(1)乃至(3)記載の半導電性エンドレスベルト;
を要旨とするものである。
According to the present invention,
(1) In a semiconductive endless belt in which an ion conductive material is blended with a thermoplastic resin, the semiconductive endless belt measures the amount of oil absorbed according to the thermoplastic resin, the ion conductive material, and JIS K5101-13. A semiconductive endless belt, characterized in that it is made of porous silica having a weight of 50 to 350 ml / 100 g;
(2) The semiconductive endless belt according to (1), wherein the thermoplastic resin is a fluororesin having a melting point of 190 ° C. or lower:
(3) The semiconductive endless belt according to (1) or (2), wherein the ion conductive material is a polymer type antistatic agent;
(4) The semiconductive endless belt according to any one of (1) to (3), wherein the average particle size of the porous silica is 0.5 to 15 μm;
Is a summary.
本発明の半導電性エンドレスベルトは、イオン伝導性材料を配合されているにも拘わらず、半導電性エンドレスベルトに配合されている特定の多孔質シリカが、半導電性エンドレスベルト中に配合されているイオン伝導性材料に由来する微量の熱分解生成物を吸着し、熱分解生成物である低分子量成分が半導電性エンドレスベルト表面へブリードアウトするのを抑制する。その結果、本発明の半導電性エンドレスベルトは画像形成装置内で接触する感光体の表面を汚染させないという効果を有している。また、本発明の半導電性エンドレスベルトは、イオン伝導性材料を用いているため、イオン伝導性材料を用いた半導電性エンドレスベルトの特徴である電気抵抗の面内バラツキやロット間バラツキが小さい、電気抵抗の制御が容易であり、所望の電気抵抗を有する半導電性エンドレスベルトを安定して製造できるというという特徴をも有している。さらに、本発明の半導電性エンドレスベルトを搭載した画像形成装置で印刷を行うと、白抜けのない均一で高品質の画像が得られるという効果をも有している。 Although the semiconductive endless belt of the present invention contains an ion conductive material, the specific porous silica compounded in the semiconductive endless belt is compounded in the semiconductive endless belt. A small amount of thermal decomposition product derived from the ion conductive material is adsorbed, and the low molecular weight component which is the thermal decomposition product is prevented from bleeding out to the surface of the semiconductive endless belt. As a result, the semiconductive endless belt of the present invention has an effect of not contaminating the surface of the photosensitive member in contact with the image forming apparatus. In addition, since the semiconductive endless belt of the present invention uses an ion conductive material, there is little in-plane variation or lot-to-lot variation in electrical resistance, which is a feature of the semiconductive endless belt using the ion conductive material. Also, the electric resistance can be easily controlled, and a semiconductive endless belt having a desired electric resistance can be stably manufactured. Further, when printing is performed with an image forming apparatus equipped with the semiconductive endless belt of the present invention, there is an effect that a uniform and high quality image without white spots can be obtained.
以下、本発明について詳細に説明する。
本発明に用いられる熱可塑性樹脂としては、ポリエチレン、ポリプロピレンなどのオレフィン系樹脂、ポリスチレン、ABS樹脂などのスチレン系樹脂、アクリル樹脂、ポリフッ化ビニリデン、フッ化ビニリデン共重合体、エチレンとテトラフルオロエチレンとの共重合体などのフッ素系樹脂、ポリ乳酸、ポリエチレンテレフタレート、ポリブチレンテレフタレートなどのポリエステル、ポリカーボネート、脂肪族ポリアミドなどが挙げられる。
Hereinafter, the present invention will be described in detail.
Examples of the thermoplastic resin used in the present invention include olefin resins such as polyethylene and polypropylene, styrene resins such as polystyrene and ABS resin, acrylic resins, polyvinylidene fluoride, vinylidene fluoride copolymers, ethylene and tetrafluoroethylene, Fluorine resins such as copolymers, polyesters such as polylactic acid, polyethylene terephthalate and polybutylene terephthalate, polycarbonates, aliphatic polyamides and the like.
これらのうち、熱可塑性樹脂としては、難燃性を有し、イオン伝導性材料の熱分解反応を抑えるためにも比較的低温で加工できる、融点が190℃以下のフッ素系樹脂が好ましい。融点が190℃以下のフッ素系樹脂としては、ポリフッ化ビニリデン、フッ化ビニリデン−ヘキサフルオロプロピレン共重合体、フッ化ビニリデン−テトラフルオロエチレン共重合体を挙げることができる。 Of these, the thermoplastic resin is preferably a fluororesin having a flame resistance and a melting point of 190 ° C. or lower that can be processed at a relatively low temperature in order to suppress the thermal decomposition reaction of the ion conductive material. Examples of the fluorine-based resin having a melting point of 190 ° C. or lower include polyvinylidene fluoride, vinylidene fluoride-hexafluoropropylene copolymer, and vinylidene fluoride-tetrafluoroethylene copolymer.
本発明に用いられるイオン伝導性材料としては高分子型帯電防止剤が好ましく、ポリエーテルエステルアミド、ポリエーテルエステル、ポリエーテルアミド、ポリエチレンオキサイド、エチレンオキサイドとプロピレンオキサイドとの共重合体、ポリエピクロルヒドリン、エチレンオキサイドとエピクロルヒドリンとの共重合体などのポリエチレンオキサイド鎖を有する重合体、側鎖に4級アンモニウム塩を有する重合体、側鎖にスルホン酸塩を有する重合体等が挙げられる。これらの中でも、得られた半導電性エンドレスベルトの電気抵抗の環境依存性(温度と湿度の変動による電気抵抗の変化)が小さいので、イオン伝導性材料としてポリエチレンオキサイド、またはエチレンオキサイドとプロピレンオキサイドとの共重合体が好ましい。 As the ion conductive material used in the present invention, a polymer type antistatic agent is preferable, polyether ester amide, polyether ester, polyether amide, polyethylene oxide, a copolymer of ethylene oxide and propylene oxide, polyepichlorohydrin, Examples thereof include a polymer having a polyethylene oxide chain, such as a copolymer of ethylene oxide and epichlorohydrin, a polymer having a quaternary ammonium salt in the side chain, and a polymer having a sulfonate in the side chain. Among these, since the environmental dependence of the electrical resistance of the obtained semiconductive endless belt (change in electrical resistance due to fluctuations in temperature and humidity) is small, polyethylene oxide or ethylene oxide and propylene oxide can be used as an ion conductive material. These copolymers are preferred.
イオン伝導性材料として用いられる高分子型帯電防止剤は、重量平均分子量が10万以上のものが好ましい。また、低分子量成分はブリードアウト現象を起こす恐れがあるため、分子量3000以下の低分子量成分を含有していないイオン伝導性材料が好ましい。さらに好ましくは分子量8000以下の低分子量成分を含有していないイオン伝導性材料が好ましい。なお、重量平均分子量は、蒸留水を溶離液としポリエチレンオキサイドを標準試料とし、GPC(ゲルパーミエーションクロマトグラフィー)を用いて測定した値である。
これらの添加量は、半導電性エンドレスベルトに要求される電気抵抗にもよるが、イオン伝導性材料の添加量が多いと成形加工時の熱分解により生成する低分子量成分が多くなるため、熱可塑性樹脂100重量部に対し10重量部以下が好ましい。また、エンドレスベルトへ半導電性を付与させるためには熱可塑性樹脂100重量部に対しイオン伝導性材料を0.3重量部以上配合するのが好ましい。
The polymer antistatic agent used as the ion conductive material preferably has a weight average molecular weight of 100,000 or more. Moreover, since a low molecular weight component may cause a bleed-out phenomenon, an ion conductive material containing no low molecular weight component having a molecular weight of 3000 or less is preferable. More preferably, an ion conductive material containing no low molecular weight component having a molecular weight of 8000 or less is preferable. The weight average molecular weight is a value measured using GPC (gel permeation chromatography) using distilled water as an eluent and polyethylene oxide as a standard sample.
The amount of these additives depends on the electrical resistance required for the semiconductive endless belt, but if the amount of ion-conductive material added is large, the amount of low molecular weight components generated by thermal decomposition during molding increases, The amount is preferably 10 parts by weight or less with respect to 100 parts by weight of the plastic resin. In order to impart semiconductivity to the endless belt, it is preferable to blend 0.3 parts by weight or more of the ion conductive material with respect to 100 parts by weight of the thermoplastic resin.
上記のように、イオン伝導性材料として用いる高分子型帯電防止剤は分子量3000以下の低分子量成分を含有していないことが好ましい。しかしながら、そのようなイオン伝導性材料を用いても、熱可塑性樹脂へイオン伝導性材料を添加・混合するコンパウンド工程、および得られたコンパウンドをチューブ状に押出す成形工程、得られたチューブを所定長さに切断後周長を均一にする加熱工程にて、イオン伝導性材料が高温下に晒された場合、イオン伝導性材料が熱分解反応を起こし分子量3000以下の低分子量成分を生成する恐れがあるため、これらの加工温度は240℃以下とするのが好ましい。 As described above, it is preferable that the polymer antistatic agent used as the ion conductive material does not contain a low molecular weight component having a molecular weight of 3000 or less. However, even if such an ion conductive material is used, a compound process for adding and mixing the ion conductive material to the thermoplastic resin, a molding process for extruding the obtained compound into a tube shape, and the obtained tube are predetermined. When the ion conductive material is exposed to a high temperature in the heating process for making the circumference uniform after cutting into length, the ion conductive material may cause a thermal decomposition reaction to generate a low molecular weight component having a molecular weight of 3000 or less. Therefore, these processing temperatures are preferably 240 ° C. or lower.
本発明の半導電性エンドレスベルトには、上記イオン伝導性材料に加えて、電気抵抗を下げる目的で、イオン電解質を併用することもできる。イオン電解質としては、過塩素酸リチウム、過塩素酸ナトリウム、過塩素酸カリウム、過塩素酸アンモニウム、テトラブチルアンモニウムの硫酸水素塩、テトラエチルアンモニウムテトラフルオロほう酸塩、テトラブチルアンモニウムテトラフルオロほう酸塩、塩化リチウム、チオシアン酸リチウム、チオシアン酸ナトリウム、チオシアン酸カリウムなどのアルカリ金属塩、アンモニウム塩、ほう酸塩などを用いることができる。 In addition to the ion conductive material, an ion electrolyte can be used in combination with the semiconductive endless belt of the present invention for the purpose of lowering electric resistance. Examples of ion electrolytes include lithium perchlorate, sodium perchlorate, potassium perchlorate, ammonium perchlorate, tetrabutylammonium hydrogen sulfate, tetraethylammonium tetrafluoroborate, tetrabutylammonium tetrafluoroborate, lithium chloride Alkali metal salts such as lithium thiocyanate, sodium thiocyanate, potassium thiocyanate, ammonium salts, borates and the like can be used.
本発明に用いることのできる多孔質シリカは、ケイ酸ソーダと硫酸とを混合しケイ酸ゾルを生成させ、それを徐々に重合、ゲル化させてコロイド状シリカとし、それを粉砕することにより得ることができる。多孔質シリカとしては、その中でも、JIS K5101−13に規定される吸油量が50〜350ml/100g、さらには80〜350ml/100gのものを好適に用いることができる。吸油量が50ml/100g未満のシリカは、イオン伝導性材料に起因する低分子量成分のブリードアウトを抑制する効果が不充分で好ましくない。 The porous silica that can be used in the present invention is obtained by mixing sodium silicate and sulfuric acid to form a silicate sol, gradually polymerizing and gelling it to form colloidal silica, and then pulverizing it. be able to. Among these, those having an oil absorption of 50 to 350 ml / 100 g, further 80 to 350 ml / 100 g as defined in JIS K5101-13 can be suitably used as the porous silica. Silica having an oil absorption of less than 50 ml / 100 g is not preferable because the effect of suppressing bleed out of low molecular weight components due to the ion conductive material is insufficient.
また、多孔質シリカの平均粒子径は、0.5〜15μmが好ましい。多孔質シリカの平均粒子径が0.5μm未満の場合は、多孔質シリカと熱可塑性樹脂とを加熱混練する際、多孔質シリカの二次凝集物ができやすいので好ましくなく、平均粒子径が15μmを超える場合は、半導電性エンドレスベルトとした場合、多孔質シリカの平均粒子径が大きいために得られたエンドレスベルトの表面粗さが大きくなるため好ましくない。
さらに、多孔質シリカの比表面積は、100〜1000m2/gが好ましい。多孔質シリカの比表面積が100m2/g未満の場合は、比表面積が小さいために吸油量が小さいので好ましくなく、比表面積が1000m2/gを超える多孔質シリカは平均細孔径が小さすぎ、イオン伝導性材料の熱分解反応により生成した低分子量成分を吸着する能力が小さくなるため好ましくない。
The average particle size of the porous silica is preferably 0.5 to 15 μm. When the average particle size of the porous silica is less than 0.5 μm, it is not preferable because when the porous silica and the thermoplastic resin are heat-kneaded, secondary aggregates of the porous silica are easily formed, and the average particle size is 15 μm. In the case of exceeding the semi-conductive endless belt, the surface roughness of the endless belt obtained because the average particle diameter of the porous silica is large is not preferable.
Furthermore, the specific surface area of the porous silica is preferably 100 to 1000 m 2 / g. When the specific surface area of the porous silica is less than 100 m 2 / g, the specific surface area is small, which is not preferable because the oil absorption is small, and the porous silica having a specific surface area exceeding 1000 m 2 / g has an average pore diameter that is too small. This is not preferable because the ability to adsorb low molecular weight components generated by the thermal decomposition reaction of the ion conductive material is reduced.
上記多孔質シリカの添加量は、熱可塑性樹脂100重量部に対して0.05〜2.0重量部が好ましい。さらには、0.1〜1.0重量部が好ましい。多孔質シリカの添加量が0.05重量部未満の場合は、多孔質シリカの添加量が少ないためその効果が小さいので好ましくなく、2.0重量部を超える場合は得られた半導電性エンドレスベルトの表面粗さが大きくなるので好ましくない。 The amount of the porous silica added is preferably 0.05 to 2.0 parts by weight with respect to 100 parts by weight of the thermoplastic resin. Furthermore, 0.1-1.0 weight part is preferable. When the addition amount of the porous silica is less than 0.05 parts by weight, the effect is small because the addition amount of the porous silica is small, which is not preferable. When the addition amount exceeds 2.0 parts by weight, the obtained semiconductive endless Since the surface roughness of a belt becomes large, it is not preferable.
更に、本発明の半導電性エンドレスベルトには、上記以外に、さまざまな目的で熱安定剤、補強剤、滑剤、相容化剤、着色剤、改質剤などの各種添加剤を配合してもよい。 Furthermore, in addition to the above, the semiconductive endless belt of the present invention contains various additives such as a heat stabilizer, a reinforcing agent, a lubricant, a compatibilizer, a colorant, and a modifier for various purposes. Also good.
以下に、本発明の半導電性エンドレスベルトの製造方法を説明する。
本発明の半導電性エンドレスベルト用コンパウンドは、熱可塑性樹脂、イオン伝導性材料、多孔質シリカ、さらに必要に応じてイオン電解質などの各種添加剤を通常のニーダー、ロール、バンバリーミキサー、二軸混練機等で混練・ペレット化することによって製造することができる。
Below, the manufacturing method of the semiconductive endless belt of this invention is demonstrated.
The compound for a semiconductive endless belt according to the present invention is a conventional kneader, roll, Banbury mixer, biaxial kneader containing various additives such as a thermoplastic resin, an ion conductive material, porous silica and, if necessary, an ionic electrolyte. It can be produced by kneading and pelletizing with a machine or the like.
このようにして得られたコンパウンドは、環状ダイを備えた押出し機に供給し、所定周長のチューブ状に製膜することにより、半導電性エンドレスベルト用原反を得ることができる。もしくは、多層の環状ダイを装着した少なくとも1台の押出し機へ上記コンパウンドを供給して共押出しし、多層の半導電性エンドレスベルト用原反を得ることができる。
得られた半導電性エンドレスベルト用原反は、所定長さにカット後、周長精度を上げるために原反周長より少し大きい円筒状金型へ被せ加熱することにより、周長が均一な目的とする半導電性エンドレスベルトを得ることができる。
The compound thus obtained is supplied to an extruder equipped with an annular die and formed into a tube having a predetermined circumference, whereby a semiconductive endless belt original fabric can be obtained. Alternatively, the compound can be supplied and co-extruded to at least one extruder equipped with a multilayer annular die to obtain a multilayer semi-conductive endless belt raw material.
The obtained semi-conductive endless belt material is cut into a predetermined length, and then heated over a cylindrical mold slightly larger than the original material circumference to increase the accuracy of the circumference, so that the circumference is uniform. The intended semiconductive endless belt can be obtained.
なお、多層の半導電性エンドレスベルトの場合は、イオン伝導性材料を含有する層へ当該層の熱可塑性樹脂100重量部に対し、多孔質シリカを0.05重量部〜2.0重量部添加するのが好ましい。もしくは、イオン伝導性材料を含有する層より表層側の他の層へ先に記載した量の多孔質シリカを添加することもできる。 In the case of a multilayer semiconductive endless belt, 0.05 to 2.0 parts by weight of porous silica is added to a layer containing an ion conductive material with respect to 100 parts by weight of the thermoplastic resin of the layer. It is preferable to do this. Alternatively, the amount of porous silica described above can be added to the other layer on the surface layer side of the layer containing the ion conductive material.
なお、このようにして得られた半導電性エンドレスベルトへ離型性、滑り性、耐磨耗性などの特性を付与するために、エンドレスベルト表面へこれらの特性を付与する塗工剤を塗工することもできる。 In order to impart properties such as releasability, slipperiness, and wear resistance to the semiconductive endless belt thus obtained, a coating agent that imparts these properties is applied to the endless belt surface. It can also be crafted.
上記のように、本発明の半導電性エンドレスベルトを得るためには、熱可塑性樹脂とイオン伝導性材料、多孔質シリカなどとを混練するコンパウンド化工程、得られたコンパウンドからチューブ状の半導電性エンドレスベルト用原反を得る押出し工程、エンドレスベルト原反を金型へ被せ周長精度を上げる加熱工程があり、半導電性エンドレスベルト用原料はそれぞれの工程で加熱されるが、イオン伝導性材料の熱分解による低分子量成分の生成を抑えるためには、各工程の温度は240℃以下とするのが好ましい。 As described above, in order to obtain the semiconductive endless belt of the present invention, a compounding step of kneading a thermoplastic resin, an ion conductive material, porous silica and the like, and a tube-shaped semiconductive from the obtained compound. There are extruding process to obtain the raw material for the conductive endless belt, heating process for covering the endless belt raw material on the mold to increase the circumference accuracy, and the raw material for the semiconductive endless belt is heated in each process, but the ionic conductivity In order to suppress the production of low molecular weight components due to thermal decomposition of the material, the temperature of each step is preferably 240 ° C. or lower.
次に、実施例によって、本発明を具体的に説明する。得られた半導電性エンドレスベルトの評価方法は次に示す通りである。なお、実施例、および比較例で用いた多孔質シリカの特性を表1に示す。 Next, the present invention will be described specifically by way of examples. The evaluation method of the obtained semiconductive endless belt is as follows. Table 1 shows the characteristics of the porous silica used in the examples and comparative examples.
<多孔質シリカの特性>
多孔質シリカの平均粒子径、比表面積、及び吸油量は下記のようにして求めた。
[平均粒子径(レーザー法)]
多孔質シリカの平均粒子径は、多孔質シリカの粒子にレーザー光を照射し、そこから得られる散乱パターンから多孔質シリカの平均粒子径を求めた。
[比表面積]
多孔質シリカの比表面積は、簡易BET法により測定した。
すなわち、まず脱ガスした多孔質シリカの重量を測定し、その多孔質シリカへ窒素ガスを吹き込み試料表面に窒素ガスを吸着させる。そして窒素ガスの圧力変化に対する吸着量の変化をプロットすることにより、多孔質シリカ表面にだけ吸着した窒素ガス分子吸着量をBET吸着等温式より求めた。
[吸油量]
多孔質シリカの吸油量は、JIS K5101−13に準拠し、多孔質シリカ100gが吸収する精製あまに油の体積(ml)で示した。
<Characteristics of porous silica>
The average particle diameter, specific surface area, and oil absorption of the porous silica were determined as follows.
[Average particle size (Laser method)]
The average particle diameter of the porous silica was determined by irradiating the porous silica particles with laser light and determining the average particle diameter of the porous silica from the scattering pattern obtained therefrom.
[Specific surface area]
The specific surface area of the porous silica was measured by a simple BET method.
That is, first, the weight of the degassed porous silica is measured, nitrogen gas is blown into the porous silica, and nitrogen gas is adsorbed on the sample surface. Then, the amount of adsorption of nitrogen gas molecules adsorbed only on the surface of the porous silica was determined from the BET adsorption isotherm by plotting the variation of the amount of adsorption against the pressure change of nitrogen gas.
[Oil absorption]
The amount of oil absorption of the porous silica was represented by the volume (ml) of refined sesame oil absorbed by 100 g of porous silica in accordance with JIS K5101-13.
<体積抵抗率、表面抵抗率>
体積抵抗率は、三菱化学(株)製ハイレスタURSプローブを用い、印加電圧250V、23℃、50%RH条件下で測定した。
表面抵抗率は、三菱化学(株)製ハイレスタURSプローブを用い、印加電圧500V、23℃、50%RH条件下で測定した。
体積抵抗率、および表面抵抗率は任意の10点を測定した平均値で、そのバラツキは最大値を最小値で除した値で表した。
<Volume resistivity, surface resistivity>
The volume resistivity was measured using a Hiresta URS probe manufactured by Mitsubishi Chemical Corporation under an applied voltage of 250 V, 23 ° C., and 50% RH.
The surface resistivity was measured using a Hiresta URS probe manufactured by Mitsubishi Chemical Corporation under an applied voltage of 500 V, 23 ° C., and 50% RH.
The volume resistivity and the surface resistivity are average values obtained by measuring 10 arbitrary points, and the variation is represented by a value obtained by dividing the maximum value by the minimum value.
<引張り強度、および引張り破断伸び>
オートグラフAGS−100(島津製作所製)を用いて、JIS K7127に準拠して2号試験片を作製し、引張り速度30mm/minで引張った時の最大加重と引張り破断伸びを測定した。
<Tensile strength and elongation at break>
Using Autograph AGS-100 (manufactured by Shimadzu Corporation), No. 2 test piece was prepared according to JIS K7127, and the maximum load and tensile elongation at break when it was pulled at a pulling speed of 30 mm / min were measured.
<表面粗さ>
接触式表面粗さ計サーフコム575A(東京精密社製)を用いて、JIS B0601−1982に準拠して、中心線平均粗さRaを測定した。
<Surface roughness>
Centerline average roughness Ra was measured using a contact type surface roughness meter Surfcom 575A (manufactured by Tokyo Seimitsu Co., Ltd.) in accordance with JIS B0601-1982.
<ブリードアウトの評価>
短冊状の試料上へ直径12mmの金属ローラを置き、50℃、相対湿度90%中へ30日間放置後、常態へ取り出し、金属ローラを置いていた試料表面の状態を観察することにより、ブリードアウトの有無を判定した。すなわち、金属ローラを置いていた試料表面を目視で観察し、試料表面に異物が観察されない場合を○、異物が観察された場合を×とした。
<Evaluation of bleed-out>
Bleed out by placing a metal roller with a diameter of 12 mm on a strip-shaped sample, leaving it in a normal state for 30 days in 50 ° C. and 90% relative humidity, and observing the state of the sample surface on which the metal roller was placed. The presence or absence of was determined. That is, the surface of the sample on which the metal roller was placed was visually observed. A case where no foreign matter was observed on the surface of the sample was indicated as ◯, and a case where foreign matter was observed was indicated as ×.
ポリフッ化ビニリデン100重量部、エチレンオキサイドとプロピレンオキサイドとの共重合体(プロピレンオキサイド含量10%、蒸留水を溶離液としポリエチレンオキサイドを標準試料とした時の重量平均分子量:85万)3重量部、過塩素酸リチウム0.2重量部、フェノール系熱安定剤0.2重量部、多孔質シリカA0.2重量部を設定温度180℃の二軸混練機へ供給し、半導電性エンドレスベルト用コンパウンドを得た。次いで、環状ダイスを装着した押出し機(設定温度210℃)へこのコンパウンドを供給し、直径180mmのチューブを得た。このチューブを長さ320mmに切断し、外径183mmの円筒金型へ被せ、150℃で60分間加熱することにより、半導電性エンドレスベルトを得た。得られた半導電性エンドレスベルトの特性を表2に示す。 100 parts by weight of polyvinylidene fluoride, 3 parts by weight of a copolymer of ethylene oxide and propylene oxide (propylene oxide content 10%, weight average molecular weight when using distilled water as an eluent and polyethylene oxide as a standard sample), Supplying 0.2 parts by weight of lithium perchlorate, 0.2 parts by weight of a phenol-based heat stabilizer, and 0.2 parts by weight of porous silica A to a biaxial kneader at a set temperature of 180 ° C., a compound for a semiconductive endless belt Got. Next, this compound was supplied to an extruder (set temperature 210 ° C.) equipped with an annular die to obtain a tube having a diameter of 180 mm. This tube was cut into a length of 320 mm, covered with a cylindrical mold having an outer diameter of 183 mm, and heated at 150 ° C. for 60 minutes to obtain a semiconductive endless belt. Table 2 shows the characteristics of the obtained semiconductive endless belt.
多孔質シリカとして、多孔質シリカBを用いた以外は実施例1と同様にして半導電性エンドレスベルトを得た。得られた半導電性エンドレスベルトの特性を表2に示す。 A semiconductive endless belt was obtained in the same manner as in Example 1 except that porous silica B was used as the porous silica. Table 2 shows the characteristics of the obtained semiconductive endless belt.
エチレンオキサイドとプロピレンオキサイドとの共重合体の配合量を4重量部とした以外は実施例1と同様にして半導電性エンドレスベルトを得た。得られた半導電性エンドレスベルトの特性を表2に示す。 A semiconductive endless belt was obtained in the same manner as in Example 1 except that the amount of the copolymer of ethylene oxide and propylene oxide was changed to 4 parts by weight. Table 2 shows the characteristics of the obtained semiconductive endless belt.
多孔質シリカとして、多孔質シリカAを0.3重量部用いた以外は実施例1と同様にして半導電性エンドレスベルトを得た。得られた半導電性エンドレスベルトの特性を表2に示す。 A semiconductive endless belt was obtained in the same manner as in Example 1 except that 0.3 part by weight of porous silica A was used as the porous silica. Table 2 shows the characteristics of the obtained semiconductive endless belt.
[比較例1]
多孔質シリカを用いなかった以外は実施例1と同様にして半導電性エンドレスベルトを得た。得られた半導電性エンドレスベルトの特性を表2に示す。
[Comparative Example 1]
A semiconductive endless belt was obtained in the same manner as in Example 1 except that porous silica was not used. Table 2 shows the characteristics of the obtained semiconductive endless belt.
[比較例2]
多孔質シリカとして、多孔質シリカCを用いた以外は実施例1と同様にして半導電性エンドレスベルトを得た。得られた半導電性エンドレスベルトの特性を表2に示す。
[Comparative Example 2]
A semiconductive endless belt was obtained in the same manner as in Example 1 except that porous silica C was used as the porous silica. Table 2 shows the characteristics of the obtained semiconductive endless belt.
[比較例3]
エチレンオキサイドとプロピレンオキサイドとの共重合体を4重量部とした以外は比較例2と同様にして半導電性エンドレスベルトを得た。得られた半導電性エンドレスベルトの特性を表2に示す。
[Comparative Example 3]
A semiconductive endless belt was obtained in the same manner as in Comparative Example 2 except that the copolymer of ethylene oxide and propylene oxide was changed to 4 parts by weight. Table 2 shows the characteristics of the obtained semiconductive endless belt.
以上の結果より、吸油量が50ml/100g以上の多孔質シリカを添加した実施例1、2、3および4の半導電性エンドレスベルトは、高温高湿下に長時間放置しても半導電性エンドレスベルト表面へのブレードアウト物は認められず、感光体を汚染する恐れがないことを確認した。また、多孔質シリカを添加したことによる体積抵抗率、表面抵抗率、引張り強度、引張り破断伸び、表面粗さへの影響は見られなかった。それに対し、多孔質シリカを添加しなかった比較例1や吸油量が50ml/100g未満の多孔質シリカを添加した比較例2、および3の半導電性エンドレスベルトは、高温高湿下へ長時間放置するとブリードアウトが見られた。 From the above results, the semiconductive endless belts of Examples 1, 2, 3 and 4 to which porous silica having an oil absorption of 50 ml / 100 g or more was added were semiconductive even when left for a long time under high temperature and high humidity. No blade-outs were found on the endless belt surface, and it was confirmed that there was no fear of contaminating the photoreceptor. Moreover, the influence on volume resistivity, surface resistivity, tensile strength, tensile elongation at break, and surface roughness due to the addition of porous silica was not observed. On the other hand, Comparative Example 1 in which no porous silica was added, Comparative Example 2 in which porous silica having an oil absorption of less than 50 ml / 100 g was added, and the semiconductive endless belts in 3 were used for a long time under high temperature and high humidity. When left untreated, a bleed-out was observed.
本発明で得られた半導電性エンドレスベルトは、イオン伝導性材料を用いているにも拘わらず、高温高湿下へ長時間放置してもブリードアウトが認められないため感光体表面を汚染する恐れがなく、電子写真方式の画像形成装置の転写搬送ベルト、あるいは中間転写ベルトとして好適に用いることができる。 Although the semiconductive endless belt obtained by the present invention uses an ion conductive material, it does not bleed out even if left in a high temperature and high humidity for a long time, so it contaminates the surface of the photoreceptor. There is no fear, and it can be suitably used as a transfer conveyance belt or an intermediate transfer belt of an electrophotographic image forming apparatus.
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