JPS6239208A - Manufacture of raw polyester master polymer - Google Patents

Manufacture of raw polyester master polymer

Info

Publication number
JPS6239208A
JPS6239208A JP60179206A JP17920685A JPS6239208A JP S6239208 A JPS6239208 A JP S6239208A JP 60179206 A JP60179206 A JP 60179206A JP 17920685 A JP17920685 A JP 17920685A JP S6239208 A JPS6239208 A JP S6239208A
Authority
JP
Japan
Prior art keywords
pigment
polyester
kneading
rotational power
polymer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP60179206A
Other languages
Japanese (ja)
Inventor
Masuo Murai
益夫 村井
Yu Amano
天野　祐
Yoshito Koike
小池　義人
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Ester Co Ltd
Original Assignee
Nippon Ester Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nippon Ester Co Ltd filed Critical Nippon Ester Co Ltd
Priority to JP60179206A priority Critical patent/JPS6239208A/en
Publication of JPS6239208A publication Critical patent/JPS6239208A/en
Pending legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/375—Plasticisers, homogenisers or feeders comprising two or more stages
    • B29C48/385—Plasticisers, homogenisers or feeders comprising two or more stages using two or more serially arranged screws in separate barrels

Abstract

PURPOSE:To enable to manufacture a polyester master polymer which is obtained by dispersing a pigment highly uniformly and has a high concentration of pigment, by kneading with rotational power of specific magnitude by limiting a scope of the mixture ratio between polyester and the pigment at a first step. CONSTITUTION:At the first kneading step, it is necessary to set the mixture ratio between polyester and pigment at a weight ratio of 60:40-40:60. Kneading is performed further at the second step; it is desirable to set the concentration of pigment at this time at 10-40wt%. With this construction, the dispersability of pigment can be improved and it is possible to lower the temperature of the polyester raised through shearing force at the time of kneading at the first step and to control thermal decomposition. It is necessary to make rotational power at the time of the kneading more than 0.03kW per 1kg of a kneading thing. With this construction, at the low rotational power, dispersion of the pigment becomes insufficient because of lack of shearing force. However, it is wastefulness in energy to raise the rotational power excessively and the rotational power to the extent of 0.07-0.2kW is desirable.

Description

【発明の詳細な説明】 （産業上の利用分野） 本発明は顔料を含有した繊維、フィルム等の製造に使用
される原着ポリエステルマスターポリマーを製造する方
法に関するものであり、ポリエステルと顔料とをスクリ
ュー型２軸混練押出機中で特定の条件で２段階で混練し
て顔料が均一に分散した原着ポリエステルマスターポリ
マーを製造する方法に関するものである。Detailed Description of the Invention (Industrial Field of Application) The present invention relates to a method for producing a spun-dyed polyester master polymer used in the production of pigment-containing fibers, films, etc. The present invention relates to a method for producing a doped polyester master polymer in which pigments are uniformly dispersed by kneading in two stages under specific conditions in a screw-type twin-screw kneading extruder.

（従来の技術） ポリエステル、特にポリエチレンテレフタレート又はこ
れを主体とするポリエステルは１機械的。(Prior Art) Polyester, especially polyethylene terephthalate or a polyester mainly composed of polyester, has a mechanical property.

化学的な性能の優れた素材として、繊維、フィルム等の
成形物として広く使用されているが、Ｒ料を混合した原
着ポリエステルとして用いられることも多い。As a material with excellent chemical performance, it is widely used as molded products such as fibers and films, but it is also often used as a spun-dyed polyester mixed with an R material.

原着成形物を製造する場合、顔料を高濃度で含有したマ
スターポリマーを造り、これを顔料を含有しないベース
ポリマーに添加して成形するのが普通である。When producing a molded product, it is common to prepare a master polymer containing a high concentration of pigment, add this to a base polymer that does not contain pigment, and then mold the product.

原着ポリエステルを製造する方法としては、ポリエステ
ルの合成時に顔料を添加する方法とポリエステルと顔料
とをニーグー、バンバリーミキサ−等で混合する方法と
がある。しかし、前者の方法では多品種少量生産には対
応しがたく、一方。Methods for producing spun-dyed polyester include a method in which a pigment is added during polyester synthesis, and a method in which a polyester and a pigment are mixed in a Negoo mixer, a Banbury mixer, or the like. However, the former method is difficult to support high-mix, low-volume production.

後者の方法では顔料をポリエステル中に高度に均一に分
散させることが困難であったり、長時間を要するという
問題があり、特に顔料濃度の高いマスターポリマーを製
造する場合、顔料を高度に均一に分散させることは困難
であった。The latter method has the problem that it is difficult or takes a long time to disperse the pigment highly uniformly in the polyester, especially when producing a master polymer with a high pigment concentration. It was difficult to do so.

なお、特開昭５８−２１２９０８号公報には、２軸混練
押出機を用いて溶融ポリマーに顔料等の添加物を混合す
る際、定量供給されるポリマーを分流させ。In addition, JP-A No. 58-212908 discloses that when an additive such as a pigment is mixed into a molten polymer using a twin-screw kneading extruder, the polymer that is supplied in a fixed amount is divided into streams.

その一部を添加物と混合１分散させた後、２軸混練押出
機の下流部で残りのポリマーを合流させる方法が開示さ
れているが、ここに開示された方法は、そのまま溶融紡
糸して繊維を製造するものである。A method has been disclosed in which a portion of the polymer is mixed with additives and dispersed, and then the remaining polymer is merged downstream of a twin-screw kneading extruder. It manufactures fibers.

（発明が解決しようとする問題点） 本発明は、顔料が高度に均一に分散した。顔料濃度の高
いポリエステルマスターポリマーを製造することのでき
る節易な方法を提供しようとするものである。(Problems to be Solved by the Invention) In the present invention, the pigment is highly uniformly dispersed. The object of the present invention is to provide an easy method for producing a polyester master polymer with a high pigment concentration.

（問題点を解決するための手段） 本発明は、上記目的を達成するもので、その要旨は、ポ
リエステルと顔料とをスクリュー型２軸混練押出機中で
、２段階で混練して原着ポリエステルマスターポリマー
を製造するに際し、第１段階目でのポリエステルと顔料
との混合比率を６０：４０〜４０　：　６０の重量比と
し、混練物ＩＫｇ当たり０．０３ＫＷ以上の回転動力で
混練することを特徴とする原着ポリエステルマスターポ
リマーの製造法にある。(Means for Solving the Problems) The present invention achieves the above object, and its gist is to knead polyester and pigment in two stages in a screw-type twin-screw kneading extruder to produce a spun-dyed polyester. When producing the master polymer, the mixing ratio of polyester and pigment in the first stage is set to a weight ratio of 60:40 to 40:60, and kneading is performed with a rotational power of 0.03 KW or more per Ikg of kneaded material. There is a method for producing a spun-dyed polyester master polymer.

本発明において５回転動ノｊとは、混練時の消費電力か
ら混練物のない空運転時の消費電力を差し引き、混練物
ＩＫｇ当たりの消費電力で表したものである。In the present invention, the 5-rotation dynamic nozzle is the power consumption during kneading minus the power consumption during idle operation with no kneaded material, and is expressed as power consumption per Ikg of kneaded material.

本発明において、第１段階目の混練部へ供給するポリエ
ステルは重縮合反応器から払い出された溶融状態のもの
でも、一旦ベレント状に成形したものでも、いずれでも
よい。In the present invention, the polyester supplied to the first-stage kneading section may be either a molten polyester discharged from a polycondensation reactor or a polyester once formed into a belent shape.

第１段階目の混練部では、ポリエステルと顔料との混合
比率を６０　：　４０〜４０　：　６０の重量比とする
ことが必要である。顔料濃度を高くすることにより溶融
状態での粘度を高めて高剪断力を発生させるのである。In the first-stage kneading section, it is necessary to set the mixing ratio of polyester and pigment to a weight ratio of 60:40 to 40:60. By increasing the pigment concentration, the viscosity in the molten state is increased and high shear forces are generated.

しかし、顔料濃度を高くしすぎると。However, if the pigment concentration is too high.

粘度が高くなりすぎて流動性が失われたり、剪断力によ
る混練機押出機内部の温度上昇によるポリエステルの分
解が生じたり１　さらには混練機押出機内のシャフトや
ディスクの摩耗、焼きつき等のトラブルが発生する。The viscosity may become too high and fluidity may be lost, and the polyester may decompose due to the temperature rise inside the kneader extruder due to shearing force.1 Furthermore, troubles such as wear and seizure of the shaft and disk inside the kneader extruder may occur. occurs.

第２段階目の混練部でさらに混練するが、このときの顔
料濃度は１０〜４０重量％となるようにするのが好まし
い。これにより、顔料の分散性を向上させることができ
るとともに、第１段階目の混練時の剪断力により上昇し
たポリエステルの温度を下げ、熱分解を抑制することが
できる。なお、顔料濃度をあまり低くするとマスターポ
リマーとして使用するのに適さなくなる。Further kneading is carried out in the second stage kneading section, and the pigment concentration at this time is preferably 10 to 40% by weight. Thereby, it is possible to improve the dispersibility of the pigment, and also to lower the temperature of the polyester, which has risen due to the shear force during the first stage of kneading, and to suppress thermal decomposition. Incidentally, if the pigment concentration is too low, it becomes unsuitable for use as a master polymer.

また１本発明においては、混練時の回転動力を混練物Ｉ
Ｋｇ当たり０．０３ＫＷ以上とすることが必要である。In addition, in the present invention, the rotational power during kneading is changed to the kneaded material I.
It is necessary to set it as 0.03KW or more per kg.

これより低い回転動力では、剪断力が不足して顔料の分
散が不十分となる。しかし１回転動力をむやみに高くす
ることは、エネルギーの無駄であり、０．０７〜０．２
　ＫＷ程度が好ましい。If the rotational power is lower than this, the shearing force will be insufficient and the pigment will not be sufficiently dispersed. However, increasing the power per revolution unnecessarily is a waste of energy, and it is 0.07 to 0.2
KW or so is preferable.

本発明において、ポリエステルとしてはポリエチレンテ
レフタレート又はこれを主体とするポリエステルが代表
的なものであり、改質剤を含有したものでもよい。In the present invention, the polyester is typically polyethylene terephthalate or a polyester mainly composed of polyethylene terephthalate, and may also contain a modifier.

また２本発明における顔料としては、無機顔料及び耐熱
性の良い有機顔料を使用することができる。顔料の具体
例としては、二酸化チタン、シリカ、カーボンブラック
、酸化鉄、カドミウムイエロー、銅フタロシアニンブル
ー、銅フタロシアニングリーン、ポリアゾ系顔料、キナ
クリドン系顔料、スレン系顔料、ベンジジン系顔料、チ
オインジゴ系顔料、ペリレン系顔料、ペリノン系顔料。Further, as the pigment in the present invention, inorganic pigments and organic pigments with good heat resistance can be used. Specific examples of pigments include titanium dioxide, silica, carbon black, iron oxide, cadmium yellow, copper phthalocyanine blue, copper phthalocyanine green, polyazo pigments, quinacridone pigments, thren pigments, benzidine pigments, thioindigo pigments, and perylene. pigments, perinone pigments.

ジオキサジン系顔料等が挙げられる。Examples include dioxazine pigments.

（実施例） 次に実施例により本発明を具体的に説明する。(Example) Next, the present invention will be specifically explained with reference to Examples.

実施例において「部」は単位時間当たりの重量部を表す
。In the examples, "parts" represent parts by weight per unit time.

実施例１〜７及び比較例１〜４ 極限粘度〔η）　０．６ＢのＰＥＴペレットと二酸化チ
タン（ＴｉＯｚ）ｉｉ＆粉末とをスクリュー型２軸混練
押出機を用いて第１表に示した混合比率で、混練部の温
度を２７０℃（比較例１のみ２８５℃）に設定し。Examples 1 to 7 and Comparative Examples 1 to 4 PET pellets with an intrinsic viscosity [η) of 0.6B and titanium dioxide (TiOz) II & powder were mixed at the mixing ratio shown in Table 1 using a screw-type twin-screw kneading extruder. The temperature of the kneading section was set at 270°C (285°C only in Comparative Example 1).

第１表に示した回転動力で２段階で連続的に混練し、ベ
レット化してマスターペレットを得た。The mixture was continuously kneaded in two stages using the rotational power shown in Table 1, and pelletized to obtain master pellets.

このマスターベレットの顔料分散度合を次のようにして
評価した結果を第１表に示す。Table 1 shows the results of evaluating the degree of pigment dispersion of this master pellet as follows.

（１）マスターベレットの顔料分散度 ポリマー７〜１０　ｍｇをスライドガラス上で溶融し、
カバーガラスをかけ、顕微鏡で１０部以上の顔料粒子の
個数を測定して次の４段階で評価した。(1) Melt 7 to 10 mg of master pellet pigment dispersion polymer on a glass slide,
A cover glass was placed on the sample, and the number of pigment particles of 10 parts or more was measured using a microscope and evaluated on the following four scales.

（Ａ、、　　Ｂであれば合格。） Ａ：１０部以上の顔料粒子が１個／６ｍｇ以下Ｂ：１０
部以上の顔料粒子が２〜５個／６ｍｇＣ：１０μ以上の
顔料粒子が６〜１０個／６ｍｇＤ：１０μ以上の顔料粒
子が１１個／６ｍｇ以上（２）バック圧上昇率 マスターベレットと顔料を含有しないＰＥＴペレットと
を顔料濃度が０．５％となるように混合し。(Pass if A, B.) A: 1 pigment particle of 10 parts or more / 6 mg or less B: 10
(2) Contains back pressure increase rate master pellet and pigment PET pellets with no pigment were mixed so that the pigment concentration was 0.5%.

常法により、３５ｇ／分・錘の吐出量で溶融紡糸し。Melt spinning was carried out by a conventional method at a discharge rate of 35 g/min/spindle.

２０日間連続運転したときの紡糸口金バンク圧上昇率を
調べた。The spinneret bank pressure increase rate during continuous operation for 20 days was investigated.

第１表 実施例８ スクリュー型２軸混練押出機を用いてＰＥＴベレントと
カーボンブランクとを、混練部の温度を２７０℃に設定
し、　０．１１に讐の回転動力で２段階で連続的に混練
し、ベレット化してマスターベレットを得た。Table 1 Example 8 Using a screw-type twin-screw kneading extruder, PET berent and carbon blank were mixed continuously in two stages with the temperature of the kneading section set at 270°C and the rotational power of the other end at 0.11°C. The mixture was kneaded and made into pellets to obtain a master pellet.

Ｐ　Ｅ　’Ｉ’とカーボンブラックとの混合比率は、第
１段：ＰＥ７５部、カーボンブランク５部とし、第２段
で供給するＰＥＴを２０部とした。The mixing ratio of P E 'I' and carbon black was 1st stage: 75 parts of PE, 5 parts of carbon blank, and 20 parts of PET supplied in the second stage.

このマスターベレットと顔料を含有しないＰＥＴペレ７
）とを顔料濃度が１．０％となるように混合して溶融紡
糸した。This master pellet and PET pellet that does not contain pigment 7
) were mixed so that the pigment concentration was 1.0% and melt-spun.

紡出糸の顔料の分散度合を実施例１に準じて評価したと
ころ、２０部以上の顔料粒子は３個／６ｍｇ。When the degree of dispersion of the pigment in the spun yarn was evaluated according to Example 1, the number of pigment particles of 20 parts or more was 3/6 mg.

バック圧上昇率は１０％であった。The back pressure increase rate was 10%.

（発明の効果） 本発明によれば、ポリエステルに顔料が高度に均一に分
散した原着ポリエステルマスターポリマーが容易に得ら
れる。そしてこのマスターポリマーを使用すれば、特に
繊維を製造する場合、紡糸性がよく、パック圧上昇が抑
制され、高品質の原着繊維を生産性よく製造することが
できる。(Effects of the Invention) According to the present invention, a solution-dyed polyester master polymer in which a pigment is highly uniformly dispersed in polyester can be easily obtained. If this master polymer is used, especially when manufacturing fibers, the spinnability is good, pack pressure increase is suppressed, and high-quality spun-dyed fibers can be manufactured with good productivity.

Claims (1)

【特許請求の範囲】[Claims] （１）ポリエステルと顔料とをスクリュー型２軸混練押
出機中で、２段階で混練して原着ポリエステルマスター
ポリマーを製造するに際し、第１段階目でのポリエステ
ルと顔料との混合比率を６０：４０〜４０：６０の重量
比とし、混練物１Ｋｇ当たり０．０３ＫＷ以上の回転動
力で混練することを特徴とする原着ポリエステルマスタ
ーポリマーの製造法。(1) When kneading polyester and pigment in a screw-type twin-screw extruder in two stages to produce a spun-dyed polyester master polymer, the mixing ratio of polyester and pigment in the first stage was set to 60: 1. A method for producing a doped polyester master polymer, which comprises kneading at a weight ratio of 40 to 40:60 and at a rotational power of 0.03 KW or more per 1 kg of kneaded material.
JP60179206A 1985-08-14 1985-08-14 Manufacture of raw polyester master polymer Pending JPS6239208A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP60179206A JPS6239208A (en) 1985-08-14 1985-08-14 Manufacture of raw polyester master polymer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP60179206A JPS6239208A (en) 1985-08-14 1985-08-14 Manufacture of raw polyester master polymer

Publications (1)

Publication Number Publication Date
JPS6239208A true JPS6239208A (en) 1987-02-20

Family

ID=16061780

Family Applications (1)

Application Number Title Priority Date Filing Date
JP60179206A Pending JPS6239208A (en) 1985-08-14 1985-08-14 Manufacture of raw polyester master polymer

Country Status (1)

Country Link
JP (1) JPS6239208A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5213733A (en) * 1991-06-03 1993-05-25 Industrial Technology Research Institute Method of making synthetic fibers containing photochromic pigment
WO1996001875A1 (en) * 1994-07-12 1996-01-25 Cabot Corporation Dispersible carbon black pellets
US7300967B2 (en) 2004-11-12 2007-11-27 Eastman Chemical Company Polyester polymer and copolymer compositions containing metallic titanium particles
US8987408B2 (en) 2005-06-16 2015-03-24 Grupo Petrotemex, S.A. De C.V. High intrinsic viscosity melt phase polyester polymers with acceptable acetaldehyde generation rates
JP2015206016A (en) * 2014-04-23 2015-11-19 Dic株式会社 Resin coloring master batch, resin composition and method for producing molded article thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5213733A (en) * 1991-06-03 1993-05-25 Industrial Technology Research Institute Method of making synthetic fibers containing photochromic pigment
US5422181A (en) * 1991-06-03 1995-06-06 Industrial Technology Research Institute Synthetic fibers containing photochromic pigment and their preparation
WO1996001875A1 (en) * 1994-07-12 1996-01-25 Cabot Corporation Dispersible carbon black pellets
US7300967B2 (en) 2004-11-12 2007-11-27 Eastman Chemical Company Polyester polymer and copolymer compositions containing metallic titanium particles
US8987408B2 (en) 2005-06-16 2015-03-24 Grupo Petrotemex, S.A. De C.V. High intrinsic viscosity melt phase polyester polymers with acceptable acetaldehyde generation rates
JP2015206016A (en) * 2014-04-23 2015-11-19 Dic株式会社 Resin coloring master batch, resin composition and method for producing molded article thereof

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