JPH02269120A - Drying of polyester polymer particle - Google Patents

Drying of polyester polymer particle

Info

Publication number
JPH02269120A
JPH02269120A JP8857289A JP8857289A JPH02269120A JP H02269120 A JPH02269120 A JP H02269120A JP 8857289 A JP8857289 A JP 8857289A JP 8857289 A JP8857289 A JP 8857289A JP H02269120 A JPH02269120 A JP H02269120A
Authority
JP
Japan
Prior art keywords
polyester polymer
acetone
particles
polymer particles
drying
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
JP8857289A
Other languages
Japanese (ja)
Inventor
Masaki Yamamoto
正樹 山本
Hiroshi Naito
寛 内藤
Tsutomu Tejima
手島 勉
Toru Makino
槙野 徹
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.)
Kanebo Ltd
Original Assignee
Kanebo 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 Kanebo Ltd filed Critical Kanebo Ltd
Priority to JP8857289A priority Critical patent/JPH02269120A/en
Publication of JPH02269120A publication Critical patent/JPH02269120A/en
Pending legal-status Critical Current

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  • Processes Of Treating Macromolecular Substances (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)
  • Polyesters Or Polycarbonates (AREA)

Abstract

PURPOSE:To prevent mutual fusion of particles and fusion to a wall face and to smoothly heat and dry particles of polyester polymer by previously subjecting particles of polyester polymer to surface treatment with acetone and heating and drying. CONSTITUTION:Previously particles of polyester polymer are subjected to surface treatment with acetone and heated and dried. Direct immersion in acetone, contacting with an atmospheric gas of acetone, immersion in an aqueous solution of acetone, treatment with vapor of acetone may be cited as the surface treatment with acetone.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、ポリエステル重合体粒子の乾燥方法に関する
ものである。
DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for drying polyester polymer particles.

C従来の技術〕 ポリエステル重合体粒子を溶融成形する場合、通常重縮
合反応が完了した重合体を反応槽から吐出し、固化せし
め切断し、粒子状にした後そのポリエステル重合体粒子
を押出成形に供せしめる工程をとる。
C. Prior art] When polyester polymer particles are melt-molded, the polymer after the polycondensation reaction is usually discharged from a reaction tank, solidified and cut to form particles, and then the polyester polymer particles are extruded. Take the process of making it available.

この場合、ポリエステル重合体粒子には、冷却固化によ
る冷却水や、空気中の水分の為、0.1〜押出し成形に
供すると加水分解等の劣化や成形品中にボイドを生成す
るため一般にポリエステル重合体を100℃以上のガラ
ス転移温度以上で真空乾燥又は通気乾燥する必要がある
。しかし、ポリエステル重合体粒子特に第3成分を共重
合させたような粘着しやすいポリエステル重合体粒子を
いきなりガラス転移温度以上の高温で乾燥すると、粒子
が互いに融着し、塊状となり、乾燥容器からの排出が困
難になったり、押出成形時の粒子食込み不良による成形
むらなどのトラブルが生じるという問題がある。
In this case, the polyester polymer particles are exposed to cooling water due to cooling and solidification and moisture in the air, so if the polyester polymer particles are subjected to extrusion molding, they will deteriorate due to hydrolysis etc. and voids will be formed in the molded product. It is necessary to dry the polymer in vacuum or through ventilation at a glass transition temperature of 100° C. or higher. However, if polyester polymer particles, especially sticky polyester polymer particles that have been copolymerized with a third component, are suddenly dried at a high temperature above the glass transition temperature, the particles will fuse together and form a lump, causing the particles to be removed from the drying container. There are problems such as difficulty in discharging and uneven molding due to poor particle penetration during extrusion molding.

ポリエステル重合体粒子のM着防止を開示した゛公知文
献としては、特公昭56−46967号公報、特開昭6
3−207823号公報をあげることができる。特公昭
5(i−46967号公報は、昌結晶性重合体粒子と難
結晶性重合体粒子を混合して加熱乾燥する方法が1!案
されているが、押出成形した後のポリエステル重合体粒
子が混合比により変ったり成形むらが生じる等の欠点が
ある。
Publicly known documents disclosing the prevention of M adhesion of polyester polymer particles include Japanese Patent Publication No. 56-46967 and Japanese Patent Application Laid-open No. 6
3-207823 can be mentioned. Japanese Patent Publication No. 5 (I-46967) proposes a method of mixing crystalline polymer particles and difficult-to-crystalline polymer particles and heating and drying the mixture, but the polyester polymer particles after extrusion molding There are disadvantages such as change in the mixing ratio depending on the mixing ratio and uneven molding.

化炭素共存化で予めポリエステル重合体粒子を加熱処理
した後、乾燥する方法が提案されているが、共重合比率
が高いポリエステル重合体粒子においては・乾燥時の融
着防止効果が充分とはいえない。
A method has been proposed in which polyester polymer particles are heat-treated in advance to coexist with carbon and then dried, but for polyester polymer particles with a high copolymerization ratio, the effect of preventing fusion during drying is sufficient. do not have.

〔発明が解決しようとする問題点〕[Problem that the invention seeks to solve]

本発明の目的は、ポリエステル重合体粒子特に共重合ポ
リエステル重合体粒子を加熱乾燥するに際し、粒子が互
いにあるいは壁面に融着することを防止して、加熱乾燥
を円滑に実施する方法を提供するところにある。
An object of the present invention is to provide a method for smoothly carrying out heat drying of polyester polymer particles, particularly copolymerized polyester polymer particles, by preventing the particles from fusing to each other or to a wall surface. It is in.

〔問題点を解決する為の手段〕[Means for solving problems]

本発明者等は、かかる問題点を解決する為a意研究し、
本発明を達成した。すなわち本発明は、ポリエステル重
合体粒子を加熱乾燥するに際して、予めポリエステル重
合体粒子をアセトンにて表面処理した後に加熱乾燥する
ことを特徴とするポリエステル重合体粒子の乾燥方法で
ある。
The present inventors have conducted a research to solve such problems,
The present invention has been achieved. That is, the present invention is a method for drying polyester polymer particles, which is characterized in that, when drying polyester polymer particles by heating, the polyester polymer particles are surface-treated with acetone in advance and then dried by heating.

本発明において、ポリエステル重合体とは、縮合重合可
能な芳香族ジカルボン酸成分とジオール成分からなる縮
合重合体である。具体的には、第3成分を比較的多■に
共重合させたポリエステル共重合体に効果が顕著であり
、ポリエチレンテレツクレート共重合体、ポリブチレン
テレフタレート共重合体、ポリエチレン−2−6−ナフ
タレート共重合体があげられる。また共重合体を構成す
る第3成分としての酸成分は、たとえば、イソフクル酸
、ナフタレンジカルボン酸、ジフェニルジカルボン酸、
ジフェノキシエタンジカルボン酸。
In the present invention, the polyester polymer is a condensation polymer consisting of an aromatic dicarboxylic acid component and a diol component that can undergo condensation polymerization. Specifically, the effect is remarkable for polyester copolymers in which a relatively large amount of the third component is copolymerized; Examples include copolymers. Further, the acid component as the third component constituting the copolymer is, for example, isofucric acid, naphthalene dicarboxylic acid, diphenyl dicarboxylic acid,
Diphenoxyethanedicarboxylic acid.

ジクロルテレフタル酸、ジブロムテレフタル酸。Dichloroterephthalic acid, dibromoterephthalic acid.

5−ソデイウムスルホイソフタル酸、pオー1−シ安患
香酸、アジピン酸、セバシン酸、ヘキサヒドロテレフタ
ル酸、ナフトエ酸、ヒドロキシステアリン酸等がある。
Examples include 5-sodium sulfoisophthalic acid, p-1-sulfoisophthalic acid, adipic acid, sebacic acid, hexahydroterephthalic acid, naphthoic acid, and hydroxystearic acid.

また共重合せしめるグリコール成分としては、エチレン
グリコール(ブチレンテレフタレート共重合の場合)、
ジエチレングリコール、114ブタンジオール(ポリエ
チレンテレフタレート、ポリエチレンナフタレート共重
合体の’A合) 、  1.3 フチレンゲリコール、
l、5ベンタンジオール、ネオペンチルグリコール、1
.6ヘキサンジオール73メチル1.5ベンタンジオー
ル、119ノナンジオール、1,10デカンジオール、
114シクロヘキサンジメタツール、ビスバラエトキシ
ビスフェノールA、にスパラエトキシビスフェノールS
等が例示され、第3成分として2種類以上のものを共重
合してもよい、この場合第3成分の組成比が10モル%
以上(複数併用の場合合計モル比率)の場合特に融着防
止効果が著しい。
In addition, the glycol components to be copolymerized include ethylene glycol (in the case of butylene terephthalate copolymerization),
Diethylene glycol, 114 butanediol ('A combination of polyethylene terephthalate and polyethylene naphthalate copolymer), 1.3 phthylene gelicol,
l, 5bentanediol, neopentyl glycol, 1
.. 6 hexanediol 73 methyl 1.5 bentanediol, 119 nonanediol, 1,10 decanediol,
114 cyclohexane dimetatool, bisparaethoxybisphenol A, bisparaethoxybisphenol S
etc., and two or more types may be copolymerized as the third component. In this case, the composition ratio of the third component is 10 mol%.
Above (total molar ratio in the case of multiple combinations), the effect of preventing fusion is particularly remarkable.

ポリエステル重合体粒子の大きさは、任意であるが、通
常は一辺の長さが5mm以下のものが好ましい、形状は
立方体、直方体1円柱体などの任意の形をとることがで
きる。
The size of the polyester polymer particles is arbitrary, but it is usually preferable to have a side length of 5 mm or less, and the shape can be any shape such as a cube, rectangular parallelepiped, and one cylinder.

ポリエステル重合体には結晶核剤を混合使用してもよい
、結晶核剤としては、たとえばシリカ。
A crystal nucleating agent may be used in combination with the polyester polymer. Examples of the crystal nucleating agent include silica.

タルク、カーボンブランク、#X酸ナトリウム、炭酸カ
ルシウム、硫酸バリウム、塩化リチウム、ベンゼンスル
ホン酸ナトリウムなどがあり、配合量はi、omm%以
下が望ましい。
Examples include talc, carbon blank, sodium #X acid, calcium carbonate, barium sulfate, lithium chloride, sodium benzenesulfonate, etc., and the blending amount is preferably i.omm% or less.

またポリエステル重合体に、シリコンオイル。Also polyester polymer and silicone oil.

変性シリコン系化合物、ポリエチレングリコール等を混
合して使用することが好ましい。
It is preferable to use a mixture of modified silicone compounds, polyethylene glycol, and the like.

ポリエステル重合体をアセトンにて表面処理する方法は
、′アセトンに直接ポリエステル重合体を漫ン貞する方
法、アセトンの雰囲気ガスにポリエステル重合体粒子を
接触させる方法、アセトン水溶液中にポリエステル重合
体粒子を浸漬する方法、アセトンとポリエステル重合体
粒子を密閉容器内に入れ、水原気封入し lO気圧以下
の加圧系で撹拌する方法等があり、その時の表面処理温
度は常温でもよい。
Methods for surface treatment of polyester polymers with acetone include methods such as dipping the polyester polymer directly into acetone, contacting the polyester polymer particles with acetone atmospheric gas, and placing the polyester polymer particles in an aqueous acetone solution. There is a method of immersion, a method of placing acetone and polyester polymer particles in a closed container, enclosing water, and stirring in a pressurized system below 10 atmospheres, and the surface treatment temperature at this time may be room temperature.

ポリエステル重合体粒子の乾燥時の温度(T)は、ポリ
エステル重合体の結晶開始温度(T c )と融点(T
m)を有する場合、次式 TC5T≦Tm−20℃を満たす範囲の温度が好ましく
、’l’c、Tmが現われないポリエステル重合体の場
合は次式 Tg≦T≦Tg+50℃を満たす範囲の温度が好ましい
、この場合78以上では、乾燥効果が少なく、Tg+5
0℃を越えるとチップの変形が見られることがある。
The temperature (T) during drying of the polyester polymer particles is determined by the crystallization initiation temperature (T c ) and the melting point (T
m), the temperature is preferably in the range that satisfies the following formula TC5T≦Tm-20°C, and in the case of a polyester polymer in which 'l'c and Tm do not appear, the temperature is in the range that satisfies the following formula Tg≦T≦Tg+50°C is preferable; in this case, if it is 78 or more, the drying effect is small and Tg+5
If the temperature exceeds 0°C, deformation of the chip may be observed.

〔作用〕[Effect]

ポリエステル重合体粒子を予めアセトンによって処理す
る方法によって、ポリエステル重合体の融着防止できる
作用としては、明らかではないが、1!リ工ステル重合
体粒子表面がアセトンで構造変化されること等が考えら
れる。
Although it is not clear how the method of pre-treating polyester polymer particles with acetone can prevent the fusion of polyester polymers, 1! It is thought that the surface of the reengineered stell polymer particles is structurally changed by acetone.

〔発明の効果〕〔Effect of the invention〕

本発明によれば、ポリエステル重合体粒子特に共重合ポ
リエステル重合体粒子を加熱乾燥するに際し、粒子が互
いにあるいは壁面に融着することを防止して、加熱乾燥
を円滑に実施する方法を提供することができる。
According to the present invention, there is provided a method for smoothly performing heat drying of polyester polymer particles, particularly copolymerized polyester polymer particles, by preventing the particles from fusing to each other or to a wall surface. I can do it.

ポリエステル重合体粒子の乾燥が充分なことにより、後
の成形工程及び得られる成形品のトラブルが解決され、
繊維をはじめとし、シート、フィルム用ポリマーとして
広く使用されているポリエステル成形品の品質を高める
ことができ産業上その有用性は大きい。
Sufficient drying of the polyester polymer particles solves problems in the subsequent molding process and the resulting molded products.
It has great industrial utility because it can improve the quality of polyester molded products, which are widely used as polymers for fibers, sheets, and films.

〔実施例〕〔Example〕

以下実施例を掲げて、本発明を説明する。 The present invention will be explained below with reference to Examples.

まず重合体粒子の融着度合の測定方法を記述する。First, a method for measuring the degree of fusion of polymer particles will be described.

直径3cmの硬質ガラス試験管に高さ5cmのチップを
充填し熱風乾燥機又は真空静置乾燥機中に立てて所定温
度で所定時間加熱する。その後試験管を(頃むけること
によって粒子を取り出し、その状況によって次の4段階
に分類する。
A hard glass test tube with a diameter of 3 cm is filled with chips with a height of 5 cm, placed in a hot air dryer or a vacuum stationary dryer, and heated at a predetermined temperature for a predetermined time. The particles are then removed by rolling the test tube and classified into the following four stages depending on the situation.

1級二 粒子間の融着は殆どなく、1つぶずつバラバラ
になって取り出せる。
Class 1/2: There is almost no fusion between the particles, and they can be taken out one by one.

2級二 粒子間の融着は多少あるが、試験管をタンピン
グして振動を与えることにより粒子が離れ取り出せる。
Class 2: There is some fusion between the particles, but the particles can be separated by tamping the test tube and applying vibration.

3級二 粒子間の融着はあるが、スパチュラにて掻き取
る事により容易に取り出せるが、ブロックを形成する。
Class 3: There is some fusion between the particles, which can be easily removed by scraping with a spatula, but they form a block.

4級二 粒子間の融着かあり、スパチュラにて措き取る
事が出来ず、試験管からは取り出せない。
Grade 4 2: There is fusion between particles, which cannot be removed with a spatula and cannot be removed from the test tube.

実施例1 長径3mm、短径2mm、高さ3mmの楕円柱状のポリ
エチレンテレフタレート・ナフタレート共重合体粒子(
テレフタル酸成分70モル%、イソフクル酸成分30モ
ル%、IV=0.69.Tg=69℃、水分率0.15
%)を約50gビーカーに取り10ccのアセトンにて
粒子表面を常温にて潤おし、アセトンを充分揮発又は切
った。この時ポリエステル共重合体粒子表面は、°透明
であったものが表面が僅か失透した。これを直jl 3
 c mの試験管に5cmの高さ充填し、110℃X1
5時間の真空静置乾燥機にて乾燥し、粒子水分率はo、
 o o a%であった。
Example 1 Oval cylindrical polyethylene terephthalate/naphthalate copolymer particles with a major axis of 3 mm, a minor axis of 2 mm, and a height of 3 mm (
Terephthalic acid component 70 mol%, isofucric acid component 30 mol%, IV=0.69. Tg=69℃, moisture content 0.15
%) in a beaker, the particle surface was moistened with 10 cc of acetone at room temperature, and the acetone was sufficiently volatilized or removed. At this time, the surface of the polyester copolymer particles was slightly transparent, but the surface became slightly devitrified. Directly do this 3
Fill a cm test tube to a height of 5 cm and heat at 110℃
Dry in a vacuum stationary dryer for 5 hours, particle moisture content is o,
It was o o a%.

比較例1 実施例1で用いたと同じポリエステル共重合体粒子をア
セトンで処理せずに、実施例1と同様の方法で真空減圧
乾燥した。
Comparative Example 1 The same polyester copolymer particles used in Example 1 were dried under reduced pressure in the same manner as in Example 1 without being treated with acetone.

表−1 の結果の如( 実施例は全く融着は見られ ないことがわかる。Table-1 As the result of ( No fusion was observed in the example. It turns out that there isn't.

Claims (1)

【特許請求の範囲】[Claims] ポリエステル重合体粒子を加熱乾燥するに際して、予め
ポリエステル重合体粒子をアセトンにて表面処理した後
に加熱乾燥することを特徴とするポリエステル重合体粒
子の乾燥方法。
1. A method for drying polyester polymer particles, which comprises first surface-treating the polyester polymer particles with acetone and then drying them by heating.
JP8857289A 1989-04-07 1989-04-07 Drying of polyester polymer particle Pending JPH02269120A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP8857289A JPH02269120A (en) 1989-04-07 1989-04-07 Drying of polyester polymer particle

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP8857289A JPH02269120A (en) 1989-04-07 1989-04-07 Drying of polyester polymer particle

Publications (1)

Publication Number Publication Date
JPH02269120A true JPH02269120A (en) 1990-11-02

Family

ID=13946577

Family Applications (1)

Application Number Title Priority Date Filing Date
JP8857289A Pending JPH02269120A (en) 1989-04-07 1989-04-07 Drying of polyester polymer particle

Country Status (1)

Country Link
JP (1) JPH02269120A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0611133A3 (en) * 1993-02-09 1996-05-08 Johnson & Johnson Orthopaedics Process of preparing an absorbable polymer.

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0611133A3 (en) * 1993-02-09 1996-05-08 Johnson & Johnson Orthopaedics Process of preparing an absorbable polymer.

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