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JPH0286604A - Method for purifying polymer - Google Patents

Method for purifying polymer

Info

Publication number
JPH0286604A
JPH0286604A JP63238398A JP23839888A JPH0286604A JP H0286604 A JPH0286604 A JP H0286604A JP 63238398 A JP63238398 A JP 63238398A JP 23839888 A JP23839888 A JP 23839888A JP H0286604 A JPH0286604 A JP H0286604A
Authority
JP
Japan
Prior art keywords
polymer
extractant
extractor
molten state
contact
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
JP63238398A
Other languages
Japanese (ja)
Inventor
Hisashi Miyagawa
久司 宮川
Takayori Shinohara
篠原 孝順
Tetsuo Maeda
前田 徹男
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.)
Toyo Engineering Corp
Original Assignee
Toyo Engineering Corp
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 Toyo Engineering Corp filed Critical Toyo Engineering Corp
Priority to JP63238398A priority Critical patent/JPH0286604A/en
Priority to GB8920786A priority patent/GB2223022B/en
Priority to DE3931498A priority patent/DE3931498A1/en
Priority to KR1019890013598A priority patent/KR950008562B1/en
Publication of JPH0286604A publication Critical patent/JPH0286604A/en
Priority to US07/654,964 priority patent/US5237048A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F6/00Post-polymerisation treatments
    • C08F6/06Treatment of polymer solutions
    • C08F6/10Removal of volatile materials, e.g. solvents
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F6/00Post-polymerisation treatments
    • C08F6/001Removal of residual monomers by physical means
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/54Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

PURPOSE:To remove volatile matters from a polymer effectively, by bringing the polymer in a molten state into contact with an extractant. CONSTITUTION:In a process wherein volatile matters contained in a thermoplastic polymer is removed by treating the polymer with an extractant under a high pressure, the polymer in a molten state is brought into contact with the extractant. Here, the term 'the polymer in a molten state' means a liq. polymerization compsn. of the polymer, the melt of powder or pellets of the polymer, or a mixture thereof. As the extractant, any of carbon dioxide, nitrous oxide, carbon disulfide, an aliphatic hydrocarbon such as ethane, ethylene or propane, a halogenated hydrocarbon, an aromatic hydrocarbon such as benzene, toluene or xylene, and an alcohol such as methanol or ethanol can be used. They are used in a liq. or supercritical state; the latter is pref.

Description

【発明の詳細な説明】 (産業上の利用分野) この発明は、重合体の精製方法に関するものであり、さ
らに詳しくは溶融状態の重合体中に含有される揮発性物
質を高圧下に抽出除去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 purifying a polymer, and more specifically to a method for extracting and removing volatile substances contained in a molten polymer under high pressure. It's about how to do it.

(従来の技術) 重合体の揮発性物質を除去する方法として、特公昭61
−29245号公報および特公昭61−52163号公
報には、溶融した熱可塑性樹脂を」 ベント式押出機で処理する方法、あるいは特開昭59−
166506号公報には、重合液組成物を垂直発泡゛型
子熱器と真空槽を直結した揮発分離器を用いて連続的に
脱揮発する方法などが提案されている。さらに、近年は
超臨界流体を使用する高圧抽出方法が提案されており、
特公昭59−46972号公報にはテトラヒドロフラン
−、アルキレンオキシド−5またはテトラヒドロフラン
/アルキレンオキシド−重合物に含まれるオリゴマー性
環状エーテル類の減少方法として、前記重合体を超臨界
状態にあるガスと接触させる方法が開示されている。
(Prior art) As a method for removing volatile substances from polymers,
JP-A-29245 and Japanese Patent Publication No. 61-52163 disclose a method of processing a molten thermoplastic resin with a vented extruder, or JP-A No. 59-59-
Japanese Patent No. 166506 proposes a method of continuously devolatilizing a polymerization liquid composition using a volatilization separator in which a vertical foaming type heater and a vacuum tank are directly connected. Furthermore, in recent years, high-pressure extraction methods using supercritical fluid have been proposed.
Japanese Patent Publication No. 59-46972 describes a method for reducing oligomeric cyclic ethers contained in tetrahydrofuran, alkylene oxide-5, or tetrahydrofuran/alkylene oxide polymers, in which the polymer is brought into contact with a gas in a supercritical state. A method is disclosed.

(発明が解決しようとする課題) しかしながら、前記特公昭61−29245号公報、特
公昭61−52163号公報および特開昭59−166
506号公報に記載の方法は、処理後の重合体中に残留
する揮発性物質濃度を、概略400ppm程度まで減少
させるのが限界であり、前記の残留揮発性物質濃度以下
の市場要求に対応することは不可能であった。また、特
公昭59−46972号公報に記載の方法は、常温で液
状の重合体から不純物を高圧抽出除去する方法であるが
重合体中に残留する不純物をある程度の濃度以下に減少
させるような高度抽出には限界がある。
(Problems to be Solved by the Invention) However, the aforementioned Japanese Patent Publication No. 61-29245, Japanese Patent Publication No. 61-52163 and Japanese Patent Application Laid-open No. 59-166
The method described in Publication No. 506 has a limit of reducing the concentration of volatile substances remaining in the polymer after treatment to approximately 400 ppm, and meets the market demand for a concentration of residual volatile substances below the above. That was impossible. In addition, the method described in Japanese Patent Publication No. 59-46972 is a method of removing impurities by high-pressure extraction from a liquid polymer at room temperature. There are limits to extraction.

(課題を解決するための手段) 本発明者らは、前記した従来の重合体の精製に際しての
問題を克服するため鋭意研究を重ねた結果、溶融状態の
重合体を抽出剤と接触させることにより、揮発性物質の
除去が効率的に行え、重合体中に残留する揮発性物質濃
度を概略tooppm以下に減少させ得ることを見出し
、この知見に基づきこの発明をなすに至った。
(Means for Solving the Problems) As a result of intensive research to overcome the problems in the conventional purification of polymers described above, the present inventors found that by bringing a molten polymer into contact with an extractant, It was discovered that volatile substances can be efficiently removed and the concentration of volatile substances remaining in a polymer can be reduced to about toppm or less, and based on this knowledge, the present invention has been made.

すなわち、この発明は、重合体を抽出剤により高圧下に
処理し、重合体中に含有される揮発性物質を除去するに
当り、溶融状態の重合体を抽出剤と接触させることを特
徴とする重合体の精製方法を提供するものである。
That is, the present invention is characterized in that the polymer is treated under high pressure with an extractant to remove volatile substances contained in the polymer, and the polymer in a molten state is brought into contact with the extractant. A method for purifying a polymer is provided.

この発明方法を実施するに際し、より好適な重合体は、
例えばポリエチレン、ポリプロピレン、ポリスチレン、
アクリルニトリル−スチレン−コポリマー、アクリルニ
トリル−ブタジェン−スチレン−ターポリマー、ポリ酢
酸ビニル、ポリアクリレート、ポリメタクリレート、ポ
リ塩化ビニル、ポリ塩化ビニリデン、フッ素系プラスチ
ック、ポリアクリロニトリル、ポリビニルエーテル、ポ
リビニルケトン、ポリエーテル、熱可塑性ポリエステル
、ポリアミド、ジエン系プラスチック、ポリウレタン系
プラスチックなど、耐熱性高分子としては、ポリキシリ
レン、ポリカーボネート、ポリフェニレンオキシド、ポ
リスルホンなどの熱可塑性樹脂である。
When carrying out the method of this invention, more suitable polymers are:
For example, polyethylene, polypropylene, polystyrene,
Acrylonitrile-styrene copolymer, acrylonitrile-butadiene-styrene terpolymer, polyvinyl acetate, polyacrylate, polymethacrylate, polyvinyl chloride, polyvinylidene chloride, fluorine-based plastic, polyacrylonitrile, polyvinyl ether, polyvinyl ketone, polyether Examples of heat-resistant polymers include thermoplastic resins such as polyxylylene, polycarbonate, polyphenylene oxide, and polysulfone.

この発明において、溶融状態の重合体とは、前記の重合
体の重合液組成物、粉状もしくはベレ・ント状などの重
合体を加熱′a融した溶融物あるいは重合液組成物と粉
状もしくはベレット状などの重合体を加熱溶融した溶融
物との混合物などを意味するものである。
In this invention, the polymer in a molten state refers to a polymer solution composition of the above-mentioned polymer, a melt obtained by heating and melting a polymer in powder or bead shape, or a polymer solution composition in powder or bead form. It means a mixture of a pellet-shaped polymer or the like with a melt obtained by heating and melting it.

この発明に使用される抽出剤は、抽出処理される溶融状
態の重合体に対して適宜選択して使用さ二窒素、二硫化
炭素、エタン、エチレン、プロパン、ブタン、ペンタン
、ヘキサン等の脂肪族炭化水素、ハロゲン化炭化水素、
ベンゼン、トルエン、キシレン等の芳香族炭化水素、メ
タノール、エタノール等のアルコール類(b)前記物質
の2種類以上の混合物が挙げられる。
The extractant used in this invention is appropriately selected and used for the molten polymer to be extracted. Hydrocarbons, halogenated hydrocarbons,
Aromatic hydrocarbons such as benzene, toluene and xylene; alcohols such as methanol and ethanol; and (b) mixtures of two or more of the above substances.

この発明において使用される抽出剤は、液状または超臨
界状態であるが、超臨界状態で用いるのがより好ましい
、この場合の抽出器内の圧力と温度は、精製される溶融
状態の重合体および使用される抽出剤により異なるか、
一般的に圧力は20〜500 Ka/c12 Gが好ま
しく、温度は精製される重合体の溶融温度以上が好まし
い。
The extractant used in this invention is in a liquid or supercritical state, but it is more preferable to use it in a supercritical state. In this case, the pressure and temperature in the extractor are such that the molten polymer to be purified It depends on the extractant used.
Generally, the pressure is preferably 20 to 500 Ka/c12G, and the temperature is preferably higher than the melting temperature of the polymer to be purified.

この発明における抽出対象となる揮発性物質は前記、溶
融状態の重合体中に含有される未反応モノマー、溶剤、
オリゴマーなどの揮発性不純物である。
The volatile substances to be extracted in this invention are the unreacted monomers contained in the molten polymer, the solvent,
Volatile impurities such as oligomers.

この発明方法を実施するに際し、使用される抽出器は充
填塔型、棚段塔型あるいはスプレー基型などが好適であ
るが、抽出処理される7B融状態の重合体と使用される
抽出剤との接触が良好な抽出器であればよく、特に限定
されるものではない。
When carrying out the method of this invention, the extractor used is preferably a packed column type, tray column type, or spray base type, but it is preferable that the extractor used is a packed column type, tray column type, or spray base type. There are no particular limitations as long as the extractor has good contact with the extractor.

また、抽出器は複数個並列に設けて連続的に抽出が行え
るようにしてもよいし、抽出器を複数個直列に設けても
よい。
Further, a plurality of extractors may be provided in parallel so that extraction can be performed continuously, or a plurality of extractors may be provided in series.

(発明の効果) この発明方法によれば溶融状態の重合体の精製を効果的
に行うことができ、揮発性物質抽出度の極めて高い溶融
状態の重合体を得ることができる。
(Effects of the Invention) According to the method of the invention, a molten polymer can be effectively purified, and a molten polymer with an extremely high degree of extraction of volatile substances can be obtained.

また、この発明方法から得られた重合体の成形物は残留
揮発性物質濃度の規制の厳しい市場要求に充分対応でき
るものである。
In addition, the polymer molded product obtained by the method of the present invention can fully meet the market requirements for strict regulation of the concentration of residual volatile substances.

(実施例) 次に本発明を実施例および比較例に基づきさらに詳細に
説明する。
(Examples) Next, the present invention will be described in more detail based on Examples and Comparative Examples.

実施例1 抽出器内に揮発性物質濃度450ppmを含むペレット
状のポリスチレン20gを充填し、加熱溶融させたのち
、抽出剤として二酸化炭素を供給し、抽出器内の圧力を
徐々に上げていった。I&終的に抽出器内の圧力245
にg/cn2 G、温度150℃で1時間保持した後、
二酸化炭素の供給を停止した。抽出器内の圧力が大気圧
になったあと、ポリスチレンを取り出し、分析に供した
0分析の結果、揮発性物質濃度は50ppmに減少した
Example 1 After filling an extractor with 20 g of polystyrene pellets containing a volatile substance concentration of 450 ppm and heating and melting them, carbon dioxide was supplied as an extractant and the pressure inside the extractor was gradually increased. . I & finally the pressure in the extractor 245
g/cn2 G, after holding at a temperature of 150°C for 1 hour,
Carbon dioxide supply was stopped. After the pressure inside the extractor reached atmospheric pressure, the polystyrene was taken out and subjected to analysis. As a result of zero analysis, the volatile substance concentration was reduced to 50 ppm.

比較例1 実施例1と同じペレット状ポリスチレンで実施した。す
なわち、抽出器内に揮発性物質濃度450ppmを含む
ベレット状のポリスチレン20gを充填し、抽出剤とし
て二酸化炭素を供給し、抽出器内の圧力を徐々に上げて
いった。最終的に抽出器内の圧力245 /c112 
G、温度30℃で4時間保持した後、二酸化炭素の供給
を停止した。抽出器内の圧力が大気圧になったあと、ポ
リスチレンを取り出し、分析に供した。分析の結果、揮
発性物質濃度は410ppmであった。
Comparative Example 1 The same pelleted polystyrene as in Example 1 was used. That is, the extractor was filled with 20 g of pellet-shaped polystyrene containing a volatile substance concentration of 450 ppm, carbon dioxide was supplied as an extractant, and the pressure inside the extractor was gradually increased. Finally the pressure inside the extractor is 245/c112
G. After maintaining the temperature at 30° C. for 4 hours, the supply of carbon dioxide was stopped. After the pressure inside the extractor reached atmospheric pressure, the polystyrene was taken out and subjected to analysis. As a result of analysis, the volatile substance concentration was 410 ppm.

実施例2 溶融状態のポリスチレンで実施した。抽出器内に揮発性
物質濃度2500ppmを含むポリスチレン重合液20
gを充填し、抽出剤として二酸化炭素を供給し、抽出器
内の圧力を徐々に上げていった。I&終的に抽出器内の
圧力245K(1/CI2 G、温度220℃で1時間
保持した後、二酸化炭素の供給を停止した。抽出器内の
圧力が大気圧になったあと、ポリスチレンを取り出し、
分析に供した。
Example 2 Conducted with polystyrene in molten state. Polystyrene polymerization solution containing 2500 ppm of volatile substances in the extractor
The pressure inside the extractor was gradually increased by supplying carbon dioxide as an extractant. Finally, the pressure inside the extractor was maintained at 245K (1/CI2G) and the temperature at 220℃ for 1 hour, and then the supply of carbon dioxide was stopped. After the pressure inside the extractor reached atmospheric pressure, the polystyrene was taken out. ,
It was submitted for analysis.

分析の結果、揮発性物質濃度は90ppmであった。As a result of analysis, the volatile substance concentration was 90 ppm.

Claims (1)

【特許請求の範囲】[Claims] (1)重合体を抽出剤により高圧下に処理し、重合体中
に含有される揮発性物質を除去するに当り、溶融状態の
重合体を抽出剤と接触させることを特徴とする重合体の
精製方法。(2)重合体が熱可塑性樹脂である特許請求
の範囲第1項記載の重合体の精製方法。
(1) The polymer is treated with an extractant under high pressure to remove volatile substances contained in the polymer, and the molten polymer is brought into contact with the extractant. Purification method. (2) The method for purifying a polymer according to claim 1, wherein the polymer is a thermoplastic resin.
JP63238398A 1988-09-22 1988-09-22 Method for purifying polymer Pending JPH0286604A (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
JP63238398A JPH0286604A (en) 1988-09-22 1988-09-22 Method for purifying polymer
GB8920786A GB2223022B (en) 1988-09-22 1989-09-14 Method for purifying polymer
DE3931498A DE3931498A1 (en) 1988-09-22 1989-09-21 METHOD FOR CLEANING A POLYMER
KR1019890013598A KR950008562B1 (en) 1988-09-22 1989-09-21 Method for purifying polymer
US07/654,964 US5237048A (en) 1988-09-22 1991-02-13 Method for purifying polymer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP63238398A JPH0286604A (en) 1988-09-22 1988-09-22 Method for purifying polymer

Publications (1)

Publication Number Publication Date
JPH0286604A true JPH0286604A (en) 1990-03-27

Family

ID=17029608

Family Applications (1)

Application Number Title Priority Date Filing Date
JP63238398A Pending JPH0286604A (en) 1988-09-22 1988-09-22 Method for purifying polymer

Country Status (4)

Country Link
JP (1) JPH0286604A (en)
KR (1) KR950008562B1 (en)
DE (1) DE3931498A1 (en)
GB (1) GB2223022B (en)

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DE4201046A1 (en) * 1992-01-17 1993-07-22 Bayer Ag METHOD FOR CLEANING POLYMER SOLUTIONS
US5350813A (en) * 1992-07-27 1994-09-27 Novacor Chemicals (International) S.A. Fluid assisted devolatilization
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KR102144877B1 (en) * 2016-09-26 2020-08-14 주식회사 엘지화학 Method for preparing eco-friendly aromatic vinyl-vinyl cyanide compolymer
US10723858B2 (en) 2018-09-18 2020-07-28 Greenmantra Recycling Technologies Ltd. Method for purification of depolymerized polymers using supercritical fluid extraction
CN113648678B (en) * 2021-07-30 2023-04-07 珠海健科医用材料有限公司 Polysulfone polymer and purification method thereof
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0940711A (en) * 1995-07-28 1997-02-10 Japan Exlan Co Ltd Improved method for producing acrylonitrile polymer melt

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DE3931498A1 (en) 1990-03-29
KR900004774A (en) 1990-04-13
KR950008562B1 (en) 1995-08-03
GB2223022A (en) 1990-03-28
GB2223022B (en) 1992-09-16
GB8920786D0 (en) 1989-11-01

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