JPS63309537A - Separation of resin from fluorocarbon resin solution - Google Patents

Separation of resin from fluorocarbon resin solution

Info

Publication number
JPS63309537A
JPS63309537A JP62145374A JP14537487A JPS63309537A JP S63309537 A JPS63309537 A JP S63309537A JP 62145374 A JP62145374 A JP 62145374A JP 14537487 A JP14537487 A JP 14537487A JP S63309537 A JPS63309537 A JP S63309537A
Authority
JP
Japan
Prior art keywords
solvent
fluororesin
resin
fluorocarbon resin
solution
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
JP62145374A
Other languages
Japanese (ja)
Inventor
Hiroshi Kimura
博 木村
Kazunori Chiba
和典 千葉
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.)
AGC Inc
Original Assignee
Asahi Glass 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 Asahi Glass Co Ltd filed Critical Asahi Glass Co Ltd
Priority to JP62145374A priority Critical patent/JPS63309537A/en
Publication of JPS63309537A publication Critical patent/JPS63309537A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/62Plastics recycling; Rubber recycling

Abstract

PURPOSE:To obtain a solid fluorocarbon resin of a low residual solvent content in good efficiency, by dispersing an organic solvent solution of a fluorocarbon resin in a specified solvent in the form of fine particles to thereby deposit the fine particulate fluorocarbon resin. CONSTITUTION:A solution is obtained by dissolving a fluorocarbon resin of an intrinsic viscosity of 0.1-2.0dl/g (in tetrahydrofuran at 30 deg.C) and a glass transition temperature >=30 deg.C (e.g., polytetrafluoroethylene) in an organic solvent (e.g., tert-butanol). A solvent (e.g., water) which does not dissolve the fluorocarbon resin but dissolves the solvent for the fluorocarbon resin is circulated at a high speed by a pump 3 from a Venturi part 1 to a resin recovery rank 2. Said fluorocarbon resin solution is fed from a line 4 to the Venturi part 1 and is finely dispersed by a vortex of the solvent passing the Venturi part 1 to thereby deposit fine particulate fluorocarbon resin 5, and subjected to solid/liquid separation in the resin recovery tank 2 to recover the fluorocarbon resin.

Description

【発明の詳細な説明】 [産業上の利用分野コ 本発明は、フッ素樹脂溶液からの樹脂分離法に関するも
のである。
DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for separating resin from a fluororesin solution.

[従来の技術] 従来、塗料用などを目的として各種溶剤に可溶なフッ素
樹脂か知られている。例えば、特公昭55−44083
号、特公昭60−21686号、特公昭6121644
号、特開昭61−57609号、特開昭61−1417
1:1号など。しかしながら、これら溶剤可溶性フッ素
樹脂は、一般に、キシレンなどの有機溶剤に溶解させた
状態で流通されるため、運搬において、危険か伴う。ま
た、塗料以外の用途への展開か難しいなどの問題点かあ
った。
[Prior Art] Fluororesins that are soluble in various solvents have been known for use in paints and the like. For example, Tokuko Sho 55-44083
No., Special Publication No. 60-21686, Special Publication No. 6121644
No., JP-A-61-57609, JP-A-61-1417
1:1 etc. However, these solvent-soluble fluororesins are generally distributed in a state dissolved in an organic solvent such as xylene, which can be dangerous during transportation. There were also problems, such as the difficulty of expanding the product to uses other than paint.

また、合成樹脂溶液から、樹脂を回収する方法としては
、溶液を加熱することにより直接溶剤を蒸発させ固体樹
脂を分離回収する方法や、水蒸気を溶液中に吹き込み溶
剤を水の共沸蒸発により、溶剤を除去し、樹脂を分離回
収する方法や、溶剤として水可溶性の溶剤か用いられた
場合、溶液を水中に投入することにより、溶剤を水に溶
解させて、樹脂を分離する方法などが知られている。
In addition, methods for recovering resin from a synthetic resin solution include a method in which the solvent is directly evaporated by heating the solution and the solid resin is separated and recovered, and a method in which water vapor is blown into the solution and the solvent is removed by azeotropic evaporation of water. There are methods to remove the solvent and separate and recover the resin, and methods to separate the resin by dissolving the solvent in water by pouring the solution into water when a water-soluble solvent is used as the solvent. It is being

[発明の解決しようとする問題点] 従来の合成樹脂溶液から樹脂を回収する方法を、溶剤可
溶性フッ素樹脂溶液に適用した場合、装置壁に融着接着
を起こし、固体フッ素樹脂の回収か困難であるという問
題点があった。
[Problems to be solved by the invention] When the conventional method for recovering resin from a synthetic resin solution is applied to a solvent-soluble fluororesin solution, fusion adhesion occurs on the equipment wall, making it difficult to recover the solid fluororesin. There was a problem.

[問題点を解決するための手段] 本発明は、前述の問題点を解決すべくなされたものであ
り、フッ素樹脂を有機溶剤に溶解したフッ素樹脂溶液を
、フッ素樹脂を溶解せず、フッ素樹脂溶液の溶剤を溶解
する溶媒中に、微小粒状に分散させて微粒子状フッ素樹
脂を析出させ、次いでそのフッ素樹脂を回収することを
特徴とするフッ素樹脂溶液からの樹脂の分離法を提供す
るものである。
[Means for Solving the Problems] The present invention has been made to solve the above-mentioned problems. This invention provides a method for separating a resin from a fluororesin solution, which is characterized by dispersing the solvent of the solution in a solvent to precipitate a particulate fluororesin by dispersing it in the form of fine particles, and then recovering the fluororesin. be.

本発明におけるフッ素樹脂としては、溶剤に可溶なフッ
素樹脂か採用される。この溶剤可溶性フッ素樹脂として
は、フルオロオレフィン、ビニルエーテルおよび必要に
応じ他の共単量体の共重合したフッ素樹脂、フルオロオ
レフィン−ビニルエステル系共重合体、などが例示され
る。ここて、フルオロオレフィンとしては、テトラフル
オロエチレン、クロロトリフルオロエチレン、ヘキサフ
ルオロプロピレン、ビニリデンフルオライド、ビニルフ
ルオライドなどが例示される。好ましくは、テトラフル
オロエチレン、クロロトリフルオロエチレン、ヘキサフ
ルオロプロピレンなどのパーハロオレフィン類である。
As the fluororesin in the present invention, a fluororesin that is soluble in a solvent is used. Examples of the solvent-soluble fluororesin include fluororesins obtained by copolymerizing fluoroolefins, vinyl ethers, and other comonomers as necessary, and fluoroolefin-vinyl ester copolymers. Examples of the fluoroolefins include tetrafluoroethylene, chlorotrifluoroethylene, hexafluoropropylene, vinylidene fluoride, and vinyl fluoride. Preferred are perhaloolefins such as tetrafluoroethylene, chlorotrifluoroethylene, and hexafluoropropylene.

ビニルエーテルとしては、炭素数1〜8程度の直鎖状、
分岐状あるいは脂環状のアルキルビニルエーテル、これ
らアルキルエーテルの炭素に直接結合した水素の一部ま
たは全部かフッ素て置換されたフルオロアルキルビニル
エーテル、また、水酸基、カルボン酸基、エポキシ基、
アミノ基などの官能基含有ビニルエーテルなどが例示さ
れる。また、ビニルエステル類としては、脂肪酸、ビニ
ルエステル類などが例示される。また他の共単量体とし
ては、オレフィン性不飽和結合を有する有機ケイ素化合
物、アクリル酸、メタクリル酸、アクリル酸エステル、
メタクリル酸エステルなどのアクリル糸上ツマ−、アリ
ルビニルエーテルなどが例示される。これらのビニルエ
ステル、共単量体は、水酸基、エポキシ基、アミン基、
カルホン酸基などの官能基を有していてもよい。
Vinyl ethers include linear chains with about 1 to 8 carbon atoms,
Branched or alicyclic alkyl vinyl ethers, fluoroalkyl vinyl ethers in which some or all of the hydrogens directly bonded to the carbon atoms of these alkyl ethers are substituted with fluorine, hydroxyl groups, carboxylic acid groups, epoxy groups,
Examples include vinyl ethers containing functional groups such as amino groups. Furthermore, examples of the vinyl esters include fatty acids and vinyl esters. Other comonomers include organosilicon compounds having olefinic unsaturated bonds, acrylic acid, methacrylic acid, acrylic esters,
Examples include acrylic thread binders such as methacrylic acid ester, allyl vinyl ether, and the like. These vinyl esters and comonomers have hydroxyl groups, epoxy groups, amine groups,
It may have a functional group such as a carbonic acid group.

また、これら溶剤可溶性フッ素樹脂は、テトラヒドロフ
ラン中30°Cて測定される固有粘度か0.1〜2.0
 dl/g程度であることが好ましい。またガラス転移
温度か30℃以上であることか好ましい。
In addition, these solvent-soluble fluororesins have an intrinsic viscosity of 0.1 to 2.0 when measured in tetrahydrofuran at 30°C.
It is preferable that it is about dl/g. Further, it is preferable that the glass transition temperature is 30°C or higher.

本発明において、フッ素樹脂溶液の溶剤としては、上記
フッ素樹脂を溶解する種々の溶剤か採用される。たとえ
ば、ケトン類、アルコール類、エーテル類、芳香族炭化
水素類、塩素系溶剤、フッ素系溶剤、ミネラルスピリッ
トなどの石油系溶剤などが例示される。
In the present invention, as the solvent for the fluororesin solution, various solvents that dissolve the above-mentioned fluororesin are employed. Examples include ketones, alcohols, ethers, aromatic hydrocarbons, chlorinated solvents, fluorinated solvents, and petroleum solvents such as mineral spirits.

また、本発明の方法ては、フッ素樹脂溶液を、フッ素樹
脂を溶解せず、フッ素樹脂溶液の溶剤を溶解する溶媒中
に微小粒状に投入させることか重要である。かかる溶媒
としては、フッ素樹脂およびフッ素樹脂溶液の溶剤の選
択により種々の溶媒を選択することか出来るか、工業的
には水を用いることか好ましい。溶媒としては水を用い
た場合には、フッ素樹脂溶液の溶剤として、水に可溶な
ケトン類、アルコール類、エーテル類を選ぶことか好ま
しい。またフッ素樹脂溶液を溶媒中へ微小粒状に分散さ
せて、微粒状フッ素樹脂を析出させ、次いでそのフッ素
樹脂を回収することか重要である。単にフッ素樹脂溶液
を前記溶媒中に投入するたけては、フッ素樹脂は大きな
塊となり、溶剤の除去を充分に行うことか困難になる。
Furthermore, in the method of the present invention, it is important that the fluororesin solution is introduced in the form of fine particles into a solvent that does not dissolve the fluororesin but dissolves the solvent of the fluororesin solution. As such a solvent, various solvents can be selected depending on the selection of the fluororesin and the solvent for the fluororesin solution, or it is preferable to use water from an industrial perspective. When water is used as the solvent, it is preferable to select water-soluble ketones, alcohols, and ethers as the solvent for the fluororesin solution. It is also important to disperse the fluororesin solution in the form of fine particles in a solvent, precipitate the finely divided fluororesin, and then recover the fluororesin. If the fluororesin solution is simply poured into the solvent, the fluororesin will form large lumps, making it difficult to remove the solvent sufficiently.

フッ素樹脂溶液を微小粒状に分散させる手段としては種
々の方法を採用しうる。通常は、上記#奴の乱流状の流
れにフッ素樹脂溶液を供給して分散させる方法か採用さ
れる。具体的には、後述のようなノスルから乱流状に噴
出させた溶媒の流れにフッ素樹脂溶液を供給する方法や
激しい攪拌下の溶媒中にフッ素樹脂溶液を供給する方法
かある。その他、フッ素樹脂溶液をスプレー等で微細な
粒状とし、それを溶媒に接触させるなどの方法も採用し
つる。
Various methods can be used to disperse the fluororesin solution into fine particles. Usually, a method is adopted in which a fluororesin solution is supplied to the above-mentioned turbulent flow and dispersed. Specifically, there are a method of supplying the fluororesin solution to a stream of solvent jetted out in a turbulent flow from a nostle as described below, and a method of supplying the fluororesin solution into a solvent under vigorous stirring. Other methods include making the fluororesin solution into fine particles by spraying and bringing them into contact with a solvent.

以下に本発明の方法を実施した装置の図を用いて、本発
明をさらに具体的に説明する。第1図は、本発明の方法
を実施した装置の一例である。図中、1は樹脂析出部で
あり、2段のヘンチュリーから構成されており、2は、
樹脂回収槽てあり、3は水循環用ポンプである。第2図
はベンチュリ一部の拡大図である。装置内部を水か高速
て循環されており、水温はlO°C程度に保持されてい
る。フッ素樹脂溶液は、供給ポンプにより、4より、強
制的にベンチュリ一部ヘフィートされる。フィートされ
たフッ素樹脂溶液は、ベンチュリ一部を通過する水の激
しい渦流の発生により微細に分散される。この時、フッ
素樹脂溶液の溶媒は水に溶解するため、水に不溶である
フッ素樹脂は析出される。析出したフッ素樹脂は、粒状
で、水に分解され、水の流れにより樹脂回収槽に搬送さ
れる。樹脂回収槽では、フッ素樹脂粒の水分散液を、固
・液分離操作し、粒状フッ素樹脂を回収、水は、水循環
用ポンプに供給され、装置内を循環する。また回収され
た粒状フッ素樹脂は、ざらにこ流動乾燥機により、残留
水分または溶剤か除去され、固体状のフッ素樹脂が得ら
れる。
The present invention will be explained in more detail below using the drawings of an apparatus that implements the method of the present invention. FIG. 1 is an example of an apparatus implementing the method of the present invention. In the figure, 1 is the resin precipitation part, which is composed of two stages of henturi, and 2 is the resin precipitation part.
There is a resin recovery tank, and 3 is a water circulation pump. Figure 2 is an enlarged view of a portion of the venturi. Water is circulated inside the device at high speed, and the water temperature is maintained at about 10°C. The fluororesin solution is forcibly fed to a portion of the venturi via a supply pump. The poured fluororesin solution is finely dispersed by the generation of a violent vortex of water passing through a portion of the venturi. At this time, since the solvent of the fluororesin solution is dissolved in water, the fluororesin that is insoluble in water is precipitated. The precipitated fluororesin is in the form of particles, decomposed into water, and transported to a resin recovery tank by the flow of water. In the resin recovery tank, the aqueous dispersion of fluororesin particles is subjected to a solid/liquid separation operation to recover particulate fluororesin. Water is supplied to a water circulation pump and circulated within the apparatus. Further, residual moisture or solvent is removed from the recovered granular fluororesin using a coarse fluidized dryer to obtain a solid fluororesin.

[実施例コ 以下の実施例は前記図示した装置を用いて実施した。[Example code] The following examples were carried out using the apparatus shown above.

実施例1 固有粘度か0.2dl/gてあり、ガラス転移温度か4
5℃であるフッ素樹脂のターシャリ−ブタノール50重
量%溶液を温度5℃の水が21113/分の流量で循環
する樹脂析出部へ5文/分の速度でフィートし、粒子径
0.1〜1■の粒状フッ素樹脂を回収した。この粒状フ
ッ素樹脂の乾燥後の残存溶剤量は1重量%以下であった
Example 1 The intrinsic viscosity is 0.2 dl/g, and the glass transition temperature is 4
A 50% by weight solution of fluororesin in tert-butanol at a temperature of 5°C is fed at a rate of 5 g/min to a resin precipitation section where water at a temperature of 5°C circulates at a flow rate of 21113/min, and the particle size is 0.1 to 1. Particulate fluororesin (2) was recovered. The amount of residual solvent in this granular fluororesin after drying was 1% by weight or less.

実施例2 固有粘度か0.1dl/gであり、ガラス転移点が35
℃である40重量%溶解したターシャリ−ツタノール、
セカンダリ−ツタノール混合溶剤溶液を、温度2°Cの
水か3m’/分の流量て循環する樹脂析出部へ5文/分
の速度でフィートすることにより、粒子径0.1〜0.
5■の粒状フッ素樹脂を得た。この粒状フッ素樹脂の乾
燥後の残存溶剤量は1重量%以上であった。
Example 2 The intrinsic viscosity is 0.1 dl/g and the glass transition point is 35
tert-tutanol dissolved at 40% by weight at °C;
By feeding the secondary-tutanol mixed solvent solution at a rate of 5 g/min to a resin precipitation section where water at a temperature of 2° C. was circulated at a flow rate of 3 m'/min, particle sizes of 0.1-0.
A 5-inch granular fluororesin was obtained. The amount of residual solvent in this granular fluororesin after drying was 1% by weight or more.

[発明の効果] 本発明の方法は、フッ素樹脂溶液から、固体フッ素樹脂
を極めて効率よく、分離することかできる。さらに、本
発明の方法により得られる固体フッ素樹脂は残存溶剤量
が極めて少なく、また粒状であるため、成形用として使
用する場合の作業性に極めて優れる。
[Effects of the Invention] The method of the present invention makes it possible to very efficiently separate a solid fluororesin from a fluororesin solution. Furthermore, since the solid fluororesin obtained by the method of the present invention has an extremely small amount of residual solvent and is granular, it has extremely excellent workability when used for molding.

【図面の簡単な説明】[Brief explanation of drawings]

第1図は、本発明の方法を実施する装置の一例てあり、
第2図はベンチュリ一部の拡大図である。 図において、1は樹脂析出部、2は樹脂回収槽てあり、
3は水循環用ポンプてあり、5はフッ素樹脂である。
FIG. 1 shows an example of an apparatus for implementing the method of the present invention,
Figure 2 is an enlarged view of a portion of the venturi. In the figure, 1 is the resin precipitation part, 2 is the resin recovery tank,
3 is a water circulation pump, and 5 is a fluororesin.

Claims (1)

【特許請求の範囲】 1、フッ素樹脂を有機溶剤に溶解したフッ素樹脂溶液を
、フッ素樹脂を溶解せず、フッ素樹脂溶液の溶剤を溶解
する溶媒中に、微小粒状に分散させて微粒子状フッ素樹
脂を析出さ せ、次いでそのフッ素樹脂を回収することを特徴とする
フッ素樹脂溶液からの樹脂の分離法。
[Claims] 1. A fluororesin solution obtained by dissolving a fluororesin in an organic solvent is dispersed in the form of fine particles in a solvent that does not dissolve the fluororesin but dissolves the solvent of the fluororesin solution to produce a finely divided fluororesin. 1. A method for separating a resin from a fluororesin solution, which comprises precipitating the fluororesin and then recovering the fluororesin.
JP62145374A 1987-06-12 1987-06-12 Separation of resin from fluorocarbon resin solution Pending JPS63309537A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP62145374A JPS63309537A (en) 1987-06-12 1987-06-12 Separation of resin from fluorocarbon resin solution

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP62145374A JPS63309537A (en) 1987-06-12 1987-06-12 Separation of resin from fluorocarbon resin solution

Publications (1)

Publication Number Publication Date
JPS63309537A true JPS63309537A (en) 1988-12-16

Family

ID=15383749

Family Applications (1)

Application Number Title Priority Date Filing Date
JP62145374A Pending JPS63309537A (en) 1987-06-12 1987-06-12 Separation of resin from fluorocarbon resin solution

Country Status (1)

Country Link
JP (1) JPS63309537A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6061629A (en) * 1992-01-22 2000-05-09 Mitsubishi Denki Kabushiki Kaisha Traffic navigation apparatus having a by-pass function

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6061629A (en) * 1992-01-22 2000-05-09 Mitsubishi Denki Kabushiki Kaisha Traffic navigation apparatus having a by-pass function

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