KR960010708A - Process for producing crystalline polyester powder - Google Patents

Process for producing crystalline polyester powder Download PDF

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Publication number
KR960010708A
KR960010708A KR1019940024724A KR19940024724A KR960010708A KR 960010708 A KR960010708 A KR 960010708A KR 1019940024724 A KR1019940024724 A KR 1019940024724A KR 19940024724 A KR19940024724 A KR 19940024724A KR 960010708 A KR960010708 A KR 960010708A
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KR
South Korea
Prior art keywords
solvent
phase separation
crystalline polyester
polyester
spherical powder
Prior art date
Application number
KR1019940024724A
Other languages
Korean (ko)
Other versions
KR0148831B1 (en
Inventor
최철림
김준경
임순호
이광희
박민
Original Assignee
김은영
한국과학기술연구원
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Publication date
Application filed by 김은영, 한국과학기술연구원 filed Critical 김은영
Priority to KR1019940024724A priority Critical patent/KR0148831B1/en
Priority to JP7249117A priority patent/JP2624639B2/en
Publication of KR960010708A publication Critical patent/KR960010708A/en
Application granted granted Critical
Publication of KR0148831B1 publication Critical patent/KR0148831B1/en

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/88—Post-polymerisation treatment
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
    • C08G63/16—Dicarboxylic acids and dihydroxy compounds
    • C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
    • C08G63/181—Acids containing aromatic rings
    • C08G63/183—Terephthalic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/12—Powdering or granulating
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2250/00—Compositions for preparing crystalline polymers

Abstract

본 발명은 괴상의 폴리에스테르 수지를 따라 비용매 또는 용매 특성을 나타내는 상분리용 용매를 사용하여 크기 분포가 균일한 단구정상의 폴리에스테르 분말을 얻는 결정성 폴리에스테르 구형 분말의 제조 방법에 관한 것이다. 본 발명의 목적은 종래의 방법으로 제조 불가능한 단구정상의 균일한 크기 분포를 가지는 결정성 폴리에스테르 수지 구형 분말의 제조 방법을 제공하는 것이다.The present invention relates to a method for producing a crystalline polyester spherical powder obtained by obtaining a mono-spherical polyester powder with a uniform size distribution using a phase separation solvent exhibiting nonsolvent or solvent properties along a bulk polyester resin. An object of the present invention is to provide a method for producing a crystalline polyester resin spherical powder having a uniform size distribution of monoclinic phase which cannot be produced by a conventional method.

Description

결정성 폴리에스테르 분말의 제조 방법Process for producing crystalline polyester powder

본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음Since this is an open matter, no full text was included.

Claims (7)

(a)괴상의 결정성 폴리에스테르 수지를 고온에서 상분리용 용매 중에 완전히 용해시켜 투명한 균일 용액을 형성하는 단계, (b)상기 균일 용액을 저온으로 냉각시켜 용매와 폴리에스테르 간의 상분리를 유도하여 폴리에스테르가 독립된 단구정상으로 상분리된 불균일 용액을 형성하는 단계, (c)상기 불균일 용액을 세척용 용매를 사용하여 상분리 용매만을 용해, 세척하여 제거함으로써 폴리에스테르를 상분리된 상태 그대로 분리, 침전시키는 단계, 및 (d)상기 침전물을 여과, 건조시켜 크기 분포가 균일한 독립된 단구정상의 폴리에스테르 분말을 얻는 단계로 이루어진 결정성 폴리에스테르 구형 분말의 제조 방법.(a) completely dissolving the crystalline polyester resin in a phase separation solvent at a high temperature to form a transparent homogeneous solution, (b) cooling the homogeneous solution to a low temperature to induce phase separation between the solvent and the polyester to Forming a heterogeneous solution separated from each other in a mono-monotropic phase, (c) separating and precipitating the polyester in a phase-separated state by dissolving the heterogeneous solution by dissolving, washing and removing only the phase separation solvent using a washing solvent, and (d) A method for producing a crystalline polyester spherical powder, comprising the step of filtering and drying the precipitate to obtain an independent monoclinic polyester powder having a uniform size distribution. 제1항에 있어서, 괴상의 결정성 폴리에스테르 수지는 폴리에틸렌 테레프탈레이트, 폴리부틸렌 테레프탈레이트, 및 그들의 유도체 및 공중합체로 이루어진 군으로부터 선택되는 것인 결정성 폴리에스테르 구형 분말의 제조 방법.The method for producing crystalline polyester spherical powder according to claim 1, wherein the bulk crystalline polyester resin is selected from the group consisting of polyethylene terephthalate, polybutylene terephthalate, and derivatives and copolymers thereof. 제1항에 있어서, 상분리용 용매는 폴리에스테르의 용융 온도(이하, Tm으로 약칭함)를 기준으로 할때, Tm-50℃이하의 온도에서 비용매의 특성을 나타내고, 그 이상의 온도에서는 용매의 특성을 나타내며, 상온에서의 점도가 30cP이상인 것인 결정성 폴리에스테르 분말의 제조 방법.The solvent for phase separation according to claim 1, wherein the solvent for phase separation exhibits non-solvent properties at temperatures below Tm-50 ° C, based on the melting temperature of the polyester (hereinafter abbreviated as Tm). It shows the characteristic, The manufacturing method of the crystalline polyester powder whose viscosity in normal temperature is 30 cP or more. 제3항에 있어서, 상분리용 용매는 네오펜틸글리콜디글리시딜 에테르, 폴리프로필렌글리콜디글리시딜 에테르, 비스페놀 A의 디글리시딜 에테르(DGEBA), 카르보닉모노글리시딜 에테그, 1,6-헥산디올디글리시딜 에테르, 3-메티롤프로판트리글리시딜 에테르 등의 글리시딜 에테르 유도체 및 p-2급 부틸 페놀 에테르 등의 페놀 에테르 유도체로 이루어진 군으로부터 선택되는 것인 결정성 폴리에스테르 구형 분말의 제조 방법.The solvent for phase separation according to claim 3, wherein the solvent for phase separation is neopentyl glycol diglycidyl ether, polypropylene glycol diglycidyl ether, diglycidyl ether of bisphenol A (DGEBA), carbonic monoglycidyl ether, 1 Glycidyl ether derivatives such as 6-hexanediol diglycidyl ether, 3-methyrolpropanetriglycidyl ether, and phenol ether derivatives such as p-secondary butyl phenol ether. Method for producing polyester spherical powder. 제1항에 있어서, 세척용 용매는 상분리용 용매와는 상용성이 있지만 폴리에스테르와는 상용성이 없는 것인 결정성 폴리에스테르 구형 분말의 제조 방법.The method of claim 1, wherein the washing solvent is compatible with the solvent for phase separation but not compatible with the polyester. 제1항에 있어서, 구형 분말의 직경은 1㎛ 내지 100㎛ 범위이고, 그 크기 분포를 나타내는 다분산도는 1.10이하인 결정성 폴리에스테르 구형 분말의 제조 방법.The process for producing crystalline polyester spherical powder according to claim 1, wherein the diameter of the spherical powder is in the range of 1 µm to 100 µm, and the polydispersity indicating its size distribution is 1.10 or less. 제1항에 있어서, (a)단게에서 괴상의 결정성 폴리에스테르 수지를 상분리용 용매에 무게비로 1% 내지 30% 투입하고, (b)단게에서 투명한 균일 용액을 분당 0.01℃내지 20℃의 속도로 냉각시키는 결정성 폴리에스테르 구형 분말의 제조 방법.The method according to claim 1, wherein in step (a), the bulky crystalline polyester resin is added to the solvent for phase separation in a weight ratio of 1% to 30%, and (b) a step of a transparent homogeneous solution at steps of 0.01 ° C to 20 ° C per minute Method for producing crystalline polyester spherical powder to be cooled by. ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
KR1019940024724A 1994-09-29 1994-09-29 Process for preparing crystalline polyester powder KR0148831B1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
KR1019940024724A KR0148831B1 (en) 1994-09-29 1994-09-29 Process for preparing crystalline polyester powder
JP7249117A JP2624639B2 (en) 1994-09-29 1995-09-27 Method for producing crystalline polyester spherical particle powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
KR1019940024724A KR0148831B1 (en) 1994-09-29 1994-09-29 Process for preparing crystalline polyester powder

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KR960010708A true KR960010708A (en) 1996-04-20
KR0148831B1 KR0148831B1 (en) 1998-10-15

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KR100435518B1 (en) * 2002-03-15 2004-06-10 한국화학연구원 The production of spherical polyethylene particle by emulsion crystallization
WO2009142010A1 (en) 2008-05-23 2009-11-26 三洋化成工業株式会社 Resin particle and process for production thereof
JP5429922B2 (en) * 2008-06-18 2014-02-26 独立行政法人産業技術総合研究所 Method for producing polyimide fine particle aggregate
WO2010021081A1 (en) 2008-08-19 2010-02-25 三洋化成工業株式会社 Resin particle and method for producing same
JP5467505B2 (en) 2009-09-30 2014-04-09 株式会社リコー Toner manufacturing method, toner and developer
JP5685984B2 (en) 2010-04-21 2015-03-18 株式会社リコー Toner containing crystalline polyester
JP5549997B2 (en) 2010-08-27 2014-07-16 株式会社リコー Toner for developing electrostatic image, developer, container containing developer, process cartridge, image forming apparatus, and image forming method
JP5672095B2 (en) 2010-09-30 2015-02-18 株式会社リコー Toner and developer for developing electrostatic image
JP2012098697A (en) 2010-10-04 2012-05-24 Ricoh Co Ltd Toner and developer
US8524437B2 (en) 2011-03-04 2013-09-03 Ricoh Company, Ltd. Particle producing method, particle, toner, developer, process cartridge, image forming method, image forming apparatus, and particle producing method
JP6086291B2 (en) 2011-12-15 2017-03-01 株式会社リコー Toner, developer, and toner production method
JP5817601B2 (en) 2012-03-14 2015-11-18 株式会社リコー Toner, developer, and image forming apparatus
JP2013195621A (en) 2012-03-19 2013-09-30 Ricoh Co Ltd Toner for electrostatic charge image development, two-component developer, and image forming apparatus
US10545421B2 (en) 2017-03-16 2020-01-28 Ricoh Company, Ltd. Toner, toner stored unit, image forming apparatus, and method for producing toner
EP3546502A1 (en) * 2018-03-27 2019-10-02 Friedrich-Alexander-Universität Erlangen-Nürnberg Method for producing a population of particles of polyethylene terephthalate or polybutylene terephthalate or of a copolymer comprising pet and/or pbt

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JPS591291B2 (en) * 1975-03-19 1984-01-11 株式会社クラレ Polyester material
JPS57172923A (en) * 1981-04-17 1982-10-25 Toray Ind Inc Production of polybutylene terephthalate polymer fine particle
JPS63241035A (en) * 1987-03-27 1988-10-06 Toyo Ink Mfg Co Ltd Production of polyester powder
CA2006540A1 (en) * 1988-12-23 1990-06-23 Eric Nield Non-attritive method for making polyester polycarbonate or polyamide particles, particles obtainable by the method and their use

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KR0148831B1 (en) 1998-10-15
JP2624639B2 (en) 1997-06-25
JPH08176310A (en) 1996-07-09

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