KR960041228A - Method of producing polycarbonate - Google Patents

Method of producing polycarbonate Download PDF

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KR960041228A
KR960041228A KR1019960018378A KR19960018378A KR960041228A KR 960041228 A KR960041228 A KR 960041228A KR 1019960018378 A KR1019960018378 A KR 1019960018378A KR 19960018378 A KR19960018378 A KR 19960018378A KR 960041228 A KR960041228 A KR 960041228A
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emulsion
conditions
polycarbonate
alkali metal
aqueous phase
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KR1019960018378A
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KR100457487B1 (en
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신이치 사토
마사아키 미야모토
기요지 구마
겐지 쓰루하라
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미우라 아키라
미쓰비시가가쿠가부시키가이샤
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G64/00Macromolecular compounds obtained by reactions forming a carbonic ester link in the main chain of the macromolecule
    • C08G64/20General preparatory processes
    • C08G64/22General preparatory processes using carbonyl halides
    • C08G64/24General preparatory processes using carbonyl halides and phenols
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G64/00Macromolecular compounds obtained by reactions forming a carbonic ester link in the main chain of the macromolecule
    • C08G64/20General preparatory processes
    • C08G64/205General preparatory processes characterised by the apparatus used

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polyesters Or Polycarbonates (AREA)

Abstract

본 발명은 2상 계면 축합법에 따라 수상 중의 디페놀의 알칼리 금속염과 유기상 중의 포스겐을 반응시켜 올리고머를 수득하는 것을 포함하는 플리카보네이트의 제조방법에 있어서, (1) 반응 생성물은 용해시키지만 물을 용해시키지 않는 불활성 유기용매를 함유하는 유기상과 물, 디페놀 및 알칼리 금속 수산화물을 함유하는 수상을 유화조건 하에서 접촉시켜 유탁액을 생성시키는 공정, 및 (2) 이러한 유탁액을 포스겐과 축합반응 조건하에서 기한 유화 조건보다 약한 혼합조건 하에서 접촉시켜 올리고머를 수득하는 공정을 포함함을 특징으로 하는 폴리카보네이트의 제조방법을 제공한다.The present invention relates to a method for producing polycarbonate, which comprises reacting an alkali metal salt of diphenol in an aqueous phase with a phosgene in an organic phase according to a two-phase interfacial condensation method to obtain an oligomer, wherein (1) the reaction product is dissolved but water is dissolved. Contacting an organic phase containing an inert organic solvent which does not have an inert organic solvent with an aqueous phase containing water, diphenols and alkali metal hydroxides under emulsification conditions to generate an emulsion, and (2) limiting the emulsion under phosgene and condensation reaction conditions. It provides a process for producing a polycarbonate, characterized in that it comprises a step of obtaining an oligomer by contacting under mixing conditions weaker than the emulsification conditions.

상기공정으로 색상이 우수하고 용융 성형후에 색상의 변화가 작은 폴리카보네이트를 수득할 수 있다.By the above process, a polycarbonate excellent in color and small in color change after melt molding can be obtained.

Description

폴리카보네이트의 제조방법Method of producing polycarbonate

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

제1도는 본 발명을 실시하는데 사용하는 반응장의 평면도이다. 제2도는 본 발명을 실시하는데 사용하는 별도 양태의 반응 장치의 평면도이다.1 is a plan view of a reaction field used to practice the present invention. 2 is a plan view of a reaction apparatus of another embodiment used to practice the present invention.

Claims (9)

2상 계면 축합법에 따라 수상 중의 디페놀의 알칼리 금속염과 유기상 중의 포스겐을 반응시켜 올리고머를 수득하는 것을 포함하는 플리카보네이트의 제조방법에 있어서, (1) 반응 생성물은 용해시키지만 물을 용해시키지 않는 불활성 유기용매를 함유하는 유기상과 물, 디페놀 및 알칼리 금속 수산화물을 함유하는 수상을 유화조건 하에서 접촉시켜 유탁액을 생성시키는 공정 및 (2) 이러한 유탁액을 포스겐과 축합반응 조건하에서 기한 유화 조건보다 약한 혼합조건 하에서 접촉시켜 올리고머를 수득하는 공정을 포함함을 특징으로 하는 폴리카보네이트의 제조방법.A method for producing a polycarbonate comprising reacting an alkali metal salt of diphenol in an aqueous phase with a phosgene in an organic phase according to a two-phase interfacial condensation method to obtain an oligomer, wherein (1) an inert that dissolves the reaction product but does not dissolve water. Contacting an organic phase containing an organic solvent with an aqueous phase containing water, diphenols and alkali metal hydroxides under emulsification conditions to form an emulsion, and (2) making the emulsion weaker than the emulsification conditions under condensation with phosgene. Method of producing a polycarbonate, characterized in that it comprises a step of obtaining an oligomer by contacting under mixed conditions. 제1항에 있어서, (1)의 공정의 유화조건으로서 웨이버수 We가 1×104이상이고 (2)는 공정의 조건으로서 웨이버수 We가 1×104미만인 폴리카보네이트의 제조방법.The method for producing a polycarbonate according to claim 1, wherein the number of wavers We is 1 × 10 4 or more as the emulsification condition of the step (1), and (2) the number of wavers We is less than 1 × 10 4 as the conditions of the step. 제1항에 있어서, (1)의 고정의 유화조건으로서 하기 일반식의 P/qRK 200 이상이고 (2)의 공정의 혼합조건으로서 하기 일반식의 P/q가 200 미만인 폴리카보네이트의 제조방법.The method for producing a polycarbonate according to claim 1, wherein P / qRK of the following general formula is at least 200 as the fixed emulsification condition of (1) and P / q of the following general formula is less than 200 as the mixing condition of the process of (2). P/q=Np·ρ·n3·d5/(g·q)(㎏·m/ℓ) P / q = N p · ρ · n 3 · d 5 / (g · q) (㎏ · m / ℓ) 여기서, Np는 상수로서 탱크형 믹서에서는 0.8이고 관모양 믹서에서는 2.31이며, ρ는 비중(㎏/㎥)이며, n은 교반기의 회전수(rps)이며, d는 교반기의 날개 직경(m)이며, g는 중력 가속도(m/sec2)이며, q는 유량(ℓ/sec)이다.Where N p is a constant, 0.8 in the tank mixer, 2.31 in the tubular mixer, ρ is the specific gravity (kg / m 3), n is the rotational speed (rps) of the stirrer, and d is the blade diameter (m) of the stirrer. Where g is gravitational acceleration (m / sec 2 ) and q is flow rate (l / sec). 제1항 내지 제3항 중의 어느 한 항에 있어서, 유탁액의 생성을 하나 이상의 연쇄 정지제 및/또는 하나 이상의 중축합 촉매의 존재하에 실시함을 특징으로 하는 방법.The process according to any one of claims 1 to 3, characterized in that the production of an emulsion is carried out in the presence of at least one chain stopper and / or at least one polycondensation catalyst. 제1항 내지 제4항 중의 어느 한 항에 있어서, 유탁액의 생성을 동적 믹서(기계적 유화기) 및/또는 정적 믹서 속에서 실시함을 특징으로 하는 방법.The process according to claim 1, wherein the production of the emulsion is carried out in a dynamic mixer (mechanical emulsifier) and / or in a static mixer. 제1항 내지 제5항 중의 어느 한 항에 있어서, 포스겐과의 접촉을 압력 0 내지 10㎏/㎤G, 온도 80℃ 이하에서 실시함을 특징으로 하는 방법.The method according to any one of claims 1 to 5, wherein the contact with phosgene is carried out at a pressure of 0 to 10 kg / cm 3 G and a temperature of 80 ° C or lower. 제1항 내지 제6항 중의 어느 한 항에 있어서, 포스겐과의 접촉을 피스톤 유동방식의 반응기 속에서 실시함을 특징으로 하는 방법.The process according to claim 1, wherein the contact with the phosgene is carried out in a piston flow reactor. 2상 계면 축합법에 따라 수상 중의 디페놀의 알칼리 금속염과 유기상 중의 포스겐을 반응시켜 올리고머를 수득하는 것을 포함하는 플리카보네이트의 제조방법에 있어서, (1) 반응 생성물은 용해시키지만 물을 용해시키지 않는 불활성 유기용매를 함유하는 유기상과 물, 디페놀 및 알칼리 금속 수산화물을 함유하는 수상을 유화조건 하에서 접촉시켜 유탁액을 생성시키고, (2) 이러한 유탁액을 포스겐과 축합반응 조건하에서 기한 유화 조건보다 약한 혼합조건 하에서 접촉시켜 올리고머를 수득하고 이때에 수상 중의 디페놀의 알칼리 금속염이 소실될 때까지 유화 상태를 유지시키는 것을 특징으로 하는 폴리카보네이트의 제조방법.A method for producing a polycarbonate comprising reacting an alkali metal salt of diphenol in an aqueous phase with a phosgene in an organic phase according to a two-phase interfacial condensation method to obtain an oligomer, wherein (1) an inert that dissolves the reaction product but does not dissolve water. An organic phase containing an organic solvent and an aqueous phase containing water, diphenols and alkali metal hydroxides are contacted under emulsification conditions to form an emulsion, and (2) mixing the emulsion with phosgene weaker than the emulsification conditions under condensation reaction conditions. Contacting under conditions to obtain an oligomer, wherein the emulsified state is maintained until the alkali metal salt of diphenol in the aqueous phase is lost. 2상 계면 축합법에 따라 수상 중의 디페놀의 알칼리 금속염과 유기상 중의 포스겐을 반응시켜 올리고머를 수득하는 것을 포함하는 플리카보네이트의 제조방법에 있어서, (1) 반응 생성물은 용해시키지만 물을 용해시키지 않는 불활성 유기용매를 함유하는 유기상과 물, 디페놀 및 알칼리 금속 수산화물을 함유하는 수상을 유화조건 하에서 접촉시켜 유탁액을 생성시키는 공정, (2) 이러한 유탁액을 포스겐과 축합반응 조건하에서 기한 유화 조건보다 약한 혼합조건 하에서 접촉시켜 올리고머를 수득하고 이때에 수상 중의 디페놀의 알칼리 금속염이 소실될 때까지 유탁액의 유화 상태를 유지하는 공정 및 (3) 이어서 이러한 올리고머가 용해된 유기상을 수상으로부터 분리하고 필요한 경우 추가량의 불활성 유기 용매와 동시에 물과 알카리 금속 수산화물을 함유하는 수상과 중축합 반응조건 하에 접촉시켜 폴리카보네이트를 수득하는 공정을 포함함을 특징으로 하는 폴리카보네이트의 제조방법.A method for producing a polycarbonate comprising reacting an alkali metal salt of diphenol in an aqueous phase with a phosgene in an organic phase according to a two-phase interfacial condensation method to obtain an oligomer, wherein (1) an inert that dissolves the reaction product but does not dissolve water. Contacting an organic phase containing an organic solvent with an aqueous phase containing water, diphenols and alkali metal hydroxides under emulsification conditions to produce an emulsion, (2) making the emulsion weaker than emulsification conditions under the condensation reaction conditions with phosgene. Contacting under mixed conditions to obtain an oligomer at which time the emulsion is emulsified in the emulsion until the alkali metal salt of diphenol in the aqueous phase is lost; and (3) the organic phase in which such oligomer is dissolved is separated from the aqueous phase and, if necessary, Water and alkali metal hydroxides simultaneously with additional amounts of inert organic solvents Method for producing a polycarbonate, comprising the step of obtaining a polycarbonate by contacting with an aqueous phase containing a polycondensation reaction conditions. ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
KR1019960018378A 1995-05-29 1996-05-29 Method for producing polycarbonate KR100457487B1 (en)

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JP95-152801 1995-05-29

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JPH03199231A (en) * 1989-12-27 1991-08-30 Mitsubishi Kasei Corp Production of aromatic polycarbonate

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