KR930007998A - 퍼플루오로폴리옥시알킬렌 중에 함유된 비작용성, 1 작용성 및 2 작용성군을 분리하는 방법 - Google Patents

퍼플루오로폴리옥시알킬렌 중에 함유된 비작용성, 1 작용성 및 2 작용성군을 분리하는 방법 Download PDF

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KR930007998A
KR930007998A KR1019920019387A KR920019387A KR930007998A KR 930007998 A KR930007998 A KR 930007998A KR 1019920019387 A KR1019920019387 A KR 1019920019387A KR 920019387 A KR920019387 A KR 920019387A KR 930007998 A KR930007998 A KR 930007998A
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perfluoropolyoxyalkylene
solvent
nonpolar
functional
polar
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KR1019920019387A
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KR100215519B1 (ko
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토넬리 클라우디오
투리 스테파노
기아노티 기우세페
레비 마리넬라
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카를로 코글리아티
오시몬트 에스.피.에이.
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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
    • C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
    • C08G8/28—Chemically modified polycondensates
    • C08G8/30—Chemically modified polycondensates by unsaturated compounds, e.g. terpenes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • 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
    • C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/002—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from unsaturated compounds
    • C08G65/005—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from unsaturated compounds containing halogens
    • C08G65/007—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from unsaturated compounds containing halogens containing fluorine
    • 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
    • C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/30—Post-polymerisation treatment, e.g. recovery, purification, drying

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Polyethers (AREA)

Abstract

용출제로서, 비극성 플루오르화 용매를 단독으로 사용하거나 또는 극성 용매와의 혼합물을 사용하여 퍼플루오로폴리옥시알킬렌을 컬럼 크로마토그래피하는 것으로 구성되어 있는, 하기 일반식의 퍼플루오로폴리옥시알킬렌 중의 비작용성, 1작용성 및 2작용성군을 서로 분리하는 방법.
X-O-Rf-Y
상기 식에서, Rf=화학식(CF2O), (CF2CF2O), (CF2CF2CF2O)의 단량체 단위를 함유하는 퍼플루오로폴리옥시알킬렌 사슬이고, X, Y=서로 동일하거나 상이하며 비작용성 말단기이거나 작용기 OH및/또는 NH2작용기를 갖는 말단기이며, 상기 퍼플루오로폴리옥시알킬렌의 일부인 적어도 X 또는 Y는 -OH이거나 -OH기를 함유하는 기이다.

Description

퍼플루오로폴리옥시알킬렌 중에 함유된 비작용성, 1 작용성 및 2 작용성군을 분리하는 방법
본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음
히드록실 작용기를 갖는 일반식(Ⅰ)의 퍼플루오로폴리옥시알킬렌 샘플에 대한 크로마토그래피 분석에 있어서, 용출된 용매 부피의 함수로서 중합체 용출 밴드의 프로필을 나타낸 것이다.

Claims (8)

  1. (a) 극성 형태의 결합 또는 상호작용을 형성할 수 있는 활성 부위 및/또는 기, 또는 수소 결합을 함유하는 화합물로 구성된 고체상을, 비극성 플루오르화 용매를 사용하여 일반식(Ⅰ)의 퍼플루오로폴리옥시알킬렌의 히드록시 말단기로 처리함으로써 고정상을 제조하고; (b) 상기한 비극성 플루오르화 용매 최소향 중의 퍼플루오로폴리옥시알킬렌 용액을 컬럼 상부에 제공함으로써 고정상에 의해 퍼플루오로폴리옥시알킬렌을 흡착시키고; (c) 상기한 비극성 용매를 컬럼 상부에 공급함으로써 흡착된 퍼플루오로폴리옥시알킬렌을 용출시키고; (d) 극성 용매에 대한 비극성 용매의 부피비가 바람직하게는 9/1~1/1인 상기한 비극성 용매와 극성 용매로 구성된 혼합물을 컬럼 상부에 공급함으로써 퍼플루오로폴리옥시알킬렌을 계속해서 용출시키고; (e) 고정상을 함유하는 컬럼을 순수한 비극성 용매로 세척하고; (f) 임의로, 상기 (c)~(e)단계에 따라 크로마토그래피 분석을 행할 추가의 퍼플루오로폴리옥시알킬렌 샘플을 고정상에 다시 채우는 것으로 구성되어 있는 방법에 따라 퍼플루오로폴리옥시알킬렌을 컬럼 크로마토그래프 처리함을 특징으로 하는, 하기 일반식(Ⅰ)의 퍼플루오로폴리옥시알킬렌을 구성하는 고분자 비작용성, 1작용성 및 2작용성 군의 1종류 이상을 분리하는 방법.
    X-O-Rf-Y (Ⅰ)
    상기 식에서, Rf=수평균 분자량이 약 500~10,000이며 통계적으로 사슬을 따라 배열된 화학식 (CF2CF2O), (CF2O), (CF2CF2CF2O)의 하나 이상의 퍼플루오로옥시알킬렌 단위를 함유하는 퍼플루오로폴리옥시알킬렌 사슬이고, X, Y=서로 동일하거나 상이하며 화학식 -CF2-CH2O(CH2CH2O)sH, -CF2-CF2CH2O(CH2CH2O)sH, -CF2CH2NH2의 작용성기, 또는 식 -CF2CF2CF3, -CF2CF2Cl, -CF2CF3, -CF2Cl, -CF3, -CFCL2, -CF2Br, -CFBr2의 비작용성기이며, s=0 이상 2이하이다. (단, 고분자의 일부인 X및/또는 Y가 -CF2-CH2O(CH2CH2O)sH 및/또는 -CF2-CF2CH2O(CH2CH2O)sH 및/또는 -CF2CH2NH2기인 경우).
  2. 제1항에 있어서, (a)단계 이전에, 비극성 플루오르화 용매 및 극성 용매로 구성되어 있으며 실리카에 대해 용출강도 ε가 0.2 이상인 혼합물을 사용하여, 고정상을 형성하는 고체 생성물을 처리하는 (A) 단계가 선행되는 분리 방법.
  3. 제2항에 있어서, 비극성 플루오르화 용매와 극성 용매로 구성된 혼합물이 0.3~0.6의 용출강도 ε를 나타내는 분리 방법.
  4. 제1항에 있어서, 비극성 플루오르화 용매가 1,1,2-트리클로로-1,2,2-트리플루오로에탄인 분리 방법.
  5. 제1항에 있어서, 고정상이 실리카겔로 구성되어 있는 분리 방법.
  6. 제1항에 있어서, 고정상이 평균 공극 지름이 200Å 미만인 활성 알루미나로 구성되어 있는 분리방법.
  7. 제1항에 있어서, 극성 용매의 용출강도 ε가 실리카에 대하여 0.30 이상인 분리방법.
  8. 제2항에 있어서, 극성 용매의 용출강도 ε가 실리카에 대하여 0.30 이상인 분리방법.
    ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.
KR1019920019387A 1991-10-21 1992-10-21 퍼플루오로폴리옥시알킬렌중에함유된비작용성,1작용성및2작용성군을분리하는방법 KR100215519B1 (ko)

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ITMI912774A IT1251965B (it) 1991-10-21 1991-10-21 Procedimento per separare tra loro le specie non funzionali, monofunzionali e bifunzionali presenti nei perfluoropoliossialchileni.
ITMI91A002774 1991-10-21

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US (1) US5262057A (ko)
EP (1) EP0538827B1 (ko)
JP (1) JP3283594B2 (ko)
KR (1) KR100215519B1 (ko)
AR (1) AR247893A1 (ko)
AT (1) ATE190331T1 (ko)
AU (1) AU649572B2 (ko)
BR (1) BR9203979A (ko)
CA (1) CA2081085C (ko)
CZ (1) CZ287428B6 (ko)
DE (1) DE69230745T2 (ko)
ES (1) ES2144406T3 (ko)
IT (1) IT1251965B (ko)
RU (1) RU2105971C1 (ko)
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RU2105971C1 (ru) 1998-02-27
CA2081085C (en) 2003-12-09
KR100215519B1 (ko) 1999-08-16
CZ287428B6 (cs) 2000-11-15
JPH06145339A (ja) 1994-05-24
ZA927972B (en) 1993-04-26
AR247893A1 (es) 1995-04-28
AU2723892A (en) 1993-04-22
EP0538827A3 (en) 1993-05-26
JP3283594B2 (ja) 2002-05-20
ATE190331T1 (de) 2000-03-15
ITMI912774A0 (it) 1991-10-21
BR9203979A (pt) 1993-04-27
DE69230745T2 (de) 2000-09-07
AU649572B2 (en) 1994-05-26
EP0538827B1 (en) 2000-03-08
CZ313992A3 (en) 1993-05-12
US5262057A (en) 1993-11-16
ES2144406T3 (es) 2000-06-16
IT1251965B (it) 1995-05-27
ITMI912774A1 (it) 1993-04-21
CA2081085A1 (en) 1993-04-22
DE69230745D1 (de) 2000-04-13
EP0538827A2 (en) 1993-04-28

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