KR960700280A - 에틸렌 공중합법(ethylene interpolymerizations) - Google Patents
에틸렌 공중합법(ethylene interpolymerizations)Info
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- KR960700280A KR960700280A KR1019950703120A KR19950703120A KR960700280A KR 960700280 A KR960700280 A KR 960700280A KR 1019950703120 A KR1019950703120 A KR 1019950703120A KR 19950703120 A KR19950703120 A KR 19950703120A KR 960700280 A KR960700280 A KR 960700280A
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Abstract
본 발명은 에틸렌/
Description
본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음
Claims (22)
- (A) 하나 이상의 반응기중에서 알루미늄 조촉매를 함유하지 않거나 또는 단지 소량의 알루미늄 조촉매를 함유하는 동질 촉매 조성물의 존재하에 용액중합 조건하에서 에틸렌과 하나 이상의 다른-올레핀을 접촉반응시킴으로써 좁은 조성 분포 및 좁은 분자량 분포를 갖는 제1공중합체 용액을 제조하고; (B) 하나 이상의 다른 반응기중에서 이질 지글러 촉매의 존재하의 용액중합 조건 및 상기 (A) 단계중에 사용된 온도보다 높은 중합온도에서 에틸렌과 하나 이상의 다른-올레핀을 접촉 반응시킴으로써 넓은 조성 분포 및 분자량 분포를 갖는 제2공중합체 용액을 형성시키고(상기 지글러 촉매는 (ⅰ) 할로겐화 마그네슘 또는 실리카로부터 유도된 고형 지지체 성분 및 (ⅱ) 일반식 TrX´4-q(OR1)q, TrX´4-qOR2 q, VOX´3 및 VO(OR1)3으로 나타낸 전이금속성분을 포함하고, 여기서, Tr은 IVB, VB 또는 VIB족 금속이고, q는 0 내지 4의 수이고, X´는 할로겐이고, R´는 1 내지 20개의 탄소원자를 갖는 알킬 그룹, 아릴 그룹 또는 사이클로알킬 그룹이고, R2는 알킬 그룹, 아릴 그룹, 아르알킬 그룹 또는 치환된 아르알킬 그룹이다): (C) 제1공중합체의 용액을 제2중합체의 용액과 혼합하여 에틸렌/-올레핀 공중합체 조성물을 포함하는 고온의 중합체 용액을 형성시키고; (D) 상기 단계 (C)의 중합체 용액으로부터 용매를 제거하고 에틸렌/-올레핀 공중합체 조성물을 회수함을 특징으로 하는 에틸렌/-올레핀 공중합체 조성물의 제조방법.
- 제1항의 방법에 의해서 제조딘 에틸렌/-올레핀 공중합체 조성물.
- 제1항에 있어서, 단계(A) 및 (B)의-올레핀이 각각 1-옥텐인 방법.
- 제3항의 방법에 의해서 제조된 에틸렌/1-옥텐 공중합체 조성물.
- 제1항에 있어서, 상기 동질 촉매 조성물이 원소 주기율표의 제4족의 금속 및 제한-유도 잔기(constrain-inducing moiety)로 치환된 비편재화된-결합된 잔기를 포함하는 금속 배위 착제를 포함하고, 상기 착제가 비편재화된-결합된 잔기의 질량중심과 하나 이상의 잔류 치환기의 중심 사이의 금속에서의 각이 이러한 제한-유도성 치환기가 없는 유사한-결합된 잔기를 함유하는 유사한 착체에서의 이러한 각보다 더 작도록 하는, 금속 원자에 대한 제한된 기하학적 구조를 가지나, 단 하나 이상의 비편재화된 치환된-결합된 잔기를 포함하는 이들 착체에서 각 금속원자에 대해 이들 중 1개만이 환형의 비편재화된 치환된-결합된 잔기인 방법.
- 제5항에 있어서, 동질 촉매 조성물이 또한 활성화와 조촉매를 포함하는 방법.
- 제5항에 있어서, 배위 착제가 하기 일반식에 상응하는 방법:상기식에서, m은 원소주기율표의 4족의 금속이고; Cp*는 5결합방식으로 M에 결합된 사이클로펜타디에닐 또는 치환된 사이클로펜타디에닐기이고; Z는 붕소, 또는 원소주기율표의 14족 원소, 및 선택적으로는 황 또는 산소를 포함하는 잔기이고, 이때 이 잔기는 20개 이하의 비수소 원자를 함유하며, 선택적으로는, Cp*과 Z는 함께 축합 고리 시스템을 형성하며; X는 각각 독립적으로 30개 이하의 비수소 원자를 갖는 음이온성 리간드기이고; n은 1 또는 2이고; Y는 질소, 인, 산소 또는 황을 함유하여 20개 이하의 비수소 원자를 가지는, Z 및 M에 결합된 음이온성 또는 비이온성 리간드 기이며, 선택적으로는 Y와 Z는 함께 축합 고리 시스템을 형성한다.
- 제5항에 있어서, 배위 착제가 하기 일반식에 상응하는 방법:상기식에서, R´는 각각 수소, 알킬, 아릴, 실릴 및 20개 이하의 비수소 원자를 갖는 이들의 조합체로 이루어진 군으로부터 독립적으로 선택되며; X는 각각 독립적으로 수소화물, 할로, 아킬, 아릴, 실릴, 아릴옥시, 알콕시, 아미드, 실록시 및 20개 이하의 비수소 원자를 갖는 이들의 조합체로 이루어진 군으로부터 선택되며; Y는 -O-, -S-, -NR*-, -PR*- 또는 OR*, SR*, NR*2또는 PR*2로 이루어진 군으로부터 선택된 중성의 2개 전자 공여 리간드이고; M은 전술한 바와 같고; Z는 SiR*2, CR*2, SiR*2SiR*2, CR*2CR*2, CR*=CR*, CR*2SiR*2, BR*이고; R*은 각각, 수소, 알킬, 아릴, 실릴, 할로겐화된 알킬, 20개 이하의 비수소 원자를 갖는 할로겐화된 아릴기, 및 이들의 혼합물로 이루어진 군으로부터 독립적으로 선택되거나, 또는 Y,Z 또는 Y 및 Z 모두로부터의 2개 이상의 R*기는 축합 고리 시스템을 형성하고; n은 1 또는 2 이다.
- 제5항에 있어서, 금속 배위 착체가 하기 일반식에 상응하는 아미도실란-또는 아미도알칸디일-화합물인 방법:상기식에서, M은 5방식으로 사이클로펜타디에닐기에 결합된 티탄, 지르코늄 또는 하프늄이고; R´는 각각 수소, 알킬, 아릴 및 7개 이하의 탄소원자를 갖는 이들의 조합체, 또는 실릴로 이루어진 군으로부터 독립적으로 선택되고; E는 규소 또는 탄소이며; X는 각각 독립적으로 수소화물, 할로, 탄소원자 10개 이하의 알킬, 아릴, 아릴옥시 또는 알콕시이거나, 또는 실릴이고; m은 1 또는 2이고; n은 1 또는 2이다.
- 제5항에 있어서, 금속 배위 착제가 하기 일반식에 상응하는 한계 전하 분리구조를 자는 이온성 촉매인 방법:상기식에서, M은 원소주기율표의 4족의 금속이고; Cp*는 5결합방식으로 M에 결합된 사이클로펜타디에닐 또는 치환된 사이클로펜타디에닐기이고; Z는 붕소, 또는 원소주기율표의 14족 원소, 및 선택적으로는 황 또는 산소를 포함하는 잔기이고, 이때 이 잔기는 20개 이하의 비수소 원자를 함유하며, 또 경우에 따라 Cp*와 Z는 함께 축합 고리 시스템을 형성하고; X는 각각 독립적으로 30개 이하의 비수소 원자를 갖는 음이온성 리간드기이며; n은 1 또는 2이고; XA*-는-XB(C6F5)3이다.
- 제1항에 있어서, 동질 촉매 조성물이 이질 촉매의 반응성비의 절반 미만의 반응성비를 갖는 방법.
- (A) 알루미늄 조촉매를 함유하지 않거나 또는 단지 소량의 알루미늄 조촉매를 함유하는 동질 촉매 성분을 함유하는 하나이상의 반응기중에서 적절한 용액중합 온도 및 압력하에서 에틸렌과 하나이상의 다른-올레핀을 용액중합 방법으로 중합시켜 좁은 조성분포 및 좁은 분자량 분포를 갖는 제1공중합체를 포함하는 제1공중합체 용액을 제조하고; (B) 상기 (A)단계의 공중합체 용액을 용액중합 조건 및 상기 (A)단계중에 사용된 온도보다 높은 중합온도에서 이질 지글러 촉매, 에틸렌 및 하나 이상의 다른 올레핀을 함유하는 하나 이상의 다른 반응기중에 통과시킴으로써 에틸렌/-올레핀 공중합체 조성물을 포함하는 고온의 중합체의 용액을 형성시키고(상기 지글러 촉매는 (ⅰ) 할로겐화 마그네슘 또는 실리카로부터 유도된 고형 지지체 성분 및 (ⅱ) 일반식 TrX´4-q(OR1)q, TrX´4-qOR2 q, VOX´3 및 VO(OR1)3으로 나타낸 전이금속성분을 포함하고, 여기서, Tr은 IVB, VB 또는 VIB족 금속이고, q는 0 내지 4의 수이고, X´는 할로겐이고, R´는 1 내지 20개의 탄소원자를 갖는 알킬 그룹, 아릴 그룹 또는 사이클로알킬 그룹이고, R2는 알킬 그룹, 아릴 그룹, 아르알킬 그룹 또는 치환된 아르알킬 그룹이다): (C) 상기 단계(B)의 중합체의 용액으로부터 용매를 제거하고 에틸렌/-올레핀 공중합체 조성물을 회수함을 특징으로 하는, 에틸렌/-올레핀 공중합체 조성물의 제조방법.
- 제12항의 방법에 의해서 제조된 에틸렌/-올레핀 공중합체 조성물.
- 제12항에 있어서,-올레핀이 1-옥텐인 방법.
- 제14항의 방법에 의해서 제조된 에틸렌/1-옥텐 공중합체 조성물.
- 제12항에 있어서, 상기 동질 촉매 조성물이 원소 주기율표의 제4족의 금속 및 제한-유도 잔기(constrain-inducing moiety)로 치환된 비편재화된-결합된 잔기를 포함하는 금속 배위 착제를 포함하고, 상기 착제가 비편재화된-결합된 잔기의 질량중심과 하나 이상의 잔류 치환기의 중심 사이의 금속에서의 각이 이러한 제한-유도성 치환기가 없는 유사한-결합된 잔기를 함유하는 유사한 착체에서의 이러한 각보다 더 작도록 하는, 금속 원자에 대한 개선된 기하학적 구조를 가지며, 또한 하나 이상의 비편재화된 치환된-결합된 잔기를 포함하는 이들 착체에서 각 금속원자에 대해 이들 중 1개만이 환형의 비편재화된 치환된-결합된 잔기인 방법.
- 제12항에 있어서, 동질 촉매 조성물이 또한 활성화 조촉매를 포함하는 방법.
- 제16항에 있어서, 금속 배위 착체가 하기 일반식에 상응하는 방법:상기식에서, M은 원소주기율표의 4족의 금속이고; Cp*는 5결합방식으로 M에 결합된 사이클로펜타디에닐 또는 치환된 사이클로펜타디에닐기이고; Z는 붕소, 또는 원소주기율표의 14족 원소, 및 선택적으로는 황 또는 산소를 포함하는 잔기이고, 이때 이 잔기는 20개 이하의 비수소 원자를 함유하며, 선택적으로는, Cp*과 Z는 함께 축합 고리 시스템을 형성하며; X는 각각 독립적으로 30개 이하의 비수소 원자를 갖는 음이온성 리간드기이고; n은 1 또는 2이고; Y는 질소, 인, 산소 또는 황을 함유하여 20개 이하의 비수소 원자를 가지는, Z 및 M에 결합된 음이온성 또는 비이온성 리간드 기이며, 선택적으로는 Y와 Z는 함께 축합 고리 시스템을 형성한다.
- 제16항에 있어서, 금속 배위 착체가 하기 일반식에 상응하는 방법:상기식에서, R´는 각각 수소, 알킬, 아릴, 실릴 및 20개 이하의 비수소 원자를 갖는 이들의 조합체로 이루어진 군으로부터 독립적으로 선택되며; X는 각각 독립적으로 수소화물, 할로, 알킬, 아릴, 실릴, 아릴옥시, 알콕시, 아미드, 실록시 및 20개 이하의 비수소 원자를 갖는 이들의 조합체로 이루어진 군으로부터 선택되며; Y는 -O-, -S-, -NR*-, -PR*- 또는 OR*, SR*, NR*2또는 PR*2로 이루어진 군으로부터 선택된 중성의 2개 전자 공여 리간드이고; M은 전술한 바와 같고; Z는 SiR*2, CR*2, SiR*2SiR*2, CR*2CR*2, CR*=CR*, CR*2SiR*2, BR*이고; R*은 각각, 수소, 알킬, 아릴, 실릴, 할로겐화된 알킬, 20개 이하의 비수소 원자를 갖는 할로겐화된 아릴기, 및 이들의 혼합물로 이루어진 군으로부터 독립적으로 선택되거나, 또는 Y,Z 또는 Y 및 Z 모두로부터의 2개 이상의 R*기는 축합 고리 시스템을 형성하고; n은 1 또는 2 이다.
- 제16항에 있어서, 금속 배위 착제가 하기 일반식에 상응하는 아미도 실란-또는 아미도알칸디일-화합물인 방법:상기식에서, M은 5방식으로 사이클로펜타디에닐기에 결합된 티탄, 지르코늄 또는 하프늄이고; R´는 각각 수소, 알킬, 아릴 및 7개 이하의 탄소원자를 갖는 이들의 조합체, 또는 실릴로 이루어진 군으로부터 독립적으로 선택되고; E는 규소 또는 탄소이며; X는 각각 독립적으로 수소화물, 할로, 탄소원자 10개 이하의 알킬, 아릴, 아릴옥시 또는 알콕시이거나, 또는 실릴이고; m은 1 또는 2이고; n은 1 또는 2이다.
- 제16항에 있어서, 금속 배위 착제가 하기 일반식에 상응하는 한계 이하 분리구조를 갖는 이온성 촉매인 방법:상기식에서, M은 원소주기율표의 4족의 금속이고; Cp*는 5결합방식으로 M에 결합된 사이클로펜타디에닐 또는 치환된 사이클로펜타디에닐기이고; Z는 붕소, 또는 원소주기율표의 14족 원소, 및 선택적으로는 황 또는 산소를 포함하는 잔기이고, 이때 이 잔기는 20개 이하의 비수소 원자를 함유하며, 또 경우에 따라 Cp*와 Z는 함께 축합 고리 시스템을 형성하고; X는 각각 독립적으로 30개 이하의 비수소 원자를 갖는 음이온성 리간드기이며; n은 1 또는 2이고; XA*-는-XB(C6F5)3이다.
- 제12항에 있어서, 동질 촉매 조성물이 이질 촉매의 반응성비의 절반미만의 반응성비를 갖는 방법.※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.
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- 1994-01-28 EP EP94910097A patent/EP0681592B1/en not_active Expired - Lifetime
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- 1994-01-28 DE DE69425556T patent/DE69425556T2/de not_active Expired - Lifetime
- 1994-01-28 RU RU95116450A patent/RU2113443C1/ru active
- 1994-01-28 CZ CZ19951963A patent/CZ288678B6/cs unknown
- 1994-01-28 KR KR1019950703120A patent/KR100301978B1/ko not_active IP Right Cessation
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- 1994-01-28 AT AT00100889T patent/ATE254635T1/de active
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