KR960700280A - 에틸렌 공중합법(ethylene interpolymerizations) - Google Patents

에틸렌 공중합법(ethylene interpolymerizations)

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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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브라이언 더블유. 에스 콜타머
로버트 에스. 카드웰
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스티븐 에스. 그레이스
더 다우 케미칼 캄파니
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Abstract

본 발명은 에틸렌/

Description

에틸렌 공중합법(ETHYLENE INTERPOLYMERIZATIONS)
본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음

Claims (22)

  1. (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.
  2. 제1항의 방법에 의해서 제조딘 에틸렌/-올레핀 공중합체 조성물.
  3. 제1항에 있어서, 단계(A) 및 (B)의-올레핀이 각각 1-옥텐인 방법.
  4. 제3항의 방법에 의해서 제조된 에틸렌/1-옥텐 공중합체 조성물.
  5. 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.
  6. 제5항에 있어서, 동질 촉매 조성물이 또한 활성화와 조촉매를 포함하는 방법.
  7. 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.
  8. 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.
  9. 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.
  10. 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*--XB(C6F5)3이다.
  11. 제1항에 있어서, 동질 촉매 조성물이 이질 촉매의 반응성비의 절반 미만의 반응성비를 갖는 방법.
  12. (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.
  13. 제12항의 방법에 의해서 제조된 에틸렌/-올레핀 공중합체 조성물.
  14. 제12항에 있어서,-올레핀이 1-옥텐인 방법.
  15. 제14항의 방법에 의해서 제조된 에틸렌/1-옥텐 공중합체 조성물.
  16. 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.
  17. 제12항에 있어서, 동질 촉매 조성물이 또한 활성화 조촉매를 포함하는 방법.
  18. 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.
  19. 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.
  20. 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.
  21. 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*--XB(C6F5)3이다.
  22. 제12항에 있어서, 동질 촉매 조성물이 이질 촉매의 반응성비의 절반미만의 반응성비를 갖는 방법.
    ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.
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