KR910007974A - 알루미늄 알킬의 첨가에 의해 개선된 올레핀 중합용 메탈로센 촉매 - Google Patents

알루미늄 알킬의 첨가에 의해 개선된 올레핀 중합용 메탈로센 촉매 Download PDF

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KR910007974A
KR910007974A KR1019900016067A KR900016067A KR910007974A KR 910007974 A KR910007974 A KR 910007974A KR 1019900016067 A KR1019900016067 A KR 1019900016067A KR 900016067 A KR900016067 A KR 900016067A KR 910007974 A KR910007974 A KR 910007974A
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윤 존
제이. 엘더 마이클
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피나 테크놀로지. 인코포레이티드
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    • C08F4/44—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides
    • C08F4/60—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides together with refractory metals, iron group metals, platinum group metals, manganese, rhenium technetium or compounds thereof
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    • C08F4/60—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides together with refractory metals, iron group metals, platinum group metals, manganese, rhenium technetium or compounds thereof
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    • C08F4/60—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides together with refractory metals, iron group metals, platinum group metals, manganese, rhenium technetium or compounds thereof
    • C08F4/62—Refractory metals or compounds thereof
    • C08F4/64—Titanium, zirconium, hafnium or compounds thereof
    • C08F4/659—Component covered by group C08F4/64 containing a transition metal-carbon bond
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Abstract

내용 없음

Description

알루미늄 알킬의 첨가에 의해 개선된 올레핀 중합용 메탈로센 촉매
본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음

Claims (32)

  1. a) 알루미늄 알킬을 올레핀과 혼합시키고, b) 메탈로센 촉매를 제조하고, c) 촉매를 알루미늄 알킬-올레핀 혼합물과 혼합시킴을 특징으로 하는 올레핀의 중합화 방법.
    상기에서, 알루미늄 알킬의 일반식이 AlR3이며, R이 할로겐, 산소, 수소화물, 알킬, 알콕시 또는 아릴이고, R은 각각 동일하거나 다르며, 하나 이상의 R은 알킬이고, 메탈로센은 중성 메탈로센 화합물 및 이온화 화합물로 부터 형성된 이온쌍이다.
  2. 제1항에 있어서, R이 탄소수 6이하의 알킬 또는 알콕시이거나 탄소수 10이항의 아릴인 방법.
  3. 제2항에 있어서, 메탈로센 : 이온화 화합물 : 알루미늄 알킬의 몰비가 0.5 : 1: 0.5 내지 5: 1: 350인 방법.
  4. 제3항에 있어서, 메탈로센 : 이온화 화합물 : 알루미늄 알킬의 몰비가 0.625 : 1: 1.5 내지 1:5 : 1 :77인 방법.
  5. 제4항에 있어서, 메탈로센 : 이온화 화합물 : 알루미늄 알킬의 몰비가 1: 1: 1인 방법.
  6. 제5항에 있어서, 알루미늄 알킬이 트리에틸알루미늄 및 트리메틸알루미늄으로 이루어진 그룹중에서 선택되는 방법.
  7. 제6항에 있어서, 알루미늄 알킬이 트리에틸알루미늄인 방법.
  8. 제1항에 있어서, (a) 이온화 이온계 화합물을 메탈로센의 중성 메틸유도체와 혼합하고, (b) 이온화 이온계 화합물과 메탈로센의 중성 메틸유도체 사이에서 접촉시켜, 메탈로센 양이온이 촉매로서 작용하는 이온쌍을 생성시키는 단계를 포함하는 방법으로 촉매를 제조하고, 여기에서, 메탈로센의 중성 유도체의 일반식은 Cp2MR*p이며, 이때 Cp는 시클로펜타디에닐 또는 치환된 시클로펜타디에닐그룹이고, 이때 각각의 Cp는 동일하거나 상이하며, M은 제III, IV, V 또는 VI족 금속이고, R*는 수화물, 할로겐, 아미드 또는 히드로카빌 라디칼이며, 이때 각각의 R*는 동일하거나 상이하고, 단 단지 1개의 R*만은 수화물이며 p는 1내지 4이고, 또한 이온화 이온계 화합물은 환성부분을 함유하지 않으며, 카보늄, 옥소늄 또는 설포늄 양이온을 함유하고, 또한, 이온화 이온계 화합물의 양이온은 배위되지 않거나 단지 느슨하게 메탈로센 양이온과 배위할 뿐이며, 메탈로센 양이온과는 화학적으로 반응하지 않는 방법.
  9. 제8항에 있어서, 올레핀이 프로필렌인 방법.
  10. 제8항에 있어서, R이, 탄소수가 20이하인 알킬, 아릴, 알케닐, 알킬아릴 및 아릴알킬중에서 선택한 히드로카빌 라디칼인 방법.
  11. 제10항에 있어서, M이, 티탄, 지르코늄 및 하프늄 중에서 선택한 제IV족 금속인 방법.
  12. 제11항에 있어서, M이 하프늄 또는 지르코늄인 방법.
  13. 제12항에 있어서, 메탈로센의 중성 메틸유도체를 에틸렌비스(테트라히드로인데닐) 지르코늄 디메틸, 에틸렌비스(인데닐)지르코늄 디메틸, 메틸렌비스(인데닐)하프늄 디메틸 및 이소프로필리덴(시클로펜타디에닐-1-플루오레닐)지르코늄 디메틸중에서 선택하는 방법.
  14. 제13항에 있어서, 이온화 이온계 화합물이 트리페닐카베늄 테트라키스(펜타플루오로페닐)보로네이트인 방법.
  15. 제1항에 있어서, (a) 1개의 양자와 반응할 수 있는 1개 이상의 치환체를 함유하며 또한 티탄, 지르코늄 및 하프늄중에서 선택한 금속을 함유하는 메탈로센의 중성 메틸 유도체로 이루어진 1개 이상의 제1화합물과, 1개의 양자를 수여할 수 있는 양이온 및 두 화합물 사이에서의 반응의 결과로서 형성된 음이온을 함유하는 1개 이상의 제2화합물을 적합한 용매 또는 희석제중에서 혼합하고, (b) 제2화합물의 양이온에 의해 제공된 양자가 제1화합물의 리간드와 반응하기에 충분한 시간 동안 단계 (a)에서의 접촉을 유지시키고, (c) 활성 촉매를 단계(b)로부터인 직접 생성물로서 또는 단계(b)로부터인 1개 이상의 직접적인 생성물의 분해생성물로서 회수하는 단계를 포함하여 촉매를 제조하는 방법.
  16. 제15항에 있어서, 올레핀이 프로필렌인 방법.
  17. 제16항에 있어서, 메탈로센의 중성 메틸 유도체가 하기 일반식을 갖는 방법.
    Cp2MR'p
    상기식에서, Cp는 각각 동일하거나 상이하며, 사이클로펜타디에닐 또는 치환된 사이클로펜타디에닐 그룹이고, M은 그룹 (III), (IV), (V) 또는 (VI) 금속이며 R'는 각각 동일하거나 상이하며, 하이드로카빌 라디칼이고, p는 1내지 4이다.
  18. 제17항에 있어서, M을 티타늄, 지르코늄 및 하프늄 중에서 선택하는 방법.
  19. 제18항에 있어서, M이 지르코늄인 방법.
  20. 제19항에 있어서, R'를 탄소수 20이하의 알킬, 아릴, 알케닐, 알킬아릴 및 아릴알킬 중에서 선택하는 방법.
  21. 제10항에 있어서, 메탈로센의 중성 메틸 유도체를 에틸렌 비스(테트라하이드로인데닐)지르코늄 디메틸 및 에틸렌 비스(인데닐)지르코늄 디메틸중에서 선택하는 방법.
  22. 제21항에 있어서, 첫번째 화합물이 에틸렌 비스(인데닐) 지르코늄 디메틸인 방법.
  23. 제22항에 있어서, 두번째 화합물이 N,N-디메틸아닐륨 테트라키스 (펜타플루오로페닐) 보로네이트인 방법.
  24. 제1항에 있어서, 촉매를 a) 일반식 Cp2MR"2(R"X) [여기서, Cp는 사이클로펜타디에닐 또는 치환된 사이클로펜타디에닐이고, M은 그룹 (III), (IV), (V) 또는 (VI) 금속이며, X는 할로겐이고, R'은 합한 알킬이다]의 사이클로펜타디에닐 금속 화합물을 테트라페닐보레이트 금속 화합물과 합하고, b) 테트라페닐보레이트 금속 화합물의 금속에 의해 사이클로펜디에닐 금속 화합물로부터 X-또는 R-이온의 추출을 허용하기에 충분한 시간동안 단계 a)중에서의 접촉을 유지시키고, c) 일반식 [Cp2MR"]+[BPh1]-의 이온쌍을 형성시키는 단계에 의해 제조하는 방법.
  25. 하기 일반식의 메탈로센 촉매 및 일반식 AlR3(여기서, R은 동일하거나 상이하며, 各各 할로겐, 산소, 수화물, 알킬, 알콕시 또는 아릴이고, R중의 하나 이상은 알킬이다)의 알루미늄 알킬을 포함함을 특징으로 하는 촉매계.
    [Cp2MR"P-1]+[A]-
    상기식에서, [Cp2MR"P-1]+는 메탈로센 양이온이고, Cp는 동일하거나 상이하며, 사이클로펜타디에닐 또는 치환된 펜타디에닐이고, M은 동일하거나 상이하며, 각각 수화물, 할로겐, 아미드 또는 하이드로카빌 라디칼이고, 하나의 R"를 제외한 나머지 R"은 수화물이고, p는 1내지 4이고, [A]-는 음이온이다.
  26. 제25항에 있어서, R이 알킬, 아릴, 알케닐, 알킬아릴 및 20개 이하의 탄소원자를 갖는 아릴알킬로 이루어진 그룹중에서 선택된 하이드로카빌 라디칼인 촉매.
  27. 제26항에 있어서, R이 알킬, 탄소수 6개 이하의 알콕시 또는 탄소수 10개 이하의 아릴인 촉매.
  28. 제27항에 있어서, M이 티탄, 지르코늄 및 하프늄으로 이루어진 그룹중에서 선택된 그룹(IV)금속인 촉매.
  29. 제28항에 있어서, 메탈로센의 천연 메틸 유도체가 에틸렌비스(테트라하이드로인데닐)지르코늄 디메틸, 에틸렌비스(인데닐) 지르코늄 디메틸, 에틸렌비스(인데닐)하프늄 디메틸 및 이소프로필리덴(사이클로펜타디에닐-1-플로오로레닐) 지르코늄 디메틸로 이루어진 그룹중에서 선택된 촉매.
  30. 제29항에 있어서, 음이온이 테트라키스(펜타플루오로레닐)보레이토 음이온인 촉매.
  31. 제30항에 있어서, 알루미늄 알킬이 트리에틸알루미늄 및 트리메틸알루미늄으로 이루어진 그룹중에서 선택된 촉매.
  32. 제31항에 있어서, 알루미늄 알킬이 트리에틸알루미늄인 촉매.
    ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.
KR1019900016067A 1989-10-30 1990-10-10 알루미늄 알킬의 첨가에 의해 개선된 올레핀 중합용 메탈로센 촉매 KR100196613B1 (ko)

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US41922289A 1989-10-30 1989-10-30
US419222 1989-10-30

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CN1051365A (zh) 1991-05-15
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ATE137247T1 (de) 1996-05-15
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US5519100A (en) 1996-05-21
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CN1037686C (zh) 1998-03-11
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CA2027122A1 (en) 1991-05-01
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JP2939321B2 (ja) 1999-08-25
DE69026679T2 (de) 1996-09-26
EP0426638A2 (en) 1991-05-08
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