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KR960010719A - 고활성 이중 금속 시안나이드 촉매 - Google Patents

고활성 이중 금속 시안나이드 촉매 Download PDF

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KR960010719A
KR960010719A KR1019950029366A KR19950029366A KR960010719A KR 960010719 A KR960010719 A KR 960010719A KR 1019950029366 A KR1019950029366 A KR 1019950029366A KR 19950029366 A KR19950029366 A KR 19950029366A KR 960010719 A KR960010719 A KR 960010719A
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polyether
metal cyanide
complexing agent
organic complexing
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비 르 카크
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존 엠. 와그너
아르코케미칼 테크놀로지,엘,피.
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Abstract

본 발명은 고활성 이중 금속 시안나이드(DMC) 촉매에 관한 것이다. 상기 촉매는 DMC 복합물, 및 유기 착화제, 및 촉매에 대하여 약 500 이상의 수평균분자량을 갖는 5 내지 80중량%의 폴리에테르를 함유한다. 또한, 본 발명은 상기 촉매의 제조방법에 관한 것이다. 상기 촉매는 제조가 용이하고, 우수한 활성도를 가지며, 원한다면, 폴리머로부터 빠르게 제거된다.

Description

고활성 이중 금속 시안나이드 촉매
본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음
제1도는 본 발명에 따른 100ppm 촉매로 중합반응시키는 동안 시간에 대한 프로필렌 옥사이드의 소모량을 나타낸 그래프로서, 촉매의 활성도(코발트(g)/분(min)에 대한 전환된 폴리프로필렌 옥사이드(㎏)로 표시)는 그 경사점에서 곡선의 기울기로 결정된다.

Claims (35)

  1. (a) 이중 금속 시안나이드 화합물; (b) 유기 착화제; 및 (c) 촉매의 양에 대하여 약 500 이상의 수평균분자량을 갖는 폴리에테르 5 내지 80중량%로 이루어져 에폭시화합물 중합반응에 사용되며; 상기 폴리에테르 부재하에 제조된 촉매와 비교하여 에폭시화합물 중합반응에 대해 증진된 활성도를 갖는 것을 특징으로 하는 고체 이중 금속 시안나이드 촉매.
  2. 제1항에 있어서, 상기 이중 금속 시안나이드 화합물이 징크 헥사시아노코발테이트인 것을 특징으로 하는 촉매.
  3. 제1항에 있어서, 상기 유기 착화제가 삼차-부틸 알콜인 것을 특징으로 하는 촉매.
  4. 제1항에 있어서, 상기 폴리에테르가 1000 내지 10,000의 수평균분자량을 갖는 폴리에테르 폴리올인 것을 특징으로 하는 촉매.
  5. 제1항에 있어서, 상기 폴리에테르가 2,000 내지 4,000의 수평균분자량을 갖는 폴리(옥시프로필렌) 디올인 것을 특징으로 하는 촉매.
  6. 제1항에 있어서, 상기 촉매가 10 내지 70중량%의 폴리에테르를 함유하는 것을 특징으로 하는 촉매.
  7. 제1항에 있어서, 상기 촉매가 15 내지 60중량%의 폴리에테르를 함유하는 것을 특징으로 하는 촉매.
  8. (a) 징크 헥사시아노코발테이트 화합물; (b) 삼차-부틸 알콜; 및 (c) 촉매의 양에 대하여 약 1000 내지 5000의 수평균분자량을 갖는 폴리에테르 폴리올 10 내지 70중량%로 이루어져 에폭시화합물 중합반응에 사용되며; 상기 폴리에테르 폴리올 부재하에 제조된 촉매와 비교하여 에폭시화합물 중합반응에 대해 증진된 활성도를 갖는 것을 특징으로 하는 고체 이중 금속 시안나이드 촉매.
  9. 제8항에 있어서, 상기 폴리에테르 폴리올이 2,000 내지 4,000의 수평균분자량을 갖는 폴리(옥시프로필렌)디올인 것을 특징으로 하는 촉매.
  10. 제8항에 있어서, 상기 촉매가 15 내지 60중량%의 폴리에테르 폴리올을 함유하는 것을 특징으로 하는 촉매.
  11. 제8항에 있어서, 상기 촉매가 5.75(br), 4.82(br), 3.76(d-스페이싱, 옹거스트롱)의 X-레이 회절무늬를 가지며, 약 5.07, 3.59, 2.54, 2.28(d-스페이싱, 옹거스트롱)에서 고결정 징크 헥사시아노코발테이트에 상응하는 감지신호가 나타나지 않는 것을 특징으로 하는 촉매.
  12. 제8항에 있어서, 상기 촉매가 5 내지 10중량%의 코발트를 함유하는 것을 특징으로 하는 촉매.
  13. 약 500 이상의 수평균분자량을 갖는 폴리에테르 존재하에서 반응시키며, 5 내지 80중량%의 폴리에테르를 함유하는 것을 특징으로 하는 고체 이중 금속 시안나이드 촉매의 제조방법.
  14. 제13항에 있어서, 상기 폴리에테르가 1000 내지 10,000의 수평균분자량을 갖는 폴리에테르 폴리올인 것을 특징으로 하는 방법.
  15. 제13항에 있어서, 상기 폴리에테르가 2000 내지 4000의 수평균분자량을 갖는 폴리(옥시프로필렌) 디올인 것을 특징으로 하는 방법.
  16. 제13항에 있어서, 상기 이중 금속 시안나이드 촉매가 징크 헥사시아노코발테이트인 것을 특징으로 하는 방법.
  17. 제14항에 있어서, 상기 이중 금속 시안나이드 촉매가 15 내지 60중량%의 폴리에테르 폴리올을 함유하는 것을 특징으로 하는 방법.
  18. 제13항에 있어서, 상기 촉매가 유기 착화제 존재하에서 제조됨을 특징으로 하는 방법.
  19. 제18항에 있어서, 상기 유기 착화제가 삼차-부틸 알콜임을 특징으로 하는 방법.
  20. (a) 촉매 슬러리를 제조하기 위해 유기 착화제 존재하에서 금속염 수용액(과량)과 금속 시안나이드염을 충분히 혼합, 반응시키는 단계; (b) 상기 촉매 슬러리와 약 500 이상의 수평균분자량을 갖는 폴리에테르를 화합시키는 단계; (c) 상기 슬러리로부터 폴리에테르-함유 고체 촉매를 분리시키는 단계; (d) 부가적인 유기 착화제를 함유하는 수용액으로 폴리에테르-함유 고체 촉매를 세척시키는 단계; 및 (e) 고체 이중 금속 시안나이드 촉매에 대하여 5 내지 80중량%의 폴리에테르를 함유하는 고체 이중 금속 시안나이드 촉매를 회수하는 단계로 이루어지며, 에폭시화합물 중합반응에 사용되는 고체 이중 금속 시안나이드 촉매의 제조방법.
  21. 제20항에 있어서, 상기 이중 금속 시안나이드 촉매가 징크 렉사시아노코발테이트인 것을 특징으로 하는 방법.
  22. 제20항에 있어서, 상기 유기 착화제가 삼차-부틸 알콜인 것을 특징으로 하는 방법.
  23. 제20항에 있어서, 상기 폴리에테르가 1000 내지 10,000의 수평균분자량을 갖는 폴리에테르 폴리올인 것을 특징으로 하는 방법.
  24. 제20항에 있어서, 상기 폴리에테르가 2000 내지 4000의 수평균분자량을 갖는 폴리(옥시프로필렌) 디올인 것을 특징으로 하는 방법.
  25. 제20항에 있어서, 상기 촉매 슬러리가 저-전단 혼합방법을 사용하는 상기 (b)단계에서 폴리에테르와 혼합됨을 특징으로 하는 방법.
  26. 제20항에 있어서, 상기 (d)단계의 유기 착화제 수용액이 부가적인 폴리에테르를 더욱 포함하는 것을 특징으로 하는 방법.
  27. 제26항에 있어서, 상기 (d)단계 이후에 세척된 폴리에테르-함유 고체 촉매가 부가적인 유기 착화제로 다시 세척됨을 특징으로 하는 방법.
  28. 제26항에 있어서, 상기 (d)단계 이후에 세척된 폴리에테르-함유 고체 촉매가 폴리에테르와 유기 착화제의 혼합물로 다시 세척됨을 특징으로 하는 방법.
  29. (a) 촉매 슬러리를 제조하기 위해 유기 착화제 존재하에서 금속염 수용액(과량)과 금속 시안나이드염을 충분히 혼합, 반응시키는 단계; (b) 상기 촉매 슬러리와 부가적인 유기 착화제 수용액을 함유하는 희석제를 충분히 혼합시키는 단계; (c) 상기 (b)단계에서 얻은 촉매 슬러리와 약 500 이상의 수평균분자량을 갖는 폴리에테르를 화합시키는 단계; (d) 상기 슬러리로부터 폴리에테르-함유 촉매를 분리시키는 단계; 및 (e) 고체 이중 금속 시안나이드 촉매에 대하여 5 내지 80중량%의 폴리에테르를 함유하는 고체 이중 금속 시안나이드 촉매를 회수하는 단계로 이루어지며, 에폭시화합물 중합반응에 사용되는 고체 이중 금속 시안나이드 촉매의 제조방법.
  30. 제29항에 있어서, 상기 (d)단계 이후에 상기 폴리에테르-함유 고체 촉매가 부가적인 유기 착화제로 세척됨을 특징으로 하는 방법.
  31. 제29항에 있어서, 상기 (d)단계 이후에 상기 폴리에테르-함유 고체 촉매가 부가적인 폴리에테르와 유기 착화제의 혼합물로 세척됨을 특징으로 하는 방법.
  32. 제1항의 촉매 존재하에서 에폭시화합물과 하이드록실기-함유개시제를 반응시키는 것을 특징으로 하는 에폭시화합물의 중합공정.
  33. 제8항의 촉매 존재하에서 에폭시화합물과 하이드록실기-함유개시제를 반응시키는 것을 특징으로 하는 에폭시화합물의 중합공정.
  34. 제1항의 촉매를 사용하여 제조된 폴리에테르 폴리올.
  35. 제8항의 촉매를 사용하여 제조된 폴리에테르 폴리올.
    ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.
KR1019950029366A 1994-09-08 1995-09-07 고활성이중금속시안나이드촉매 KR100355336B1 (ko)

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DE69508009T2 (de) 1999-08-12
HUT73052A (en) 1996-06-28
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ATE177123T1 (de) 1999-03-15
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CA2157312C (en) 2008-02-19
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US5482908A (en) 1996-01-09
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AU688548B2 (en) 1998-03-12
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DE69508009D1 (de) 1999-04-08
CN1072687C (zh) 2001-10-10
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US5536883A (en) 1996-07-16
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