KR910007572A - 은 함량이 높은 산화알킬렌 촉매 - Google Patents

은 함량이 높은 산화알킬렌 촉매 Download PDF

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KR910007572A
KR910007572A KR1019900016607A KR900016607A KR910007572A KR 910007572 A KR910007572 A KR 910007572A KR 1019900016607 A KR1019900016607 A KR 1019900016607A KR 900016607 A KR900016607 A KR 900016607A KR 910007572 A KR910007572 A KR 910007572A
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매그너스 토스테인슨 이어린드
모한 바신 마단
라지 세예드모니르 세예드
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티모씨 엔. 비숍
유니온 카바이드 케미칼즈 앤드 플라스틱스 캄파니 인코포레이티드
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D301/00—Preparation of oxiranes
    • C07D301/02—Synthesis of the oxirane ring
    • C07D301/03—Synthesis of the oxirane ring by oxidation of unsaturated compounds, or of mixtures of unsaturated and saturated compounds
    • C07D301/04—Synthesis of the oxirane ring by oxidation of unsaturated compounds, or of mixtures of unsaturated and saturated compounds with air or molecular oxygen
    • C07D301/08—Synthesis of the oxirane ring by oxidation of unsaturated compounds, or of mixtures of unsaturated and saturated compounds with air or molecular oxygen in the gaseous phase
    • C07D301/10—Synthesis of the oxirane ring by oxidation of unsaturated compounds, or of mixtures of unsaturated and saturated compounds with air or molecular oxygen in the gaseous phase with catalysts containing silver or gold
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/48—Silver or gold
    • B01J23/50—Silver
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/66—Silver or gold
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/31—Density
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/61—Surface area
    • B01J35/612—Surface area less than 10 m2/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/63—Pore volume
    • B01J35/635—0.5-1.0 ml/g

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
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  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract

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Description

은 함량이 높은 산화알킬렌 촉매
본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음

Claims (80)

  1. 촉매를 기준으로 표면적이 적어도 약 0.7㎡/g이고 공극 용적이 적어도 약 0.5㏄/g인 불활성의 내화성 고체 지지체상의 적어도 약30중량%의 함침된 은 금속 및 촉매의 효율을 증진시키기 위한 촉진량의 적어도 하나의 촉진제를 함유하는, 알켄의 증기상 에폭시화에 의한 알킬렌 옥사이드 제조용 촉매.
  2. 제1항에 있어서, 촉매의 총 중량을 기준으로 함침된 은 금속의 양이 약 30 내지 약 60중량%인 촉매.
  3. 제2항에 있어서, 촉매의 총 중량을 기준으로 함침된 은 금속의 양이 약 35 내지 약 45중량%인 촉매.
  4. 표면적이 적어도 약 0.7㎡/g이고 공극 용적이 적어도 약 0.5㏄/g인 불활성의 내화성 고체 지지체상의 적어도 약0.4g은/㎤ 촉매(벌크밀도)의 양의 함침된 은 금속 및 촉매의 효율을 증진시키기 위한 촉진량의 적어도 하나의 촉진제를 함유하는, 알켄의 증기상 에폭시화에 의한 알킬렌 옥사이드 제조용 촉매.
  5. 제4항에 있어서, 함침된 은 금속은 양이 0.4 내지 약 2.0g은/㎤ 촉매(벌크밀도)의 범위인 촉매.
  6. 제4항에 있어서, 함침된 은 금속은 양이 0.54 내지 약 0.91g은/㎤ 촉매(벌크밀도)의 범위인 촉매.
  7. 제1항에 있어서, 지지체의 형태가 소형판 형태인 촉매.
  8. 제7항에 있어서, 지지체가 α-알루미나인 촉매.
  9. 제8항에 있어서, 지지체가 적어도 98%순도의 α-알루미나인 촉매.
  10. 제1항에 있어서, 지지체가 불소-함유물질을 함유하는 촉매.
  11. 제10항에 있어서, 불소-함유물질을 함유하는 지지체의 형태가 소형판 형태인 촉매.
  12. 제1항에 있어서, 적어도 하나의 촉진제가 원소주기율표의 3b 내지 7b족 또는 3a 내지 7a족에서 선택된 적어도 하나의 원소를 포함하는 화합물인 촉매.
  13. 제12항에 있어서, 알칼리 금속 또는 알칼리 토금속 양이온을 함유하는 촉매.
  14. 제12항에 있어서, 적어도 하나의 촉진제가 표준 에틸렌 옥사이드 공정조건하에서 측정했을 때 촉매의 효율 및 활성중 적어도 하나를 증진시키는 촉매.
  15. 제12항에 있어서, 산소를 제외한 원자번호가 7 내지 83이고 원소주기율표의 3b 내지 7b족 또는 3a 내지 7a족에서 선택되는 원소의 할라이드 및/또는 산소 음이온을 함유하는 촉매.
  16. 제15항에 있어서, 산소음이온이 설페이트를 포함하는 촉매.
  17. 제15항에 있어서, 산소음이온이 몰리브데이트를 포함하는 촉매.
  18. a)표면적이 적어도 약 0.7㎡/g이고 공극용적이 적어도 약 0.5㏄/g인 내화성 고체 지지체를 제동하고, b)지지체를 용존 은 화합물을 함유하는 1차 함침 용액으로 함침시키며, c)은 화합물을 함유하는 함침된 지지체를 함침 용액으로부터 제거하고 함침된 지지체를 은 화합물로부터 은 금속을 형성하는 조건에 노출시킨 다음, d)지지체를 추가의 용존 은 화합물을 함유하는 2차 함침 용액으로 함침시키며, e)추가의 은 화합물을 함유하는 함침 지지체를 2차 함침 용액으로부터 제거하고 함침된 지지체를 추가의 은 화합물로부터 은 금속을 형성하는 조건에 노출시킨 다음, f)필요하다면, 지지체의 총 중량을 기준으로 지지체중에 함유된 은 금속의 양이 적어도 30중량%에 도달할 때까지 단계(d)와 (e)를 반복함을 특징으로 하여, 알켄의 증기상 에폭시화에 의한 알킨렌옥사이드 제조용 촉매를 제조하는 방법.
  19. 제18항에 있어서, 함침 용액이 촉매의 효율을 증진시키는 적어도 하나의 촉진제를 함유하는 방법.
  20. 제19항에 있어서, 적어도 하나의 촉진제가 최종은 함침용액에만 존재하는 방법.
  21. 제20항에 있어서, 촉진제가 몰리브데이트를 포함하는 방법.
  22. 제18항에 있어서, 지지체를 은 화합물 용액 및 형성된 은 금속으로 함침시키기 전 및/또는 후에, 지지체를 촉매의 효율을 증진시키는 적어도 하의 촉진제를 함유하는 용액과 접촉시키는 방법.
  23. 제18항에 있어서, 은 화합물의 농도가 1차 함침용액에서보다는 2차 함침용액에서 비교적 더 높은 방법.
  24. 제18항에 있어서, 지지체를 1차 함침용액으로 함침시킨 후, 그러나 함침된 지지체를 침착된 은 화합물로 부터 은 금속이 형성되는 조건에 노출시키기 전에, 촉매를 적절한 용매로 세정하여 폐색된 은 화합물을 제거하는 방법.
  25. 제18항에 있어서, 은 화합물로부터 은 금속을 형성하는 조건이 지지체를 가열하는 과정 또는 은 이온→은 금속을 감소시키는 화학물질 처리과정을 포함하는 방법.
  26. 제18항에 있어서, 촉매를 총 중량을 기준으로 함침된 은 금속의 양이 30 내지 약 60중량%의 범위인 방법.
  27. 제18항에 있어서, 촉매를 총 중량을 기준으로 함침된 은 금속의 양이 35 내지 약 45중량%의 범위인 방법.
  28. 제18항에 있어서, 지지체의 형태가 소형판 형태인 방법.
  29. 제28항에 있어서, 지지체가 α-알루미나인 방법.
  30. 29항에 있어서, 지지체가 적어도 98%순도의 α-알루미나인 방법.
  31. 제18항에 있어서, 지지체가 불소-함유 물질을 함유하는 방법.
  32. 제31항에 있어서, 불소-함유 물질을 함유하는 방법.
  33. 제19항에 있어서, 적어도 하나의 촉진제가 원소주기율표의 3b 내지 7b족 또는 3a 내지 7a족에서 선택된 적어도 하나의 원소를 포함하는 화합물인 촉매.
  34. 제32항에 있어서, 알칼리 금속 또는 알칼리 토금속 양이온을 함유하는 방법.
  35. 제33항에 있어서, 적어도 하나의 촉진제가 표준 에틸렌 옥사이드 공정조건하에서 측정했을 때 촉매의 안정성, 효율 및 활성중 적어도 하나를 증진시키는 방법.
  36. 제33항에 있어서, 산소를 제외한 원자번호가 7 내지 83이고 원소주기율표의 3b 내지 7b족 또는 3a 내지 7a족에서 선택되는 원소의 할라이드 및/또는 산소 음이온을 함유하는 방법.
  37. 제36항에 있어서, 산소음이온이 설페이트를 포함하는 방법.
  38. 제36항에 있어서, 산소음이온이 몰리브데이트를 포함하는 방법.
  39. 알켄과 산소를 알켄, 산소 및 가스상 억제제를 함유하는 스트림이 알킬렌 옥사이드 생성 조건하에 제1항에 따른 촉매의 고정층에 공급되고 알킬렌 옥사이드가 촉매의 고정층으로부터의 유출물중에 제공되는 증기상으로 반응시킴으로써 알킬렌 옥사이드를 제조하는 방법.
  40. 제39항에 있어서, 알킬렌 옥사이드가 에틸렌 옥사이드이고 알켄이 에틸렌인 방법.
  41. 표면적이 적어도 약 0.7㎡/g이고 공극용적이 적어고 약 0.5㏄/g인 불활성의 내화성 고체 지지체상의 보다 적은 양의 은을 함유하는 유사 촉매와 비교하여 적어도 약 5°C에서 표준 에틸렌 옥사이드 생성 조건하에 측정하여 촉매의 활성을 증가시키기에 충분한 양의 합침된 은 금속 및 촉매의 효율을 증진시키기 위한 촉진량의 적어도 하나의 촉진제를 함유하는, 알켄의 증기상 에폭시화에 의한 알킬렌 옥사이드 제조용 촉매.
  42. 제41항에 있어서, 활성이 적어도 약 10°C까지 증가되는 촉매.
  43. 표면적이 적어도 약 0.7m²/g이고 공극용적이 적어도 약 0.5cc/g이며 중간 크기 공극의 직경이 약 3내지 2μ인 불활성의 내화성 고체 지지체상에 함침되며, 촉매를 기준으로 하여 적어도 25중량%의 은을 함유하는 알켄의 증기상 에폭시화에 의한 알킬렌 옥사이드 제조용 촉매.
  44. 43항에 있어서, 공극의 약 10 내지 25용적%가 0.5 내지 1μ의 공극 직경을 갖고 공극의 적어도 10용적%가 약 1 내지 10μ의 공극 직경을 가지며, 공극의 적어도 20용적%가 약 10 내지 100μ의 공극 직경을 갖는 촉매.
  45. 제44항에 있어서, 촉매의 효율을 증가시키기 위한 적어도 하나의 촉진젤을 함유하는 촉매.
  46. 제45항에 있어서, 적어도 하나의 촉진제가 양이온성 촉진제인 촉매.
  47. 제46항에 있어서, 양이온 촉진제가 칼륨, 루비듐 및 세슘중 적어도 하나를 포함하는 촉매.
  48. 제46항에 있어서, 적어도 하나의 촉진제가 음이온성 촉진제를 포함하는 촉매.
  49. 제46항에 있어서, 음이온성 촉진제가 산소를 제외한 원자번호가 7 내지 83이고 원소주기율표의 3b 내지 7b족 또는 3a 내지 7a족에서 선택된 원소의 할라이드 및 또는 산소 음이온중의 적어도 하나를 포함하는 촉매.
  50. 제49항에 있어서, 음이온성 촉진제가 설페이트, 플루오로설페이트, 나이트레이트, 망가네이트, 바나데이트, 크로메이트, 몰리브데이트, 텅스테이트, 레네이트 및 세레이트중 적어도 하나를 포함하는 촉매.
  51. 제50항에 있어서, 양이온성 촉진제가 알칼리 금속 및 알칼리토금속중 적어도 하나를 포함하는 촉매.
  52. 제51항에 있어서, 양이온성 촉진제가 세슘, 루비듐 및 칼륨중 적어도 하나를 포함하는 촉매.
  53. 제52항에 있어서, 담체가 α-알루미나를 포함하는 촉매.
  54. 제43항에 있어서, 담체가 α-알루미나를 포함하는 촉매.
  55. 제54항에 있어서, 담체의 공극 용적 분표가 하기와 같은 촉매.
  56. 공극 직경(μ) 공극% (용적%)
  57. 0.1미만 0내지 5
  58. 0.1내지 0.5 5내지 20
  59. 0.5내지 1.0 10내지 25
  60. 1.0내지 1.0 10내지 40
  61. 10내지 100 30내지 55
  62. 100이상 6내지 20
  63. 제55항에 있어서, 담체의 산도가 비가역성 암모니아 흡수로 측정하여 약 1.5미만인 촉매.
  64. 제43항에 있어서, 촉매의 효율을 촉진시키기 위한 적어도 하나의 촉매를 추가로 함유하는 촉매.
  65. 제57항에 있어서, 중간 크기 공극의 직경 및 공극 분포가, 촉매가 표준에틸렌 옥사이드 공정조건하 2.0%σ 에틸렌 옥사이드에서 약12 내지 15중량%의 은을 함유하는 것을 제외하고는 동일한 다른 촉매에 의해 유사한 조건하에서 나타나는 것보다 비교적 더 큰 효율 및 낮은 온도를 나타내는 촉매.
  66. 제58항에 있어서, 효율의 증가가 적어도 약 2효율% 포인트인 촉매.
  67. 에틸렌 및 산소를 에틸렌, 산소 및 가스상 억제제를 함유하는 스트림이 에틸렌 옥사이드 생성조건하에 제43항에 따른 촉매의 고정층에 공급되고 에틸렌 옥사이드가 촉매 고정층으로부터의 유출물중에 제공되는 증기상으로 반응시키므로써 에틸렌 옥사이드를 제조하는 방법.
  68. 에틸렌 및 산소를 에틸렌, 산소 및 가스상 억제제를 함유하는 스트림이 에틸렌 옥사이드 생성조건하에 제53항에 따른 촉매의 고정층에 공급되고 에틸렌 옥사이드가 촉매 고정층으로부터의 유출물중에 제공되는 증기상으로 반응시키므로써 에틸렌 옥사이드를 제조하는 방법.
  69. 표면적이 적어도 약 0.7㎡/g이고 공극용적이 적어고 약 0.5㏄/g이며 공극 분포가 공극의 약 10내지 25용적%는 공극 직경이 0.5 내지 1μ익 공극의 적어도 10용적%는 공극 직경이 약 1 내지 10μ이며 공극의 적어도 20용적%는 공극 용적이 약 10 내지 100μ이고 불활성이 내화성 고체 지지체에 함침되는, 촉매를 기준으로 적어도 25중량%의 은을 함유하는 알켄의 증기상 에폭시화에 의한 알킬렌 옥사이드 제조용 촉매.
  70. 제62항에 있어서, 담체가 α-알루미나를 포함하는 촉매.
  71. 제63항에 있어서, 중간크기 공극의 직경이 약 1 내지 25μ인 촉매.
  72. 제64항에 있어서, 촉매효율울 증진시키기 위한 적어도 하나의 촉진제를 함유하는 촉매.
  73. 제64항에 있어서, 적어도 하나의 촉진제가 음이온성 촉진제를 포함하는 촉매.
  74. 제66항에 있어서, 음이온성 촉진제가 산소를 제외한 원자번호가 7 내지 83이고 원소주기율표의 3b 내지 7b족 또는 3a 내지 7a족에서 선택되는 원소의 할라이드 및 또는 산소음이온중을 포함하는 촉매.
  75. 제67항에 있어서, 양이온성 촉진제가 알칼리금속 및 알칼리토금속중 적어도 하나를 포함하는 촉매.
  76. 제68항에 있어서, 양이온성 촉진제가 세슘, 루비듐 및 칼륨중 적어도 하나를 포함하는 촉매.
  77. 제69항에 있어서, 중간 크기 공극의 직경 및 공극 분포가, 촉매가 표준에틸렌 옥사이드 공정조건하 2.0%σ 에틸렌 옥사이드에서 약 12 내지 15중량%의 은을 함유하는 것을 제외하고는 동일한 다른 촉매에 의해 유사한 조건하에서 나타나는 것보다 비교적 더 큰 효율 및 낮은 온도를 나타내는 촉매.
  78. 제70항에 있어서, 중간 크기 공극의 직경 및 공극 분포가, 촉매가 표준에틸렌 옥사이드 공정조건하 2.0%σ 에틸렌 옥사이드에서 약 12 내지 15중량%의 은을 함유하는 것을 제외하고는 동일한 다른 촉매에 의해 유사한 조건하에서 나타나는 것보다 비교적 더 큰 효율 및 낮은 온도를 나타내는 촉매.
  79. 에틸렌 및 산소를 에틸렌, 산소 및 가스상 억제제를 함유하는 스트림이 에틸렌 옥사이드 생성조건하에 제64항에 따른 촉매의 고정층에 공급되고 에틸렌 옥사이드가 촉매 고정층으로부터의 유출물중에 제공되는 증기상으로 반응시키므로써 에틸렌 옥사이드를 제조하는 방법.
  80. ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.
KR1019900016607A 1989-10-18 1990-10-17 은 함량이 높은 알킬렌 옥사이드 촉매 KR960012093B1 (ko)

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US556828 1990-07-23
US07/556,828 US5187140A (en) 1989-10-18 1990-07-23 Alkylene oxide catalysts containing high silver content
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ATE176907T1 (de) 1999-03-15
AU5036793A (en) 1994-01-13
CN1060839A (zh) 1992-05-06
US5187140A (en) 1993-02-16
DE69032957T2 (de) 1999-08-12
DE69032957T4 (de) 1999-10-21
JP3030512B2 (ja) 2000-04-10
JPH03207447A (ja) 1991-09-10

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