KR970706066A - 비균질 촉매(heterogeneous catalysts) - Google Patents

비균질 촉매(heterogeneous catalysts)

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Publication number
KR970706066A
KR970706066A KR1019970701861A KR19970701861A KR970706066A KR 970706066 A KR970706066 A KR 970706066A KR 1019970701861 A KR1019970701861 A KR 1019970701861A KR 19970701861 A KR19970701861 A KR 19970701861A KR 970706066 A KR970706066 A KR 970706066A
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sol
hydrolysis
titanium
alkoxylated
silicon
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KR1019970701861A
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KR100391533B1 (ko
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알폰스 바이케르
도미니크 두토이트
레모 후테르
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클라우스너 프리돌린, 보러 롤란드
에프 호프만-라 롯슈 아크티엔게젤샤프트
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D263/00—Heterocyclic compounds containing 1,3-oxazole or hydrogenated 1,3-oxazole rings
    • C07D263/52—Heterocyclic compounds containing 1,3-oxazole or hydrogenated 1,3-oxazole rings condensed with carbocyclic rings or ring systems
    • C07D263/54—Benzoxazoles; Hydrogenated benzoxazoles
    • C07D263/56—Benzoxazoles; Hydrogenated benzoxazoles with only hydrogen atoms, hydrocarbon or substituted hydrocarbon radicals, directly attached in position 2
    • C07D263/57—Aryl or substituted aryl radicals
    • 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
    • C07D301/19—Synthesis of the oxirane ring by oxidation of unsaturated compounds, or of mixtures of unsaturated and saturated compounds with organic hydroperoxides
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00—Medicinal preparations containing organic active ingredients
    • A61K31/33—Heterocyclic compounds
    • 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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063—Titanium; Oxides or hydroxides thereof
    • 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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/08—Silica
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/03—Precipitation; Co-precipitation
    • B01J37/031—Precipitation
    • B01J37/033—Using Hydrolysis
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/03—Precipitation; Co-precipitation
    • B01J37/036—Precipitation; Co-precipitation to form a gel or a cogel
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D277/00—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings
    • C07D277/60—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings condensed with carbocyclic rings or ring systems
    • C07D277/62—Benzothiazoles
    • C07D277/64—Benzothiazoles with only hydrocarbon or substituted hydrocarbon radicals attached in position 2
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
    • C07D303/02—Compounds containing oxirane rings
    • C07D303/04—Compounds containing oxirane rings containing only hydrogen and carbon atoms in addition to the ring oxygen atoms

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
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  • Life Sciences & Earth Sciences (AREA)
  • Pharmacology & Pharmacy (AREA)
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  • Medicinal Chemistry (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Catalysts (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Silicon Compounds (AREA)
  • Epoxy Compounds (AREA)

Abstract

본 발명은 선택적으로 예비가수분해된 알콕시화규소 및 알콕시화티탄(이의 가수분해능은 킬레이트 형성에 의해 감소된다)으로부터 산성 또는 염기성 가수분해 조건하에서 줄을 제조하고, 이 졸을 겔화하고 시효시키고, 이렇게 제조된 시효된 겔을 졸의 제조시 사용된 용매 및 가수분해시 생성된 알콜을 초임계 이산화탄소로 추출함으로써 건조시키고, 필요한 경우, 상기로부터 생성되는 에어로겔을 산소를 함유하는 기체 스트림에서 1000℃이하의 온도에서 하소함으로써 제조가능한 실리카-티타니아 혼합된 산화물 촉매에 관한 것이다. 이러한 촉매는 특히 올레핀성 불포화 화합물의 유기 하이드로퍼옥시드와의 에폭시화를 촉매하는데 사용될 수 있다.

Description

비균질 촉매(HETEROGENEOUS CATALYSTS)
본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음

Claims (12)

  1. 선택적으로 예비가수분해된 알콕시화규소 및 알콕시화티탄(이의 가수분해능은 킬레이트 형성에 의해 감소된다)으로부터 산성 또는 염기성 가수분해 조건하에서 졸을 제조하고, 이 졸을 겔화하고 시효시키고, 이렇게 제조된 시효된 겔을 졸의 제조시 사용된 용매 및 가수분해시 생성된 알콜을 초임계 이산화탄소로 추출함으로써 건조시키고, 필요한 경우, 상기로부터 생성되는 에어로겔을 산소를 함유하는 기체 스트럼에서 1000℃ 이하의 온도에서 하소함으로써 제조가능한 실리카-티타니아 혼합된 산화물 촉매.
  2. 제1항에 있어서, 알콕시화규소가 화학식 Si(OR2)4(여기서, R2는 각각 C1-4알킬이다)의 화합물, 바람직하게는 테트라메톡시실란인 촉매.
  3. 제1항 또는 제2항에 있어서, 가수분해능이 킬레이트 형성에 의해 감소되는 알콕시화티탄이 화학식 Ti(OR1)4(여기서, R2는 각각 C1-4알킬이다)의 화합물, 바람직하게는 테트라이소프로필 오르토티타네이트이며, 리간드로서 아세틸아세톤을 갖는 촉매.
  4. 제1항 내지 제3항 중 어느 한 항에 있어서, 졸이 산성 가수분해 조건하에서 제조되고, 염산이 이러한 목적을 위한 산으로서 사용되는 촉매.
  5. 제1항 내지 제4항 중 어느 한 항에 있어서, 가수분해 매질 및 결과적으로 생성되는 졸에서 규소 : 티탄의 몰 비가 약 1 : 1 내지 약 70 : 1, 바람직하게는 약 3: 1 내지 약 12 : 1의 범위인 촉매.
  6. 제1항 내지 제5항 중 어느 한 항에 있어서, 알콕시화규소 및 알콕시화티탄(이의 가수분해능은 킬레이트 형성에 의해 감소된다)의 가수분해시 용매로서 물외에 이소프로판올이 사용되는 촉매.
  7. 제1항 내지 제6항 중 어느 한 항에 있어서, 무수 불활성 기체, 바람직하게는 질소에 졸을 노출시킴으로써 겔화 및 시효가 수행되는 촉매.
  8. 제1항 내지 제7항 중 어느 한 항에 있어서, 약 31 내지 약 5O℃ 범위의 온도 및 약 200 내지 약 270바아 범위의 압력에서, 졸의 생성시 사용된 용매 및 가수분해시 생성된 알콜을 초임계 이산화탄소로 추출함으로써 시효된 겔의 건조가 수행되는 촉매.
  9. 제1항 내지 제8항 중 어느 한 항에 있어서, 산소 함량이 15 내지 25부피%인 산소-함유 기체 스트림에 의해 에어로겔이 하소되는 촉매.
  10. 표면에서 티탄: 규소 원자 비가 약 1 : 19 내지 약 3:7인 것외에, 가능한 한 원자끼리 각각이 산소 원자를 통해 가교되어 있는 규소 및 티탄 성분의 혼합을 갖고, BET(Brunauer-Emmett-Teller) 표면적이 약 500 내지 약 800㎡/g이고, 기공도가 약 2 내지 약 6Onm인 실리카-티타니아 혼합된 산화물 촉매.
  11. 선택적으로 예비가수분해된 알콕시화규소 및 알콕시화티탄(이의 가수분해능은 킬레이트 형성에 의해 감소된다)으로부터 산성 또는 염기성 가수분해 조건하에서 졸을 제조하고, 이 졸을 겔화하고 시효시키고, 이렇게 제조된 시효된 겔을 졸의 제조시 사용된 용매 및 가수분해시 생성된 알콜을 초임계 이산화탄소로 추출함으로써 건조시키고, 필요한 경우, 상기로부터 생성되는 에어로겔을 산소를 함유하는 기체 스트림에서 1000℃ 이하의 온도에서 하소하는 것을 포함하는, 실리카-티타니아 혼합된 산화물 촉매의 제조 방법.
  12. 유기 하이드로퍼옥시드와의 촉매 반응에 의한 올레핀성 불포화 화합물의 에폭시화를 위한 액상 공정에서의,제1항 내지 제1O항 중 어느 한 항에 따른 촉매의 용도.
    ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.
KR10-1997-0701861A 1994-09-22 1995-09-08 비균질촉매 KR100391533B1 (ko)

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CH2882/94-6 1994-09-22
CH288294 1994-09-22

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KR100391533B1 KR100391533B1 (ko) 2003-10-17

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US (1) US5935895A (ko)
EP (1) EP0783371B1 (ko)
JP (1) JP3843126B2 (ko)
KR (1) KR100391533B1 (ko)
CN (1) CN1070730C (ko)
AT (1) ATE167641T1 (ko)
DE (1) DE69503142T2 (ko)
DK (1) DK0783371T3 (ko)
ES (1) ES2119473T3 (ko)
WO (1) WO1996009117A1 (ko)

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EP0783371A1 (en) 1997-07-16
WO1996009117A1 (en) 1996-03-28
JPH10505785A (ja) 1998-06-09
CN1158578A (zh) 1997-09-03
EP0783371B1 (en) 1998-06-24
ES2119473T3 (es) 1998-10-01
DE69503142D1 (de) 1998-07-30
CN1070730C (zh) 2001-09-12
DE69503142T2 (de) 1998-11-05
US5935895A (en) 1999-08-10
DK0783371T3 (da) 1999-04-06
KR100391533B1 (ko) 2003-10-17
ATE167641T1 (de) 1998-07-15

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