KR950011451A - 하이드리도 카르보닐트리스(트리오가노포스포러스)로듐의 제조방법 - Google Patents

하이드리도 카르보닐트리스(트리오가노포스포러스)로듐의 제조방법 Download PDF

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KR950011451A
KR950011451A KR1019930022084A KR930022084A KR950011451A KR 950011451 A KR950011451 A KR 950011451A KR 1019930022084 A KR1019930022084 A KR 1019930022084A KR 930022084 A KR930022084 A KR 930022084A KR 950011451 A KR950011451 A KR 950011451A
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rhodium
triorganophosphorus
carbon monoxide
distillation residue
compound
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KR0134494B1 (ko
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이상무
최정욱
정승문
김진도
이기혁
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최근선
주식회사 럭키
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Priority to US08/245,659 priority patent/US5414101A/en
Priority to DE69418418T priority patent/DE69418418T2/de
Priority to EP94116502A priority patent/EP0649851B1/en
Priority to JP6254066A priority patent/JP2588374B2/ja
Publication of KR950011451A publication Critical patent/KR950011451A/ko
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    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J31/00Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/16Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
    • B01J31/18Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
    • B01J31/1845Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms the ligands containing phosphorus
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    • B01J31/16Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
    • B01J31/18Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
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    • B01J31/16Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
    • B01J31/24Phosphines, i.e. phosphorus bonded to only carbon atoms, or to both carbon and hydrogen atoms, including e.g. sp2-hybridised phosphorus compounds such as phosphabenzene, phosphole or anionic phospholide ligands
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    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B01J31/00Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/40Regeneration or reactivation
    • B01J31/4015Regeneration or reactivation of catalysts containing metals
    • B01J31/4023Regeneration or reactivation of catalysts containing metals containing iron group metals, noble metals or copper
    • B01J31/4038Regeneration or reactivation of catalysts containing metals containing iron group metals, noble metals or copper containing noble metals
    • B01J31/4046Regeneration or reactivation of catalysts containing metals containing iron group metals, noble metals or copper containing noble metals containing rhodium
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/49Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reaction with carbon monoxide
    • C07C45/50Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reaction with carbon monoxide by oxo-reactions
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    • C07F15/0073Rhodium compounds
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    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
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Abstract

하이드로포르밀화반응 증류잔류물에 함유되어 있는 로듐화합물을 출발물질로 하여 하이드리도카르보닐트리스(트리오가노포스포러스)로듐을 제조함에 있어서, 비활성화된 로듐촉매화합물 함유 증류잔류물을 산화제로 처리한 후 일산화탄소와 산소의 혼합기체존재하에서 로듐-카르보닐화합물로 전환시키고 이들 반응액으로부터 단리함이 없이 직접 수산기 함유화합물, 알칼리금속 하이드록사이드, 포름알데히드, 트리오가노포스포러스 리간드와 반응시키고 일산화탄소와 수소로 후처리함으로서 고수율로 하이드리도카르보닐트리스(트리오가노포스포러스) 로듐을 합성하는 유기단일상 반응임을 특징으로 하는 제조방법.

Description

하이드리도 카르보닐트리스(트리오가노포스포러스)로듐의 제조방법
본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음

Claims (15)

  1. 하이드로포르밀화반응 증류잔류물에 함유되어있는 로듐화함물을 출발물질로하여 하이드리도카르보닐트리스(트리오가노포스포러스)로듐을 제조함에 있어서, 비활성화된 로듐촉매화합물함유 증류잔류물을 산화제로 처리한 후 일산화탄소와 산소의 혼합기 체존재하에서 로듐-카르보닐화합물로 전환시키고 이를 반응액으로부터 단리함이없이 직접 수산기 함유화합물, 알카리금속 하이드록사이드, 포름알데히드, 트리오가노포스포러스 리간드와 반응시키고 일산화탄소와 수소로 후처리함으로서 고수율로 하이드리도카르보닐트리스(트리오가노포스포러스)로듐을 합성하는 유기단일상 반응임을 특징으로 하는 제조방법.
  2. 제1항에 있어서, 산화제는 산소 또는 공기이며, 처리온도 및 압력이 60-120℃, 1-10기압임을 특징으로하는 제조방법.
  3. 제1항에 있어서, 증류잔류물중 로듐농도는 1500-30000ppm임을 특징으로하는 제조방법.
  4. 제1항에 있어서, 로듐-카르보닐화합물로 전환시 일산화탄소와 산소의 분압비를 5:1-30:1로하고 총압력을 10-100기압으로하여 반응시킴을 특징으로 하는 제조방법.
  5. 제2항에 있어서, 로듐-카르보닐화합물로 전환시의 반응은도는 80-120℃임을 특징으로 하는 제조방법.
  6. 제1항에 있어서, 수산기 함유화합물이 에탄올임을 특징으로하는 제조방법.
  7. 제6항에 있어서, 사용되는 수산기 함유화합물의 양이 사용되는 증류잔류물양의 1-10중량배임을 특징으로하는 제조방법.
  8. 제1항에 있어서, 알카리금속 하이드록사이드가 포타슘 하이드록사이드임을 특징으로 하는 제조방법.
  9. 제8항에 있어서, 알카리금속 하이드록사이드를 로듐몰수에 4-20몰배 사용함을 특징으로 하는 제조방법.
  10. 제1항에 있어서, 포름알데히드는 물이 거의 함유되지않은 메탄올 : 포름알데히드의 중량비가 5 : 1-1 : 1인 혼합물을 사용하고 증류잔류물의 0.1-10중량% 사용함을 특징으로 하는 제조방법.
  11. 제1항에 있어서, 트리오가노포스포러스 리간드는 트리페닐포스핀, 트리페닐포스파이트임을 특징으로 하는 제조방법.
  12. 제11항에 있어서, 사용되는 트리오가노포스포러스 리간드의 양은 로듐몰수에 4-20몰배 사용함을 특징으로하는 제조방법.
  13. 제1항에 있어서, 후처리시 일산화탄소처리후에 수소를 처리함을 특징으로 하는 제조방법.
  14. 제13항에 있어서, 일산화탄소처리시 온도 및 압력이 55-70℃, 1-100기압임을 특징으로 하는 제조방법.
  15. 제13항에 있어서, 수소처리시 온도 및 압력이 60-80℃, 1-100기압임을 특징으로 하는 제조방법.
    ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.
KR1019930022084A 1993-10-20 1993-10-20 하이드리도카르보닐트리스(트리오가노포스포러스)로듐의 제조방법 KR0134494B1 (ko)

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Application Number Priority Date Filing Date Title
KR1019930022084A KR0134494B1 (ko) 1993-10-20 1993-10-20 하이드리도카르보닐트리스(트리오가노포스포러스)로듐의 제조방법
US08/245,659 US5414101A (en) 1993-10-20 1994-05-18 Preparation of hydridocarbonyl tris (triorganophosphorus) rhodium compounds
DE69418418T DE69418418T2 (de) 1993-10-20 1994-10-19 Verfahren zur Herstellung einer Hydridocarbonyltris(triorganophosphor)-Rhodium-Verbindung
EP94116502A EP0649851B1 (en) 1993-10-20 1994-10-19 Process for preparation of hydridocarbonyltris (triorganophosphorus) rhodium compound
JP6254066A JP2588374B2 (ja) 1993-10-20 1994-10-20 ヒドリドカルボニルトリス(トリオガノホスホラス)ロジウム化合物の製造方法

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KR1019930022084A KR0134494B1 (ko) 1993-10-20 1993-10-20 하이드리도카르보닐트리스(트리오가노포스포러스)로듐의 제조방법

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KR0134494B1 KR0134494B1 (ko) 1998-04-20

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US (1) US5414101A (ko)
EP (1) EP0649851B1 (ko)
JP (1) JP2588374B2 (ko)
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DE (1) DE69418418T2 (ko)

Cited By (1)

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CN112892603A (zh) * 2019-12-03 2021-06-04 中国科学院大连化学物理研究所 一种用于氮甲酰化反应的固体多相催化剂及其制备和应用

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DE10048301A1 (de) * 2000-09-29 2002-04-11 Oxeno Olefinchemie Gmbh Stabilisierung von Rhodiumkatalysatoren für die Hydroformylierung von Olefinen
EP2136917B1 (en) 2007-04-18 2011-08-17 ExxonMobil Chemical Patents Inc. Improvements in oxidative demetalling
CN102382143B (zh) * 2010-08-31 2014-05-28 中国石油化工股份有限公司 一种烯烃氢甲酰化均相络合催化剂的制备方法
CN102503985B (zh) * 2011-10-25 2014-12-17 中国海洋石油总公司 一种三(三苯基膦)羰基氢铑的制备方法
EP3990176A1 (en) * 2019-06-27 2022-05-04 Dow Technology Investments LLC Process to prepare solution from hydroformylation process for precious metal recovery

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US446074A (en) * 1891-02-10 Attachment for metal-planers
JPS5850234B2 (ja) * 1980-10-23 1983-11-09 三菱化学株式会社 第8族貴金属固体錯体の取得方法
US4363764A (en) * 1980-12-30 1982-12-14 Union Carbide Corporation Preparation of rhodium complex compounds
US4446074A (en) * 1981-12-24 1984-05-01 Union Carbide Corporation Preparation of rhodium complex compounds
DE3822037A1 (de) * 1988-06-30 1990-01-04 Hoechst Ag Verfahren zur abtrennung und wiedergewinnung von rhodium aus den produkten der oxosynthese

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112892603A (zh) * 2019-12-03 2021-06-04 中国科学院大连化学物理研究所 一种用于氮甲酰化反应的固体多相催化剂及其制备和应用
CN112892603B (zh) * 2019-12-03 2022-04-12 中国科学院大连化学物理研究所 一种用于氮甲酰化反应的固体多相催化剂及其制备和应用

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JPH07252285A (ja) 1995-10-03
DE69418418D1 (de) 1999-06-17
DE69418418T2 (de) 1999-09-16
US5414101A (en) 1995-05-09
EP0649851A1 (en) 1995-04-26
KR0134494B1 (ko) 1998-04-20
JP2588374B2 (ja) 1997-03-05

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