Preparation method of acetylacetonatocarbonyltriphenylphosphine rhodium, and olefin hydroformylation method

A technology of acetone triphenylphosphine and acetone dicarbonyl rhodium is applied in a field of preparation and olefin hydroformylation, can solve the problems of low catalytic activity, decreased catalytic activity and the like, and achieves the effect of solving low yield

Active Publication Date: 2014-04-09
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0009] The purpose of the present invention is to overcome the problem that the existing triphenylphosphinecarbonyl rhodium acetylacetonate catalyst is used for the hydroformylation reaction of propylene and synthesis gas with low catalytic activity or obvious decline in catalytic activity, and to provide a catalyst with high catalytic activity The method for rhodium acetylacetonate triphenylphosphinecarbonyl, in addition also provides a method for olefin hydroformylation containing the preparation method of triphenylphosphinecarbonylrhodium acetylacetonate

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  • Preparation method of acetylacetonatocarbonyltriphenylphosphine rhodium, and olefin hydroformylation method
  • Preparation method of acetylacetonatocarbonyltriphenylphosphine rhodium, and olefin hydroformylation method
  • Preparation method of acetylacetonatocarbonyltriphenylphosphine rhodium, and olefin hydroformylation method

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preparation example Construction

[0022] The invention provides a kind of preparation method of triphenylphosphine carbonyl rhodium acetylacetonate, it is characterized in that, the method comprises:

[0023] (1) Under the conditions of the precipitation reaction, the rhodium trichloride aqueous solution is contacted with the precipitating agent, so that the rhodium element is precipitated, and the precipitation of the rhodium-containing element is obtained;

[0024](2) Washing the precipitate containing rhodium elements until the chloride ion content in the precipitate containing rhodium elements is lower than 1000ppm;

[0025] (3) Under the conditions of the reaction for synthesizing rhodium dicarbonyl acetylacetonate, dissolving the precipitation of the rhodium-containing element obtained in step (2) and then contacting acetylacetone to obtain a reaction solution containing rhodium dicarbonyl acetylacetonate;

[0026] (4) Under the conditions of the reaction for synthesizing rhodium acetylacetonate tripheny...

Embodiment 1

[0072] This example is used to illustrate the preparation method of triphenylphosphinecarbonylrhodium acetylacetonate provided by the present invention.

[0073] (1) Precipitation reaction: In a 1500ml beaker, add 250.00ml of rhodium trichloride aqueous solution with a Rh concentration of 1.000mol / L, under magnetic stirring, control the reaction temperature at 10°C, and drop NaOH with a concentration of 1.00mol / L About 750ml of solution, monitoring solution pH value change, stops dropwise when solution pH value=8.0, obtains the reaction solution that contains rhodium hydroxide precipitation.

[0074] (2) Washing the precipitate: filter the reaction solution containing the rhodium hydroxide precipitate under reduced pressure to separate the rhodium hydroxide precipitate. Wash three times with deionized water at a temperature of 10°C, and finally wash once with 10°C cyclohexane. After vacuum drying at 25°C, a yellow rhodium hydroxide precipitate was obtained. The content of ch...

Embodiment 2

[0082] This example is used to illustrate the preparation method of triphenylphosphinecarbonylrhodium acetylacetonate provided by the present invention.

[0083] (1) Precipitation reaction: In a 1000ml beaker, add 150.0ml of rhodium trichloride aqueous solution with a Rh concentration of 2.000mol / L. Under magnetic stirring, control the reaction temperature to be 7°C, add about 300ml of KOH solution with a concentration of 3.00mol / L dropwise, monitor the change in pH value of the solution, stop the dropwise addition when the pH value of the solution=7.0, and obtain a precipitate containing rhodium hydroxide reaction solution.

[0084] (2) Washing the precipitate: filter the reaction solution containing the rhodium hydroxide precipitate under reduced pressure to separate the rhodium hydroxide precipitate. Wash three times with deionized water at 8°C, and finally wash once with 7°C cyclohexane. After vacuum drying at 25°C, the resulting yellow rhodium hydroxide precipitates. T...

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Abstract

The invention discloses a preparation method of acetylacetonatocarbonyltriphenylphosphine rhodium. The preparation method comprises following steps: (1) under precipitation reaction conditions, a rhodium trichloride aqueous solution is contacted with a precipitating agent so as to precipitate rhodium and obtain a sediment containing rhodium; (2) the sediment containing rhodium is washed until chloride ion content is less than 1000ppm; (3) under acetylacetonato dicarbonylrhodium synthesis conditions, the sediment containing rhodium, which is obtained in step (2), is dissolved, and is contacted with acetylacetone so as to obtain a reaction liquid containing acetylacetonato dicarbonylrhodium; and (4) under acetylacetonatocarbonyltriphenylphosphine rhodium synthesis conditions, acetylacetonatocarbonyltriphenylphosphine rhodium in the reaction liquid is contacted with triphenylphosphine. The invention also discloses an olefin hydroformylation method. The preparation method of acetylacetonatocarbonyltriphenylphosphine rhodium is capable of reducing chloride ion content of products, increasing product synthesis yield, and improving catalytic activity of acetylacetonatocarbonyltriphenylphosphine rhodium.

Description

technical field [0001] The invention relates to a preparation method of triphenylphosphine carbonyl rhodium acetylacetonate and a method for olefin hydroformylation, in particular to a method of using rhodium trichloride hydrate as a raw material to prepare acetylacetonate by forming a precipitation of rhodium-containing elements. A method for acetone triphenylphosphinecarbonylrhodium, and a method for hydroformylation of olefins and synthesis gas comprising the preparation method of acetylacetonate triphenylphosphinecarbonylrhodium. Background technique [0002] Triphenylphosphinecarbonyl rhodium acetylacetonate (Rh(acac)(PPh 3 )(CO)) is α-olefin and syngas (CO and H 2 A good catalyst precursor for the hydroformylation reaction to generate normal and isomeric aldehydes. For example, propylene and syngas in Rh(acac)(PPh 3 ) (CO) in the presence of a homogeneous catalyst precursor to generate n-butyraldehyde and isobutyraldehyde; in addition, it can also be used for methan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F19/00C07C47/02C07C45/50
Inventor 吕顺丰刘博秦燕璜李彤王世亮
Owner CHINA PETROLEUM & CHEM CORP
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