Preparation method of acetylacetonato dicarbonylrhodium, and olefin hydroformylation method

A technology of acetone dicarbonyl rhodium and acetyl is applied in the field of hydroformylation reaction of olefin and synthesis gas, and can solve problems such as poor catalytic activity and the like

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

[0007] The purpose of the invention is to overcome the existing poor catalytic activity of rhodium acetylacetonate and improve the yield of rhodium acetylacetonate, and provide a method for preparing rhodium acetylacetonate with high catalytic activity and high yield, Also provide a kind of method that contains the olefin hydroformylation of this acetylacetonate rhodium dicarbonyl preparation method in addition

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  • Preparation method of acetylacetonato dicarbonylrhodium, and olefin hydroformylation method
  • Preparation method of acetylacetonato dicarbonylrhodium, and olefin hydroformylation method
  • Preparation method of acetylacetonato dicarbonylrhodium, and olefin hydroformylation method

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preparation example Construction

[0019] The invention provides a kind of preparation method of rhodium acetylacetonate dicarbonyl, it is characterized in that, the method comprises:

[0020] (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;

[0021] (2) Washing the precipitate containing rhodium elements until the chloride ion content in the precipitate containing rhodium elements is lower than 1000ppm;

[0022] (3) Under the conditions of the reaction for synthesizing rhodium dicarbonyl acetylacetonate, the precipitation of the rhodium-containing element obtained in step (2) is dissolved and then contacted with acetylacetone.

[0023] According to the present invention, in the preparation method of rhodium acetylacetonate dicarbonyl, step (1) is used to precipitate rhodium trichloride hydrate into a precipit...

Embodiment 1

[0059] This embodiment is used to illustrate the preparation method of rhodium acetylacetonate dicarbonyl provided by the present invention.

[0060] (1) Precipitation reaction: In a 1500ml beaker, add 250.0ml 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 The solution is about 750ml, monitor the change of the pH value of the solution, and stop dropping when the pH value of the solution=8.0. A reaction solution containing precipitated rhodium hydroxide was obtained.

[0061] (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. ...

Embodiment 2

[0067] This embodiment is used to illustrate the preparation method of rhodium acetylacetonate dicarbonyl provided by the present invention.

[0068] (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 at 7°C, add about 300ml of KOH solution with a concentration of 3.00mol / L dropwise, monitor the change of the pH value of the solution, and stop the dropwise addition when the pH value of the solution is 7.0. A reaction solution containing precipitated rhodium hydroxide was obtained.

[0069] (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 cyclohexane at 7°C. After vacuum drying at 25°C, a yellow rhodium hydroxide precipitate was obtained. ...

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Abstract

The invention discloses a preparation method of acetylacetonato dicarbonylrhodium. 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; and (3) under acetylacetonato dicarbonylrhodium synthesis conditions, the sediment containing rhodium, which is obtained in step (2), is dissolved, and is contacted with acetylacetone. The invention also discloses an olefin hydroformylation method. The preparation method of acetylacetonato dicarbonylrhodium is capable of reducing chloride ion content of products, increasing product synthesis yield, and improving catalytic activity of acetylacetonato dicarbonylrhodium.

Description

technical field [0001] The invention relates to a method for preparing rhodium dicarbonyl acetylacetonate and a method for hydroformylation of olefins, in particular to a method of using rhodium trichloride hydrate as a raw material to prepare rhodium dicarbonyl acetylacetonate through precipitation of rhodium-containing elements The method, and the method for carrying out the hydroformylation reaction of olefins and synthesis gas comprising the preparation method of rhodium acetylacetonate dicarbonyl. Background technique [0002] Rhodium dicarbonyl acetylacetonate (Rh(CO) 2 (acac)) is the combination of α-olefins 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(CO) 2 (acac) n-butyraldehyde and isobutyraldehyde are produced in the presence of a homogeneous catalyst precursor. [0003] "Simple method of preparing acetylacetonate dicarbonyl rhodium (I)" (Ru...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00B01J31/24C07C45/50C07C47/02
Inventor 吕顺丰李彤王世亮刘博秦燕璜
Owner CHINA PETROLEUM & CHEM CORP
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