Preparation method of acetylacetonatodicarbonyl rhodium

A technology of rhodium dicarbonyl acetone and acetylacetone, which is applied in the field of rhodium dicarbonyl acetylacetonate synthesis, can solve the problems of many steps, low yield, and low synthesis yield of rhodium dicarbonyl acetylacetonate, etc., and achieve great economic benefits Effect

Active Publication Date: 2012-03-14
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods either have many steps or low yields, and are judged as inapplicable methods
[0009] In a word, in the prior art, the synthesis yield of rhodium acetylacetonate dicarbonyl is not very high, especially when it is used as a large-scale preparation method, there is still a need for further improvement

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add a small amount of deionized water to dimethylformamide to make the water content reach 0.5% (mass percentage).

[0024] To 5.00 g of rhodium trichloride trihydrate, add 100 ml of the above-mentioned dimethylformamide for controlling the water content. With stirring, first raise the temperature to 140°C to dissolve all the rhodium trichloride trihydrate, then raise the temperature and control the temperature at 148±2°C. When the color of the solution changed from deep red to orange red, add 25ml of acetylacetone. After the addition, time the reaction time for a total of 1 hour. Stop heating and mix to cool down to 40°C naturally. The reaction mixture was poured into deionized water, and the ratio of the amount of deionized water to the amount of the reaction mixture was 6:1 (volume ratio). Immediately after pouring, a red precipitate was produced, which was allowed to stand for 8 hours after stirring slightly. Afterwards, it was filtered, dried, and recrystallized ...

Embodiment 2

[0030] According to the step of embodiment 1, just change the ratio of reaction mixture and water addition, obtain different yield results and list the following table:

[0031] Amount of water added: reaction mixture (volume ratio)

[0032] The data in the table shows that the amount of water added affects the product yield. Best results were obtained with the ligand at 6:1.

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Abstract

The invention discloses a preparation method of acetylacetonatodicarbonyl rhodium. The method comprises the following steps: (1) adding a defined amount of water in dimethylformamide; (2) dissolving trihydrate rhodium chloride in dimethylformamide, refluxing; adding acetylacetone in the mixture, refluxing again; (4) stopping heating to ensure that the reaction mixture is naturally cooled, pouring the mixture in deionized water, stirring; and (5) filtering the mixture, drying and recrystallizing. Compared with the prior art, the yield of rhodium can be increased to 95%, which brings a lot of economic benefit.

Description

technical field [0001] The present invention relates to a kind of synthetic method of noble metal organic compound, specifically a kind of synthetic method of rhodium acetylacetonate dicarbonyl. Background technique [0002] Rhodium dicarbonyl acetylacetonate (Rh(CO) 2 C 5 h 7 o 2 ) are often used as catalysts in organic synthesis reactions. For example, catalysts for the hydroformylation of olefins. Because the natural resources of metal rhodium are rare and expensive, the preparation method of rhodium compound has always been paid attention to. The method innovation or the improvement of the original method aims to improve the old yield or simplify the preparation steps to achieve the purpose of improving efficiency. [0003] The preparation method of rhodium dicarbonyl acetylacetonate was first published in J.Chem.Soc., 3156,1964. In the method, dirhodium dichlorotetracarbonyl and acetylacetone are used as raw materials, petroleum ether is used as a solvent, sodium ...

Claims

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Application Information

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IPC IPC(8): C07F15/00
Inventor 王红红郭浩然王蕴林
Owner CHINA PETROLEUM & CHEM CORP
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