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A kind of preparation method of acetylacetonate bifefors rhodium catalyst

A technology of acetylacetone and rhodium catalysts, which is applied in the direction of carbon monoxide reaction preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems such as the complicated process of water-soluble hexachlororhodium salt, and achieve the effect of high catalytic activity

Active Publication Date: 2017-11-03
TIANJIN BOHUA YONGLI CHEM IND
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process does not produce water-soluble rhodium trichloride in the end
And it is more complicated in the process of preparing water-soluble hexachlororhodium

Method used

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  • A kind of preparation method of acetylacetonate bifefors rhodium catalyst
  • A kind of preparation method of acetylacetonate bifefors rhodium catalyst

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Effect test

preparation example Construction

[0019] The preparation method of the rhodium acetylacetonate bifivers catalyst of the present invention includes the following steps:

[0020] (1) Pass chlorine gas into the tube furnace as the protective gas, and put the rhodium powder and sodium chloride powder with a mass ratio of 4:1 into the tube furnace and heat it to 400-1000°C for reaction, heating for 60 -Get soluble rhodium salt after 120 minutes;

[0021] (2) Dissolve the soluble rhodium salt in water to form a rhodium salt solution, recover the unreacted rhodium powder in the rhodium salt solution, then add a precipitation agent to the rhodium salt solution to completely precipitate the rhodium ions in the solution, and then deposit the rhodium precipitate Filter and wash to separate the rhodium precipitate from chloride and sodium ions;

[0022] (3) Adding an organic acid to the rhodium precipitate to completely dissolve the rhodium precipitate to obtain an organic rhodium solution, thereby preventing the prepared produ...

Embodiment 1

[0036] (1) Pass chlorine gas into the tube furnace as a protective gas, and put 4g of rhodium powder and 1g of sodium chloride powder into the tube furnace and heat to 400°C for reaction, and obtain soluble rhodium salt after heating for 60 minutes;

[0037] (2) Dissolve the soluble rhodium salt in water to form a rhodium salt solution, recover the unreacted rhodium powder in the rhodium salt solution, then add sodium hydroxide to the rhodium salt solution to completely precipitate the rhodium ions in the solution, and then precipitate the rhodium Filtration and washing to separate the rhodium precipitate from chloride and sodium ions;

[0038] (3) Adding formic acid to the rhodium precipitate to completely dissolve the rhodium precipitate to obtain a rhodium solution, thereby preventing the prepared product from containing chloride ions;

[0039] (4) Mix the rhodium solution with N,N-dimethylformamide (DMF) to form a mixed solution. Under the protection of nitrogen, heat to 120°C an...

Embodiment 2

[0045] (1) Pass chlorine gas into the tube furnace as a protective gas, and put 6g rhodium powder and 1.5g sodium chloride powder into the tube furnace and heat to 700°C for reaction. After heating for 100 minutes, a soluble rhodium salt is obtained. ;

[0046] (2) Dissolve the soluble rhodium salt in water to form a rhodium salt solution, recover the unreacted rhodium powder in the rhodium salt solution, then add potassium hydroxide to the rhodium salt solution to completely precipitate the rhodium ions in the solution, and then precipitate the rhodium Filtration and washing to separate the rhodium precipitate from chloride and sodium ions;

[0047] (3) Adding acetic acid to the rhodium precipitate to completely dissolve the rhodium precipitate to obtain a rhodium solution, thereby preventing the prepared product from containing chloride ions;

[0048] (4) Mix the rhodium solution with N,N-dimethylformamide (DMF) to form a mixed solution. Under the protection of nitrogen, heat to 1...

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Abstract

The invention discloses a preparation method of an acetylacetonate bifefos rhodium catalyst, comprising the following steps: (1) placing rhodium powder and sodium chloride powder in a tubular furnace for heating and reaction to obtain a soluble rhodium salt; (2) Dissolving the soluble rhodium salt in water to form a rhodium salt solution, recovering unreacted rhodium powder in the rhodium salt solution, then adding a precipitant to the rhodium salt solution to completely precipitate the rhodium ions in the solution, then filtering and washing the rhodium precipitate (3) prepare organic rhodium solution, acetylacetonate dicarbonyl rhodium and acetylacetonate bifefos rhodium successively. The catalytic activity of the metal rhodium catalyst prepared by the method is higher than 80%, and the positive-to-iso ratio of the product is above 15.

Description

Technical field [0001] The invention relates to a preparation process and application of a rhodium acetylacetonate bifivers catalyst. Background technique [0002] The rhodium acetylacetonate bififurs catalyst is aimed at olefins and syngas (CO and H 2 The mixed gas), a good catalyst for hydroformylation to generate normal aldehydes and iso-aldehydes. For example, butene and synthesis gas are catalyzed by the acetylacetone bifivers rhodium homogeneous catalyst to produce valeraldehyde, and ethylene and synthesis gas are catalyzed by the acetylacetone bifivers rhodium homogeneous catalyst to produce propionaldehyde. The catalytic activity of the rhodium bifurcation catalyst is far better than that of the traditional acetylacetonate triphenylphosphorhodium. It has a more obvious effect on C4 (mixed butene) after ether. It also uses mixed butene to prepare 2- The best carbonylation catalyst for PH. [0003] Rhodium is a relatively rare noble metal. The key technology for preparing r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C07C47/02C07C45/50
Inventor 李亚斌侯强安继民郭东升李治水张思学宁宇
Owner TIANJIN BOHUA YONGLI CHEM IND