Preparation method of rhodium catalyst

A rhodium catalyst, rhodium ethylene dimer technology, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as high risk factor, high equipment requirements, and easy-to-corrosion reactors. Achieve the effects of low equipment requirements, shortened reaction time, and reduced toxic waste gas

Active Publication Date: 2021-10-12
SUZHOU SINOCOMPOUND TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method involves high-pressure reaction conditions, which requires high equipment, and there are chloride ions in the reaction, which are easy to corrode the reactor under high-pressure conditions, and the risk factor of this process is relatively high.

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  • Preparation method of rhodium catalyst
  • Preparation method of rhodium catalyst
  • Preparation method of rhodium catalyst

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preparation example Construction

[0030] One embodiment of the present invention provides a kind of preparation method of rhodium catalyst, comprises the steps:

[0031] Introduce ethylene or diene into the aqueous solution of trivalent rhodium salt, and add zinc powder under protective atmosphere to carry out reduction reaction to obtain rhodium catalyst, which is monovalent rhodium ethylene dimer or monovalent rhodium diene diolefin Polymer.

[0032] In the process of the above-mentioned reduction reaction, the zinc powder gradually dissolves, trivalent rhodium is reduced to monovalent rhodium, and at the same time coordinates with ethylene or diene to form a water-insoluble rhodium catalyst, which is then precipitated from the reaction solution, while by-products such as zinc chloride The product is soluble in water, easy to separate, and the yield of the product is high.

[0033] The preparation method of above-mentioned rhodium catalyst adopts zinc powder to reduce trivalent rhodium salt under protective...

Embodiment 1

[0059] Example 1: Add 10.0 g of rhodium trichloride trihydrate and 150 mL of deionized water into a 250 mL three-necked flask, stir at room temperature for 30 minutes to completely dissolve the rhodium trichloride; first replace the atmosphere with argon gas three times, and then replace it with ethylene gas Three times, and ethylene gas was passed into the reaction solution at a ventilation rate of 0.5L / min; 2.4g of zinc powder was added in batches under stirring conditions at room temperature (in this invention, 25°C±5°C, the same below); the pH meter was online Check the pH value. When the pH value is 2.1, orange-red precipitation begins to appear in the reaction solution. When the pH value is 3.8, the zinc powder is added, and the color of the reaction solution gradually fades. When the pH value is 4.1, it remains unchanged within 1-2 minutes. Stop ventilation. The precipitate was filtered anaerobically, washed with weakly acidic deionized water, and dried to obtain 6.3 g ...

Embodiment 2

[0064] Example 2: Add 10.0 g of rhodium trichloride trihydrate and 150 mL of deionized water into a 250 mL three-necked flask, stir at room temperature for 30 minutes to completely dissolve the rhodium trichloride; first replace the atmosphere with argon gas three times, and then replace it with ethylene gas Three times, and ethylene gas was passed into the reaction solution at a ventilation rate of 0.5L / min; 2.7g of zinc powder was added in batches under stirring at room temperature; the pH value was detected online with a pH meter, and orange began to appear in the reaction solution when the pH value was 2.2. Red precipitation, when the pH value is 3.8, the zinc powder is added, the color of the reaction solution gradually fades, when the pH value is 4.3, it remains unchanged within 1-2 minutes, and the aeration is stopped. The precipitate was filtered anaerobically, washed with weakly acidic deionized water, and dried to obtain 6.7 g of orange-red powder.

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Abstract

The invention relates to a preparation method of a rhodium catalyst. The preparation method comprises the following steps: introducing ethylene or adding dialkene into an aqueous solution of trivalent rhodium salt, and adding zinc powder in a protective atmosphere for reduction reaction to obtain the rhodium catalyst which is a monovalent rhodium ethylene dimer or a monovalent rhodium dialkene dimer. The zinc powder is used for reducing the trivalent rhodium salt under the protective atmosphere, the rhodium catalyst of the monovalent rhodium ethylene dimer or the monovalent rhodium diene dimer is prepared through the one-pot method, the reaction time is greatly shortened, the problems that the multi-step reaction operation is tedious and the yield is reduced are solved, in addition, the zinc powder is used as the reducing agent, and generation of toxic waste gas is reduced. The preparation method is simple in process, free of high temperature and high pressure, easy to separate and capable of improving the yield and purity of the product.

Description

technical field [0001] The invention relates to the field of chemical catalysis, in particular to a preparation method of a rhodium catalyst. Background technique [0002] Catalysis is of great significance to chemical engineering. Most chemical reactions require the participation of catalysts, and the chemical reactions that require the participation of noble metals account for more than half. Especially for some high-selectivity, directional, low-temperature and low-pressure reactions, the participation of noble metals is difficult to replace. However, rhodium is very expensive, and there is very little content in the earth's crust, and the cost of rhodium catalysts is very high. As an important catalytic material, rhodium catalyst is widely used in the fields of petrochemical, pharmaceutical, fine chemical and environmental protection, especially in the field of asymmetric catalysis. It can be widely used in many chemical and pharmaceutical intermediates under the action...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J37/16B01J37/30C07F15/00
CPCB01J31/2291B01J31/2213B01J31/2295B01J37/16B01J37/30C07F15/0073B01J2531/822B01J2531/0225B01J2531/0238
Inventor 孙明明朱志伟郑晟敏
Owner SUZHOU SINOCOMPOUND TECH
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