Preparation method of rhodium-ruthenium composite catalyst for preparing ethyl alcohol through acetic acid hydrogenation

A composite catalyst, a technology for hydrogen preparation, applied in catalyst activation/preparation, preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of low conversion rate and selectivity, and achieve high conversion rate and selectivity of ethanol. Good effect and simple preparation process

Inactive Publication Date: 2017-02-22
ZHONGRONG TECH CORP LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The present invention aims at the problem that the catalyst prepared in the prior art is applied to the hydrogenation of acetic acid to prepare ethanol and has low conversion rate and selectivity, and provides a novel rhodium-ruthenium composite catalyst and a preparation method thereof

Method used

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  • Preparation method of rhodium-ruthenium composite catalyst for preparing ethyl alcohol through acetic acid hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041]Weigh 1 g of rhodium(III) chloride hydrate, 0.5 g of anhydrous ruthenium trichloride, and 0.5 g of cobalt nitrate hexahydrate, and prepare 100 mL of an aqueous solution of the metal salt in a volumetric flask. Add ammonia water with a concentration of 25-28% to the aqueous solution of the metal salt at 50°C until the final pH value is 7.5; add 20g of γ-alumina to the solution and continue stirring for 4 hours to make the precipitate adsorb on the carrier γ-tri On aluminum oxide, the quasi-catalyst was obtained; then the quasi-catalyst was filtered to remove impurities therein, washed with water, and dried at 100°C for 12 hours to obtain the catalyst; the catalyst was taken out and roasted in a muffle furnace, from room temperature to The temperature was raised to 400°C at a rate of 5°C / min, kept for 4 hours for calcination, and then slowly lowered to room temperature. The prepared catalyst is called Cat-1.

Embodiment 2

[0043] Weigh 1.0 g of rhodium (II) acetate dimer, 0.8 g of ruthenium acetate, 2.0 g of molybdenum acetate, and 2.0 g of nickel nitrate in a volumetric flask to make 1 L of metal salt aqueous solution, and place it in a large beaker. Add 0.10 mol / L sodium hydroxide aqueous solution to the aqueous solution of metal salt under the environment of 80 ℃ until the end point pH value is 6.5; catalyst; then the quasi-catalyst was filtered to remove impurities therein, washed with water, and dried at 120°C for 8 hours to obtain the catalyst; the catalyst was taken out and roasted in a muffle furnace, and the temperature was raised from room temperature at a rate of 5°C / min to 550 ° C, and keep 8h roasting, and then slowly cool down to room temperature. The prepared catalyst is called Cat-2.

Embodiment 3

[0045] Weigh 0.5g of rhodium(III) chloride hydrate, 1.0g of anhydrous ruthenium trichloride, and 2.0g of manganese acetate tetrahydrate into a 1000mL volumetric flask to prepare a metal salt solution. Add 1.0mol / L sodium carbonate aqueous solution to the aqueous solution of the metal salt at 60°C until the final pH value is 8.0; add 50g of ceria to the solution and continue to stir for 6 hours to make the precipitate adsorb on the carrier ceria , to obtain the quasi-catalyst; then the quasi-catalyst was filtered to remove impurities therein, washed with water, and dried in a dry environment at 120°C for 10 hours to obtain the catalyst; the catalyst was taken out and roasted in a muffle furnace, from room temperature at 5°C / min The temperature was raised to 650°C and kept for 10h for calcination; then the temperature was slowly lowered to room temperature to obtain the desired titanium dioxide-supported catalyst called Cat-3.

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Abstract

The invention provides a preparation method of a rhodium-ruthenium composite catalyst for preparing ethyl alcohol through acetic acid hydrogenation. According to the method, rhodium and ruthenium or oxide thereof is adopted as a main catalyst, metal or oxide thereof is adopted as a promoter, and any one or more of silicon dioxide, aluminum oxide, titanium dioxide, cerium dioxide, zirconium dioxide and silicon carbide are adopted as carriers. The preparation method is a deposition-precipitation method and includes the steps that an alkaline solution is dropwise added into a mixed solution prepared from rhodium, ruthenium and M salt, precipitates are formed, the carriers are added into the solution, and precipitation substances are adsorbed on the carriers after the materials are evenly stirred for a period of time; filtering and washing are carried out to filter out impurities; drying and calcining are carried out, and supported metal oxide is obtained. A hydrogenation reaction is carried out in a tubular fixed bed reactor, firstly, the catalyst is reduced in the reducing atmosphere, and then the high conversion rate and selectivity are obtained by controlling the reaction temperature and pressure, the volume air speed, the hydrogen-acid ratio and other parameters. The preparation method is simple, high repeatability is achieved, and the catalytic effect is high.

Description

technical field [0001] The invention relates to a method for preparing a catalyst, in particular to a method for preparing a rhodium-ruthenium composite catalyst for preparing ethanol by hydrogenating acetic acid, and belongs to the technical field of chemical catalyst preparation. Background technique [0002] Ethanol is an important bulk chemical product, which is widely used in food, medicine, new materials, chemical industry and other fields. It is also an ideal high-octane non-polluting vehicle fuel and its additives. Ethanol can be blended into fuel ethanol after adding denaturant, which can be added to automobiles as fuel for automobiles, greatly reducing the pollution to the environment when gasoline is burned. [0003] The main synthesis methods of ethanol are biological fermentation and chemical synthesis. One of the raw materials of the bio-fermentation method is various food crops, but there are problems such as "competition with the people for food and land wit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J23/656B01J23/60C07C29/149C07C31/08
CPCB01J23/60B01J23/6562B01J23/8913B01J23/8993B01J37/0236B01J37/031B01J37/16C07C29/149C07C31/08
Inventor 代淑梅吴超勇
Owner ZHONGRONG TECH CORP LTD
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