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Ester hydrogenation catalyst and preparation method thereof, and ester hydrogenation reaction method

A technology for hydrogenation of esters and catalysts, applied in chemical instruments and methods, preparation of hydroxyl compounds, metal/metal oxide/metal hydroxide catalysts, etc., can solve problems such as inapplicability, and achieve high hydrogenation activity

Active Publication Date: 2016-03-02
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0006] The purpose of the present invention is to overcome the defect that existing ester hydrogenation catalysts are not suitable for the hydrogenation reaction of ester compounds containing a small amount of residual acetic acid, and provide a new preparation method of ester hydrogenation catalysts, prepared by the method Obtained ester hydrogenation catalyst and method for catalyzing ester hydrogenation reaction using the ester hydrogenation catalyst

Method used

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  • Ester hydrogenation catalyst and preparation method thereof, and ester hydrogenation reaction method
  • Ester hydrogenation catalyst and preparation method thereof, and ester hydrogenation reaction method

Examples

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preparation example Construction

[0016] The preparation method of ester hydrogenation catalyst provided by the invention comprises the following steps:

[0017] (1) adjusting the pH value of the water-soluble aluminum salt solution to 4-10 with a first alkaline substance to obtain slurry A;

[0018] (2) prepare mixed solution B and mixed solution C that all contain water-soluble copper salt solution and water-soluble zinc salt solution, the copper / zinc mol ratio in described mixed solution B<the copper / zinc mol in described mixed solution C Compare;

[0019] (3) Mix the mixed solution B with the slurry A to obtain a mixture E, and adjust the pH value of the mixture E to 4-10 with a second alkaline substance, then add the mixed solution C and the water-soluble A solution D of at least one of a platinum compound, a water-soluble palladium compound and a water-soluble tin compound to obtain a mixture F, and then adjust the pH value of the mixture F to 4-10 with a third alkaline substance, followed by solid-liqu...

preparation example 1

[0044] In this preparation example, a three-stage precipitation method is used to prepare copper-zinc-aluminum composite oxides.

[0045] 150.01 g (0.40 mol) of aluminum nitrate nonahydrate was dissolved in 300 mL of deionized water to obtain an aqueous solution of aluminum nitrate. The pH value of the aluminum nitrate aqueous solution was titrated to 7.0 with a 1 mol / L aqueous sodium hydroxide solution under stirring to obtain a white turbid slurry A. 72.48 g of copper nitrate trihydrate was dissolved in 128 g of deionized water, and the resulting solution was divided into two portions of 20.48 g and 180 g. 89.25 g of zinc nitrate hexahydrate was dissolved in 150 g of deionized water, and the obtained solution was divided into two portions of 23.25 g and 216 g. 20.48 g of copper nitrate aqueous solution (the content of copper nitrate is 0.03 mol) and 216 g of zinc nitrate aqueous solution (the content of zinc nitrate is 0.27 mol) were mixed to obtain mixed solution B. A mix...

preparation example 2

[0050] In this preparation example, a three-stage precipitation method is used to prepare copper-zinc-aluminum composite oxides.

[0051]150.01 g (0.40 mol) of aluminum nitrate nonahydrate was dissolved in 300 mL of deionized water to obtain an aqueous solution of aluminum nitrate. The pH value of the aluminum nitrate aqueous solution was titrated to 6.0 with a 1 mol / L aqueous sodium hydroxide solution under stirring to obtain a white turbid slurry A. 99.87g of copper sulfate pentahydrate was dissolved in 150g of deionized water, and the obtained solution was divided into two parts of 24.87g and 225g. 59.50 g of zinc nitrate hexahydrate was dissolved in 90 g of deionized water, and the obtained solution was divided into two parts of 119.50 g and 30 g. 24.87g of copper sulfate aqueous solution (the content of copper sulfate is 0.04mol) and 119.50g of zinc nitrate aqueous solution (the content of zinc nitrate is 0.15mol) were mixed to obtain mixed solution B. Mix 225 g of copp...

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Abstract

The present invention provides an ester hydrogenation catalyst and a preparation method thereof, and an ester hydrogenation reaction method. The ester hydrogenation catalyst preparation method comprises: (1) adjusting the pH value of a water-soluble aluminum salt solution to 4-10 to obtain a slurry A; (2) preparing a mixing solution B containing a water-soluble copper salt solution and a water-soluble zinc salt solution and a mixing solution C containing a water-soluble copper salt solution and a water-soluble zinc salt solution, wherein the copper / zinc molar ratio in the mixing solution B is less than the copper / zinc molar ratio in the mixing solution C; and (3) mixing the mixing solution B and the slurry A, adjusting the pH value of the obtained mixture E to 4-10, adding the mixing solution C and a solution D containing at least one selected from a water-soluble platinum compound, a water-soluble palladium compound and a water-soluble tin compound, adjusting the pH value of the obtained mixture F to 4-10, and carrying out solid-liquid separation, drying and calcining. The ester hydrogenation catalyst obtained by using the method has high cyclohexanol selectivity and use stability in the presence of trace acetic acid.

Description

technical field [0001] The invention relates to a method for preparing an ester hydrogenation catalyst, an ester hydrogenation catalyst prepared by the method and a method for using the ester hydrogenation catalyst to catalyze ester hydrogenation reaction. Background technique [0002] Cyclohexanol is an important solvent and intermediate in organic synthesis, which can be dehydrogenated to cyclohexanone with high selectivity. Cyclohexanone is a raw material for the manufacture of nylon, caprolactam and adipic acid, and is also widely used as a solvent in the production processes of paints, pesticides, dyes, aviation lubricants, fats, waxes, film release, stain removal, and spot removal. [0003] There are many types of cyclohexanol production processes. According to different raw materials, it can be divided into phenol method and benzene method. The former uses phenol as a raw material to hydrogenate cyclohexanol directly, and its disadvantages are that the raw material ...

Claims

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Application Information

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IPC IPC(8): B01J23/80C07C29/149C07C35/08
Inventor 郜亮夏玥穜温朗友宗保宁慕旭宏俞芳
Owner CHINA PETROLEUM & CHEM CORP
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