Catalyst for preparing glycolate through hydrogenating oxalate, preparation method for catalyst and use of catalyst

A glycolic acid ester and oxalic acid ester technology is applied in the preparation of carboxylic acid esters, molecular sieve catalysts, chemical instruments and methods, etc., and can solve the problems of low glycolic acid ester selectivity and poor catalyst activity.

Inactive Publication Date: 2016-05-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] One of the technical problems to be solved by the present invention is that there are technical problems of poor catalyst activity and low glycolate selectivity in the prior art, and a new catalyst for the hydrogenation of oxalate to glycolate is provided

Method used

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  • Catalyst for preparing glycolate through hydrogenating oxalate, preparation method for catalyst and use of catalyst
  • Catalyst for preparing glycolate through hydrogenating oxalate, preparation method for catalyst and use of catalyst
  • Catalyst for preparing glycolate through hydrogenating oxalate, preparation method for catalyst and use of catalyst

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Experimental program
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Effect test

Embodiment 1

[0037] Prepare 50ml silver acetate solution I containing 4.5% silver, then dissolve 35g P123 in 1.2L aqueous solution containing 1.5mol / L acetic acid, stir well to obtain solution II, then add 75ml tetraethyl orthosilicate dropwise under stirring into solution II to obtain solution III and to obtain slurry IV after stirring for 20 hours. Add the prepared solution I to the slurry IV under stirring, transfer the slurry to the crystallization kettle for aging at 50°C for 12 hours after stirring evenly, after the crystallization is completed, use sodium hydroxide to degrade the pH in the crystallization kettle for 5. Take out the product and filter, then wash the filter cake with ethanol and deionized water, dry at 120°C, and roast at 500°C. Hydrogen glycolate catalyst cat-A1. Catalyst samples were taken for ICP and BET characterization tests, and the test results are shown in Table 1.

Embodiment 2

[0039]Prepare 50ml solution I of silver acetate and cobalt nitrate containing 4.5% silver and 0.045% cobalt, then dissolve 35g P123 in 1.2L aqueous solution containing 1.5mol / L acetic acid, stir well to obtain solution II, and then dissolve 75ml Ethyl orthosilicate was added dropwise to solution II to obtain solution III, and after stirring for 14 hours, slurry IV was obtained. Add the prepared solution I into the slurry IV under stirring, and transfer the slurry to the crystallization tank at 40°C for aging for 12 hours after stirring evenly. After the crystallization is completed, adjust the pH in the crystallization tank with sodium hydroxide to 5. Take out the product and filter, then wash the filter cake with ethanol and deionized water, dry at 120°C, and roast at 500°C. Hydrogen glycolate catalyst cat-A2. Catalyst samples were taken for ICP and BET characterization tests, and the test results are shown in Table 1.

Embodiment 3

[0041] Prepare 50ml solution I of silver acetate and nickel nitrate containing 4.5% silver and 0.22% nickel, then dissolve 35g P123 in 1.2L aqueous solution containing 1.5mol / L acetic acid, stir well to obtain solution II, and then dissolve 69ml Ethyl orthosilicate was added dropwise to solution II to obtain solution III, and then 2 g of alumina was added and stirred for 4 hours to obtain slurry IV. Add the prepared solution I to the slurry IV under stirring, and transfer the slurry to the crystallization tank at 100°C for aging for 12 hours after stirring evenly. . Take out the product and filter, then wash the filter cake with ethanol and deionized water, dry at 120°C, and roast at 500°C. Hydrogen glycolate catalyst cat-A3. Catalyst samples were taken for ICP and BET characterization tests, and the test results are shown in Table 1.

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Abstract

The invention relates to a catalyst for preparing glycolate through hydrogenating oxalate, a preparation method for the catalyst and use of the catalyst. The catalyst is mainly used for solving the problem in the prior art that catalysts are poor in activity and low in glycolate selectivity. Through adopting the technical scheme that the catalyst which contains the following ingredients in percentage by weight is prepared by in-situ synthesis: (1) 0.5-15wt% of silver or oxides thereof; (2) 0-4wt% of at least one metal of VIII-group metals or oxides thereof; (3) 0-3wt% of at least one element of VA-group elements or oxides thereof; and (4) 78-99.5wt% of at least one carrier selected from silica, alumina, zirconia, titania and molecular sieves, the problem is better solved, and the catalyst can be applied to the industrial production for preparing glycolate through hydrogenating oxalate.

Description

technical field [0001] The invention relates to a method for preparing a catalyst for hydrogenating oxalate to synthesize glycolate, in particular to a method for preparing a catalyst for catalytically hydrogenating dimethyl oxalate to synthesize methyl glycolate. Background technique [0002] Due to its unique molecular structure and the chemical properties of both alcohols and esters, glycolic acid esters can undergo carbonylation reactions, hydrolysis reactions, oxidation reactions, etc., and become an important chemical raw material. It can be widely used in many fields such as chemical industry, medicine, pesticide, feed, spices and fuel. [0003] Due to the wide application and high market demand of glycolic acid ester, there are also many researches on its synthesis process at home and abroad, mainly including one-step synthesis method of glyoxal and methanol, formaldehyde carbonylation monoester synthesis method, ester methylal and formic acid method , coupling meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/50B01J23/89B01J29/44B01J27/185C07C69/675C07C67/31
Inventor 龚海燕刘国强孙凤侠
Owner CHINA PETROLEUM & CHEM CORP
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