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Catalyst for production of hydroxyacetic acid ester by oxalate through hydrogenation

A technology of glycolate and oxalate, applied in physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, preparation of carboxylate, etc., can solve the problem of low selectivity of glycolate

Inactive Publication Date: 2012-08-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is the low selectivity of hydrogenation product glycolate in the prior art, and a new catalyst for producing glycolate by hydrogenation of oxalate is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 100 grams of alumina composite carrier with a weight ratio of alumina to silica of 4:1. The catalyst is prepared according to the content of 20 parts Cu, 5 parts Ba and 2 parts Fe. The steps are as follows: select copper nitrate, prepare an impregnation solution according to the Cu loading amount, immerse the silica carrier in the solution for 20 hours, and then vacuum dry for 6 hours Obtained solid I. Select barium nitrate and ferric nitrate, and prepare the impregnation solution according to the load of barium and iron. In order to prevent the hydrolysis of metal ions to form hydroxides or oxide precipitation, a small amount of nitric acid is added to the impregnation solution to make the pH of the impregnation solution = 4-6 , Then the above solid substance I was soaked in the dipping solution for 12 hours, dried into a solid after being fully absorbed, and pulverized to obtain a solid substance II; Add the solid substance II to an appropriate amount of Tianqing...

Embodiment 2

[0026] According to the various steps and conditions of Example 1, except that the carrier of the catalyst is a composite carrier with a weight ratio of alumina and silica of 1:1, and the composition of the catalyst is 21 parts Cu and 4 parts Cu 2 O, 0.5 parts of Zn / SiO 2 , Using dimethyl oxalate as raw material, at a reaction temperature of 170℃, and a weight space velocity of 0.5 hours -1 , The hydrogen / ester molar ratio is 80:1, and the reaction pressure is 2.8MPa. The raw materials are contacted with the catalyst to react to produce an effluent containing methyl glycolate. The reaction result is: the conversion rate of dimethyl oxalate is 82 %, the selectivity of glycolate is 83%.

Embodiment 3

[0028] According to the various steps and conditions of Example 1, except that the carrier of the catalyst is a composite carrier with a weight ratio of alumina and silica of 0.1:1, the composition of the catalyst is 15 parts Cu, 10 parts Cr, and 1 part Cu. 2 O, using dimethyl oxalate as raw material, at a reaction temperature of 150°C, and a weight space velocity of 0.4 hours -1 When the hydrogen / ester molar ratio is 60:1 and the reaction pressure is 1.0 MPa, the conversion rate of dimethyl oxalate is 75%, and the selectivity of methyl glycolate is 73%.

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Abstract

The invention relates to a catalyst for production of hydroxyacetic acid ester by oxalate through hydrogenation, which mainly solves the technical problem of low selectivity of hydroxyacetic acid ester in hydrogenated products in the prior art. The catalyst comprises the following components as per parts by weight: 5 to 80 parts of active component, 0 to 40 parts of assistant and 1 t0 30 parts of carriers, wherein the active component is copper, oxide of copper of copper mixture; the assistant is at least one of zinc, lanthanum, barium, nickel or iron or oxide of zinc, lanthanum, barium, nickel or iron; and the carrier is a complex carrier chosen from alumina and silicon oxide, and the weight ratio of the alumina and silicon oxide is 0.01 to 30:1. The catalyst for production of hydroxyacetic acid ester by oxalate through hydrogenation can solve the problem well, and can be used for industrial production of hydroxyacetic acid ester.

Description

Technical field [0001] The invention relates to a catalyst for producing glycolate by hydrogenation of oxalate, in particular to a catalyst for producing glycolate by hydrogenation of dimethyl oxalate or diethyl oxalate. Background technique [0002] Glycolate has a unique molecular structure: it has aH, hydroxyl and ester functional groups at the same time, which makes it have the chemical properties of alcohol and ester, and can undergo carbonylation, hydrolysis, oxidation, etc., making it an important chemical raw material . Glycolate is an excellent solvent for many celluloses, resins and rubbers. Its downstream products glycolic acid, glycine, dimethyl malonate and glyoxylic acid also have a wide range of applications. [0003] At present, there is no mature environment-friendly production process of glycolic acid ester in China. The chloroacetic acid method is still used for production, and the process is to mix and stir chloroacetic acid with caustic soda solution. Heat ...

Claims

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Application Information

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IPC IPC(8): B01J23/745B01J23/80B01J23/86B01J23/72B01J23/755B01J23/78B01J23/83C07C69/675C07C67/31
Inventor 刘俊涛王万民刘国强
Owner CHINA PETROLEUM & CHEM CORP
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