Method for producing glycolic acid ester through adding hydrogen in oxalic ester

A glycolic acid ester and oxalic acid ester technology, which is applied in the preparation of carboxylate, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of low selectivity of glycolic acid esters

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 prod

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Weigh 100 g of silica support. The catalyst is prepared according to the content of 20 parts of Cu, 5 parts of Ba and 2 parts of Fe / carrier. The steps are as follows: select copper nitrate, prepare an impregnation solution according to the Cu loading capacity, impregnate the silica carrier in the solution for 20 hours, and then dry it in vacuum Solid I was obtained in 6 hours. Select barium nitrate and ferric nitrate, prepare the impregnating solution according to the load of barium and iron, in order to prevent the hydrolysis of metal ions to form hydroxide or oxide precipitation, add a small amount of nitric acid to the impregnating solution, so that the pH of the impregnating solution is 4~6 , and then the above solid I was soaked in the impregnation solution for 12 hours, dried into a solid after being fully absorbed, and crushed to obtain the solid II; the solid II was mixed with an appropriate amount of Tianqing powder, and an appropriate amount of forming agent w...

Embodiment 2

[0021] According to each step and condition of embodiment 1, only the composition of catalyst is 21 parts of Cu, 4 parts of Cu 2 O and 0.5 parts Zn / SiO 2 , with dimethyl oxalate as raw material, at a reaction temperature of 170°C and a weight space velocity of 0.5 hours -1 , the hydrogen / ester molar ratio is 80:1, and the reaction pressure is under the condition of 2.8MPa, the raw material is contacted with the catalyst, and the reaction generates the effluent containing methyl glycolate, and the reaction result is: the conversion rate of dimethyl oxalate is 84.7 %, the selectivity of glycolate was 85.1%.

Embodiment 3

[0023] According to each step and condition of embodiment 1, only the composition of catalyst is 15 parts of Cu, 10 parts of Cr, 1 part of Cu 2 O / Al 2 o 3 , with dimethyl oxalate as raw material, at a reaction temperature of 150°C and a weight space velocity of 0.4 hours -1 , the molar ratio of hydrogen / ester is 60:1, and the reaction pressure is 1.0 MPa, the conversion rate of dimethyl oxalate is 78.3%, and the selectivity of methyl glycolate is 76.2%.

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PUM

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Abstract

The invention relates to a method for producing glycolic acid ester through adding hydrogen in oxalic ester, which mainly solves the technical problem in the prior art that the selectivity of the glycolic acid ester is low in a hydrogenated production. The invention adopts the technical scheme that under conditions that the reaction temperature is 100-250 DEG C, the weight space velocity is 0.2-5 h<-1>, the molar ratio of hydrogen to ester is (10-100):1, and the reaction pressure is 0-6.0 MPa, raw materials, namely the oxalic ester, are in contact with a catalyst to generate an effluence containing the glycolic acid ester, wherein the catalyst, in parts by weight, comprises 5-80 parts of active component, 0-40 parts of additive and 1-90 parts of carrier. Due to the adoption of the technical scheme, the problem is better solved, and the method can be used in the industrial production of glycolic acid ester.

Description

technical field [0001] The invention relates to a method for producing glycolate by hydrogenation of oxalate, in particular to a method for producing glycolate by hydrogenating catalyzed dimethyl oxalate or diethyl oxalate. Background technique [0002] With its unique molecular structure: it has a-H, hydroxyl and ester functional groups at the same time, which makes it have the chemical properties of alcohol and ester, and can undergo carbonylation reaction, hydrolysis reaction, oxidation reaction, etc., and has become an important chemical raw material . Glycolate is an excellent solvent for many celluloses, resins, and rubbers. Its downstream products such as glycolic acid, glycine, dimethyl malonate and glyoxylic acid also have extensive application value. [0003] At present, there is no mature production process of environmentally friendly glycolic acid ester in China. It is still produced by the chloroacetic acid method, and the process is to mix and stir the chlor...

Claims

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Application Information

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IPC IPC(8): C07C69/675C07C67/31B01J23/78B01J23/80B01J23/85B01J23/745B01J29/46
Inventor 杨为民刘俊涛孙凤侠李蕾
Owner CHINA PETROLEUM & CHEM CORP
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