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Method for increasing selectivity of glycollic acid ester

A glycolate and selectivity technology, which is applied in the preparation of carboxylate, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problem of low selectivity of glycolate

Active 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 technical problem of glycolic acid ester selectivity that exists in the method for previous document, a kind of new method that improves glycolic acid ester selectivity is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Weigh 500 grams of a silicon oxide carrier with a specific surface area of ​​400 square meters per gram, and configure the catalyst according to the content of 35 parts of active copper oxide. After soaking in the solution for 24 hours, vacuum-dry at room temperature for 12 hours to obtain a solid. The solid was then dried at 120°C for 12 hours and calcined at 450°C for 4 hours to obtain the desired CuO / SiO 2 catalyst.

[0016] Weigh the prepared CuO / SiO 2 200 grams of catalyst is loaded into a tubular reactor with a diameter of 24 mm, using dimethyl oxalate as a raw material, at a reaction temperature of 180 ° C, and a weight space velocity of 0.4 hours -1 , the hydrogen / ester molar ratio is 60: 1, and the reaction pressure is under the condition of 3.0MPa, the raw material is contacted with the copper-containing oxide catalyst to react, and the reaction result is: the conversion rate of dimethyl oxalate is 82%, methyl glycolate The selectivity to ester was 86.4%. ...

Embodiment 2

[0018] The copper-containing oxide catalyst prepared according to the various steps and conditions of [Example 1] has 28 parts by weight of the copper oxide component.

[0019] Weigh the prepared CuO / SiO 2 200 grams of catalyst is loaded into a tubular reactor with a diameter of 24 mm, using dimethyl oxalate as a raw material, at a reaction temperature of 140 ° C, and a weight space velocity of 0.8 hours -1 , the hydrogen / ester molar ratio is 50:1, and the reaction pressure is under the condition of 5.0MPa, the raw material is contacted with the copper-containing oxide catalyst to react, and the reaction result is: the conversion rate of dimethyl oxalate is 80.1%, and the conversion rate of glycolic acid ester is 80.1%. The selectivity is 82.3%.

Embodiment 3

[0021] The copper-containing oxide catalyst prepared according to the various steps and conditions of [Example 1] has 25 parts by weight of the copper oxide component.

[0022] Weigh the prepared CuO / SiO 2 200 grams of catalyst is loaded into a tubular reactor with a diameter of 24 mm, using dimethyl oxalate as a raw material, at a reaction temperature of 190 ° C, and a weight space velocity of 0.5 hours -1 , the hydrogen / ester molar ratio is 60:1, and the reaction pressure is under the condition of 4.0MPa, the raw material is contacted with the copper-containing oxide catalyst to react, and the reaction result is: the conversion rate of dimethyl oxalate is 90.8%, and the conversion rate of glycolic acid ester The selectivity is 91.8%.

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Abstract

The invention relates to a method for increasing selectivity of glycollic acid ester. The technical problem of low selectivity of the glycollic acid ester in the prior art is solved. The method comprises the following steps of: taking oxalate as a raw material, and contacting the raw material with a copper-containing oxide catalyst under the conditions of reaction temperature at 100-210 DEG C, weight hourly space velocity at 0.2-5 per hour, mole ratio of hydrogen to ester at (10-100):1 and reaction pressure at 0.5-6.0MPa, thereby generating a reaction effluent containing the glycollic acid ester, wherein the reaction is started by the copper-containing oxide catalyst under oxide state, and on the basis of weight part of the catalyst, the copper-containing oxide catalyst comprises 10-60 weight parts of copper and copper oxide components. According to the technical scheme, the problem is more efficiently solved. The method is suitable for the industrial production for increasing the yield of glycollic acid ester.

Description

technical field [0001] The invention relates to a method for improving the selectivity of glycolate, in particular to a method for improving the selectivity of glycolate by hydrogenating dimethyl oxalate or hydrogenating 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 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/675C07C67/31B01J23/72B01J23/755
Inventor 刘俊涛孙凤侠蒯骏
Owner CHINA PETROLEUM & CHEM CORP
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