Method for synthesizing glycolic acid ester by gas-phase hydrogenation of oxalate

A technology of glycolic acid ester and oxalic acid ester, which is applied to the preparation of carboxylate, chemical instruments and methods, and the preparation of organic compounds, etc.

Active Publication Date: 2015-09-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the conversion rate of dimethyl oxalate can be as high as

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The catalyst was prepared at the content of 15 parts of copper oxide + 5 parts of cobalt oxide + 80 parts of silicon dioxide. The steps are as follows: 1 liter of copper nitrate and cobalt acetate solution containing the required concentration is used as solution I, 80 grams of silicon dioxide is added to solution I under stirring to obtain slurry II, and then 3 mol / liter of ammonium bicarbonate Add water as a precipitant to slurry II, control the end point pH to 6.5, age at 90°C for 4 hours, then filter and wash the slurry, dry the obtained filter cake at 80-120°C for 10 hours, and roast at 500°C for 5 hours After roasting, it can be pressed into tablets to obtain the catalyst for the hydrogenation of oxalate to methyl glycolate.

[0018] The catalyst is loaded into a fixed-bed reactor, and the temperature is programmed to increase with hydrogen for reduction. Among them, the hydrogen volume space velocity is 800 hours -1 , the temperature was raised to 300° C., and ...

Embodiment 2

[0021] The catalyst was prepared according to the content of 10 parts of copper oxide + 1 part of barium oxide + 89 parts of aluminum oxide. The steps are as follows: 1 liter of copper nitrate and barium nitrate solution containing the required concentration is used as solution I, 80 grams of alumina is added to solution I under stirring to obtain slurry II, and then 3 mol / liter of ammonia water is used as a precipitant Add it to slurry II, control the end point pH to 6.5, age at 90°C for 4 hours, then filter and wash the slurry, dry the obtained filter cake at 80-120°C for 10 hours, bake at 450°C for 5 hours, press The catalyst for the hydrogenation of oxalate to methyl glycolate can be obtained by molding the sheet.

[0022] The catalyst is loaded into a fixed-bed reactor, and the temperature is programmed to increase with hydrogen for reduction. Among them, the volume space velocity of hydrogen is 1000 hours -1 , the temperature was raised to 250° C., and the temperature ...

Embodiment 3

[0025] The catalyst was prepared according to the content of 40 parts of copper oxide + 3 parts of calcium oxide + 57 parts of mesoporous molecular sieve. The steps are as follows: 1 liter of copper nitrate and calcium nitrate solution containing the required concentration is used as solution I, 80 grams of mesoporous molecular sieves are added to solution I under stirring to obtain slurry II, and then 3 mol / liter of ammonium bicarbonate is used as Add the precipitant to the slurry II, control the end point pH to 6.5, age at 90°C for 4 hours, then filter and wash the slurry, and dry the obtained filter cake at 80-120°C for 10 hours, then roast at 400°C for 5 hours, and then The catalyst for the hydrogenation of oxalate to methyl glycolate can be obtained after tableting.

[0026] The catalyst is loaded into a fixed-bed reactor, and the temperature is programmed to increase with hydrogen for reduction. Among them, the hydrogen volume space velocity is 500 hours -1 , the tempe...

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Abstract

The invention relates to a method for synthesizing glycolic acid ester by gas-phase hydrogenation of oxalate, and is used for mainly solving the technical problem of low yield of glycolic acid ester in the prior art. The problem is better solved through adopting the technical scheme that the method comprises the steps: taking oxalate as a raw material, pre-mixing with hydrogen gas containing a dilution gas, then under conditions of the temperature of 120 DEG C-250 DEG C, the pressure of 0.5-5 MPa, the oxalate weight space velocity of 0.1-6 h<-1> and the hydrogen gas-oxalate molar ratio of 10-150, carrying out a contact reaction with a catalyst, and generating an effluent containing glycolic acid ester. The method can be used in industrial production of glycolic acid ester.

Description

technical field [0001] The invention relates to a method for synthesizing glycolate by gas-phase hydrogenation of oxalate, in particular to a method for synthesizing methyl glycolate by gas-phase hydrogenation of dimethyl oxalate. Background technique [0002] Due to its unique molecular structure and the chemical properties of both alcohols and esters, methyl glycolate can undergo carbonylation reactions, hydrolysis reactions, oxidation reactions, etc., and has 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 methyl glycolate, there are 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 method, chloroacetic acid method, formaldehyde ...

Claims

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Application Information

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IPC IPC(8): C07C69/675C07C67/31
CPCB01J23/72B01J23/75B01J23/755B01J23/78B01J23/80B01J23/83B01J23/885B01J23/8892B01J23/8926C07C67/31C07C69/675
Inventor 龚海燕刘俊涛李蕾
Owner CHINA PETROLEUM & CHEM CORP
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