Method for synthesizing glycolate from oxalate

A glycolic acid ester and oxalic acid ester technology, which is applied in the preparation of carboxylate esters, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of low yield of glycolic acid esters and achieve good technical effects

Active Publication Date: 2021-01-12
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the current methods of hydrogenation of oxalate esters to glycolate reported in relevant literature and patents, oxalate esters are reacted with pure hydrogen, and the yield of glycolate esters is generally low.

Method used

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  • Method for synthesizing glycolate from oxalate
  • Method for synthesizing glycolate from oxalate
  • Method for synthesizing glycolate from oxalate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A certain amount of silver nitrate, palladium nitrate and ammonium molybdate is added to 1 liter of deionized water, and it is mixed with solution I containing 0.07mol / L silver nitrate, 0.0036mol / L palladium nitrate and 0.01mol / L ammonium molybdate, under stirring The specific surface area of ​​81g is 448.33m 2 / g, average pore diameter 12.51nm, pore volume 1.09cm 3 The ratio of silicon dioxide per gram to 10g silicon aluminum is 316, and the specific surface area is 220.4m 2 / g, average pore diameter 3.44nm, pore volume 0.45cm 3 / g of ZSM-5 was added to solution I to obtain slurry II, and then 3mol / L ammonium bicarbonate water was added to slurry II as a precipitant, and the pH at the end point was controlled to be 6.5, aged at 100°C for 6 hours, and then After filtering and washing the slurry, the obtained filter cake was dried at 120°C for 10 hours, calcined at 400°C for 5 hours, and pressed into tablets after calcined to obtain the catalyst CA1 for oxalate ester s...

Embodiment 2

[0042] A certain amount of silver nitrate, palladium nitrate and ammonium molybdate is added to 1 liter of deionized water, and it is mixed with solution I containing 0.04mol / L silver nitrate, 0.002mol / L palladium nitrate and 0.01mol / L ammonium molybdate, under stirring The specific surface area of ​​84.5g is 448.33m 2 / g, average pore diameter 12.51nm, pore volume 1.09cm 3 The ratio of silicon dioxide per gram to 10g silicon aluminum is 316, and the specific surface area is 220.4m 2 / g, average pore diameter 3.44nm, pore volume 0.45cm 3 / g of ZSM-5 was added to solution I to obtain slurry II, and then 3mol / L ammonium bicarbonate water was added to slurry II as a precipitant, and the pH at the end point was controlled to be 6.5, aged at 100°C for 6 hours, and then After filtering and washing the slurry, the obtained filter cake was dried at 120°C for 10 hours, calcined at 400°C for 5 hours, and pressed into tablets after calcined to obtain the catalyst CA2 for synthesizing g...

Embodiment 3

[0044] A certain amount of silver nitrate, palladium nitrate and ammonium molybdate is added to 1 liter of deionized water, and it is mixed with solution I containing 0.14mol / L silver nitrate, 0.0068mol / L palladium nitrate and 0.01mol / L ammonium molybdate, under stirring The specific surface area of ​​74g is 448.33m 2 / g, average pore diameter 12.51nm, pore volume 1.09cm 3 The ratio of silicon dioxide per gram to 10g silicon aluminum is 316, and the specific surface area is 220.4m 2 / g, average pore diameter 3.44nm, pore volume 0.45cm 3 / g of ZSM-5 was added to solution I to obtain slurry II, and then 3mol / L ammonium bicarbonate water was added to slurry II as a precipitant, and the pH at the end point was controlled to be 6.5, aged at 100°C for 6 hours, and then The slurry was filtered and washed, and the obtained filter cake was dried at 120°C for 10 hours, calcined at 400°C for 5 hours, and pressed into tablets after calcined to obtain the catalyst CA3 for synthesizing gl...

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Abstract

The invention provides a method for synthesizing glycolate from oxalate, which comprises the following step: in the presence of a catalyst, carrying out contact reaction on the oxalate and a mixed gascontaining hydrogen and carbon monoxide to generate the glycolate. According to the method, the carbon monoxide is added while the hydrogen is introduced in the reaction of synthesizing the glycolate, so that the selectivity of methyl glycolate is improved.

Description

technical field [0001] The invention relates to a method for synthesizing glycolate from oxalate. Background technique [0002] Glycolic acid ester is an important chemical raw material because of its hydroxyl and ester group structure and the chemical properties of both alcohols and esters. It can undergo hydrolysis reactions, carbonylation reactions, oxidation reactions, etc. It can be widely used in many fields such as fuel, pesticide, medicine, spices, feed and chemical industry. [0003] Due to the wide use of glycolate, there are many studies on it at home and abroad. At present, the main production route in foreign countries is the carbonylation route using formaldehyde as a raw material. At about 70.9MPa and high temperature, formaldehyde aqueous solution and CO are condensed to form glycolic acid under the action of catalysts such as concentrated sulfuric acid or boron trifluoride, and then Glycolic acid is esterified with methanol to obtain methyl glycolate. The...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/675C07C67/31B01J23/68B01J35/10
CPCC07C67/31B01J23/686B01J35/1019B01J35/1061B01J35/1038C07C69/675Y02P20/52
Inventor 龚海燕刘俊涛孙凤侠
Owner CHINA PETROLEUM & CHEM CORP
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