Production method for preparing glyoxylate from glycollate

A glycolic acid ester and glyoxylic acid ester technology is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., which can solve the problems of easy over-oxidation, high separation cost, difficult product separation, etc. The process and steps are simple to operate, and the effect of good technical effect

Active Publication Date: 2019-12-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main technical problem to be solved is that the glycolic acid esters in the prior art are prone to over-oxidation in the process of preparing glyoxylic acid esters, and the separation of products is difficult and the separation cost is high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh Cu(NO 3 ) 2 ·3H 2 O, Zn(NO 3 ) 2 ·6H 2 O, Zr(NO 3 ) 4 ·5H 2 O solid and silica sol (40wt%), Cu(NO 3 ) 2 ·3H 2 O, Zn(NO 3 ) 2 ·6H 2 O and Zr(NO 3 ) 4 ·5H 2 O solid is dissolved in deionized water to make a mother liquor, and sodium hydroxide is used as an alkaline precipitant to make a 1mol / l solution, and flow co-precipitation to pH=10, and the precipitation temperature is 75°C, and continue to add silica sol under stirring conditions , aged at 80°C for 1h, put the obtained colloid into the reaction kettle, treated at 120°C for 16h, took out the product, cooled, washed and filtered, dried at 100°C for 24h, and roasted at 500°C for 3h, the roasted The particles were compressed into tablets to make catalyst C-1.

[0028] Weigh 5g of the catalyst and put it in a fixed bed reactor, reduce the catalyst at 180°C and raise the temperature of the reactor to 210°C, vaporize the glycolic acid ester in a 160°C vaporization furnace, and control the volume spa...

Embodiment 2

[0030] Weigh Cu(NO 3 ) 2 ·3H 2 O, Zn(NO 3 ) 2 ·6H 2 O, Zr(NO 3 ) 4 ·5H 2 O solid and silica sol (40wt%), Cu(NO 3 ) 2 ·3H 2 O, Zn(NO 3 ) 2 ·6H 2 O and Zr(NO 3 ) 4 ·5H 2 O solid is dissolved in deionized water to make a mother liquor, and sodium hydroxide is used as an alkaline precipitant to make a 1mol / l solution, and co-precipitate to pH=11, and the precipitation temperature is 80°C, and continue to add silica sol under stirring conditions , aged at 80°C for 1h, put the obtained colloid into the reaction kettle, treated at 140°C for 24h, took out the product, cooled, washed and filtered, dried at 110°C for 24h, and roasted at 550°C for 3h, the roasted The particles were compressed into tablets to make Catalyst C-2.

[0031] Weighed 5g of catalyst and put it in a fixed-bed reactor, and reacted according to the conditions of Example 1. The results are shown in Table 1.

Embodiment 3

[0033] Weigh Cu(NO 3 ) 2 ·3H 2 O, Zn(NO 3 ) 2 ·6H 2 O, Zr(NO3 ) 4 ·5H 2 O solid and tetraethyl orthosilicate (analytical grade), Cu(NO 3 ) 2 ·3H 2 O, Zn(NO 3 ) 2 ·6H 2 O and Zr(NO 3 ) 4 ·5H 2 O solid is dissolved in deionized water to make mother liquor, and sodium carbonate is used as alkaline precipitant to make 1mol / l solution, co-precipitate to pH=12, precipitation temperature is 65°C, continue to add orthosilicic acid under stirring condition Ethyl ester, aged at 70°C for 1h, put the obtained colloid into the reaction kettle, treated at 160°C for 16h, took it out, cooled, washed and filtered the product, dried at 120°C for 24h, and roasted at 550°C for 3h, roasted Good particles are compressed into tablets to make Catalyst C-3.

[0034] Weighed 5g of catalyst and put it in a fixed-bed reactor, and reacted according to the conditions of Example 1. The results are shown in Table 1.

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PUM

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Abstract

The invention relates to a production method for preparing glyoxylate from glycollate. A purpose of the invention is mainly to solve the problems of excessive oxidation of glycollate, difficulty in product separation and high cost in the prior art. According to the invention, glyoxylate is prepared by directly dehydrogenating glycollate; the catalyst comprises the following components that cu andZn are used as active components, ZrO2 and SiO2 are used as carriers, and a ratio of Cu to Zn to Zr to Si is 1:0-2:1-4:1-7; the reaction conditions comprise that the temperature is 160-240 DEG C, andthe feeding volume space velocity of glycollate is 0.4-1.0 h<-1>; with the method, the conversion rate of glycollate reaches 99%, and the selectivity of glyoxylate reaches 96%; and the method can wellsolve the problems in the prior art, and can be used for industrial production of glyoxylate from glycollate.

Description

technical field [0001] The invention provides a production method for preparing glyoxylic acid ester from glycolic acid ester, which belongs to the technical field of organic chemical industry. Background technique [0002] Glyoxylate has both the chemical properties of aldehyde and ester, and can undergo various chemical reactions, especially hydrolysis to produce glyoxylic acid. Glyoxylic acid is the simplest aldehyde acid, which has both aldehyde and carboxylic acid functional groups and their corresponding chemical properties. It is an important fine chemical intermediate and can be used to produce oral penicillin, vanillin, ethyl vanillin, almond Important products such as acid and allantoin have active chemical properties and can simultaneously undergo aldehyde and acid reactions, cyclization, and condensation reactions. [0003] At present, there are three main industrial production methods of glyoxylic acid, which are glyoxal oxidation, oxalic acid electrolytic redu...

Claims

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Application Information

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IPC IPC(8): C07C69/738C07C67/313B01J23/80B01J37/03B01J37/18
CPCC07C67/313B01J23/80B01J23/002B01J37/031B01J37/18C07C69/738Y02P20/584
Inventor 李婷婷于杨袁浩然张觅
Owner CHINA PETROLEUM & CHEM CORP
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