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Method for producing glyoxylate through oxydehydrogenation of glycollate

A technology of glycolic acid ester and glyoxylic acid ester is applied in the field of oxidative dehydrogenation of glycolic acid ester to produce glyoxylic acid ester, and can solve the problems of low yield of glyoxylic acid ester and the like

Active Publication Date: 2017-12-08
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 yield of glyoxylate produced by oxidative dehydrogenation of glycolate in the prior art, and a new method for producing glyoxylate by oxidative dehydrogenation of glycolate is provided

Method used

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  • Method for producing glyoxylate through oxydehydrogenation of glycollate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Prepare 100ml of ammonium molybdate and ammonium metavanadate aqueous solution I containing 12.5% ​​molybdenum and 3.4% vanadium, add 84g of alumina carrier, and stir for 5 hours to obtain slurry II; then mix 100ml of nitric acid containing 4% iron under stirring Slowly add the iron solution to the slurry II, stir for 2 hours, pour the slurry into a 500ml autoclave, and place it at 180°C for 15 hours, then cool and filter, wash with deionized water, dry at 100°C, and dry at 250°C Calcined for 4 hours, and then pressed into tablets to obtain catalyst CA1. The catalyst samples were taken for X-fluorescence (XRF) characterization test to determine the catalyst components as shown in Table 1.

[0031] Take by weighing 6g catalyzer in fixed bed reactor, adopt NO and air and methyl glycolate as raw material, wherein the oxygen molar ratio contained in NO and air is 6, and the oxygen and methyl glycolate molar ratio in air is 0.8, in The reaction temperature is 80°C, the react...

Embodiment 2

[0033] Prepare 100ml of ammonium molybdate and ammonium metavanadate aqueous solution I containing molybdenum 6.3%, vanadium 3.4, add 90g zirconia carrier, stir for 5 hours to obtain slurry II; then mix 100ml iron nitrate containing 4% iron under stirring Slowly add the solution to the slurry II, stir for 2 hours, pour the slurry into a 500ml autoclave, and place it at 180°C for 15 hours, then cool and filter, wash with deionized water, dry at 100°C, and roast at 250°C After 4 hours, the catalyst CA2 was obtained by pressing into tablets, and the catalyst samples were taken for X-fluorescence (XRF) characterization test to determine the catalyst components as shown in Table 1.

[0034] Weigh 6g of catalyst in a fixed-bed reactor and react according to the conditions of [Example 1]. The reaction results are shown in Table 2.

Embodiment 3

[0036] Prepare 100ml of ammonium molybdate and ammonium metavanadate aqueous solution I containing 0.25% molybdenum and 0.2 vanadium, add 97g of alumina carrier, stir for 5 hours to obtain slurry II; then mix 100ml of ferric nitrate containing 4% iron under stirring Slowly add the solution to the slurry II, stir for 2 hours, pour the slurry into a 500ml autoclave, and place it at 180°C for 15 hours, then cool and filter, wash with deionized water, dry at 100°C, and roast at 250°C After 4 hours, the catalyst CA3 was obtained by pressing into tablets, and the catalyst samples were taken for X-fluorescence (XRF) characterization test to determine the catalyst components as shown in Table 1.

[0037] Weigh 6g of catalyst in a fixed-bed reactor and react according to the conditions of [Example 1]. The reaction results are shown in Table 2.

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Abstract

The invention relates to a method for producing glyoxylate through oxydehydrogenation of glycollate. The invention mainly aims to overcome the problem of low yield of glyoxylate in the prior art. The method provided by the invention comprises a reaction step of contacting a nitrogen oxide and oxygen-containing gas with glycollate in the presence of a catalyst to produce glyoxylate. The catalyst comprises the following components by weight: a) 0.3 to 20 parts of a mixture of molybdenum and vanadium; b) 0.05 to 15 parts of at least one metal selected from a group consisting of copper, palladium, manganese, nickel, cerium, bismuth, potassium, lanthanum, magnesium, tin, iron, calcium and cobalt; and c) 65 to 99.8 parts of a carrier. With such a technical scheme, the above problem is overcome, and the method is applicable to industrial production of glyoxylate through oxydehydrogenation of glycollate.

Description

technical field [0001] The invention relates to a method for producing glyoxylate by oxidative dehydrogenation of glycolate. Background technique [0002] Glyoxylate has both the chemical properties of aldehyde and ester, and can undergo various reactions, especially glyoxylic acid can be prepared by hydrolysis. Glyoxylic acid is an organic intermediate for the synthesis of spices, medicine, food, varnish raw materials, dyes, plastic additives, etc. It can be used to produce oral penicillin, vanillin, mandelic acid and allantoin, etc. Consumption has also been on the rise. [0003] The production methods of glyoxylic acid are different according to the starting materials, and there are about a dozen kinds at present. The most commonly used in industry are oxalic acid electrolytic reduction method, glyoxal nitric acid oxidation method, maleic acid (anhydride) ozonation method, etc. At present, the domestic glyoxylic acid industry has encountered two major problems: first, ...

Claims

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Application Information

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IPC IPC(8): C07C67/313C07C69/67B01J23/28B01J23/31B01J23/34B01J23/652B01J23/887B01J29/03B01J29/04
CPCB01J23/28B01J23/31B01J23/34B01J23/6525B01J23/8877B01J29/0341B01J29/045B01J2229/18C07C67/313C07C69/716
Inventor 龚海燕宋海峰李蕾
Owner CHINA PETROLEUM & CHEM CORP
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