Method for preparing ethanol acid by catalytic oxidation of biformyl

A technology of glyoxal catalysis and glyoxylic acid, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate, etc., can solve problems such as unsatisfactory yield of glyoxylic acid and low conversion rate of glyoxylic acid , to achieve the effect of stable quality, improved conversion rate and high product purity

Inactive Publication Date: 2009-06-24
SHANGHAI HUAYI GRP CO
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  • Abstract
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Problems solved by technology

[0008] The technical problem solved by the present invention is to provide a method for preparing glyoxylic acid by catalytic oxidation of glyoxal, so as to overcome the shortcomings of low conversion rate of glyoxal and unsatisfactory yield of glyoxylic acid in the prior art

Method used

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  • Method for preparing ethanol acid by catalytic oxidation of biformyl

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Embodiment 1

[0022] 1. Prepare the catalyst: Add 10g of ammonium metavanadate, 5g of ammonium dichromate, 2.5g of ammonium niobium oxalate and 20g of water into a reactor with stirring and a thermometer, dissolve under stirring, add 20g of 20-100 mesh (0.0009- 0.00018m) coarse-porous microsphere silica gel, maintained at 20-30°C for 24 hours, filtered the obtained catalyst precursor and dried at 80°C for 4 hours, then placed in a tube furnace, introduced nitrogen, and maintained at a temperature of 250±10°C for activation After 3 hours, 35 g of activated catalysts were prepared and cooled to room temperature for use;

[0023] 2. In the autoclave with heating, stirring and thermometer, add 40wt% glyoxal 95.5g (0.66mol) respectively, step (1) catalyst 1g, import oxygen, control reaction pressure 0.15MPa, temperature 55 ± 5 ℃, reacted for 6 hours, filtered the obtained reaction product at room temperature, and left the mother liquor after removing the catalyst overnight;

[0024] 3. Filter t...

Embodiment 2

[0026] 1. Prepare the catalyst: Add 10g of ammonium metavanadate, 2g of ammonium dichromate, 1g of ammonium niobium oxalate and 25g of water into a reactor with stirring and a thermometer, dissolve under stirring, add 20g of 20-100 mesh (0.0009-0.00018 m) Coarse-porous microsphere silica gel, maintained at 20-30°C for 24 hours, filtered the obtained catalyst precursor and dried at 90°C for 2.5 hours, then placed in a tube furnace, introduced nitrogen, and maintained at a temperature of 280±10°C for activation 2 Hours, 30 g of activated catalysts were prepared and cooled to room temperature for use.

[0027] 2. In the autoclave with heating, stirring and thermometer, add 50wt% glyoxal 152.5g (1.31mol) respectively, step (1) catalyst 2g, import oxygen, control reaction pressure 0.13MPa, temperature 60 ± 5 ℃, reacted for 4 hours, filtered the obtained reaction product at room temperature, and left the mother liquor after removing the catalyst overnight;

[0028] 3. Filter the mo...

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Abstract

The invention discloses a method for preparing glyoxylate by catalytic oxidation of oxalic aldehyde; in the method, 20-100 mesh microballoon silochrom are added into aqueous solution which is composed of ammonium metavanadate, niobium ammonium oxalate and ammonium dichromate for being soaked, and activated under the protection of nitrogen, thus preparing a catalyst; the oxalic aldehyde water solution is used as raw material, oxygen is led in in the presence of the catalyst in the invention, and catalytic oxidation reaction is carried out by pressurizing, thus obtaining the target product of glyoxylate in the invention. The yield of the glyoxylate obtained by the method can be more than or equal to 57 percent in a single reaction and the purity is more than 99 percent. Compared with the prior art, the conversion rate of the oxalic aldehyde and the productive rate of the glyoxylate are improved, the product purity is high and the quality is stable, thus being suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of glyoxylic acid, in particular to a method for preparing glyoxylic acid by catalytic oxidation of glyoxal. Background technique [0002] Glyoxylic acid is an important chemical raw material. It is an important raw material for the synthesis of vanillin, ethyl vanillin, allantoin, p-hydroxyphenylglycine and p-hydroxyphenylacetic acid. It has a wide range of applications in the synthesis of spices and medicines. application. [0003] The structural formula of glyoxylic acid is as follows: [0004] [0005] In the prior art, the preparation methods of glyoxylic acid mainly include the nitric acid oxidation method of glyoxal and the electrolytic reduction method of oxalic acid, and the nitric acid oxidation method of glyoxal is due to the production of NO x Compounds are eliminated because of their strong corrosiveness, and the preparation method of electrolytic reduction of oxalic acid is cumbersome in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/153C07C51/235B01J31/04
Inventor 宋振蒋旭亮
Owner SHANGHAI HUAYI GRP CO
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