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Method for producing glyoxylic acid by glyoxal oxide water solution

A glyoxylic acid, aqueous solution technology, applied in chemical instruments and methods, preparation of organic compounds, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of large consumption of nitric acid and poor selectivity of glyoxylic acid and other problems, to achieve the effect of reducing the consumption of nitric acid, facilitating the post-processing of the product, and stabilizing the oxidation reaction process

Active Publication Date: 2018-05-08
广东玖翼化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the invention is to provide a 2 and nano-SiO 2 The coated heteropoly acid is used as a catalyst, and the method of synergistically oxidizing glyoxal aqueous solution with air and nitric acid to produce glyoxylic acid solves the problems of large consumption of nitric acid and poor selectivity of glyoxylic acid in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Na 2 WO 4 2H 2 O 39.5g (0.12mol) was dissolved in 100mL of 50-60°C deionized water to obtain an aqueous sodium tungstate solution, and Na 2 HPO 3 12H 2 O 4.2g (0.03mol) was dissolved in 50mL of deionized water to obtain a disodium hydrogen phosphate aqueous solution, mixed for 1 hour under stirring, then 25mL of concentrated hydrochloric acid was added to adjust the pH value of the aqueous solution to 1-2, and hydrogen peroxide with a mass concentration of 3% was added 5mL aqueous solution, filter the insoluble impurities in the solution, cool the filtrate to room temperature, and extract the generated H with 90mL ether three times in a separating funnel. 3 PW 12 o 40 , after combining, the extract was washed with a small amount of water, and the aqueous phase was separated to obtain H 3 PW 12 o 40 99g of ether solution with a concentration of 29.4% by mass.

[0033] Add 800mL of deionized water, 800mL of ether, 0.4g of cetyltrimethylammonium bromide, 200g of ...

Embodiment 2

[0039] Na 2 MoO 4 2H 2 O 29.0g (0.12mol) is dissolved in 100mL hot deionized water to obtain sodium molybdate aqueous solution, Na 2 SiO 3 9H 2 O 3.4g (0.012mol) was dissolved in 50mL deionized water to obtain sodium silicate aqueous solution, mixed under stirring for 2h, then added concentrated hydrochloric acid 30mL to adjust the pH value of the aqueous solution to 1, adding 5mL of hydrogen peroxide aqueous solution with a mass concentration of 3%, The insoluble impurities in the separation solution were filtered, the filtrate was cooled to room temperature, and the generated H was extracted three times with 90 mL ether in a separatory funnel. 4 SiMo 12 o 40 , after combining, the extract was washed with a small amount of water, and the aqueous phase was separated to obtain H 4 SiMo 12 o 40 100 g of an ether solution with a concentration of 18% by mass.

[0040] The nano-SiO that embodiment 1 makes 2 Hollow sphere 10g impregnated in 10g mass percentage concentrati...

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Abstract

The invention relates to a method for producing glyoxylic acid by a glyoxal oxide water solution. The glyoxylic acid is produced through adopting heteropoly acid catalysts including nano TiO2 and nanoSiO2 cladded phosphotungstic acid, silicotungstic acid, phosphomolybdic acid, silicomolybdic acid and the like, and cooperating two oxidants including air and nitric acid with the glyoxal oxide watersolution. According to the technical scheme, the method comprises three parts including preparation of the cladded heteropoly acid catalysts, production of the glyoxylic acid and post-treatment of areaction solution; quality indexes of a glyoxylic acid product are as follows: 50 percent to 51 percent of the glyoxylic acid, 0.4 percent to 0.7 percent of oxalic acid, 0.1 percent to 0.2 percent ofglyoxal, 0 to 0.01 percent of heavy metal, 0 to 0.1 percent of ignition residues, 82 percent to 87 percent of glyoxylic acid yield and 10 percent to 15 percent of oxalic acid yield. By adopting the method provided by the invention, the problems in the prior art that the corrosion on production requirement is serious, the consumption amount of the nitric acid is great and the glyoxylic acid selectivity is not good are solved.

Description

technical field [0001] The invention relates to a method for producing glyoxylic acid by oxidizing glyoxal, in particular a method for producing glyoxylic acid by synergistically oxidizing a glyoxal aqueous solution with air and nitric acid by using heteropolyacid as a catalyst, belonging to the field of pharmacy and chemical industry. Background technique [0002] Glyoxylic acid is a fine chemical with a wide range of uses, mainly used in the production of pharmaceutical and chemical products such as p-hydroxyphenylhydantoin, vanillin and hydroxyphosphine carboxylic acid. The industrial production methods of glyoxylic acid mainly include glyoxal oxidation, oxalic acid reduction and maleic anhydride ozonation. The glyoxal oxidation method can use various oxidants to oxidize glyoxal aqueous solution under acidic conditions to prepare glyoxylic acid. The commonly used oxidants mainly include nitric acid, nitrogen oxides, chlorine gas, air and their combinations. At present, g...

Claims

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Application Information

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IPC IPC(8): C07C51/27C07C59/325B01J31/16B01J27/188B01J35/10
CPCC07C51/27B01J23/002B01J23/28B01J27/188B01J2523/00B01J35/61B01J35/647C07C59/325B01J2523/41B01J2523/47B01J2523/68
Inventor 李建生王韬王泽江
Owner 广东玖翼化工有限公司
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