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Method for preparing glyoxylic acid by oxidizing glyoxal with N2O

A technology of glyoxylic acid and glyoxal, applied in chemical instruments and methods, catalyst activation/preparation, preparation of organic compounds, etc., can solve problems such as pollution and achieve high selectivity

Pending Publication Date: 2022-07-19
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the pollution problem etc. that glyoxylic acid present production technique exists, the present invention proposes to use N for the first time. 2 O is used as an oxidant, and the process of preparing glyoxylic acid by oxidizing glyoxal under the action of a catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Preparation of catalyst:

[0028] Catalyst A:

[0029] A certain amount of SAPO-11 molecular sieve was immersed in ferric nitrate solution, in which iron accounted for 0.5% of the mass of the molecular sieve; stirred at room temperature for 6 hours, dried at 110 °C for 9 hours, and then calcined at 400 °C for 4 hours in an air atmosphere to obtain Fe / SAPO-11 molecular sieve;

[0030] Take a certain amount of manganese acetylacetonate and TS-1 molecular sieve (silicon to titanium ratio is 30), the content of manganese element accounts for 3% of the TS-1 molecular sieve, heat the manganese acetylacetonate to sublimation, and the steam after sublimation is mixed with TS-1 molecular sieve. Mn / TS-1 molecular sieve was obtained by reacting at 350℃ for 8h;

[0031] Catalyst A was obtained by mixing Fe / SAPO-11 molecular sieve and Mn / TS-1 molecular sieve in a mass ratio of 4:1.

[0032] Catalyst B:

[0033] A certain amount of SAPO-34 molecular sieve was immersed in a ferri...

Embodiment 2

[0053] 10 g of catalyst A was placed in a fixed bed under N 2 Pretreatment at 300 °C for 2 h in an atmosphere. Glyoxal space velocity is 1.5h -1 , the glyoxal concentration is 10wt%, N 2 The molar ratio of O and glyoxal was 8, and the reaction was carried out under the condition of normal pressure of 200°C. After the reaction was stabilized for 5 h, the product was analyzed by gas chromatography.

Embodiment 3

[0055] 10 g of catalyst B was placed in a fixed bed under N 2 Pretreatment at 300 °C for 2 h in an atmosphere. Glyoxal space velocity is 0.8h -1 , 20% glyoxal concentration, N 2 The molar ratio of O and glyoxal was 18, and the reaction was carried out under the condition of normal pressure of 280°C. After the reaction was stabilized for 5 h, the product was analyzed by gas chromatography.

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PUM

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Abstract

The invention discloses a novel glyoxylic acid synthesis method. Glyoxylic acid is prepared by oxidizing glyoxal with N2O under the action of a catalyst. The catalyst is formed by mixed loading of a Fe / SAPO molecular sieve and a Mn / TS-1 molecular sieve. The invention provides a process for preparing glyoxylic acid by catalytically oxidizing glyoxal with N2O for the first time, and the prepared catalyst has higher product selectivity and good stability and can be used for continuous fixed bed reaction or intermittent tank reactors.

Description

technical field [0001] The present invention relates to a kind of novel preparation method of glyoxylic acid, with N 2 O is the oxidant to catalyze the oxidation of glyoxal to obtain glyoxylic acid. Background technique [0002] Glyoxylic acid is the simplest keto acid composed of an aldehyde group and a carboxyl group. It is also an important organic chemical intermediate. It is widely used in the fields of synthetic fragrances, medicine, cosmetics, and fine chemicals. [0003] At present, there are three main process routes for the synthesis of glyoxylic acid. Among them, the ozone method selects maleic anhydride as the raw material, the production process is clean and pollution-free, the selectivity of the product is high, and high-purity products can be obtained; however, the preparation of ozone requires a lot of electric energy, and the production cost is high. The second is the oxalic acid electrolytic reduction method. The raw materials of this method are easy to o...

Claims

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Application Information

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IPC IPC(8): C07C51/27C07C59/147B01J29/80B01J37/02B01J37/08B01J37/10
CPCC07C51/27B01J29/80B01J37/0201B01J37/088B01J37/10B01J29/85B01J29/48B01J2229/18C07C59/147
Inventor 范立耸王锐付松丁大康冯民昌李俊平
Owner WANHUA CHEM GRP CO LTD