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Preparation method of methyl glyoxylate

A technology of methyl glyoxylate and methyl glycolate is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., and can solve the problem of high catalyst cost, complex catalyst preparation, poor catalyst reusability, etc. problems, to reduce production costs, solve control and catalyst costs, and achieve good reusability

Inactive Publication Date: 2022-05-27
上海卿沅新材料科技有限公司
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  • Description
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AI Technical Summary

Problems solved by technology

The main technical problem to be solved is the problem of complex catalyst preparation, high catalyst cost and poor reusability of the catalyst in the process of preparing methyl glyoxylate from methyl glycolate in the prior art. The invention provides a A new catalyst preparation process for the selective oxidation of methyl glycolate to methyl glyoxylate

Method used

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Examples

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preparation example Construction

[0019] The present invention provides a technical solution: a method for preparing methyl glyoxylate. In a reaction kettle, methyl glycolate is added to prepare methyl glyoxylate by oxidation of a catalyst. The catalyst comprises the following components: Co 3 O 4 , CuO, MnO 2 As the active component, TiO 2 , CeO 2 , ZrO 2 As a carrier, the molar ratio of the active component to methyl glycolate is 1:100~1000.

[0020] The active component is non-precious metal oxide Co 3 O 4 , CuO, MnO 2 one or more of them. The carrier is TiO 2 , CeO 2 , ZrO 2 one or more of them.

[0021] The preparation method of the catalyst:

[0022] In the first step, the raw material salt of the active component and the precipitant oxalic acid or citric acid are weighed in proportion, and a certain proportion of the carrier is added, placed in a mechanical grinding tank, and stirred and mixed;

[0023] In the second step, the grinding balls of different materials are placed in the grinding...

Embodiment 1

[0028] Weigh basic copper carbonate, oxalic acid and CeO according to the loading of 10% 2 The carrier is placed in a grinding jar, and grinding balls of a certain quality are added, mixed with the raw materials evenly, adjusted to a speed of 800, ground for 4 hours, washed, vacuum dried overnight, and calcined at 400 °C for 4 hours;

[0029] Weigh 10 mmol of methyl glycolate in a 50 mL reactor, add 10 mL of anhydrous toluene, and be 1:500 feed intake according to the metal active component ratio to methyl glycolate, add a certain amount of catalyst, wash 0.5 MPa air, heated to 100 ℃, and reacted for 4 h, the conversion rate of methyl glycolate was 53%, and the selectivity of methyl glyoxylate was 89%.

example 2

[0031] Weigh basic copper carbonate, oxalic acid and CeO according to the loading amount of 20% 2 The carrier is placed in a grinding jar, and grinding balls of a certain quality are added, mixed with the raw materials evenly, adjusted to a speed of 800, ground for 4 hours, washed, vacuum dried overnight, and calcined at 400 °C for 4 hours;

[0032] Weigh 10 mmol of methyl glycolate in a 50 mL reactor, add 10 mL of anhydrous toluene, and be 1:500 feed intake according to the metal active component ratio to methyl glycolate, add a certain amount of catalyst, wash 0.5 MPa air, heated to 100 ℃, and reacted for 4 h, the conversion rate of methyl glycolate was 68%, and the selectivity of methyl glyoxylate was 85%.

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PUM

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Abstract

The invention discloses a preparation method of methyl glyoxylate, methyl glyoxylate is added, the methyl glyoxylate is prepared through oxidation of a catalyst, the catalyst comprises Co3O4, CuO and MnO2 as active components and TiO2, CeO2 and ZrO2 as carriers, and the molar ratio of the active components to the methyl glyoxylate is 1: (100-1000). The conversion rate of methyl glycolate reaches 93%, and the selectivity of methyl glyoxylate reaches 98%. The method can well solve the problems of selectivity control and catalyst cost in the prior art, and can be used for industrial production of methyl glyoxylate.

Description

technical field [0001] The application relates to a method for preparing methyl glyoxylate, which belongs to the field of chemical material preparation. Background technique [0002] In the process of coal-based synthesis gas to ethylene glycol, the efficient utilization of methyl glycolate as a by-product is of great significance to improve the process efficiency of synthesis gas to ethylene glycol and reduce the production cost of glyoxylic acid. At present, an important way to use methyl glycolate is to convert it into downstream chemicals such as glycolic acid, methyl malonate, glycine, and methyl glyoxylate, and the way to convert it to methyl glyoxylate is particularly noteworthy. . Because the glyoxylic acid obtained by one-step hydrolysis of methyl glyoxylate is widely used in the preparation of medicines, cosmetics, perfumes, and agricultural chemicals, it plays a very important role in chemical synthesis and is a very important fine chemical product. [0003] The...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/313C07C69/716B01J23/75B01J23/83B01J23/889
CPCC07C67/313B01J23/002B01J23/83B01J23/8892B01J23/75B01J2523/00C07C69/716B01J2523/17B01J2523/72B01J2523/845B01J2523/47B01J2523/48Y02P20/584
Inventor 王佳青
Owner 上海卿沅新材料科技有限公司
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