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Method for preparing methyl glycolate and by-producing methyl methoxyacetate

A technology for by-producing methyl methoxyacetate and methyl glycolate is applied to the preparation of carboxylic acid by the reaction of carbon monoxide, the preparation of carbon monoxide or formate, and the preparation of carboxylate, which can solve the problem of polluting the environment and affecting the catalytic reaction performance. , low conversion rate of raw materials, etc., to achieve the effect of increasing the ratio of CO and aldehyde groups

Active Publication Date: 2017-11-10
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A.T.Bell et al. used methyl formate instead of gaseous CO and formaldehyde for carbonylation reaction, but since the decomposition of methyl formate and release of CO is a rate-controlling step, it affects the performance of the catalytic reaction
[0028] In summary, the current synthetic methods of methyl glycolate all have problems such as too long synthetic route, low raw material conversion rate or low product selectivity, and environmental pollution during the synthetic process.

Method used

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  • Method for preparing methyl glycolate and by-producing methyl methoxyacetate
  • Method for preparing methyl glycolate and by-producing methyl methoxyacetate
  • Method for preparing methyl glycolate and by-producing methyl methoxyacetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Weigh 20 kg of methylal (DMM), 300 g of NKC-9 catalyst, and 4 kg of water into the reactor. kg (the molar ratio of DMM to aldehyde group is 2:1), 7.8 kg (the molar ratio of DMM to aldehyde group is 1:1), 15.6 kg (the molar ratio of DMM to aldehyde group is 0.5:1), and then 1.0 MPa carbon monoxide gas is introduced, if After evacuating the gas in the kettle without leaking, repeat the above operation 2 times (replacing the air in the reactor). Introduce a certain amount of gas (6.0 MPa) again to test for leaks, and let it stand for 15 minutes. If the pressure indicator does not drop, it means that there is no air leakage in the device. Then empty the gas in the kettle and fill the kettle with 6.0 MPa CO gas again. , heated up, the stirring speed of the reactor was 500 rpm, the reaction pressure was 6.0MPa, the reaction temperature was 130°C, and the reaction time was 6 h. The effects of different ratios of DMM and aldehyde groups on the reaction are shown in Table 1.

...

Embodiment 2

[0062] Weigh 20 kg of methylal (DMM), 3.9 kg of paraformaldehyde (the molar ratio of DMM to aldehyde group is 2:1), and 300 g of Y molecular sieve catalyst are loaded into the reaction kettle, and the amount of water added is the mass of methylal, respectively. 3%, 5%, 10%, 20%, 30%, and then pass in 1.0MPa carbon monoxide gas. If there is no leakage, after emptying the gas in the kettle, repeat the above operation twice (replace the air in the reactor). Introduce a certain amount of gas (6.0 MPa) again to test for leaks, and let it stand for 15 minutes. If the pressure indicator does not drop, it means that there is no air leakage in the device. Then empty the gas in the kettle and fill the kettle with 6.0 MPa CO gas again. , heated up, the stirring speed of the reactor was 500 rpm, the reaction pressure was 6.0 MPa, the reaction temperature was 130°C, and the reaction time was 6 h. The reaction results are shown in Table 2.

[0063] The impact of the addition of table 2 diff...

Embodiment 3

[0068] Weigh 20 kg of methylal (DMM), 3.9 kg of paraformaldehyde (the molar ratio of DMM to aldehyde group is 2:1), 4 kg of water, and 300 g of phosphotungstic acid catalyst are loaded into the reaction kettle, and then 1.0 MPa Carbon monoxide gas, if there is no leakage, after emptying the gas in the kettle, repeat the above operation twice (replace the air in the reactor). Introduce a certain amount of gas (6.0 MPa) again to test for leaks, and let it stand for 15 minutes. If the pressure indicator does not drop, it means that there is no air leakage in the device. Then empty the gas in the kettle and fill the kettle with 6.0MPa CO gas again. , heated up, the stirring speed of the reactor was 500 rpm, the reaction pressure was 6.0 MPa, the reaction temperatures were 90°C, 100°C, 110°C, 130°C, 150°C, and the reaction time was 6 h. The reaction results are shown in Table 3.

[0069] Table 3 Effects of different reaction temperatures on the conversion of raw materials and produ...

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Abstract

The invention provides a method for preparing methyl glycolate and by-producing methyl methoxyacetate, and relates to a chemical industry raw material preparation method. According to the method, by using methylal as a solvent, using trioxymethylene, formaldehyde tetramer or paraformaldehyde and methylal as a formaldehyde source, and using a solid acid or a liquid acid as a catalyst, in the presence of a right amount of water in a system, methyl glycolate is subjected to one-step high-conversion-rate and high-selectivity synthesis and methyl methoxyacetate is by-produced. According to the present invention, the reaction system can be performed under a low water condition, and the methyl methoxyacetate is the high added value pharmaceutical intermediate, and has excellent solubility, wherein organic matters can be dissolved in the methyl methoxyacetate, and the methyl methoxyacetate can be dissolved in water at any proportions, so the dissolving of the formaldehyde can be promoted, the formaldehyde can be dissolved in the methyl methoxyacetate, and a lot of CO in the gas phase can be dissolved in the methyl methoxyacetate during the reaction process so as to make the surface of the catalyst in the liquid phase contact more CO so as to significantly improve the ratio of CO to the aldehyde group in the liquid phase.

Description

technical field [0001] The invention relates to a method for preparing chemical raw materials, in particular to a method for preparing methyl glycolate and producing methyl methoxyacetate by-product. Background technique [0002] Methyl glycolate (HOCH 2 COOCH 3 ), abbreviated as MG, is a colorless liquid with a pleasant smell, with a melting point of 74°C, a boiling point of 150°C, and a density of 1.168g / cm 3 , soluble in water, and soluble in alcohol and ether in any proportion. Methyl glycolate has α-H, hydroxyl and ester functional groups, so it has both the chemical properties of alcohols and esters, and can undergo carbonylation reactions, hydrolysis reactions, ammoniation reactions, oxidation reactions, etc. Methyl glycolate itself is an excellent solvent for many celluloses, resins and rubbers, and is easily soluble in nitrocellulose, cellulose acetate, polyvinyl acetate, etc. Methyl glycolate is also an important intermediate in organic synthesis and pharmaceut...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/675C07C67/08C07C67/37C07C69/708C07C51/12C07C59/06C07C41/56C07C43/30
CPCC07C41/56C07C51/12C07C67/08C07C67/37C07C59/06C07C43/30C07C69/675C07C69/708
Inventor 石磊陈飞姚杰
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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