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Method for simultaneously preparing methyl methoxyacetate and methyl glycolate

A technology of methyl methoxyacetate and methyl glycolate, which is applied in the field of simultaneous preparation of methyl methoxyacetate and methyl glycolate, can solve the problems of inorganic acid pollution, difficult separation of products, corrosion, etc., and achieve non-corrosion The effect of reaction equipment, saving reaction cost, and easy separation and recovery

Pending Publication Date: 2022-05-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the serious pollution of inorganic acids, and problems such as difficult separation of products and corrosion of equipment, the development of new catalysts and new processes has become the research focus of formaldehyde carbonylation

Method used

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  • Method for simultaneously preparing methyl methoxyacetate and methyl glycolate
  • Method for simultaneously preparing methyl methoxyacetate and methyl glycolate
  • Method for simultaneously preparing methyl methoxyacetate and methyl glycolate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1. Carbonylation reaction

[0031] In a stainless steel autoclave with a volume of 100mL, add 8.1g (0.1mol HCHO) of formaldehyde aqueous solution (Shanghai test, containing about 37% formaldehyde and 10% methanol), cyclohexane:isobutyric acid=5:1 (molar ratio ) mixed solvent 50mL. Quickly weigh 0.185 g (0.2 mmol, CAT / HCHO=0.2%) of tris(triphenylphosphine)rhodium carbonyl hydride and put it into the kettle, stir and mix well, then seal the reaction kettle, replace the air in the kettle with CO for 3 times, Introduce high-pressure CO to 7MPa, and react at 120°C for 3h. After the reaction was over, the reactor was cooled to room temperature, all the reaction solution was taken out and placed in a separatory funnel, and left to stand until the layers were separated, such as figure 1 shown. Filter the dark liquid in the lower layer through a microporous membrane to obtain a light brown-yellow carbonylation product, which is set aside.

[0032] 2. Esterification reaction ...

Embodiment 2

[0036] 1. Recovery of reaction solvent

[0037] The upper layer of the liquid after the carbonylation reaction in Example 1 was taken out, filtered through a microporous membrane, and set aside.

[0038] 2. Carbonylation reaction

[0039] Put the filtered upper solvent into a 100mL stainless steel autoclave, add 8.1g (0.1mol formaldehyde) of formaldehyde aqueous solution (Shanghai test, containing about 37% formaldehyde and 10% methanol), and add 8mL of isobutyric acid. Quickly weigh 0.185 g (0.2 mmol, CAT / HCHO=0.2%) of tris(triphenylphosphine)rhodium carbonyl hydride and put it into the kettle, stir and mix well, then seal the reaction kettle, replace the air in the kettle with CO for 3 times, Introduce high-pressure CO to 7MPa, and react at 120°C for 3h. After the reaction, the reactor was cooled to room temperature, all the reaction solution was taken out and placed in a separatory funnel, and allowed to stand until the layers were separated. Filter the dark liquid in th...

Embodiment 3

[0044] 1. Carbonylation reaction

[0045] In a stainless steel autoclave with a volume of 100mL, add 5.5g (containing 0.1mol formaldehyde) of formaldehyde aqueous solution (Shanghai test, containing about 55% formaldehyde and 15% methanol), n-octane:isobutyric acid=2:1 (mol than) mixed solvent 50mL. Quickly weigh 0.196 g (0.4 mmol, CAT / HCHO=0.4%) of triphenylphosphinecarbonyl rhodium acetylacetonate into the kettle, stir and mix well, then seal the reaction kettle, replace the air in the kettle with CO for 3 times, and inject High pressure CO to 7MPa, react at 120°C for 3h. After the reaction, the reactor was cooled to room temperature, all the reaction solution was taken out and placed in a separatory funnel, and allowed to stand until layers were separated. Filter the lower layer liquid through a microporous membrane to obtain the carbonylation product, which is set aside.

[0046] 2. Esterification reaction

[0047] Put the filtered carbonylation product of the lower la...

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Abstract

The invention relates to a method for simultaneously preparing methyl methoxyacetate and methyl glycolate, which comprises the following steps: under the action of a carbonyl rhodium catalyst, carrying out carbonylation reaction on a formaldehyde monomer source substance containing methanol and CO in a mixed solvent; and adding methanol into the solvent-removed product to carry out esterification reaction to generate methyl methoxyacetate and methyl glycolate. The method has the characteristics that the cheap and easily available formaldehyde aqueous solution is adopted as the raw material, trioxymethylene or paraformaldehyde does not need to be adopted as a formaldehyde monomer source, the catalyst is non-corrosive to reaction equipment, and direct separation of a product and a solvent can be realized before esterification reaction.

Description

technical field [0001] The invention relates to the field of petrochemical industry, in particular to a method for simultaneously preparing methyl methoxyacetate and methyl glycolate. Background technique [0002] Methyl methoxyacetate is a very valuable intermediate, which can be used in the dynamic resolution of chiral amine compounds, the synthesis of vitamin B6 and sulfa-5-pyrimidine, etc., as a catalyst in polymerization reactions, and can also be used through Ethylene glycol is obtained by hydrogenation and hydrolysis, which is an important precursor of ethylene glycol. As an important organic chemical raw material, methyl glycolate can be widely used in the fields of chemical industry, polymer materials, pesticides, medicine, spices, feed and dyes. At the same time, methyl glycolate is also an important intermediate for coal-to-ethylene glycol. [0003] The synthesis methods of methyl methoxyacetate mainly include carbonylation method (using dimethoxymethane or form...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/675C07C69/708
CPCC07C67/08C07C51/12C07C51/367C07C69/675C07C69/708C07C59/06C07C59/125
Inventor 王迪吕建刚刘波周海春金萍许烽
Owner CHINA PETROLEUM & CHEM CORP
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