Method for preparing methyl methoxyacetate by industrial aqueous raw material methylal

A technology for the preparation of methyl methoxyacetate and methylal, applied in the directions of carbon monoxide or formate reaction preparation, organic chemistry, etc., can solve problems such as impossibility, and achieve low pollution, convenient source of raw materials, and few by-products. Effect

Active Publication Date: 2017-03-22
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0029] The acetal reaction of methanol and formaldehyde under the action of a catalyst to prepare methylal is still the current mainstream process route, but according to the best rectifi

Method used

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  • Method for preparing methyl methoxyacetate by industrial aqueous raw material methylal
  • Method for preparing methyl methoxyacetate by industrial aqueous raw material methylal
  • Method for preparing methyl methoxyacetate by industrial aqueous raw material methylal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Weigh 2 L of water-containing 2% methylal (DMM), 100 g of solid acid catalyst, and a certain mass of paraformaldehyde (0.0, 1.0, 3.0, 6.0, 12.0, 25.0, 35.0, 50.0, 60.0 g) into the reactor middle. Then pass in 1.0 MPa carbon monoxide gas, if there is no leak, after emptying the gas in the kettle, repeat the above operation twice (replace the air in the reaction kettle). Introduce a certain amount of gas (6.0MPa) 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 5 MPa CO gas again. , heated up, the stirring speed of the reactor was 500 rpm, the reaction pressure was 5 MPa, the reaction temperature was 110°C, and the reaction time was 6 h. The reaction results are shown in Table 1.

[0054] Table 1 Effects of different paraformaldehyde additions on the carbonylation reaction of 2% DMM in water

[0055]

[0056]...

Embodiment 2

[0058] Weigh 2 L of 10% methylal (DMM) containing water, 100 g of solid acid catalyst, and a certain mass of paraformaldehyde (0.0, 2.0, 6.0, 12.0, 25.0, 50.0, 70.0, 100.0, 120.0 g) in a reaction kettle. Then pass in 1.0 MPa carbon monoxide gas, if there is no leak, after emptying the gas in the kettle, repeat the above operation twice (replace the air in the reaction kettle). 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 5 MPa CO gas again. , heated up, the stirring speed of the reactor was 500 rpm, the reaction pressure was 5 MPa, the reaction temperature was 110 °C, and the reaction time was 6 h. The reaction results are shown in Table 2.

[0059] Table 2 Effects of different amounts of paraformaldehyde added on the carbonylation reaction of 10% DMM in water

[0060] ...

Embodiment 3

[0064] Add 100 g of solid acid catalyst into the reaction kettle, 2 L of reaction raw material DMM containing 2% water, and 12 g of paraformaldehyde. Then pass in 1.0 MPa carbon monoxide gas, if there is no leak, after emptying the gas in the kettle, repeat the above operation twice (replace the air in the reaction kettle). Introduce a certain amount of gas (6.0 MPa) again for leak detection, and let it stand for 15 minutes. If the pressure indicator does not drop, it means that the device has no air leakage. Then empty the gas in the kettle and inject 5 MPa pure CO gas. The reaction time 6 h, the reaction temperatures were 90, 100, 110, 130, 140°C, respectively.

[0065] Table 3 Effect of different reaction temperatures on the carbonylation reaction of DMM

[0066]

[0067] According to Table 3, it can be seen that with the increase of temperature, the conversion rate of raw material DMM increases continuously. When the reaction temperature is 140 °C, the conversion rate ...

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Abstract

The invention discloses a method for preparing methyl methoxyacetate by an industrial aqueous raw material methylal, and relates to the method for preparing methyl methoxyacetate. According to the method, influence of water on a carbonylation reaction is alleviated by adding a formaldehyde compound to the raw material, and the selectivity of the main product methyl methoxyacetate is improved; the preparation method includes the following process: the formaldehyde compound is added in the methylal carbonylation reaction. Under a condition without use of a solvent, provided is a brand-new methyl methoxyacetate production technological route, by adding a small amount of the formaldehyde compound to the aqueous methylal raw material, influence of trace water is removed in the methylal carbonylation reaction process, and the conversion rate of the raw material and the selectivity of the main product methyl methoxyacetate are significantly improved. The process is simple, the conversion efficiency of a catalyst after treatment is high, sources of the raw material are convenient, the amount of by-products is low, reaction posttreatment is simple, the environmental pollution is small, and a new idea and method are provided for large-scale industrialized production.

Description

technical field [0001] The invention relates to a method for preparing methyl methoxyacetate, in particular to a method for preparing methyl methoxyacetate by using industrial water-containing raw material methylal. Background technique [0002] Methyl methoxyacetate is a colorless transparent liquid with the molecular formula CH 3 OCH 2 COOCH 3 , molecular weight 104.1 English name: Methyl methoxyacetate, referred to as MMAc in industry, boiling point 129-130 ℃, flash point 35 ℃, relative density 1.0511, refractive index 1.3960, soluble in ethanol and ether, soluble in acetone, slightly soluble in water. [0003] Methyl methoxyacetate (MMAc) is an important organic chemical raw material, which can be used for the dynamic resolution of chiral amine compounds, the synthesis of vitamin B6 and sulfa-5-pyrimidine; more importantly, methoxy Methyl acetate (MMAc) can be used as an intermediate product for the further preparation of ethylene glycol monomethyl ether and ethylene...

Claims

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Application Information

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IPC IPC(8): C07C67/37C07C69/708
CPCC07C67/37C07C69/708
Inventor 石磊龚页境王玉鑫
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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