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Method for preparing methyl methoxyacetate from methanol-containing methylal

A technology of methyl methoxyacetate and methylal is applied in the preparation of organic compounds, the preparation of carbon monoxide or formate reaction, the preparation of carboxylate, etc., to achieve the effects of convenient source of raw materials, less pollution and less by-products

Active Publication Date: 2017-02-15
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0027] 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 rectification process conditions, the obtained product still contains a certain amount of methanol, so it is necessary to obtain 100 % Methanol-free pure DMM is not possible with current technology

Method used

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  • Method for preparing methyl methoxyacetate from methanol-containing methylal
  • Method for preparing methyl methoxyacetate from methanol-containing methylal
  • Method for preparing methyl methoxyacetate from methanol-containing methylal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Weigh 2L of methylal (DMM) containing a certain amount of methanol (2%, 5%, 10%, 15%, 20% (mass fraction)), 100 g of solid acid catalyst, and 320 g of paraformaldehyde 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 (6.0 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 1.

[0050]

[0051] As can be seen from Table 1, with the increase of methanol content, the conversion rate of raw material DMM and ...

Embodiment 2

[0053] Weigh 2 L of methylal (DMM) containing 10% methanol, 100 g of solid acid catalyst, and a certain mass of paraformaldehyde (8, 16, 80, 160, 320, 480, 640, 800 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 (6.0 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.

[0054]

[0055] As can be seen from Table 2, along with the increase of paraformaldehyde addition, the DMM conversion rate also increas...

Embodiment 3

[0058] Add 100 g of solid acid catalyst in the reactor, 2 L of reaction raw material DMM containing 10% methanol, 320 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 6.0 MPa pure CO gas. The reaction time 6 h, the reaction temperatures were 90, 100, 110, 130, 140°C, respectively. The reaction results are shown in Table 3.

[0059]

[0060] According to Table 3, it can be seen that with the increase of temperature (90, 100, 110, 120, 130°C), the conversion rate of raw material DMM is continuously increasing. When the reaction temperature is 130°C, the conversion rate of DMM is the highest at 99.90...

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Abstract

A method for preparing methyl methoxyacetate from methanol-containing methylal relates to a method for preparing the methyl methoxyacetate. According to the method, the influence of trace methanol in raw materials on carbonylation is eliminated by adding formaldehyde compounds into an industrial raw material, namely the methylal, so that the selectivity and the yield of the main product, namely the methyl methoxyacetate, are higher; the formaldehyde compounds are added during carbonylation of methanol-containing methylal; the formaldehyde substances are one or more paraformaldehyde mixtures of trioxymethylene, tetraoxymethylene or paraformaldehyde; the mass ratio of the added formaldehyde to the raw material methylal is 0.5% to 50%; the reaction temperature is 90 to 160 DEG C and the reaction pressure is 3.0 to 10.0 MPa. According to the method, the influence of the methanol on DMM carbonylation is eliminated by adding a small amount of formaldehyde compounds into the raw material methylal, so that treatment is simple and convenient after reaction, environmental pollution is low, and a new thought and a new 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 with methylal containing methanol as a raw material. 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 glycol...

Claims

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Application Information

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IPC IPC(8): C07C67/37C07C67/62C07C67/60C07C69/708
CPCC07C67/37C07C67/60C07C67/62C07C69/708
Inventor 石磊陈飞梁言姚杰王玉鑫
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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