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Continuous synthesis method for methyl methoxyacetate

A technology of methyl methoxyacetate and synthesis method, which is applied in the direction of carbon monoxide or formate reaction preparation, climate sustainability, sustainable manufacturing/processing, etc., and can solve the problem of large amount of wastewater treatment, difficult product separation, and unfavorable industrialization Production and other issues, to achieve the effect of low-cost large-scale industrialization, simple operation mode, and significant cost advantages

Inactive Publication Date: 2012-10-03
东莞市同舟化工有限公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

The first method uses a homogeneous catalyst, such as sulfuric acid, sulfamic acid, methanesulfonic acid, etc., and is carried out under the synergistic catalysis of metal carbonyls, which has the disadvantages of equipment corrosion, difficult catalyst recycling, and difficult product separation; the second method The third method has disadvantages such as the use of a large amount of alkali and the large amount of wastewater treatment; the third method has poor reaction selectivity or great environmental impact, which is not conducive to industrial production

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  • Continuous synthesis method for methyl methoxyacetate

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Effect test

Embodiment 1

[0039] The technological process of the continuous synthesis method of methyl methoxyacetate is as figure 1 As shown, in the carbonylation reaction section: 85%wt methylal containing methanol and CO are mixed according to the molar ratio of methylal / CO of 1:1, and the weight ratio of methylal to reaction solvent is 1:1, according to The flow rate of methylal is 30ml / h, and it is continuously pumped into carbonylation reactor 1 equipped with a solid catalyst. The reaction temperature in carbonylation reactor 1 is 100°C and the reaction pressure is 3MPa. After the carbonylation reaction, the methylal The conversion rate is 82.35%wt, no products such as CO2 have been detected, relative to the converted methylal, the selectivity of methyl methoxyacetate is 60.56% mole, and the selectivity of methyl glycolate is 15.34% mole, The high boiling point polyester selectivity is 6.75% mole. In the catalytic rectification reaction section: the carbonylation reaction liquid and anhydrous m...

Embodiment 2

[0041] The technological process of the continuous synthesis method of methyl methoxyacetate is as figure 1As shown, in the carbonylation reaction section: 99.5%wt of methylal and CO are mixed according to the molar ratio of methylal / CO of 1:3, and the weight ratio of methylal to reaction solvent is 4:1. The flow rate is 30ml / h, and it is continuously pumped into the carbonylation reactor 1 equipped with a solid catalyst. The reaction temperature in the carbonylation reactor 1 is 150°C, and the reaction pressure is 10MPa. After the carbonylation reaction, the conversion rate of methylal It is 100%wt, and no products such as CO2 have been detected. Compared with the converted methylal, the selectivity of methyl methoxyacetate is 66.78% mole, and the selectivity of methyl glycolate is 1.23% mole. The ester selectivity is 23.58% mole. In the catalytic rectification reaction section: the carbonylation reaction liquid and anhydrous methanol are continuously fed into the catalytic ...

Embodiment 3

[0043] The technological process of the continuous synthesis method of methyl methoxyacetate is as figure 1 As shown, in the carbonylation reaction section: 99.5%wt of methylal and CO are continuously pumped at a methylal / CO molar ratio of 1:3, without using a reaction solvent, at a flow rate of 30ml / h of methylal In the carbonylation reactor 1 equipped with a solid catalyst, the reaction temperature in the carbonylation reactor 1 is 110°C, and the reaction pressure is 4MPa. After the carbonylation reaction, the conversion rate of methylal is 99.8%wt, and no CO2 is detected And other products, relative to the converted methylal, the selectivity of methyl methoxyacetate is 67.96% mole, the selectivity of methyl glycolate is 0.93% mole, and the selectivity of high boiling point polyester is 24.78% mole. In the catalytic rectification reaction section: the carbonylation reaction liquid and anhydrous methanol are continuously fed into the catalytic rectification tower 2 at a weigh...

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Abstract

The invention relates to a synthesis method for methyl methoxyacetate, in particular to a continuous synthesis method for the methyl methoxyacetate. The continuous synthesis method is characterized in that: methylal and CO are used as raw materials; carbonylation reaction is performed in a carbonylation reactor in which a catalyst is filled to obtain a methyl-glycolate-containing methyl methoxyacetate rough product; then a series of separation is performed to obtain a pure product of the methyl methoxyacetate; and the methylal is recovered from a separated light component byproduct and is returned to the carbonylation reactor to realize a continuous synthesis process, wherein the purity of the methylal and the molar ratio of the methylal to the CO are any values, and the reaction pressure in the carbonylation reactor is greater than or equal to normal pressure. According to the method, the production efficiency can be effectively increased, the production process can be simplified, the emission of waste residue and wastewater in a production process can bee reduced, and the aims of continuous production and reduction of the production cost are achieved.

Description

technical field [0001] The present invention relates to the synthesis method of methyl methoxyacetate, especially a kind of continuous synthesis method of methyl methoxyacetate. Background technique [0002] Methyl methoxyacetate is an important fine chemical intermediate, which is used as an intermediate of medicine, pesticide and dyestuff, among which it is an intermediate of sulfonamide and vitamin B6 in medicine, and can also be used as a solvent. The synthetic method of methyl methoxyacetate mainly contains following 3 kinds of methods at present: one, use trioxane or paraformaldehyde and methyl formate coupling reaction, generate methyl glycolate and methyl methoxyacetate; 2. Etherification synthesis with methyl chloroacetate and sodium methoxide as raw materials; 3. Synthesis with ethylene glycol monomethyl ether as raw material through oxidation reaction. The first method uses a homogeneous catalyst, such as sulfuric acid, sulfamic acid, methanesulfonic acid, etc., ...

Claims

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Application Information

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IPC IPC(8): C07C69/708C07C67/37
CPCY02P20/10Y02P20/584
Inventor 刘新泰黄胜飘司君华徐德超宋琪
Owner 东莞市同舟化工有限公司
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