Method for preparing methyl glycolate and haloalkane as byproduct

A technology of methyl glycolate and halogenated alkanes is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., and can solve the problems of affecting catalytic reaction performance, low conversion rate of raw materials, low product selectivity, etc., Achieve the effect of raw material conversion rate and high product selectivity, no environmental pollution, and short reaction path.

Active Publication Date: 2018-01-19
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 haloalkane as byproduct
  • Method for preparing methyl glycolate and haloalkane as byproduct
  • Method for preparing methyl glycolate and haloalkane as byproduct

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Weigh 200g of methyl methoxyacetate and 600g of hydroiodic acid (mass ratio 1:3) into the reaction kettle, and react at 40, 50, 60, 70, 80, 90, and 100°C for 5 hours respectively. The results are shown in Table 1.

[0048] Table 1 Effects of different reaction temperatures on the conversion of raw materials and product selectivity

[0049]

[0050] It can be seen from Table 1 that as the reaction temperature rises, the conversion rate of methyl methoxyacetate increases gradually, and the selectivity of MG also gradually increases. After 70°C, as the temperature rises, the selectivity of MG is basically stable and maintains at 98 ~99% range.

Embodiment 2

[0052] Under the condition of 80°C, methyl methoxyacetate and hydroiodic acid were added into the reactor according to the mass ratio of 1:0.5, 1:1, 1:1.5, 1:2, 1:3, and reacted for 5 hours. The reaction results are shown in the table 2.

[0053] Table 2 Effects of different raw material mass ratios on raw material conversion and product selectivity

[0054]

[0055] As can be seen from Table 2, as the mass ratio of methyl methoxyacetate to hydroiodic acid decreases, the conversion rate of methyl methoxyacetate increases and the selectivity of MG increases. The optimum mass ratio of iodic acid is 1:3.

Embodiment 3

[0057] Weigh 200 g of methyl methoxyacetate and 600 g of hydroiodic acid (mass ratio 1:3) into the reactor, and react at 80 °C for 0.5, 1, 2, 5, and 10 hours. The reaction results are shown in the table 3.

[0058] Table 3 Effects of different reaction times on the conversion of raw materials and product selectivity

[0059]

[0060] It can be seen from Table 3 that as the reaction time increases, the conversion rate of methyl methoxyacetate gradually increases, and the selectivity of MG first increases and then decreases. After 5 h, the selectivity of MG is the highest at 98.73%. The conversion rate of ethylene glycol monomethyl ether is basically stable, and the mass selectivity of MG tends to be stable at about 98%. So the best time for the reaction is 5h.

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Abstract

The invention relates to a method for preparing methyl glycolate and haloalkane as a byproduct, which relates to the method for preparing methyl glycolate. The method takes methoxyacetic acid methyl ester and halogen (or its hydride) as raw materials, and methyl glycolate and haloalkane as the byproduct are synthesized with high selectivity through an ether bond cracking reaction. During a synthesis route, halogen hydride is strong acid, and is taken as a reaction raw material and a reaction catalyst, compared with a traditional methyl glycolate synthesis technology, The reaction path of a brand new reaction route is short, reaction condition is mild, an extra catalyst is not required, separating problem of the catalyst is not existed, the byproduct is little, the raw material conversion rate and the product selectivity are high, no pollution is generated on environment during synthesis, and the method has the advantages of energy saving and environmental protection. When the mass ratio of methoxyacetic acid methyl ester to hydroiodic acid is 1:3, the reaction temperature is 80 DEG C, the reaction time is 5 h, the raw material methoxyacetic acid methyl ester conversion rate is 86.01%, and the product methyl glycolate selectivity can reach 98.02%.

Description

technical field [0001] The invention relates to a method for preparing methyl glycolate, in particular to a method for preparing methyl glycolate and by-producting halogenated alkanes. 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 pharmaceutical synthesis....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/675C07C67/31
Inventor 石磊王岩张冬喜陈飞姚杰
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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