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Methoxyactic acid preparation method

A technology of methoxyacetic acid and oxygen, applied in the preparation of carboxylates, organic compounds, chemical instruments and methods, etc., can solve the problems of corrosion, high comprehensive production cost, cumbersome process flow, etc., and achieve mild reaction conditions, Easy operation and high catalytic efficiency

Inactive Publication Date: 2015-09-09
HUBEI UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Patent US4968840 discloses a method for preparing methoxyacetic acid by substitution reaction. The method uses methanol as a solvent. Chloroacetic acid reacts with sodium methylate under heating conditions. After the reaction, methanol is removed, methyl methoxyacetate is added, and Dry hydrogen chloride gas is used for acidification. The preparation method has a cumbersome process, and the acidification process takes a long time. The hydrogen chloride gas severely corrodes the production equipment, which brings great pressure to equipment maintenance, and the overall cost of production is high.
[0004] Patent CN101979372 discloses a method for preparing methoxyacetic acid through an oxidation reaction. The method uses ethylene glycol monomethyl ether as a raw material, industrial nitric acid as an oxidant, and performs an oxidation reaction under the catalysis of copper chloride. The amount of nitric acid required for the reaction is The amount is 1.2-3 times that of ethylene glycol monomethyl ether, the excess nitric acid is difficult to recover, and the nitrogen oxide gas produced by the reaction is difficult to purify, polluting the environment
[0005] In view of the deficiencies of the above two types of synthetic methods, especially on the serious damage to equipment and the pollution of the environment, it is urgent to design a more simple, safe and environmentally friendly methoxyacetic acid production process to adapt to the requirements of modern industrial production

Method used

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  • Methoxyactic acid preparation method

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Experimental program
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Effect test

Embodiment 1

[0023] Add 30 mL (28.8 g) of ethylene glycol monomethyl ether, 40 mL of deionized water and 0.25 g of Pt(5wt%) / C catalyst into the autoclave, adjust O 2 The pressure keeps the pressure of the reactor at 0.6 MPa and reacts at 70℃ for 7 hours. After the reactor is cooled to room temperature, the catalyst is filtered and washed to recover the catalyst. The filtrate is distilled under reduced pressure to collect the 92-94℃ / 10 ​​mmHg fraction to obtain the methoxy group. Acetic acid is 30.35g, the yield is 91%, and the purity is 99%.

Embodiment 2

[0025] Add 30 mL (28.8 g) of ethylene glycol monomethyl ether, 30 mL of deionized water and 0.15 g of Pt(5wt%) / C catalyst into the autoclave, adjust O 2 The pressure keeps the pressure of the reactor at 0.5 MPa and reacts at 60℃ for 6 hours. After the reactor is cooled to room temperature, the catalyst is filtered and washed to recover the catalyst. The filtrate is distilled under reduced pressure to collect the 92-94℃ / 10 ​​mmHg fraction to obtain the methoxy group. Acetic acid is 30.69 g, the yield is 90%, and the purity is 99%.

Embodiment 3

[0027] Put 30 mL (28.8 g) of ethylene glycol monomethyl ether, 45 mL of deionized water and 0.32 g of Pt(5wt%) / C catalyst in the autoclave, and adjust O 2 The pressure keeps the pressure of the reactor at 0.8 MPa, and reacts at 80℃ for 6 hours. After the reactor is cooled to room temperature, the catalyst is filtered and washed to recover the catalyst. The filtrate is distilled under reduced pressure to collect the 92-94℃ / 10 ​​mmHg fraction to obtain the methoxy group. Acetic acid 31.37 g, yield 92%, purity 99%.

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Abstract

The present invention relates to a methoxyactic acid preparation method, wherein Pt / C is adopted as a catalyst, oxygen is adopted as an oxidant, water is adopted as a solvent, and 2-methoxyethanol oxidation is performed to prepare the methoxyactic acid in a one-step manner. Compared with the method in the prior art, the method of the present invention has the following advantages that (1) the used solvent is the water with characteristics of low price, easy obtaining and green environmental protection, such that environment pollution can not generated; (2) the used catalyst Pt / C has the high catalysis efficiency, and can be reused only through the simple filtration after completing the reaction; (3) the reaction conditions are mild, and the operation is operate; and (4) the used oxidant is the O2 with characteristics of safety, environmental protection, low price and easy obtaining, such that waste gas and waste liquid can not be generated.

Description

Technical field [0001] The invention relates to a method for preparing methoxy acetic acid, in particular to a method for preparing methoxy acetic acid using Pt / C as a catalyst, oxygen as an oxidant, and water as a solvent. Background technique [0002] Methoxyacetic acid is an important organic chemical raw material. It synthesizes the valuable intermediate methyl methoxyacetate through esterification reaction with methanol. This intermediate can be used for the kinetic resolution of chiral amine compounds. , And can be used for vitamin B 6 , Sulfa-5-pyrimidine, etc.; In addition, methoxyacetic acid can also be used to prepare methoxyacetyl chloride, which has important uses in plant protection and pharmaceutical industry. At present, the preparation of methoxy acetic acid mainly takes two ways: substitution reaction and oxidation reaction. [0003] Patent US4968840 discloses a method for preparing methoxy acetic acid by substitution reaction. The method uses methanol as a solven...

Claims

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Application Information

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IPC IPC(8): C07C51/235C07C59/125
CPCC07C51/235C07C59/125
Inventor 聂俊琦李雄王亦鸣乐勇军杨桂春卢翠芬
Owner HUBEI UNIV
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