Method for hydrolyzing glycolic acid ester based on carbonic acid system as traceless catalyst

A glycolic acid ester and catalyst technology, applied in the preparation of carboxylate/lactone, reagents, organic chemistry, etc., can solve problems such as environmental hazards, greenhouse effect, CO2 emissions, etc., to avoid strong corrosion and toxicity , the effect of simple operation

Active Publication Date: 2022-02-18
上海卓笙环保科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Industry usually burns this by-product, but results in additional CO2 emissions
In view of the fact that excessive carbon emissions not only cause harm to the environment, but also lead to the greenhouse effect, how to convert abundant and cheap CO2 into usable resources or use it as a renewable reagent to drive chemical conversion has become a hot issue of concern.

Method used

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  • Method for hydrolyzing glycolic acid ester based on carbonic acid system as traceless catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0025] A 250 mL Hastelloy reactor was charged with 8 g of methyl glycolate (89 mmol) and 9 g of water (500 mmol). The vessel was then tightly sealed and attached to the reactor unit with 2 MPa of CO 2 Purge 3 times, then with CO 2 Saturation until the pressure remains stable at 1.5MPa. While stirring at 800 rpm, the vessel was heated to 100° C., where the reaction was continued for 3 h; the maximum pressure reached at this temperature was 6.5 MPa. After this time, the solution was cooled to ambient temperature, gas was released, and stirring was stopped. The resulting product was then analyzed by GC / MS, which indicated a glycolic acid yield of 65%;

Embodiment 2

[0027] A 250 mL Hastelloy reactor was charged with 8 g of methyl glycolate (89 mmol) and 9 g of water (500 mmol). The vessel was then tightly sealed and attached to the reactor unit with 2 MPa of CO 2 Purge 3 times, then with CO 2 Saturation until the pressure remains stable at 2MPa. While stirring at 800 rpm, the vessel was heated to 120° C., where the reaction was continued for 5 h; the maximum pressure reached at this temperature was 6.5 MPa. After this time, the solution was cooled to ambient temperature, gas was released, and stirring was stopped. The resulting product was then analyzed by GC / MS, which indicated a glycolic acid yield of 85%.

Embodiment 3

[0029] A 250 mL Hastelloy reactor was charged with 8 g of methyl glycolate (89 mmol) and 9 g of water (500 mmol). The vessel was then tightly sealed and attached to the reactor unit, purged 3 times with 2 MPa of CO , then with CO 2 Saturation until the pressure remains stable at 2MPa (water absorbs a considerable amount of CO 2 ). While stirring at 800 rpm, the vessel was heated to 150° C., where the reaction was continued for 3 h; the maximum pressure reached at this temperature was 7.5 MPa. After this time, the solution was cooled to ambient temperature, gas was released, and stirring was stopped. The resulting product was then analyzed by GC / MS, which indicated a 90% yield of glycolic acid.

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Abstract

The invention discloses a method for hydrolyzing glycolic acid ester based on a carbonic acid system as a traceless catalyst. The method comprises the following specific preparation steps: S1, adding glycolic acid ester and water into a reaction kettle; S2, introducing carbon dioxide into the reaction kettle to replace air in the kettle three times; S3, raising the temperature, introducing carbon dioxide into the kettle, continuously carrying out the stirring reaction, and stopping stirring when the reaction is finished; S4, cooling the reaction mixture; and S5, carrying out qualitative analysis by using a gas chromatograph-mass spectrometer, and carrying out quantitative analysis by using gas chromatography. According to the invention, under the condition that no other exogenous acid catalyst exists, glycolic acid is prepared by catalyzing a glycolic acid ester aqueous solution through pressurized CO2, a weakly acidic carbonic acid system formed in situ under the reaction condition is used as the catalyst, and after the reaction is finished, the required product can be directly obtained by utilizing the characteristic that the carbonic acid system is spontaneously decomposed into water and CO2 during pressure reduction, so that the step and process of separating the product from the homogeneous / heterogeneous catalyst are omitted, the operation is simple, and the process is efficient and safe.

Description

technical field [0001] The invention relates to the field of synthetic methods of glycolic acid, in particular to a method for hydrolyzing glycolate based on a carbonic acid system as a traceless catalyst. Background technique [0002] Glycolic acid, also known as glycolic acid, is an important fine chemical intermediate, which is increasingly widely used in the fields of chemical industry, medicine, textile and metallurgy. At present, chemical methods such as chloroacetic acid method, cyanidation method and formaldehyde carbonylation are generally used in industry to obtain glycolic acid. alkali, high temperature and high pressure), high requirements for reaction equipment, complicated separation and purification, and serious environmental pollution, which do not conform to the current concept of sustainable development of low carbon and environmental protection. [0003] The current conventional method for converting glycolate to glycolic acid involves the reaction of a s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/09C07C59/06
CPCC07C51/09C07C59/06Y02P20/141
Inventor 席秋波王维君
Owner 上海卓笙环保科技有限公司
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