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A kind of preparation method of easily degradable adipate polyethylene glycol polyester

A technology of polyethylene glycol polyester and polyethylene glycol, which is applied in the field of preparation of easily degradable polyethylene glycol adipate polyester, can solve the problems of loss of ethylene glycol and difficulty in making high molecular weight, and achieve improved High efficiency, cost reduction, and excellent smooth diffusion effect

Active Publication Date: 2018-06-05
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Wang Ying published "Synthesis of Polyethylene Glycol Ester" in chemical technology. Products using ethylene glycol as raw materials have loss of ethylene glycol, and it is difficult to make high molecular weight.

Method used

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  • A kind of preparation method of easily degradable adipate polyethylene glycol polyester
  • A kind of preparation method of easily degradable adipate polyethylene glycol polyester

Examples

Experimental program
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Effect test

preparation example Construction

[0028] In the preparation method of the present embodiment, the esterification reaction equation is:

[0029]

[0030] m:n=1:1-2.

[0031] The method of adding while stirring is used for compounding to add the remaining polyethylene glycol.

Embodiment 1

[0033] Add 528 grams of polyethylene glycol with a molecular weight of 528 and 146 grams of adipic acid in the flask, add 1.3 grams of p-toluenesulfonic acid and 0.4 grams of phosphorous acid catalyst under stirring, heat up to 135 ° C in 4 hours, vacuum -0.096MPa in time to remove the generated Water, keep warm for 3 hours under the reaction conditions of 135-140°C, then cool down to 80°C, add 264 grams of polyethylene glycol, stir at 70-80°C for 1 hour, and get slightly yellow (color less than 50 platinum-cobalt standard) Transparent product. This embodiment has the advantages of reasonable process, simple operation, stable product, excellent smooth diffusion lubricity, good isolation and demoulding effect, and easy biodegradation.

[0034] Get product concentration and be that 10% aqueous solution 50ml is packed in the 250ml Erlenmeyer flask, add 25% inoculum amount, shake table treatment at 30 ℃ for 5h, measure COD, calculate degradation rate 58.2%.

Embodiment 2

[0038] Add 528 grams of polyethylene glycol with a molecular weight of 528 and 146 grams of adipic acid in the flask, add 1.3 grams of p-toluenesulfonic acid and 0.4 grams of phosphorous acid catalyst under stirring, heat up to 135 ° C in 4 hours, vacuum -0.096MPa in time to remove the generated Water, keep warm at 135-140°C for 3 hours, then cool down to 80°C, add 422 grams of polyethylene glycol, stir at 70-80°C for 1 hour, and get slightly yellow (color less than 50 platinum-cobalt standard) Transparent product. This embodiment has the advantages of reasonable process, simple operation, stable product, excellent smooth diffusion lubricity, good isolation and demoulding effect, and easy biodegradation.

[0039] Take 50ml of aqueous solution with product concentration of 10% and put it in a 250ml Erlenmeyer flask, add 25% inoculum, treat it on a shaking table at 30°C for 5h, measure COD, and calculate the degradation rate of 67.8%.

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Abstract

The invention relates to a preparation method of easy-to-degrade adipic acid polyethylene glycol polyester and belongs to the technical field of ester compounds in organic chemistry. The preparation method includes: adding part of polyethylene glycol into adipic acid, stirring, adding a catalyst, and raising temperature; removing generated water in a vacuum condition, holding temperature of 120-140 DEG C for reaction for 2-5h, lowering temperature, adding remaining polyethylene glycol, and stirring at 70-80 DEG C for 0.5-2.5h to obtain a finished product. When being applied to adipic acid polyethylene glycol polyester, the preparation method has the advantages that the process is reasonable, operation is simple, and the product is stable, short in reaction period and shallow in color.

Description

technical field [0001] The invention relates to a preparation method of easily degradable adipate polyethylene glycol polyester, which belongs to the technical field of ester compound preparation in organic chemistry. Background technique [0002] Adipic acid polyethylene glycol polyester is a kind of polymer used as a diffusion lubricant in metal cutting, and used as a release agent in rubber production. It has good smoothness, dispersion, isolation and release, and has a good Environmentally friendly, it has a better release effect than polyethylene glycol alone. Due to the unique properties and wide application of oil surfactants, and the low toxicity and low irritation of oil products, the development and research of oil surfactants has attracted more and more attention. At the same time, improving the biodegradability of surfactants is an important guarantee for realizing a good cycle of the ecological environment. [0003] There are many reports on the synthesis of a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/672C08G63/87C08G63/78
CPCC08G63/672C08G63/78C08G63/87C08G2230/00
Inventor 刘志湘金一丰万庆梅陈世明余渊荣
Owner ZHEJIANG HUANGMA TECH
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