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Preparation method of modified polyethylene glycol adipate

A technology of polyethylene glycol ester and polyadipate, which is applied in the field of preparation of modified polyethylene adipate, can solve the problems of difficulty in improving biodegradability, and achieve simple equipment, mild reaction conditions, The effect of saving equipment cost and energy consumption

Active Publication Date: 2021-01-01
ZHEJIANG HUANGMA TECH +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Polyethylene glycol adipate, polyethylene glycol-polyadipate anhydride, and polyethylene glycol adipate polyester are all polymers with complex structures, and their biodegradability is compared to other ester products and Alkyl ethers are more difficult to improve

Method used

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  • Preparation method of modified polyethylene glycol adipate

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[0025] A preparation method of modified poly(ethylene glycol adipate), which comprises the following steps: adding lactic acid to polyethylene glycol at a molar ratio of polyethylene glycol: lactic acid=1.5 to 3.0:1, and adding under stirring Catalyst, heat up; remove the generated water under vacuum conditions of 600-700mbar, keep warm at 80-85°C for 1-2h, heat up to 100-120°C within 3-4h, keep warm for 1-3h; according to adipic acid: lactic acid = Add adipic acid at a molar ratio of 1.0 to 2.0:1, keep warm for 1 to 3 hours at a temperature of 160 to 165°C, adjust the vacuum to less than 10mbar, keep warm for 2 to 5 hours, and then cool down to 75 to 80°C, that is A modified polyethylene adipate was obtained.

[0026] In the above method, the molecular weight of polyethylene glycol is 200-600; the lactic acid is L-lactic acid; the catalyst is a mixture of methanesulfonic acid and phosphorous acid, wherein the weight ratio of methanesulfonic acid and phosphorous acid is 1:0.05...

Embodiment 1

[0030] Add 900 grams of polyethylene glycol with a molecular weight of 600 in the flask, add a catalyst of 90 grams of lactic acid, 5.0 grams of methanesulfonic acid and 0.7 grams of phosphorous acid under stirring, slowly heat up, if the temperature rises too quickly, the reaction will be violent. Lactic acid will come out at 650 mbar Remove the generated water in time under vacuum conditions, keep warm at 80°C for 2 hours, raise the temperature to 110°C in 3 hours, and keep warm for 2 hours; cool down to 100°C, add 146 grams of adipic acid that has been weighed using a high-level funnel, and put it at a temperature of 160°C After heat preservation for 2 hours under the reaction condition of -165°C; vacuum condition to a maximum of 10mbar, carry out polycondensation and heat preservation for 4 hours, then cool down to 80°C to obtain a slightly yellow (color less than 50 platinum-cobalt standard) transparent product, and its acid value was measured 2.1mgKOH / g, dynamic viscosity...

Embodiment 2

[0036] Add 1100 grams of polyethylene glycol with a molecular weight of 500 in the flask, add a catalyst of 90 grams of lactic acid, 4.1 grams of methanesulfonic acid and 0.6 grams of phosphorous acid under stirring, slowly heat up, if the temperature rises too quickly, the reaction will be violent. Lactic acid will come out at 650mbar Remove the generated water in time under vacuum conditions, keep warm at 80°C for 2 hours, raise the temperature to 110°C for 3 hours, and keep warm for 1 hour; cool down to 100°C, add 190 grams of adipic acid that has been weighed using a high-level funnel, and heat at 160°C After 3 hours of heat preservation under the reaction condition of -165°C; vacuum conditioning to a maximum of 10mbar for polycondensation, after 4 hours of heat preservation, the temperature was lowered to 80°C to obtain a slightly yellow (color less than 50 platinum-cobalt standard) transparent product, and its acid value was measured It is 2.2mgKOH / g, and its dynamic visc...

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Abstract

The invention discloses a preparation method of modified polyethylene glycol adipate, which belongs to the technical field of organic compound synthesis, and comprises the following steps: adding lactic acid into polyethylene glycol, adding a catalyst while stirring, heating to perform pre-esterification reaction, adding adipic acid to continue esterification after the reaction is finished, regulating the vacuum degree, and keeping the temperature to perform polycondensation reaction, and the modified polyethylene glycol adipate is obtained. The preparation method disclosed by the invention isreasonable in process and simple to operate, and the obtained product is stable and light in color, and has the advantages of excellent smooth diffusivity, good isolation demoulding effect, good biodegradability and the like.

Description

technical field [0001] The invention relates to the technical field of organic compound synthesis, in particular to a preparation method of modified polyethylene glycol adipate. Background technique [0002] Modified polyethylene glycol adipate is a high polymer and a biodegradable polyurethane material with excellent mechanical properties, tissue compatibility, biodegradability and designability, so it is used in biomedicine It has been widely used, for example, as a diffusing agent in metal cutting fluid and as a water-based release agent in rubber production. As an emulsifier, modified polyethylene glycol adipate has the characteristics of acid and alkali resistance, high temperature resistance, excellent emulsification performance, and no foam in water. In addition, the product itself is low in toxicity and low in irritation, so The development and research of polyester surfactants has attracted more and more attention. At the same time, improving the biodegradability ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/672C08G63/87
CPCC08G63/672C08G63/87C08G2230/00
Inventor 刘志湘王伟松马夏坤万庆梅叶达峰
Owner ZHEJIANG HUANGMA TECH
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