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Preparation method of biodegradable alternating polytetramide diester

A polytetramide diester, biodegradable technology, applied in the field of preparation of biodegradable alternating polytetramide diester, can solve the problems of poor crystallinity, thermal properties and mechanical properties, and achieve excellent mechanical properties and good thermal properties Effect

Inactive Publication Date: 2016-06-01
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to aim at the shortcomings of random polyester amide crystallinity, poor thermal properties and mechanical properties, to provide a polycondensation-chain extension method that does not require high vacuum degree and equipment, is pollution-free, and is easy to operate. Biodegradable Method of Alternating Polytetramide Diesters

Method used

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  • Preparation method of biodegradable alternating polytetramide diester
  • Preparation method of biodegradable alternating polytetramide diester
  • Preparation method of biodegradable alternating polytetramide diester

Examples

Experimental program
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Effect test

Embodiment 1

[0049] 1) Preparation of diamide diester: with 50 parts by weight of dimethyl adipate, 3.3 parts of hexamethylene diamine, under nitrogen protection, stepwise from 120 ° C to 180 ° C in 5 hours, cooling, filtration, Purification by recrystallization from DMF yielded the diamide diester.

[0050] 2) Weigh 41 parts of diamide diesters and 50 parts of ethanolamines in step 1) in parts by weight, gradually increase from 140° C. to 180° C. in 3 hours under nitrogen protection to the end of the reaction, recrystallize and purify with DMF to obtain Tetraamide diol-bis(ethanolamine adipyl)hexamethylenediamine, its melting point is 205~207℃.

[0051] 3) Preparation of alternating polytetraamide diester prepolymer [PreP(4A-alt-2E)-1]: Weigh 50 parts of tetraamide diol, 17.5 parts of adipic acid, 0.05 part of tetraamide diol in step 2) by weight in parts by weight % tin dichloride, under the protection of nitrogen, carry out the polycondensation reaction from 160 ° C, collect 80% of the...

Embodiment 2

[0054] Preparation of alternating polytetraamide diester prepolymer [PreP(4A-alt-2E)-2]: Weigh 50 parts of tetraamide diol, 21.4 parts of sebacic acid, 0.05% tin dichloride, under the protection of nitrogen, carry out the polycondensation reaction from 160 ° C, collect 80% of the generated water, use a decompression device, first use a water pump to gradually decompress the reaction for 2 hours, and then use an oil pump to decompress to 7 mmHg, Continue the reaction for 3 to 4 hours in the temperature range of 160 to 180 °C until the acid value is basically unchanged, to obtain PreP (4A-alt -2E)-2 prepolymer.

[0055] Weigh in parts by weight 10 parts of the above PreP(4A-alt-2E)-2 prepolymer, 0.13 parts of 1,4-phenyl-bis(2-oxazoline), and the catalyst is 0.15% tin dichloride and 0.05% p-toluenesulfonic acid was reacted for 1.5 hours at 200 °C under nitrogen protection at atmospheric pressure, and the oil pump was decompressed to 5 mmHg and reacted for 3 hours to prepare a bi...

Embodiment 3

[0057] Weigh in parts by weight PreP(4A-alt-2E)-110 parts in Example 1, step 2), 0.45 parts of chain extender N,N'-adipoylbiscaprolactam, 1,4-phenyl-bis( 2-oxazoline) 0.71 part, the catalyst is 0.15% tin dichloride, the reaction is carried out under nitrogen protection at 200 ° C normal pressure for 1.5 hours, and the oil pump decompression (pressure 5mmHg) for 3 hours to prepare an intrinsic viscosity of 0.32dL / g of biodegradable alternating polytetramide diesters.

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Abstract

The invention relates to a biodegradable alternate poly tetraamide diester preparation method, and belongs to the technical field of polyamide esters. The preparation method comprises that: an aliphatic diamine and a dicarboxylic acid ester are subjected to a reaction to prepare a diamide diester, the diamide diester reacts with alcohol amine to obtain tetraamide diol, the tetraamide diol and a dicarboxylic acid are subjected to condensation polymerization to prepare an alternate poly tetraamide diester prepolymer, and chain extenders such as bisoxazoline and diacyl di-lactam are adopted to carry out chain extension on the prepolymer to prepare the biodegradable alternate poly tetraamide diester with the 30 DEG C intrinsic viscosity of 0.26-0.45 dL / g. The biodegradable alternate poly tetraamide diester has characteristics of regular structure, good crystallinity, high melting point, good thermal property, good mechanical property, and green and pollution-free synthesis route.

Description

technical field [0001] The invention relates to a method for preparing aliphatic alternating polytetramide diester, in particular to the process of first reacting dibasic acid ester and diamine to prepare diamide diester, then reacting with alcohol amine to prepare tetraamide diol, and mixing it with diamine Alternating polytetraamide diester prepolymer prepared by polycondensation of carboxylic acid, and then chain-extended by dibasic oxazoline and diacyl bislactam to obtain biodegradable alternating polytetraamide diester with intrinsic viscosity of 0.49-0.75dL / g Ester belongs to the technical field of polyamide ester. technical background [0002] Aliphatic polyester amide (PEA) is a new type of biodegradable polymer material. Compared with aliphatic polyester, due to the introduction of amide groups, hydrogen bonds are formed between amide groups, which makes the polymer have better mechanics. At the same time, the existence of ester bonds endows the material with good ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/44
Inventor 赵京波孙会云杨万泰
Owner BEIJING UNIV OF CHEM TECH
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