Biodegradable alternate poly tetraamide diester preparation method

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: 2014-06-25
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 polyconde

Method used

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  • Biodegradable alternate poly tetraamide diester preparation method
  • Biodegradable alternate poly tetraamide diester preparation method
  • Biodegradable alternate poly tetraamide diester preparation method

Examples

Experimental program
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Embodiment 1

[0049] 1) Preparation of diamide diester: 50 parts by weight of dimethyl adipate and 3.3 parts of hexamethylenediamine, gradually from 120°C to 180°C within 5 hours under nitrogen protection, cooling, filtering, Purified by recrystallization from DMF to obtain diamide diester.

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

[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 % tin dichloride, under the protection of nitrogen, carry out polycondensation reaction from 160 ℃, after collecting 80% of the generated water, use a decompression device, first use a wate...

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 polycondensation reaction from 160 °C, collect 80% of the generated water, then use a decompression device, first use a water pump to gradually depressurize the reaction for 2 hours, and then use an oil pump to depressurize to 7mmHg, Continue to react in the temperature range of 160-180°C for 3-4 hours until the acid value is basically unchanged, and the PreP(4A-alt -2E)-2 prepolymer.

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

Embodiment 3

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

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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 present invention relates to a kind of method for preparing aliphatic alternating polytetraamide diester, be specifically related to at first prepare diamide diester with dibasic acid ester and diamine reaction, then prepare tetraamide diol with alcohol amine reaction, prepare it and diamide diol Alternating polytetramide diester prepolymers were prepared by polycondensation of basic acids, and then chain-extended by binary oxazolines and diacyl bislactams to obtain biodegradable alternating polytetramide diesters with an intrinsic viscosity of 0.49-0.75 dL / g. The 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 and the formation of hydrogen bonds between amide groups, the polymer has better mechanical properties. Performance and strength, while the presenc...

Claims

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Application Information

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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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