Method for preparing biodegradable polyesteramide through chain extension

A polyester amide, biodegradable technology, applied in the field of high molecular weight biodegradable polyester amide, can solve the problems of high equipment requirements, high vacuum degree, low content of polyester amide amide bonds, etc., to achieve time-saving reaction level, easy Easy to control and respond to the effect

Inactive Publication Date: 2011-04-20
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method requires expensive caprolactone as a raw material and a high degree of vacuum, which requires high equipment
[0006] Chinese patents CN 1,310,194A (2001), CN 1,124,304C (2003), CN101,020,746A (2007) reported the preparation of high molecular weight polyesteramides with diisocyanates or bisoxazoline chain extended aliphatic polyester prepolymers, However, the polyester amide prepared by this method has a low amide bond content, and compared with the corresponding aliphatic polyester, the thermal and mechanical properties are not significantly improved.

Method used

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  • Method for preparing biodegradable polyesteramide through chain extension
  • Method for preparing biodegradable polyesteramide through chain extension
  • Method for preparing biodegradable polyesteramide through chain extension

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] 1) Preparation of polyester amide prepolymer (PEA): take by weight 50 parts of adipic acid, 27.7 parts of 1,4-butanediol, 8.6 parts of N, N'-two (2-hydroxyethyl ) after mixing terephthalamide and 0.26 parts of dibutyltin oxide, under the protection of nitrogen, the temperature is gradually raised from 160°C to 200°C for polycondensation reaction, after collecting 70-80% of the generated water, use a decompression device instead, First use a water pump to gradually reduce the pressure for 3-4 hours, then use an oil pump to reduce the pressure to 2mmHg, and continue the reaction at a temperature range of 190-210°C for 3-4 hours to obtain an intrinsic viscosity of 0.22dL / g and an acid value of 16.7mgKOH / g, a PEA prepolymer with a hydroxyl value of 6.6mgKOH / g;

[0053] 2) Weigh 100 parts of the PEA prepolymer prepared in step 1), 2.0 parts of N, N'-terephthaloyl biscaprolactam, 1,4-phenyl-bis(2-oxazoline) in parts by weight 3.5 parts and 0.1 part of p-toluenesulfonic acid...

Embodiment 2

[0055] 1) The consumption of 1,4-butanediol is 29.3 parts, and other conditions are identical with embodiment 1 step 1), synthetic intrinsic viscosity is 0.28dL / g, acid value is 4.3mgKOH / g, hydroxyl value is 24.4mgKOH / g of PEA prepolymer;

[0056] 2) Weigh 100 parts of the PEA prepolymer prepared in step 1), 7.3 parts of N, N'-adipyl biscaprolactam, 1,4-phenyl-bis(2-oxazoline) in parts by weight 0.9 parts and 0.2 parts of p-toluenesulfonic acid were reacted at 200°C under normal pressure for 0.5 hours under the protection of nitrogen, and then reacted in a 3mmHg decompression system for 1 hour. The intrinsic viscosity of the obtained polymer was 1.05dL / g.

Embodiment 3

[0058] 1) The amount of 1,4-butanediol is 26.2 parts, the amount of N, N'-di(2-hydroxyethyl) terephthalamide is 17.1 parts, the catalyst is stannous chloride, and another 0.2 parts are added Phosphorous acid, other conditions are exactly the same as embodiment 1 step 1), and the synthetic intrinsic viscosity is the PEA prepolymer of 0.30dL / g, acid value 14.6mgKOH / g, hydroxyl value 15.0mgKOH / g;

[0059] 2) Weigh 100 parts of PEA prepolymer prepared in step 1), 4.6 parts of N, N'-adipyl biscaprolactam, and 3.1 parts of 1,4-phenyl-bis(2-oxazoline) in parts by weight , 0.1 part of p-toluenesulfonic acid, reacted at 220°C under normal pressure for 0.5 hours under the protection of nitrogen, and then reacted in a 5mmHg reduced pressure system for 2.5 hours. The intrinsic viscosity of the obtained polymer was 0.73dL / g.

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Abstract

The invention discloses a method for preparing biodegradable polyesteramide through chain extension, and relates to a method for preparing polyesteramide. The prior method for preparing the polyesteramide has the defects of environmental pollution, high requirements on equipment and vacuity, difficult control of material input ratio and the like. The method of the invention comprises the followingsteps: performing melt polycondensation on diamide-diols, dibasic acid and aliphatic diol to prepare polyesteramide prepolymer provided with terminal carboxyl group and terminal hydroxy group structures simultaneously; and performing chain extension with chain extenders of diacyl dilactam and bis-2-oxazoline to prepare the biodegradable polyesteramide of which the limiting viscosity is between 0.42 and 1.05dL / g. The method has low requirement on the vacuity, simplicity and convenience, high efficiency, time conservation, and rich and easily-obtained raw materials, and can prepare polyesteramide with different amide contents to control structures and performance of products by changing the ratio of the diamide-diols to the aliphatic diol to the dibasic acid.

Description

technical field [0001] The invention relates to a preparation method of polyester amide, in particular to a method for preparing high-molecular-weight biodegradable polyester amide with an intrinsic viscosity of 0.42-1.05 dL / g by adopting a two-step method of polycondensation and chain extension. Background technique [0002] Polyester amides (PEAs) are a new type of biodegradable polymer materials. Compared with aliphatic polyesters, due to the introduction of amide groups and the formation of hydrogen bonds between amide groups, the polymers have better mechanical properties and strength, while the presence of ester bonds endows the material with good biodegradability, making it have a wide range of application prospects. [0003] U.S. Patent No. 4,343,931 (1982) reported the synthesis of diamide diol by the reaction of glycolic acid or lactic acid and aliphatic diamines, and reacted it with dibasic acid chlorides to prepare bioabsorbable polyester amides. 3M Company has ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/44
Inventor 赵京波黄超群杨万泰
Owner BEIJING UNIV OF CHEM TECH
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