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Preparation method for biodegradable aliphatic alternating polyester amide

A polyester amide and biodegradation technology, applied in the field of biodegradable aliphatic alternating polyester amide, can solve the problems of poor crystallinity and mechanical properties of random polyester amide, and achieve easy control of the ratio and good chain extension effect. Effect

Inactive Publication Date: 2012-08-22
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a method for the preparation of biodegradable aliphatic alternating polyester amide by an easy-to-operate chain extension method for the disadvantages of random polyester amide in poor crystallinity and mechanical properties

Method used

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  • Preparation method for biodegradable aliphatic alternating polyester amide
  • Preparation method for biodegradable aliphatic alternating polyester amide
  • Preparation method for biodegradable aliphatic alternating polyester amide

Examples

Experimental program
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Embodiment 1

[0044] Embodiment 1: the preparation of polyoxamide glycol adipate prepolymer (PEA-1): with 50 parts of adipic acid, 46.3 parts of N, N'-bis (2-hydroxyethyl) ethyl Diamide, 0.05% tin dichloride, under the protection of nitrogen, carry out polycondensation reaction from 160°C, collect 70-80% of the generated water, then use a decompression device, first use a water pump to depressurize gradually for 2 hours, and then use an oil pump Reduce the pressure to 7mmHg, and continue to react in the temperature range of 160-180°C for 3-4h until the acid value remains basically unchanged, and the intrinsic viscosity is 0.08dL / g, the acid value is 54.27mgKOH / g, and the hydroxyl value is 11.53 mgKOH / g of PEA-1 prepolymer.

[0045] With 100 parts by weight of the PEA-1 prepolymer prepared above, add 3.5 parts of N, N'-adipyl biscaprolactam, 10.4 parts of 1,4-phenyl-bis(2-oxazoline) chain extender , and 0.1 part of tin dichloride and 0.05 part of p-toluenesulfonic acid catalyst, reacted at ...

Embodiment 2

[0046] Embodiment 2: the preparation of poly oxamide glycol adipate prepolymer (PEA-2): in parts by weight 50 parts of adipic acid, 50.2 parts of N, N'-bis (2-hydroxyethyl) ethyl Diamide, 0.1% tin dichloride, under the protection of nitrogen, carry out polycondensation reaction from 160°C, collect 70-80% of the generated water, then use a decompression device, first use a water pump to gradually reduce the pressure for 2 hours, and then use an oil pump Reduce the pressure to 7mmHg, and continue to react in the temperature range of 160-180°C for 3-4h until the acid value remains basically unchanged, and the intrinsic viscosity is 0.10dL / g, the acid value is 47.09mgKOH / g, and the hydroxyl value is 11.27 mgKOH / g of PEA-2 prepolymer.

[0047] With 100 parts by weight of the PEA-2 prepolymer prepared above, add 3.4 parts of N, N'-adipyl biscaprolactam, 9.1 parts of 1,4-phenyl-bis(2-oxazoline) chain extender , and 0.2 parts of tin dichloride and 0.05 parts of p-toluenesulfonic acid...

Embodiment 3

[0048] Example 3 Preparation of polyoxamide glycol sebacate prepolymer (PEA-3): 50 parts by weight of sebacic acid, 33.47 parts of N, N'-two (2-hydroxyethyl) ethylene diol Amide, 0.1% tin dichloride, under the protection of nitrogen, carry out polycondensation reaction from 170°C, collect 70-80% of the generated water, then use a decompression device, first use a water pump to depressurize gradually for 2 hours, and then use an oil pump to decompress pressure to reduce the pressure to 7mmHg, and continue to react in the temperature range of 170-180°C for 3-4 hours until the acid value basically remains unchanged, and the intrinsic viscosity is 0.20dL / g, the acid value is 48.77mgKOH / g, and the hydroxyl value is 3.91. mgKOH / g of PEA-3 prepolymer.

[0049] With 100 parts by weight of the PEA-3 prepolymer prepared in Example 3, add 1.2 parts by weight of N, N'-adipylbiscaprolactam, 9.6 parts by weight of 1,4-phenyl-bis(2-oxazoline) Chain extender, under the protection of nitrogen...

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Abstract

The invention discloses a preparation method for biodegradable aliphatic alternating polyester amide. According to the preparation method, aliphatic dicarboxylic acid and diamide diol are subjected to melt phase polycondensation to prepare alternating polyester amide prepolymer with terminal carboxyl group and terminal hydroxy group; and diacyl di-lactam and a bisoxazoline chain extender are subjected to joint chain extension to prepare the biodegradable aliphatic alternating polyester amide with the intrinsic viscosity of 0.30-0.59dL / g. The preparation method disclosed by the invention has the characteristics of simple and convenient method, mild conditions, high efficiency and the like and can be used for preparing the biodegradable aliphatic alternating polyester amide with regular structure and favorable crystallinity.

Description

technical field [0001] The present invention relates to a preparation method of aliphatic alternating polyester amide using dibasic acid and diamide diol as raw materials, especially a two-step method of polycondensation and chain extension to prepare a structure with an intrinsic viscosity of 0.30-0.59 dL / g Method for biodegradable aliphatic alternating polyester amides with regularity, good crystallinity and high molecular weight. 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, the formation of hydrogen bonds between amide groups makes the polymer have better mechanical properties. Performance and strength, while the presence of ester bonds endows the material with good biodegradability, making it have a wide range of application prospects. [0003] Timmermann et al. (Bayer company) patents WO9942514 (1999), WO9928371 (1999), DE4327024...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/44
Inventor 赵京波尹跳杨万泰
Owner BEIJING UNIV OF CHEM TECH
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