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Prepn process of biodegradable polyamidoester

A polyamide ester and biodegradation technology, which is applied in the field of high molecular weight biodegradable polyamide ester and the preparation of biodegradable polyamide ester, can solve the problem that the preparation of hydroxyl-terminated polyester prepolymer is cumbersome, time-consuming, polylactic acid Stereoregularity destruction and other problems, to achieve the effects of good crystallinity and biodegradability, simple preparation, and low temperature of chain extension reaction

Inactive Publication Date: 2007-08-22
BEIJING UNIV OF CHEM TECH
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  • Abstract
  • Description
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Problems solved by technology

In the application of Chinese patent 200510093775.9, hydroxyl-terminated polyester prepolymers (oligomers) were prepared by polycondensation, and aliphatic diacyl bis-lactams and aromatic diacyl bis-lactams were melt-chain-extended to prepare number-average molecular weights up to 50,000. Aliphatic polyester can be carried out under a lower vacuum degree and a wider feed ratio, which is easy to operate, but the preparation of the hydroxyl-terminated polyester prepolymer is still relatively cumbersome and time-consuming, and the synthesis of this method does not contain polymer Aliphatic polyester with amide structure
However, due to the high temperature of lactic acid polycondensation and chain extension reaction (above 200 ° C), it is easy to cause the destruction of the stereoregularity of polylactic acid. Even if L-lactic acid is used as raw material for polycondensation and chain extension, the final polylactic acid is completely free Stylized, unable to obtain poly(L-lactic acid)-based polyamide ester with good crystallinity and good performance

Method used

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  • Prepn process of biodegradable polyamidoester
  • Prepn process of biodegradable polyamidoester
  • Prepn process of biodegradable polyamidoester

Examples

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Embodiment 1

[0031] Embodiment 1: The preparation of polybutylene adipate (PBA): with 50 parts of adipic acid, 31 parts of butanediol, 0.24 part of dibutyltin oxide in parts by weight, under nitrogen protection, from 140 ℃ Gradually raise the temperature to 170°C for polycondensation reaction, collect 70-80% of the generated water, switch to a decompression device, and gradually reduce the pressure to 1mmHg, and react at a temperature range of 190-220°C for 4-5 hours until the acid value remains basically unchanged , the number average molecular weight obtained is 9000, the intrinsic viscosity is 0.29dL / g, and the PBA prepolymer with an acid value of 21.8mgKOH / g.

[0032] With 100 parts (parts by weight) of the prepared PBA oligomer, 4.6 parts of 1,4-phenyl-bis(2-oxazoline), 0.023 parts of p-toluenesulfonic acid, react at 200 ° C under normal pressure under nitrogen protection After 3 hours, the number average molecular weight of the obtained polymer was 27,500.

Embodiment 2

[0033] Embodiment 2: 100 parts by weight of PBA oligomer (number average molecular weight is 9000), 5.0 parts of 1,4-phenyl-bis(2-oxazoline), 0.05 part of p-toluene with the parts by weight prepared in Example 1 Sulfonic acid was reacted at 200° C. under normal pressure for 1.5 hours under the protection of nitrogen, and the intrinsic viscosity of the obtained polymer was 1.25 dL / g.

Embodiment 3

[0034] Embodiment 3: 100 parts by weight of PBA oligomer (number-average molecular weight is 9000), 5.1 parts of 1,4-phenyl-bis(2-oxazoline), 0.05 part of p-toluene with the parts by weight prepared in Example 1 Sulfonic acid was reacted at 180° C. under normal pressure for 3 hours under the protection of nitrogen, and the number average molecular weight of the obtained polymer was 26,300.

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Abstract

The present invention is preparation process of biodegradable polyamidoester. Dibasic alcohol and dibasic acid are first melt polycondensated to prepare low molecular weight polyester pre-polymer with number average molecular weight of 2000-9700 or inherent viscosity below 0.5; and the low molecular weight polyester pre-polymer is then melt and chain expanded with binary fatty oxazoline or binary aromatic oxazoline in the presence of chain expander to prepare biodegradable polyamidoester with number average molecular weight up to 39 KD and inherent viscosity up to 1.25 dL / g.

Description

technical field [0001] The present invention relates to a preparation method of aliphatic polyester, in particular to a preparation method of biodegradable polyamide ester, in particular to a two-step method of polycondensation and chain extension to prepare a polyamide with a number average molecular weight of 2.0-39,000 and an intrinsic viscosity of 0.69 Process for high molecular weight biodegradable polyesteramides of ~1.25 dL / g. Background technique [0002] The preparation of aliphatic polyester by polycondensation and chain extension is a disclosed method. This method first prepares an aliphatic polyester prepolymer with a lower molecular weight or intrinsic viscosity by polycondensation, and then uses a chain extender to extend the chain. The prepolymer Structure, chain extender selection and chain extension method have a great impact on the reaction process and product quality of synthetic different products. Chain extender for chain extension to prepare high molec...

Claims

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Application Information

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IPC IPC(8): C08G63/91C08G63/78C08G63/80C08K5/353
Inventor 赵京波罗思扬杨万泰
Owner BEIJING UNIV OF CHEM TECH
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