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Preparation method of high-molecular-weight aliphatic polyesteramide

A polyester amide, high molecular weight technology, applied in the field of polymer material preparation, can solve the problems of polyester amide products that are not easy to high molecular weight, inconsistent in structure, etc., and achieve the effects of low cost and simple operation

Active Publication Date: 2022-07-15
NORTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of this, the purpose of the present invention is to direct condensation polymerization when preparing polyester amide, the raw material of low boiling point is easy to distill out reactor together with the water that esterification produces, and the molar sum of hydroxyl and amino is excessive in the molar amount of carboxylic acid amount, resulting in difficult to obtain high-molecular-weight polyester amide products, and the different reactivity of amino groups and hydroxyl groups can easily lead to defects such as inconsistency between the obtained polyester amide product and the designed polyester amide structure, providing a high reaction rate, avoiding waste of raw materials, Preparation method of easy-to-control high molecular weight aliphatic polyester amide

Method used

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  • Preparation method of high-molecular-weight aliphatic polyesteramide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) Under nitrogen protection, react 90.1 g of 1,4-butanediol with 200.0 g of succinic anhydride at 120°C for 1 h at a stirring rate of 180 rpm to obtain component A; 44.0 g of 1,4-butanediamine React with 100.0 g of succinic anhydride at 120 °C for 1 h at a stirring rate of 180 rpm to obtain component B; 44.6 g of 4-amino-1-butanol and 100.0 g of succinic anhydride react at 120 °C with a stirring speed of 180 rpm for 1 h to obtain component B points C;

[0039] (2) Under nitrogen protection, the three components A, B, and C obtained in step (1) were added to the reaction kettle, and 236.4g of 1,6-hexanediol, 1.6g of antimony acetate were added as a catalyst and 16.3g of The triethyl phosphate was used as a heat stabilizer, and the esterification reaction was carried out by refluxing at 200 ° C with a stirring rate of 120 rpm for 2 h;

[0040] (3) the above-mentioned step (2) reaction system temperature was raised to 240 ℃, vacuumized, the pressure in the reactor was k...

Embodiment 2

[0043] (1) Under nitrogen protection, react 90.1 g of 1,4-butanediol with 200.0 g of succinic anhydride at 120°C for 1 h at a stirring rate of 180 rpm to obtain component A; 44.0 g of 1,4-butanediamine React with 100.0 g of succinic anhydride at 120 °C for 1 h at a stirring rate of 180 rpm to obtain component B;

[0044] (2) Under nitrogen protection, add the A and B two components obtained in step (1) into the reactor, add 177.3g of 1,6-hexanediol, 1.2g of antimony acetate as a catalyst, 12.2g of phosphoric acid As a heat stabilizer, triethyl ester was refluxed at 200 °C with a stirring rate of 120 rpm for 2 h to carry out the esterification reaction;

[0045] (3) the above-mentioned step (2) reaction system temperature was raised to 240 ℃, vacuumized, the pressure in the reactor was kept at 1000Pa, reacted at 120rpm stirring rate for 0.5h, then the pressure was controlled at 200Pa, and continued stirring at 120rpm Speed ​​stirring for 2h to carry out polycondensation reacti...

Embodiment 3

[0048] (1) Under nitrogen protection, react 90.1 g of 1,4-butanediol with 200.0 g of succinic anhydride at 120°C for 1 h at a stirring rate of 180 rpm to obtain component A; 44.6 g of 4-amino-1-butane The alcohol was reacted with 100.0 g of succinic anhydride at 120° C. at a stirring rate of 180 rpm for 1 h to obtain component C;

[0049] (2) Under nitrogen protection, add the A and C two components obtained in step (1) into the reactor, add 236.4g of 1,6-hexanediol, 1.3g of antimony acetate as a catalyst, 13.4g of phosphoric acid As a heat stabilizer, triethyl ester was refluxed at 200 °C with a stirring rate of 120 rpm for 2 h to carry out the esterification reaction;

[0050] (3) the above-mentioned step (2) reaction system temperature was raised to 240 ℃, vacuumized, the pressure in the reactor was kept at 1000Pa, reacted at 120rpm stirring rate for 0.5h, then the pressure was controlled at 200Pa, and continued stirring at 120rpm Speed ​​stirring for 2h to carry out polyc...

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Abstract

The invention relates to a preparation method of high molecular weight aliphatic polyesteramide, and belongs to the field of high molecular material preparation. The preparation method comprises the following steps: respectively reacting dihydric alcohol, diamine and amino alkyl alcohol with acid anhydride, mixing obtained reaction products, performing esterification reaction with high-boiling-point dihydric alcohol, a catalyst and a heat stabilizer, removing water generated by the esterification reaction, performing condensation polymerization reaction, and finally performing chain extension reaction to obtain the high-molecular-weight aliphatic polyesteramide. The dihydric alcohol, the diamine and the amino alkyl alcohol have high reaction activity with the anhydride, the reaction temperature is low, and the change of the ratio of the reaction raw materials due to the fact that the reaction raw materials with low boiling points are taken out of the reaction kettle by water generated by the reaction during direct esterification is avoided; high-boiling-point dihydric alcohol is used in the esterification stage, and a reflux reaction is carried out, so that the stability of the ratio of reaction raw materials can be ensured. The method is suitable for large-scale preparation of high-molecular-weight aliphatic polyesteramide, and is simple to operate, environment-friendly, capable of avoiding raw material waste and low in equipment requirement.

Description

technical field [0001] The invention relates to the field of polymer material preparation, in particular to a preparation method of a high molecular weight aliphatic polyester amide. Background technique [0002] Aliphatic polyesters are easy to biodegrade, and the research is relatively mature, mainly including polylactic acid (PLA), polycaprolactone (PCL), polyhydroxyalkanoate (PHA) and polybutylene succinate (PBS) and Its copolymers, etc., have been deeply researched and applied in drug controlled release systems, bone fixation devices in fractures, biodegradable materials and products. However, aliphatic dibasic acid glycol polyesters generally have a low melting point and insufficient mechanical strength, which limits their larger-scale applications. In contrast, polyamides such as nylon 6, nylon 66 and other engineering plastics have excellent mechanical properties, but are not biodegradable. In recent years, some researchers have used chemical methods to introduce a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/44
CPCC08G69/44
Inventor 危仁波周凌云王玲玲
Owner NORTHWEST UNIV