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Novel polyester chain extender and preparation method thereof

A technology of chain extender and polyester is applied in the field of novel polyester chain extender and its preparation, which can solve the problems of increasing side reactions in the reaction system, affecting the performance of the final product, and increasing the preparation cost, so as to reduce the content of terminal carboxyl groups and improve the Use value, high molecular weight effect

Inactive Publication Date: 2010-08-04
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the introduction of two chain extenders increases the preparation cost, and also increases the side reactions of the reaction system, which affects the performance of the final product

Method used

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  • Novel polyester chain extender and preparation method thereof
  • Novel polyester chain extender and preparation method thereof
  • Novel polyester chain extender and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1. The molar ratio is 1: 2 isatoic anhydride and 2-aminoalcohol are dissolved in the ratio of 20g / L in chlorobenzene, add the ZnCl of 0.08 of the total mass of isatoic anhydride and 2-aminoalcohol 2 As a catalyst, react at 100°C for 20 h, remove the chlorobenzene solvent from the reaction solution to obtain a crude product, and purify by recrystallization to obtain oxazoline aniline.

[0019] 2. Dissolve the obtained oxazoline aniline in ether at a ratio of 45 g / L. After the solid is completely dissolved, add succinic anhydride. The molar ratio of succinic anhydride to oxazoline aniline is 1:0.75, and stir at room temperature for 2 h , to obtain a suspension. The reaction solution was filtered to obtain the intermediate, which was used in the next step of synthesis.

[0020] 3. Mix the intermediate with a mass ratio of 1.0:0.3:6.0, anhydrous zinc chloride and diatomaceous earth, and grind them into fine powder. Under 380W microwave irradiation power, heat for 5min. A...

Embodiment 2

[0022] 1. be that 1: 2.4 isatoic anhydride and 2-aminoalcohol are dissolved in chlorobenzene in the ratio of 20g / L by molar ratio, add the ZnCl of 0.14% of described isatoic anhydride and 2-aminoalcohol gross mass 2 As a catalyst, it was reacted at 120°C for 23 hours, and the reaction solution was removed from the chlorobenzene solvent to obtain a crude product, which was purified by recrystallization to obtain oxazoline aniline.

[0023] 2. Dissolve the obtained oxazoline aniline in ether at a ratio of 45 g / L. After the solid is completely dissolved, add succinic anhydride. The molar ratio of succinic anhydride to oxazoline aniline is 1:0.82, and stir at room temperature for 4 h , to obtain a suspension. The reaction solution was filtered to obtain the intermediate, which was used in the next step of synthesis.

[0024] 3. Mix the intermediate with a mass ratio of 1.0:0.8:7.0, anhydrous zinc chloride and diatomaceous earth, and grind them into fine powder. Under 500W microw...

Embodiment 3

[0026] 4. be that 1: 2.8 isatoic anhydride and 2-aminoalcohol are dissolved in chlorobenzene in the ratio of 20g / L by molar ratio, add the ZnCl of 0.2% of described isatoic anhydride and 2-aminoalcohol gross mass 2 As a catalyst, react at 120°C for 26 hours, remove the chlorobenzene solvent from the reaction solution to obtain a crude product, and purify by recrystallization to obtain oxazoline aniline.

[0027] 5. Dissolve the obtained oxazoline aniline in ether at a ratio of 45 g / L. After the solid is completely dissolved, add succinic anhydride. The molar ratio of succinic anhydride to oxazoline aniline is 1:0.9, and stir at room temperature for 6 h , to obtain a suspension. The reaction solution was filtered to obtain the intermediate, which was used in the next step of synthesis.

[0028] 6. Mix the intermediate with a mass ratio of 1.0:1.2:7.5, anhydrous zinc chloride and diatomaceous earth, and grind them to a fine powder. Under 800W microwave irradiation power, heat ...

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Abstract

The invention relates to a novel polyester chain extender and a preparation method thereof. The related novel polyester chain extender can obviously improve the intrinsic viscosity of the polyester and can reduce carboxyl content in the system. The novel polyester chain extender respectively comprises o-(4,4-dimethyl oxazoline) and a butanimide structure at the ortho position of the benzene ring, wherein the imide structure can react with hydroxide radical in the polyester and can obviously improve the intrinsic viscosity of the polyester; and oxazoline can perform the chain extending reaction with carboxyl in the polyester and can reduce the carboxyl content in the system when improving the viscosity. The preparation method for the novel polyester chain extender comprises the following steps: (a) dissolving isatoic anhydride and 2-alkamine in chlorobenzene and adding a catalyst into the mixture to perform a reaction to prepare oxazoline aniline; (b) dissolving the prepared oxazoline aniline in aether, adding succinic anhydride into the mixture to perform a reaction and filtering the reaction solution to obtain an intermediate; and (c) uniformly mixing the intermediate and anhydrous zinc chloride with kieselguhr, carrying out irradiation heating on the mixture by microwave, cooling the obtained product, adding ethyl acetate into the cooled obtained product to dissolve out the product, removing the solvent and crystallizing to obtain the novel polyester chain extender.

Description

technical field [0001] The invention relates to a novel polyester chain extender and a preparation method thereof, in particular to a novel polyester chain extender capable of significantly increasing the intrinsic viscosity of polyester and reducing the carboxyl content in the system and a preparation method thereof. Background technique [0002] Polymer materials containing ester groups, such as polyethylene terephthalate, etc., during the processing of mixing, extrusion, injection molding, spinning and other processes, due to the action of oxidation, heat, and water and gas media, macromolecules will Degradation reduces the molecular weight, resulting in a decrease in material performance and affecting the processing and usability of the product. How to maximize or restore the performance of degraded polymer materials has become one of the important areas of research. Many units have conducted research on chain extenders, but there are not many related patents and techni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/91C07D413/10
Inventor 李文刚王朝生胡伟立李喆陈大钟陈向玲丁文科黄伟锋张军李羿王炯张历蒋汉雄赵万金潘磊王麒
Owner DONGHUA UNIV
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