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A kind of aromatic polyester amide and preparation method thereof

A polyester amide and aromatic technology, which is applied in the field of aromatic polyester amide and its preparation, can solve the problems of high melting point, inability to meet the requirements of high temperature application fields, and difficult processing and molding, and achieve self-reinforcing modulus, outstanding Heat resistance and modulus, effect of lowering melting point

Active Publication Date: 2019-09-10
HUANGSHAN SHENJIAN NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at the same time, new problems have emerged, the glass transition temperature of aliphatic or semiaromatic copolyesteramides ( T g ) is only 50~80 o C (see literature W Steinmann, S Walter, M Beckers, G Seide and T Gries. Thermal analysis of phase transitions and crystallization in polymeric fibers[B]. Applications of calorimetry in a wide context – differential scanning calorimetry, isothermal titration calorimetry and microcalorimetry. 2013, InTech, Croatia, Chapter 12, 277-306), cannot meet the requirements of high temperature applications
[0004] Chinese invention patent (CN103328540B) discloses a preparation method of a wholly aromatic liquid crystal polyester amide resin and a preparation method of a wholly aromatic liquid crystal polyester amide resin composition, and the Tg of the provided wholly aromatic polyester amide can reach 150~ 200°C, but its rigid molecular chain structure and strong hydrogen bond force make its melting point too high (>330°C), and it is difficult to process and shape

Method used

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  • A kind of aromatic polyester amide and preparation method thereof
  • A kind of aromatic polyester amide and preparation method thereof
  • A kind of aromatic polyester amide and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In this example, polyester amide was prepared by meta-aromatic diphenol, diacid monomer and semi-aromatic diamine monomer: 110.11g 1,3-resorcinol, 332.26g 1,3-isophthalic acid, 136.20 g 1,4-xylylenediamine, 142 mL acetic anhydride, and 49.07 mg potassium acetate. The flask was fitted with a sealed glass paddle stirrer, a nitrogen inlet tube and an insulated distillation head. A moderate nitrogen flow was introduced, and the acetylation reaction was carried out at a temperature of 140° C. for 60 minutes. The reaction mixture was heated (0.5°C / min) in a quicksand bath, and the reaction temperature rose from 140°C to 310°C. At this point, the reaction system was slowly evacuated (vacuum degree: 10 mbar), and kept at 310° C. for 30 min. The opaque melt was cooled to room temperature and the product was removed from the flask and ground to a fine powder. Finish polycondensation in a vacuum oven with a vacuum degree of 10mbar at 250°C for 24h to obtain an aromatic polyeste...

Embodiment 2

[0032] In this example, polyester amide was prepared from meta-aromatic diphenol, diacid monomer and semi-aromatic diamine monomer: 186.21g of 1,1'-biphenyl-3,4 was added to a 1000mL three-neck round bottom flask '-diphenol, 605.58g 1,1'-biphenyl-3,3'-dicarboxylic acid, 372.62g 1,4-benzenedipentylamine, 189mL acetic anhydride and 82mg sodium acetate. The flask was fitted with a sealed glass paddle stirrer, a nitrogen inlet tube and an insulated distillation head. A moderate nitrogen flow was introduced, and the acetylation reaction was carried out at a temperature of 120° C. for 60 minutes. The reaction mixture was heated (0.8°C / min) in a quicksand bath, and the reaction temperature rose from 120°C to 300°C. At this point, the reaction system was slowly evacuated (vacuum degree: 1 mbar), and kept at 300° C. for 30 min. The opaque melt was cooled to room temperature and the product was removed from the flask and ground to a fine powder. In a vacuum oven at 240°C with a vacuu...

Embodiment 3

[0041] In this example, polyester amide was prepared from meta-aromatic diphenol, diacid monomer and semi-aromatic diamine monomer: 160.17g 1,7-naphthalenediol, 756.67g 1 , 7-naphthalene dicarboxylic acid, 676.03 g 1,4-naphthalene dibutylamine, 284 mL acetic anhydride, and 81.20 mg stannous octoate. The flask was fitted with a sealed glass paddle stirrer, a nitrogen inlet tube and an insulated distillation head. A moderate nitrogen flow was introduced, and the acetylation reaction was carried out at a temperature of 140° C. for 60 minutes. The reaction mixture was heated (1.0°C / min) in a quicksand bath, and the reaction temperature rose from 140°C to 320°C. At this point, the reaction system was slowly evacuated (vacuum degree: 5 mbar), and kept at 320° C. for 15 min. The opaque melt was cooled to room temperature and the product was removed from the flask and ground to a fine powder. Finish polycondensation in a vacuum oven with a vacuum degree of 5mbar at 230°C for 24 hou...

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Abstract

The invention discloses an aromatic polyester amide and a preparation method thereof. Add meta-position fully aromatic diphenol monomer, meta-position fully aromatic diacid monomer, semi-aromatic diamine monomer, catalyst and acetic anhydride into the reactor, after acetylation reaction and transesterification reaction, in vacuum The temperature is 1-20mbar, the temperature is 300-320°C and the reaction is continued for 10-30min; after the reaction is completed, cool to room temperature in a nitrogen atmosphere, and grind the product into fine powder. After polycondensation reaction, an aromatic polyester amide is obtained. The present invention relies on the difference in aggregation state of polyester amide to obtain a polyester amide with self-enhancing modulus, tensile strength and glass transition temperature, and through meta-position all-aromatic substitution, molecular chain symmetry is destroyed and melting point is lowered. The preparation method is a one-pot polymerization reaction, which is simple and easy to control.

Description

technical field [0001] The invention relates to an aromatic polyester amide and a preparation method thereof, belonging to the technical field of high-performance polymers. Background technique [0002] Polyester amides are polymers containing ester chains and amide bonds in the main molecular chain. Aromatic polyester amide is one of the important types. As a modified polymer of polyarylate and polyarylamide, it has the advantages of both polyarylate and polyarylamide. [0003] At present, the methods for preparing aromatic polyester amides mainly include transesterification, low-temperature solution polycondensation, and interfacial polycondensation. Such as the introduction of aliphatic amide segments (such as PA66) into polyethylene terephthalate (PET) or poly(paraben-co-p-oxynaphthoate) by transesterification, Preparation of aliphatic or semi-aromatic copolyesteramide; or acetylation of aromatic monomers containing both hydroxyl and amino groups, and low-temperature s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/44
Inventor 顾嫒娟管清宝梁国正袁莉
Owner HUANGSHAN SHENJIAN NEW MATERIAL CO LTD
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