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Aromatic polyesteramide and preparation method thereof

A polyester amide and aromatic technology, applied in the field of aromatic polyester amide and its preparation, can solve the problems that cannot meet the requirements of high temperature application fields, high melting point, difficult processing and molding, etc., to achieve outstanding heat resistance and moldability amount, self-reinforcing modulus, and the effect of lowering the melting point

Active Publication Date: 2017-06-09
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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  • Aromatic polyesteramide and preparation method thereof
  • Aromatic polyesteramide and preparation method thereof
  • Aromatic polyesteramide and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In this example, polyester amide is prepared by using meta-aromatic diphenol, diacid monomer and semi-aromatic diamine monomer: add 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 24 hours to obtain an aro...

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 aromatic polyesteramide and a preparation method thereof. The preparation method includes adding meta-position wholly-aromatic diphenol monomers, meta-position wholly-aromatic diacid monomers, semi-aromatic diamine monomers, a catalyst and acetic anhydride into a reactor prior to acetylation reaction and transesterification, and continuing reacting for 10-30 minutes at a temperature of 300-320 DEG C and under a vacuum degree of 1-20 mbar; cooling a product in a nitrogen atmosphere to a room temperature after the reaction, grinding the cooled product to fine powder and subjecting the fine powder to condensation polymerization at a temperature of 200-260 DEG C and under a vacuum degree of 1-20 mbar so as to obtain the aromatic polyesteramide. The aromatic polyesteramide self-enhanced in modulus, tensile strength and glass-transition temperature is obtained based on different aggregation states of polyesteramide. Through meta-position wholly-aromatic substitution, molecular chain symmetry is destroyed and a melting point is decreased. The preparation method which is implemented through a one-pot polymerization reaction has the advantages of simplicity and easiness in 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 Applications(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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