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High-molecular-weight polyester amide resin based on 1, 2-propylene glycol and preparation method of high-molecular-weight polyester amide resin

A polyester amide and high molecular weight technology, which is applied in the field of high molecular weight polyester amide resin and its preparation, can solve the problems of poor mechanical properties, difficulty in obtaining high molecular weight polyester materials, low reactivity, etc., and achieve product mechanical properties better effect

Inactive Publication Date: 2018-07-10
SHANGHAI GENIUS ADVANCED MATERIAL (GRP) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with PTT, it has the advantages of not easy to crystallize and stable molding, but because the equilibrium constant of polyester polycondensation reaction is low (about 4), and the molecular structure of 1,2-propanediol contains both primary and secondary hydroxyl groups, secondary hydroxyl groups The presence of 1,2-propanediol makes the reactivity of 1,2-propanediol not high in the polycondensation process, and it is difficult to obtain high-molecular-weight polyester materials. The molecular weight of esters is less than 5000, and the mechanical properties are very poor, which cannot meet the requirements of engineering plastics, which greatly limits the large-scale application of 1,2-propanediol

Method used

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  • High-molecular-weight polyester amide resin based on 1, 2-propylene glycol and preparation method of high-molecular-weight polyester amide resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] (1) 45 parts of terephthalic acid, 45 parts of 1,2-propanediol, and 0.02 parts of the first catalyst zinc acetate are sequentially added to a high-pressure reactor with a condensation and vacuum device;

[0056] (2) Vacuumize the autoclave and fill it with nitrogen three times, replace the air in the autoclave to ensure that the esterification reaction is carried out under nitrogen, and heat up to 220 ° C for 2 hours under stirring and condensation until the condensate The amount of water reaches 92% of the theoretically calculated amount (the theoretically calculated amount of condensate water reaches twice the molar amount of terephthalic acid);

[0057] (3) Add 0.02 parts of the second catalyst tetra-n-butyl titanate and 0.02 parts of triphenyl phosphite, and when the temperature is raised to 260 ° C, the vacuum is pumped to 50 Pa, and the reaction is carried out for 1.5 hours;

[0058] (4) Add 10 parts of caprolactam, fill the reactor with nitrogen until the pressur...

Embodiment 2

[0061] (1) Add 25 parts of dimethyl terephthalate, 30 parts of 1,2-propanediol, and 0.01 part of the first catalyst dibutyltin oxide into a high-pressure reactor with a condensation and vacuum device;

[0062] (2) Vacuumize the autoclave and fill it with nitrogen three times, replace the air in the autoclave to ensure that the transesterification reaction is carried out under nitrogen, and heat up to 170°C for 3 hours under stirring and condensation until the condensate The amount of methanol reaches 92% of the theoretically calculated amount (the theoretically calculated amount of condensate methanol reaches twice the molar amount of dimethyl terephthalate);

[0063] (3) Add 0.01 part of the second catalyst antimony trioxide, 0.01 part of trimethyl phosphate, vacuumize to 300 Pa when the temperature is raised to 240 ° C, and react for 3 hours;

[0064] (4) Add 45 parts of caprolactam, fill the reactor with nitrogen until the pressure reaches 50kPa, and react at a constant tem...

Embodiment 3

[0067] (1) 50 parts of terephthalic acid, 45 parts of 1,2-propanediol, and 0.06 parts of the first catalyst tetraethyl titanate were sequentially added to a high-pressure reactor with a condensation and vacuum device;

[0068] (2) Vacuumize the autoclave and fill it with nitrogen three times, replace the air in the autoclave to ensure that the esterification reaction is carried out under nitrogen, and heat up to 230°C for 1 hour under stirring and condensation until the condensate The amount of water reaches 92% of the theoretically calculated amount (the theoretically calculated amount of condensate water reaches twice the molar amount of terephthalic acid);

[0069] (3) Add 0.06 parts of the second catalyst dibutyltin dilaurate, 0.06 parts of triphenyl phosphate, and vacuumize to 450Pa when the temperature is raised to 280 ° C, and react for 1 hour;

[0070] (4) Add 5 parts of lauryl lactam, fill the reactor with nitrogen until the pressure reaches 10kPa, and react at a cons...

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Abstract

The invention belongs to the technical field of high-molecular materials, and relates to high-molecular-weight polyester amide resin based on 1, 2-propylene glycol and a preparation method of the high-molecular-weight polyester amide resin. The polyester amide resin comprises, by weight, 20-65 parts of aromatic dibasic acid and / or aromatic dibasic ester, 20-70 parts of 1, 2-propylene glycol, 5-50parts of cyclic lactam, 0.01-0.06 part of first catalysts, 0.01-0.06 part of second catalysts and 0.01-0.06 part of heat stabilizers. The prepared high-molecular-weight polyester amide resin based onthe 1, 2-propylene glycol improves reaction activity of 1, 2-propylene glycol polyester molecular chains and solves the problem that the 1, 2-propylene glycol is difficult to be polymerized to obtainhigh-molecular-weight products, the 1, 2-propylene glycol can achieve high molecular weight and has excellent mechanical property, heat resistance is enhanced, and heat stability can be improved.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and relates to a high-molecular-weight polyester amide resin based on 1,2-propanediol and a preparation method thereof. Background technique [0002] Polyester refers to a linear polymer prepared by polycondensation reaction of dibasic acid and diol. According to different kinds of dibasic acids and dibasic alcohols, many kinds of polyesters can be synthesized. Currently commercialized mainly include polyethylene terephthalate (PET), polybutylene terephthalate (PBT), polyester Trimethylene terephthalate (PTT), poly-1,4-cyclohexanedimethyl terephthalate (PCT), polyethylene naphthalate (PEN) and polybutylene naphthalate ( PBN) etc. Among them, poly(trimethylene terephthalate) (PTT) is prepared by polycondensation reaction of terephthalic acid and 1,3-propanediol. It was first synthesized by Whinfield and Dickson of the British Calico Printing and Dyeing Workers Association in 1941. How...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/44
CPCC08G69/44
Inventor 杨桂生赵冬云严莉莉
Owner SHANGHAI GENIUS ADVANCED MATERIAL (GRP) CO LTD
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