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A kind of preparation method of toughened high temperature resistant polyester material poly-1.4 cyclohexane dimethanol terephthalate

A technology of cyclohexanedimethanol ester and polyterephthalic acid, which is applied in the field of polymer material production, can solve the problems that the performance and function of polymer materials are difficult to meet the needs of the industry, and achieve the improvement of branching rate and toughness. , the effect of improving heat resistance and thermal conductivity

Inactive Publication Date: 2015-08-12
HANGZHOU HANGFU NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] High-toughness and high-temperature-resistant materials have always been the research hotspots in the field of polymer materials. With the development and progress of science and technology, higher requirements have been placed on materials for industrial and special purposes. Traditional polymer materials have been difficult in terms of performance and function. To meet the needs of the industry, a lot of research has been done in the field of polymer materials in China. For example, polymer materials with photoelectric effect and luminescent polymer materials have been produced correspondingly and have achieved good applications. However, such materials are not based on high polymer materials. The improvement of the matrix of molecular materials is only achieved by adding some functional substances to the polymer material as the matrix and skeleton. A matrix material with good performance and good interface effects with functional powders is urgently needed to be developed.

Method used

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  • A kind of preparation method of toughened high temperature resistant polyester material poly-1.4 cyclohexane dimethanol terephthalate
  • A kind of preparation method of toughened high temperature resistant polyester material poly-1.4 cyclohexane dimethanol terephthalate
  • A kind of preparation method of toughened high temperature resistant polyester material poly-1.4 cyclohexane dimethanol terephthalate

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Effect test

Embodiment 1

[0031] A preparation method of toughened high-temperature-resistant polyester material poly-1.4-cyclohexanedimethylene terephthalate, comprising the following steps:

[0032] (1) Beating: Weigh purified terephthalic acid (PTA, commercially available) and 1,4 cyclohexanedimethanol (CHDM, commercially available) at a molar ratio of 1:1 and feed them into the polymerization kettle at one time , stirred and mixed evenly, then the dibutyltin oxide solution (dibutyltin oxide and solvent ethylene glycol) with a mass concentration of 1% was gradually added to the reaction system according to the dosage propeller (completed in 10 minutes), The addition amount of n-tetrabutyl titanate was 8 ppm, and the mixture was stirred at 55° C. for 3 hours.

[0033] (2) Esterification: pressurize the polymerization kettle to 0.3MPa, raise the temperature to 260°C, react for 70 minutes, then reduce the pressure to 0.04MPa, control the temperature at 270°C, react for 30 minutes, and then add heat sta...

Embodiment 2

[0037] A preparation method of toughened high-temperature-resistant polyester material poly-1.4-cyclohexanedimethylene terephthalate, comprising the following steps:

[0038] (1) Beating: Weigh purified terephthalic acid (PTA, commercially available) and 1,4 cyclohexanedimethanol (CHDM, commercially available) at a molar ratio of 1:2 and feed them into the polymerization kettle at one time , stirred and mixed evenly, then the ethylene glycol antimony solution (prepared from ethylene glycol antimony and solvent ethylene glycol) with a mass concentration of 4% was gradually added to the reaction system according to the dosage propeller (completed in 25 minutes), titanic acid The amount of n-tetrabutyl ester added was 12 ppm, and the mixture was stirred at 65° C. for 1 hour.

[0039] (2) Esterification: pressurize the polymerization kettle to 0.4MPa, raise the temperature to 280°C, react for 50 minutes, then reduce the pressure to 0.06MPa, control the temperature at 280°C, react ...

Embodiment 3

[0043] A preparation method of toughened high-temperature-resistant polyester material poly-1.4-cyclohexanedimethylene terephthalate, comprising the following steps:

[0044] (1) Beating: Weigh purified terephthalic acid (PTA, commercially available) and 1,4 cyclohexanedimethanol (CHDM, commercially available) at a molar ratio of 1:1.5 and feed them into the polymerization kettle at one time , stirred and mixed evenly, and then the n-butyl titanate solution (prepared from n-butyl titanate and solvent ethylene glycol) with a mass concentration of 2% was gradually added to the reaction system according to the dosage propeller (the addition was completed in 20 minutes), The addition amount of n-tetrabutyl titanate was 10 ppm, and the mixture was stirred at 60° C. for 2 hours.

[0045] (2) Esterification: pressurize the polymerization kettle to 0.35MPa, raise the temperature to 270°C, react for 60 minutes, then reduce the pressure to 0.05MPa, control the temperature at 275°C, react ...

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Abstract

The invention discloses a preparation method of a toughened high temperature tolerant polyester material namely poly(1,4-cyclohexylenedimethylene) terephthalate. The preparation method comprises the following steps: weighing refined terephthalic acid and 1,4-cyclohexanedimethanol according to a mole ratio of 1:1-2, taking the weighed components as the polymerization reaction monomers, feeding the weighed components into a polymerization reactor, evenly stirring, gradually adding a reaction catalyst into the polymerization reactor within 10 to 25 minutes by a metering pump propeller, adding a phosphate stabilizing agent into the reaction system, evenly stirring and mixing, and adding aluminum nitride in the mid-late period of pre-polymerization; wherein aluminum nitride will be decomposed under a high temperature condition, then nitrogen free radicals with a high reactive activity will be released, thus the branching reactions and hyperbranching reactions in the polymerization system can be realized, the polymer toughness is also improved, and at the same time the heatproof and heat conductive performance of the polymer system are both improved by the addition of aluminum nitride.

Description

technical field [0001] The invention relates to the technical field of polymer material production, in particular to a preparation method of poly-1.4-cyclohexanedimethylene terephthalate, a toughened high-temperature-resistant polyester material. Background technique [0002] High-toughness and high-temperature-resistant materials have always been the research hotspots in the field of polymer materials. With the development and progress of science and technology, higher requirements have been placed on materials for industrial and special purposes. Traditional polymer materials have been difficult in terms of performance and function. To meet the needs of the industry, a lot of research has been done in the field of polymer materials in China. For example, polymer materials with photoelectric effect and luminescent polymer materials have been produced correspondingly and have achieved good applications. However, such materials are not based on high polymer materials. The imp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/183C08G63/199C08G63/78C08G63/85
Inventor 傅伟铮邹湘坪刘水平
Owner HANGZHOU HANGFU NEW MATERIAL TECH
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