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Preparation method of toughened high temperature tolerant polyester material namely poly(1,4-cyclohexylenedimethylene) 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 achieves improved branching rate and heat resistance. The effect of improving the thermal conductivity and increasing the toughness

Inactive Publication Date: 2015-01-28
HANGZHOU HANGFU NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Preparation method of toughened high temperature tolerant polyester material namely poly(1,4-cyclohexylenedimethylene) terephthalate
  • Preparation method of toughened high temperature tolerant polyester material namely poly(1,4-cyclohexylenedimethylene) terephthalate
  • Preparation method of toughened high temperature tolerant polyester material namely poly(1,4-cyclohexylenedimethylene) terephthalate

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Embodiment 1

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

[0032] (1) Beating: Purified terephthalic acid (PTA, commercially available) and 1,4 cyclohexanedimethanol (CHDM, commercially available) were weighed in a molar ratio of 1:1 and fed into the polymerization kettle at one time , stir and mix evenly, and then add the dibutyltin oxide solution with a mass concentration of 1% (prepared by dibutyltin oxide and solvent ethylene glycol) into the reaction system according to the dose propeller step by step (the addition is completed in 10 minutes), The addition amount of n-tetrabutyl titanate was 8 ppm, and it stirred at 55 degreeC for 3 hours.

[0033] (2) Esterification: the polymerization kettle was pressurized to 0.3MPa, heated to 260°C, reacted for 70 minutes, then depressurized to 0.04MPa, controlled at 270°C, reacted for 30 minutes, and then added thermal sta...

Embodiment 2

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

[0038] (1) Beating: Purified terephthalic acid (PTA, commercially available) and 1,4 cyclohexanedimethanol (CHDM, commercially available) were weighed in a molar ratio of 1:2 and fed into the polymerization kettle at one time , stir and mix evenly, then add 4% ethylene glycol antimony solution (prepared with ethylene glycol antimony and solvent ethylene glycol) into the reaction system step by step according to the dose propeller (the addition is 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: the polymerization kettle was pressurized to 0.4MPa, heated to 280°C, reacted for 50 minutes, then depressurized to 0.06MPa, controlled at 280°C, reacted for 15 minutes, and then added thermal stabiliz...

Embodiment 3

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

[0044] (1) Beating: Purified terephthalic acid (PTA, commercially available) and 1,4 cyclohexanedimethanol (CHDM, commercially available) were weighed in a molar ratio of 1:1.5 and fed into the polymerization kettle at one time , stir and mix evenly, and then add the n-tetrabutyl titanate solution with a mass concentration of 2% (prepared by n-tetrabutyl titanate and solvent ethylene glycol) into the reaction system step by step according to the dose propeller (the addition is 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: the polymerization kettle was pressurized to 0.35MPa, heated to 270°C, reacted for 60 minutes, then depressurized to 0.05MPa, controlled at 275°C, reacted for 20 minutes, and ...

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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 a toughened and high temperature resistant polyester material poly-1.4 cyclohexane dimethanol ester. Background technique [0002] High toughness and high temperature resistant materials have always been a research hotspot in the field of polymer materials. With the development and progress of science and technology, industrial and special applications have put forward higher requirements for materials, and traditional polymer materials have been difficult to perform in terms of performance and function. To meet the needs of the industry, many discussions have been made in the field of polymer materials research in China, such as polymer materials with photoelectric effect, light-emitting polymer materials have been correspondingly produced and have achieved good applications, but such materials are not based on high The improvement of ...

Claims

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Application Information

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Patent Type & Authority Applications(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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