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Preparation method of copolycarbonate with improved thermal degradation resistance, copolycarbonate and application thereof

A copolycarbonate and performance technology, applied in the field of polycarbonate copolymers, can solve the problems of easy breakage of chemical bonds, decline in heat resistance, widening of distribution, etc., to avoid thermal degradation behavior, prolong service life, and reduce performance Effect

Active Publication Date: 2022-02-18
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Chinese patent CN101360775B describes the preparation of heat-resistant copolycarbonate containing 3,3-bis(4-hydroxyphenyl)-2-phenyl-2,3-dihydroisoindolin-1-one and bisphenol A Manufacturing method, by introducing monomers with polyphenyl ring structure, the glass transition temperature of polycarbonate can be significantly increased, but its resistance to thermal degradation and thermo-oxidative degradation is not mentioned
[0005] Chinese patent CN102971360B describes an improved method for preparing heat-resistant polycarbonate comprising 1,1-bis-(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane and bisphenol A, by controlling The sulfur content in the raw material bisphenol is used to optimize the yellowness index of the molded product, but it does not mention whether it can be beneficial to the improvement of other properties
During the powder extrusion process, the chemical bonds between the bimolecular phenolic compounds are prone to breakage, resulting in degradation of the polymer and widening of the distribution, affecting product performance
In addition, in the later use process, the bimolecular phenolic compounds in the polymer are also more susceptible to the influence of oxygen free radicals, etc., resulting in a significant decrease in heat resistance

Method used

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  • Preparation method of copolycarbonate with improved thermal degradation resistance, copolycarbonate and application thereof
  • Preparation method of copolycarbonate with improved thermal degradation resistance, copolycarbonate and application thereof
  • Preparation method of copolycarbonate with improved thermal degradation resistance, copolycarbonate and application thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0053] The purchased raw material BPTMC is purified, and the content of the bisphenol compound with the structure of formula (IV) is tested by liquid chromatography.

[0054] Purification method: Take a 5L four-neck flask, weigh 1kg of raw material BPTMC and put it into it, then add different qualities of toluene and a certain amount of pure water into the four-necked flask, and heat and reflux at 90°C. After the reflux time was about 2 hours, the heating was stopped, and after the temperature of the solution in the flask dropped to 40° C., the solution was filtered using a Buchner funnel. During the filtration process, the filter cake can be washed repeatedly with toluene and water, and then the filter cake can be heated and dried to obtain the purified raw material.

[0055] Raw materials with different content of the structural compound of formula (IV) are obtained by controlling different purification conditions. Now the source of raw material in the embodiment and the co...

Embodiment 1

[0060] Synthesize copolycarbonate prepared by formula (III) and bisphenol A, the molar ratio is 99:1.

[0061] With 306.9g (0.99mol) compound of formula (III), 2.28g (0.01mol) bisphenol A, 222.79g (1.04mol) diphenyl carbonate and 0.01g (2.5 × 10 -4 mol) sodium hydroxide was added to the reactor with a stirring and distillation device, heated to 160°C under normal pressure for 0.5 hours to melt. Then, it heated up to 210 degreeC over 1 hour, and stirred. Then, the pressure was adjusted to 2.5 KPa over 30 minutes, and it was maintained at 210° C. and 2.5 KPa for 30 minutes to conduct a transesterification reaction. Then the temperature was raised to 270° C. at a rate of 30° C. / hour, and kept at 270° C. and 2.5 KPa for 30 minutes. Then, it adjusted to 1KPa over 10 minutes, and held at 270 degreeC and 1KPa for 1 hour. It took 30 minutes to reduce the pressure to below 133 Pa, and stirred for 20 minutes under the conditions of 270° C. and below 133 Pa to carry out the polymeriza...

Embodiment 2

[0064] Synthesize copolycarbonate prepared by formula (III) and bisphenol A, the molar ratio is 99:1.

[0065] Refer to Example 1 for monomer content and synthesis steps to synthesize a copolycarbonate resin, number A2, with a weight average molecular weight of 33204.

[0066] Among them, in the bisphenol compound with the structure of formula (III), the content of formula (IV) is 495ppm.

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Abstract

The invention relates to a preparation method of copolycarbonate with improved thermal degradation resistance prepared by using BPTMC and BPA as raw materials, copolycarbonate and application thereof, the copolycarbonate comprises a structural unit with a general formula (I), and the copolycarbonate is characterized in that the raw materials contain 1-1000 ppm of bisphenol with a structure of a formula (II). According to the copolycarbonate prepared by the method disclosed by the invention, the thermal property of the copolycarbonate can be further optimized by controlling the content of the bisphenol with the structure as shown in the formula (II), and thermal degradation or thermal oxidative degradation induced by residual phenolic monomers is slowed down or avoided.

Description

technical field [0001] The invention relates to the technical field of polycarbonate copolymers, in particular to a preparation method of a copolycarbonate with improved thermal degradation resistance, a copolycarbonate and an application thereof. Background technique [0002] As an engineering plastic, polycarbonate is widely used in daily life, and the domestic conventional PC market is gradually saturated. However, in special application scenarios such as high-temperature and high-heat environments, conventional PCs cannot meet the requirements of use, and some PCs with special properties have emerged as the times require. . In the field of special PCs, it is necessary to modify PCs to improve properties such as resistance to thermal degradation. [0003] Copolycarbonate with 1,1-bis-(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane (BPTMC) and bisphenol A (BPA) structure, which has better heat resistance , can be used in some high temperature environments, such as the field...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/24C08G64/16C08L69/00
CPCC08G64/24C08G64/1608C08L69/00C08L2201/08
Inventor 黎雷王磊曾伟丁可魏志涛张珏李凤闯隋东武李强
Owner WANHUA CHEM GRP CO LTD
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