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Preparation method of copolymerized carbonic ester with improved performance, copolymerized carbonic ester and application of copolymerized carbonic ester

A technology of copolycarbonate and copolycarbonate, which is applied in the preparation of copolycarbonate and the field of copolycarbonate, can solve the problems of slowing down the polycondensation reaction, no obvious improvement in the performance of molded products, and affecting product selectivity, so as to reduce impurities content, avoid surface yellowing, and prevent the effect of sample yellowing

Active Publication Date: 2021-10-08
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] 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
[0005] Chinese patent CN107207718B describes an improved method for preparing heat-resistant polycarbonate comprising 1,1-bis-(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane and bisphenol A, by adding The addition of monohydroxyaryl compounds to the raw material mixture lowers the melting point of the monomer mixture, which further slows down the polycondensation reaction in the early stage, but does not significantly improve the corresponding performance of the molded product
[0006] Chinese patent CN101023118A 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 content of sodium chlorate in the raw material sodium hydroxide solution can optimize the color of molded products, but it does not mention the improvement of other properties
When regulating pH value, the amount of catalyst is not easy to control, but it can obviously affect the selectivity of product, if it exceeds 20mol% (based on the amount of substance of reactant TMC), then it is easy to react to produce the bisphenol compound of formula (IV) structure

Method used

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  • Preparation method of copolymerized carbonic ester with improved performance, copolymerized carbonic ester and application of copolymerized carbonic ester
  • Preparation method of copolymerized carbonic ester with improved performance, copolymerized carbonic ester and application of copolymerized carbonic ester
  • Preparation method of copolymerized carbonic ester with improved performance, copolymerized carbonic ester and application of copolymerized carbonic ester

Examples

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Effect test

preparation example 1

[0062] The raw material BPTMC is synthesized in a laboratory, and the content of the bisphenol compound with the structure of formula (IV) is tested by a liquid chromatograph.

[0063] Preparation method: Take a 5L four-necked flask, weigh 700g (5mol) TMC into it, then add 2350g (25mol) phenol into the four-necked flask, and continuously feed hydrogen chloride gas in a constant temperature water bath at 35°C for reaction. During the reaction, the pH value of the reaction solution was continuously monitored. After about 8 hours of reaction, the introduction of hydrogen chloride gas was stopped, and an appropriate amount of 5% NaOH solution was added into the flask until the pH value of the solution was close to 7.

[0064] Subsequently, the reaction solution was filtered, and the filter cake was weighed. Take a 5L four-neck flask, transfer the filter cake into the bottle, add equal mass of toluene and half mass of pure water, and heat to reflux at 95°C. After about 2 hours of...

Embodiment 1

[0069] Synthesize copolycarbonate prepared by formula (III) and bisphenol A, the molar ratio is 99:1.

[0070] 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

[0073] Synthesize copolycarbonate prepared by formula (III) and bisphenol A, the molar ratio is 99:1.

[0074] Refer to Example 1 for monomer content and synthesis steps to synthesize a copolycarbonate resin, number A2, with a weight average molecular weight of 32325.

[0075] Among them, in the bisphenol compound with the structure of formula (III), the content of formula (IV) is 452ppm.

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Abstract

The invention relates to a preparation method of a copolymerized carbonic ester with improved performance, the copolymerized carbonic ester and application of the copolymerized carbonic ester. The copolymerized carbonic ester is prepared by taking BPTMC and BPA as raw materials and comprises a structural unit of a general formula (I), and the copolymerized carbonic ester is characterized in that the raw material BPTMC contains 1-5000 ppm of bisphenol with a structure of a formula (II). According to the copolycarbonate prepared by the method disclosed by the invention, the content of impurities in a molded product can be effectively reduced by controlling the dosage of a hydrogen chloride catalyst and the like in a raw material synthesis process, so that the phenomenon that phenolic monomers induce thermal degradation or thermal oxidation degradation of polycarbonate when the product is exposed in a high-temperature load is avoided, and the mechanical, thermal and optical properties of the polycarbonate are optimized.

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 performance, a copolycarbonate and an application thereof. Background technique [0002] With the continuous expansion of domestic polycarbonate production capacity, the market is becoming increasingly saturated. However, in some special application fields, higher requirements are put forward for the performance of polycarbonate, and some polycarbonate with special performance have been produced accordingly. By adjusting the type and molar ratio of comonomers, special polycarbonates with different properties have emerged. [0003] By copolymerizing 1,1-bis-(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane (BPTMC) with bisphenol A (BPA), a more heat-resistant Polycarbonate can be used in some scenes under high temperature load, such as the field of car lights. However, in the process of use, it was found that w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/24
CPCC08G64/24
Inventor 黎雷王磊曾伟魏志涛李凤闯丁可隋东武李强
Owner WANHUA CHEM GRP CO LTD
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