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Method for preparing tetrabromo-bisphenol A polycarbonate

A technology of tetrabromobisphenol and ultramolecular weight, which is applied in the field of preparation of ultramolecular weight tetrabromobisphenol A polycarbonate, can solve the problem that the molecular weight cannot be fixed within a certain range, the target product cannot be controlled, and application value has not been found, etc. problems, to achieve the effects of low toxicity, safe operation, convenient storage and use

Inactive Publication Date: 2007-09-12
TAIZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Tetrabromobisphenol A polycarbonate with a molecular weight of less than 100,000 is generally used as a flame retardant; while tetrabromobisphenol A polycarbonate with a molecular weight of 150,000 to 250,000 has high temperature resistance and flame retardancy, and also has excellent The unique properties of light transmittance, radiation protection, impact resistance, dielectric properties, etc., so this kind of tetrabromobisphenol A polycarbonate is a new type of polymer material, which is widely used in medicine, electronics, electrical appliances, machinery, etc. , automobiles, textiles, military industry, aerospace and other fields have a wide range of applications; tetrabromobisphenol A polycarbonate with a molecular weight of more than 250,000 has not yet found its application value due to its different properties
[0003] There are many studies on tetrabromobisphenol A polycarbonate. Chang Zhi et al. synthesized tetrabromobisphenol A polycarbonate with triphosgene (BTC, commonly known as solid phosgene, also called tripolycarbonyl chloride) and tetrabromobisphenol A (TBBPA) as raw materials. Phenol A polycarbonate, but the synthetic molecular weight is low ("Chemical and Biological Engineering", 2005, 22 (5): 24-26); The polycarbonate research project was put into production in 2006, but the molecular weight was around 3500; U.S. patents US4794156, US3912687, and US4794156 introduced the reaction process of interfacial polymerization of tetrabromobisphenol A polycarbonate synthesized by phosgene method, and the molecular weight can reach 200,000 , but did not mention the use of triphosgene as a raw material
[0005] The second is that it is almost impossible for this professional and technical personnel to implement. For example, the concentration of sodium hydroxide used is "1%-50%", the temperature is "-3°C-20°C", "pH9-14", and the reaction time is "1-48°C". hour", "precipitant plus precipitation", "one-time addition of 1%-50% sodium hydroxide solution", etc., the molecular weight of the obtained product is too random, it is impossible to fix the molecular weight within a certain range, and it is impossible to control industrial production The target product with a specific molecular weight; in addition, catalysts need to be added in a temperature environment of -3°C-5°C, and the production cost is relatively high

Method used

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  • Method for preparing tetrabromo-bisphenol A polycarbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In a 3000mL four-necked flask with an electric stirrer, add 204.8g (0.376mol) of tetrabromobisphenol A, 750mL of water, 0.25g of polymerization inhibitor phenol, dissolve with 5% sodium hydroxide, and then filter cloth Filter, then add dropwise 111.7g (0.376mol) of triphosgene previously dissolved in 500mL of dichloromethane and filtered through a filter cloth at 25±3°C, after dropping, adjust the pH of the system to 10 with 15% NaOH solution, and keep warm for 30min . The reaction mixture was diluted with 1000 mL of dichloromethane, 0.2 g of 4-N,N-dimethylaminopyridine was added, 18% NaOH solution was added dropwise to maintain the pH of the reaction mixture = 10, and the mixture was stirred for 30 min. After completion of the reaction, use 5% dilute hydrochloric acid to adjust the pH to 7 to end the reaction, separate the organic layer, and wash it three times with deionized water, then add ethanol to precipitate a white solid powder, filter it to dryness, and dry it ...

Embodiment 2

[0030] In a 3000mL four-necked flask with an electric stirrer, add 204.8g (0.376mol) of tetrabromobisphenol A, 750mL of water, 0.15g of polymerization inhibitor phenol, dissolve with 5% sodium hydroxide, and then filter cloth Filter, then add dropwise 111.7g (0.376mol) of triphosgene previously dissolved in 500mL of dichloromethane and filtered through a filter cloth at 25±3°C, after dropping, adjust the pH of the system to 10 with 20% NaOH solution, and keep warm for 30min . The reaction mixture was diluted with 1000 mL of dichloromethane, 0.3 g of 4-N,N-dimethylaminopyridine was added, 20% NaOH solution was added dropwise to maintain the pH of the reaction mixture = 10, and the mixture was stirred for 60 min. After completion of the reaction, use 5% dilute hydrochloric acid to adjust the pH to 7 to end the reaction. Separate the organic layer and wash it three times with deionized water. Add ethanol to precipitate a white solid powder. Filter and dry in vacuum to obtain tetr...

Embodiment 3

[0032]In a 3000mL four-neck flask with an electric stirrer, add 204.8g (0.376mol) of tetrabromobisphenol A, 750mL of water, 0.35g of polymerization inhibitor phenol, dissolve with 5% sodium hydroxide, and then filter cloth Filter, then add dropwise 111.7g (0.376mol) of triphosgene previously dissolved in 500mL of dichloromethane and filtered through a filter cloth at 25±3°C, after dropping, adjust the pH of the system to 10 with 15% NaOH solution, and keep warm for 40min . The reaction mixture was diluted with 1000 mL of dichloromethane, 0.2 g of 4-N,N-dimethylaminopyridine was added, and 15% NaOH solution was added dropwise to maintain the reaction mixture pH=10, and stirred for 40 min. After the reaction is completed, adjust the pH to 7 with 5% formic acid to end the reaction, separate the organic layer, and wash it three times with deionized water, then add methanol to precipitate a white solid powder, filter and dry, and dry in vacuum to obtain tetrabromobisphenol with a m...

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Abstract

The invention relates to a method for preparing molecular tetrabromobisphenol-A polycarbonate. Its character shows as follow: a. it dissolves the tetrabromobisphenol-A and inhibitor in the natrium hydroxydatum, filtering. Then, it dissolves triphosgene in the halogenated alkane, filtring. b. it adds the filtered triphosgene solution to the filtered tetrabromobisphenol-A and inhibitor solution, and then it adds natrium hydroxydatum at room temperature under normal pressure, and maintains the system to be pH9-12, then it stirs the solution for 0.5-1 hours. c. it adds 10%-20% of the natrium hydroxydatum at room temperature under normal pressure, and maintains the system to be pH8-10, then it stirs the solution for 0.5-1 hours. d. it regulates the solution with acid to be neutral and takes out from the organic layer, then it washes the material with deionized water and adds fatty alcohol to precipitate white powder, then it achieves the molecular weight range of 150,000 ~ 250,000 molecular of tetrabromobisphenol-A polycarbonate through filtration and drying.

Description

technical field [0001] The invention belongs to the field of polymer materials, in particular to a preparation method of supermolecular-weight tetrabromobisphenol A polycarbonate. Background technique [0002] Tetrabromobisphenol A polycarbonate with a molecular weight of less than 100,000 is generally used as a flame retardant; while tetrabromobisphenol A polycarbonate with a molecular weight of 150,000 to 250,000 has high temperature resistance and flame retardancy, and also has excellent The unique properties of light transmittance, radiation protection, impact resistance, dielectric properties, etc., so this kind of tetrabromobisphenol A polycarbonate is a new type of polymer material, which is widely used in medicine, electronics, electrical appliances, machinery, etc. , automobiles, textiles, military industry, aerospace and other fields have a wide range of applications; tetrabromobisphenol A polycarbonate with a molecular weight of more than 250,000 has not yet found...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/24
Inventor 潘富友杨小阳徐骞
Owner TAIZHOU UNIV
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