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Preparation method of low-molecular-weight halogen flame-retardant polycarbonate

A flame retardant polycarbonate, low molecular weight technology, applied in the chemical industry, can solve the problems of difficult synthesis of halogen flame retardant polycarbonate, wide molecular weight distribution, low product qualification rate, etc., and achieves narrow molecular weight distribution, simple operation process, Efficient effect

Inactive Publication Date: 2016-04-13
甘肃银光聚银化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The preparation method of halogen flame retardant polycarbonate oligomer is very similar to ordinary phosgene polycarbonate, but bisphenol A polycarbonate is relatively easy to synthesize, but the synthesis of halogen flame retardant polycarbonate is much more difficult
Under the same conditions, the polycarbonate obtained by the reaction of phosgene and bisphenol A can have a large molecular weight, while the halogen flame-retardant polycarbonate synthesized by phosgene and polyhalogenated bisphenol A has a small molecular weight and a wide molecular weight distribution. , long reaction cycle, low product pass rate, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: In a six-necked flask with an electric stirrer, add 100 g of polyhalogenated bisphenol A, 200 g of water, and 530 g of dichloromethane as a solvent, dissolve completely with sodium hydroxide solution under stirring conditions, and add 0.73 g of catalyst triethylamine , the temperature of the system was controlled at 10°C, 33g of phosgene was introduced, and at the same time, the pH of the mixed system was adjusted between 7 and 14 with sodium hydroxide solution, and the prepolymerization reaction time was 20 minutes. After the prepolymerization reaction, increase the reaction temperature to 18°C, add 1.37g of p-tert-butylphenol as an end-capping agent, and add sodium hydroxide solution dropwise at the same time, keep the pH of the system at 7-14, and stir for 30 minutes; After layering, the oil phase was washed three times with process water and hydrochloric acid solution respectively, then the oil phase was added to the precipitant, the white solid was washed...

Embodiment 2

[0021] Example 2: In a six-necked flask with an electric stirrer, add 100 g of polyhalogenated bisphenol A, 250 g of water, and 460 g of dichloromethane as a solvent, dissolve completely with sodium hydroxide solution under stirring conditions, and add 0.5 g of catalyst triethylamine , the temperature of the system was controlled at 11° C., 35 g of phosgene was introduced, and at the same time, the pH of the mixed system was adjusted between 7 and 14 with sodium hydroxide solution, and the prepolymerization reaction time was 15 minutes. After the prepolymerization reaction, raise the reaction temperature to 20°C, add 0.86g of phenol as an end-capping agent, and dropwise add sodium hydroxide solution at the same time to keep the pH of the system at 7-14, and stir for 30 minutes; After the phases were washed three times with process water and hydrochloric acid solution, the oil phase was added to the precipitant, the white solid was washed out, filtered and dried, and a halogen f...

Embodiment 3

[0022] Example 3: In a six-necked flask with an electric stirrer, add polyhalogenated bisphenol A100g, water 300g, solvent methylene chloride 400g, dissolve completely with sodium hydroxide solution under stirring conditions, add catalyst triethylamine 1g, The temperature of the system was controlled at 12°C, 30 g of phosgene was introduced, and at the same time, the pH of the mixed system was adjusted between 7 and 14 with sodium hydroxide solution, and the prepolymerization reaction time was 20 minutes. After the prepolymerization reaction, raise the reaction temperature to 16°C, add 0.86g of phenol as an end-capping agent, and dropwise add sodium hydroxide solution at the same time to keep the pH of the system at 7-14, and stir for 20 minutes; After the phases were washed three times with process water and hydrochloric acid solution, the oil phase was added to the precipitant, the white solid was washed out, filtered and dried, and a halogen flame-retardant polymer with a nu...

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Abstract

The invention relates to a preparation method of low-molecular-weight halogen flame-retardant polycarbonate, which is characterized by comprising the following steps: a. adding polyhalo bisphenol A into a sodium hydroxide solution-haloalkane mixed system, completely dissolving by stirring at normal temperature, and meanwhile, adding a catalyst; b. introducing phosgene, meanwhile, dropwisely adding a sodium hydroxide solution to keep the pH value of the system at 7-14, and carrying out prepolymerization reaction at 0-20 DEG C for 0.2-1.5 hours; c. increasing the reaction temperature to 10-40 DEG C, adding a blocking agent, and meanwhile, dropwisely adding a sodium hydroxide solution to keep the pH value of the system at 7-14; d. after the reaction finishes, standing to stratify to obtain an organic phase, adding fatty alcohol, washing to obtain a white solid, filtering, and drying to obtain the product. By strictly controlling the prepolymerization and polycondensation reaction temperatures and the pH value of the reaction system, the synthesized product has small fluctuation of the molecular weight, and the molecular weight can be fixed within a certain range. The synthesis technique has the advantages of short period, simple operating technique and high efficiency.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of low-molecular-weight halogen flame-retardant polycarbonate. Background technique [0002] The halogen flame retardant polycarbonate oligomer prepared by polyhalogen bisphenol A and phosgene interface method has a moderate decomposition temperature, which is compatible with the decomposition temperature of various high polymers, and can be activated at the best moment when the gas phase and condensation are the same. To the flame retardant effect, the addition amount is small, the blend has good fluidity during processing, and can meet the requirements of processing small and complex parts. At the same time, it has good compatibility with polyester, no precipitation, and no blooming phenomenon on the surface of the product. Good flame retardant effect. In addition to blending with polycarbonate to produce flame retardant polycarbonate, it can also be used ...

Claims

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Application Information

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IPC IPC(8): C08G64/24
CPCC08G64/24
Inventor 齐国栋王萍付振波边祥成马建军李晓明乔鼎滕志君马瑞进崔杨赵贵荣孟蕾
Owner 甘肃银光聚银化工有限公司
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