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Bisphenol type flame-retardant polycarbonate interface method preparation method

A flame-retardant polycarbonate and phenol-type technology, which is applied in the field of preparation of bisphenol-type flame-retardant polycarbonate, can solve the problems of high production risk, high production cost, difficult operation, etc. The effect of improved safety and shortened process flow

Inactive Publication Date: 2005-01-26
WUHAN CHEM COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the phosgene method has great disadvantages: first, phosgene is highly toxic, has a low boiling point, and is a gas at room temperature. It is difficult to transport and store, and it brings potential harm to personal safety and the environment.
Second, the production process requires relatively high conditions: phosgene surge tanks and buffer tanks need to be equipped before feeding materials, the production workshop must be in a negative pressure state, and a more complicated tail gas absorption device is also required
Third, phosgene is inconvenient to use and difficult to measure accurately, which may cause side reactions
These factors lead to high production risk, high production cost and difficult operation

Method used

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  • Bisphenol type flame-retardant polycarbonate interface method preparation method
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  • Bisphenol type flame-retardant polycarbonate interface method preparation method

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0026] (1) Prepare a three-neck flask.

[0027] (2) Add NaOH 0.543g in the flask to make a 2% aqueous solution;

[0028] (3) Add 3.4g 2,2-bis(3,5-dibromo-4-hydroxyphenyl) propane (tetrabromobisphenol A) to the flask and stir slowly until all dissolve to obtain tetrabromobisphenol A sodium Salt solution, its pH value is 13.45;

[0029] (4) Adjust the temperature to 10°C-15°C and add 10ml of CH to the flask 2 Cl2 , and then add catalyst N,N-dimethylethylamine 3.4ul;

[0030] (5) Weigh 0.68g triphosgene and dissolve in 15ml CH 2 Cl 2 stand-by;

[0031] (6) Control the temperature of the system in the flask at 10°C-15°C, slowly add triphosgene solution dropwise under strong stirring, and at the same time add dropwise 5% NaOH aqueous solution prepared in advance to keep the pH value of the reaction system in the range of 13-14 Inside;

[0032] (7) After the dropwise addition is completed, the temperature is rapidly raised to 24-26 ° C, and a sufficient stirring rate is maint...

example 2

[0035] (1) Prepare a three-neck flask.

[0036] (2) Add NaOH 0.53g in the flask to make a 2% aqueous solution;

[0037] (3) Add 3.4g 2,2-bis(3,5-dibromo-4-hydroxyphenyl) propane (tetrabromobisphenol A) in the flask, stir at a slow speed until all dissolve to obtain tetrabromobisphenol A Sodium salt solution, measuring its pH value is 13.35;

[0038] (4) Adjust the temperature to 10°C-15°C and add 10ml of CH to the flask 2 Cl 2 ;

[0039] (5) add 0.103g 2,4,6-tribromophenol in the flask;

[0040] (6) Add catalyst N,N-dimethylethylamine 3.4ul in the flask;

[0041] (7) Weigh 0.68g triphosgene and dissolve in 15ml CH 2 Cl 2 stand-by;

[0042] (8) Control the temperature of the system in the flask at 10°C-15°C, slowly add triphosgene solution dropwise under strong stirring, and at the same time add dropwise 5% NaOH aqueous solution prepared in advance to keep the pH value of the reaction system in the range of 13-14 Inside;

[0043] (9) After the dropwise addition is com...

example 3

[0046] (1) Prepare a three-neck flask.

[0047] (2) add NaOH 0.371g in the flask, be made into 2% aqueous solution;

[0048] (3) Add 2.38g 2,2-bis(3,5-dibromo-4-hydroxyphenyl) propane (tetrabromobisphenol A) in the flask, stir at a slow speed until all dissolve to obtain tetrabromobisphenol A Sodium salt solution, measuring its pH value is 13.64;

[0049] (4) Weigh 0.476g triphosgene and dissolve in 20ml CH 2 Cl 2 , added to the three-necked flask at one time;

[0050] (5) Adjust the temperature of the system in the flask to 10°C-15°C and add 2.4ul of catalyst N,N-dimethylethylamine at one time, and stir for 5 minutes;

[0051] (6) Rapidly heat up to 24°C-26°C for reaction, and simultaneously add dropwise 5% NaOH aqueous solution prepared in advance to keep the pH value of the reaction system in the range of 13-14, and react for 1 hour.

[0052] (7) Wash with 21ml of 3% hydrochloric acid after completion of the reaction, wash twice with water, evaporate to dryness in vacu...

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Abstract

The invention provides a novel method for preparing Bisphenol type flame-retardant polycarbonate characterized by that, tri-phosgene is employed to substitute phosgene for reacting with bis-phenol raw material to obtain flame-proof polycarbonate. The method can realize greatly improved production safety.

Description

technical field [0001] The invention relates to a preparation method of bisphenol type flame-retardant polycarbonate. Background technique [0002] At present, in the production of polycarbonate and flame-retardant polycarbonate, the phosgene method plays a major role. Recently, US Patent 20020111456 reported a method for obtaining tetrabromobisphenol A flame-retardant polycarbonate by reacting phosgene and tetrabromobisphenol A. However, the phosgene method has great disadvantages: first, phosgene is highly toxic, has a low boiling point, and is a gas at room temperature. It is difficult to transport and store, and brings potential hazards to personal safety and the environment. Second, the production process requires relatively high conditions: a phosgene surge tank and a buffer tank must be equipped before feeding materials, the production workshop must be in a negative pressure state, and a more complicated exhaust gas absorption device is also r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/04
Inventor 喻发全吴元欣常志
Owner WUHAN CHEM COLLEGE
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