Preparation method of polycarbonate

A technology of polycarbonate and flow, which is applied in the field of preparing polycarbonate by phosgene interface method, can solve the problems of slow polycondensation reaction of phosgene and bisphenol, increase of phosgene and alkali consumption, long reaction time, etc., and meet the reaction conditions Easy to control, automatic control, and short reaction time

Inactive Publication Date: 2010-12-29
甘肃银光聚银化工有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the pH value of the system is low, the polycondensation reaction of phosgene and bisphenol is very slow, the reaction time is long, and the production efficiency is low
When the pH value of the reaction system is high, since phosgene is easily hydrolyzed during the polycondensation reaction, the consumption of phosgene and alkali is increased

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Add 300.0g of bisphenol A, 4.0g of phenol, 2.20mL of triethylamine, 1460mL of dichloromethane, and 2200mL of deionized water into the reaction kettle, and start stirring. Control the sodium hydroxide aqueous solution flow rate at 10.00g / min, pass into the sodium hydroxide aqueous solution of 30.0wt% in the reactor, pass into phosgene simultaneously, and adjust the phosgene flow rate to keep the pH value of the reaction medium at 10~11, After the reaction was carried out for 22 minutes, the flow rate of the aqueous sodium hydroxide solution was changed to 12.00 g / min, and the phosgene flow rate was adjusted to keep the pH value of the reaction medium at 10-11, and the reaction was continued for 4 minutes to end the reaction. The mixture was allowed to stand still to separate layers, and no phenols precipitated out after the aqueous phase was acidified. Take the organic phase, wash, precipitate, and filter to obtain white polycarbonate resin powder.

Embodiment 2

[0014] Add 300.0g of bisphenol A, 4.90g of phenol, 2.20mL of triethylamine, 1460mL of dichloromethane, and 2200mL of deionized water into the reaction kettle, and start stirring. Control the sodium hydroxide aqueous solution flow rate at 6.00g / min, pass into the sodium hydroxide aqueous solution of 30.0wt% in the reactor, pass into phosgene simultaneously, and adjust the phosgene flow rate to keep the pH value of the reaction medium at 10~11, After the reaction was carried out for 22 minutes, the flow rate of the aqueous sodium hydroxide solution was changed to 10.00 g / min, and the phosgene flow rate was adjusted to keep the pH value of the reaction medium at 10-11, and the reaction was continued for 6 minutes to end the reaction. The mixture was allowed to stand still to separate layers, and no phenols precipitated out after the aqueous phase was acidified. Take the organic phase, wash, precipitate, and filter to obtain white resin powder.

Embodiment 3

[0016] Add 200.0g of bisphenol A, 2.30g of phenol, 1.20mL of triethylamine, 1100mL of dichloromethane, and 1600mL of deionized water into the reaction kettle, and start stirring. Control the sodium hydroxide aqueous solution flow rate at 6.00g / min, pass into the sodium hydroxide aqueous solution of 30.0wt% in the reactor, pass into phosgene simultaneously, and adjust the phosgene flow rate to keep the pH value of the reaction medium at 9~11, After the reaction was carried out for 25 minutes, the flow rate of the aqueous sodium hydroxide solution was changed to 12.00 g / min, and the phosgene flow rate was adjusted to keep the pH value of the reaction medium at 10-11, and the reaction was continued for 2 minutes to end the reaction. The mixture was allowed to stand still to separate layers, and no phenols precipitated out after the aqueous phase was acidified. Take the organic phase, wash, precipitate, and filter to obtain white polycarbonate resin powder.

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PUM

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Abstract

The invention relates to a preparation method of polycarbonate, belonging to the technical field of preparing high molecular material, in particular to a method for preparing polycarbonate through phosgene interface method; in the course of reaction, the flow of phosgene is controlled to correspondingly regulate the flow of alkaline solution, thus the pH value of the reaction system is controlled within a proper range so as to improve the reaction rate and the conversion efficiency of phosgene and bisphenol.

Description

technical field [0001] The invention belongs to the technical field of preparation of polymer materials, in particular to a method for preparing polycarbonate through a phosgene interface method. Background technique [0002] Polycarbonate is an engineering plastic with excellent performance. It has superior optical transparency and high impact strength, excellent thermal stability, creep resistance and cold resistance, as well as good electrical insulation and flame retardancy, so it is widely used in building transparent plates, electronic appliances, optical discs, etc. It is widely used in fields such as media and automobile industry. Polycarbonates are usually prepared by an interfacial method in which phosgene and bisphenols (such as bisphenol A) are dissolved in the two solutions of a water-insoluble inert organic solvent (such as methylene chloride) and an aqueous solution (such as sodium hydroxide). React in a phase medium under the action of a catalyst. Accordin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/24
Inventor 马建军苏朝晖付振波张光宇
Owner 甘肃银光聚银化工有限公司
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