Preparation method of polycarbonate
A technology of polycarbonate and chloroformic acid, which is applied in the field of polymer material polycarbonate preparation, can solve the problems of affecting the molecular weight distribution of the product, difficult to control the molecular weight of the product, etc., and achieve the effects of short reaction time and simple operation.
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Embodiment 1
[0018] In a 1L four-necked flask, add 200 g of water, 450 g of dichloromethane, 58 g of bisphenol A, and 0.5 g of tetrabutylammonium bromide to prepare 100 g of a 28% (mass percent) NaOH solution for use. In the first stage of the reaction, the temperature of the system is controlled at about 15°C, and the prepared NaOH solution is passed through at the same time. From 3 to 7, stir the reaction for 10 minutes and then rapidly raise the temperature to 25°C. The reaction enters the second stage, and at the same time pass phosgene and drip the unfinished NaOH solution, the speed of passing light is stable at 0.4-0.6L / min, adjust the speed of dropping NaOH solution to control the pH of the system at 10-13, and control the reaction temperature Between 25 and 40°C, after 30 minutes, the lye was added dropwise, the phosgene flow was stopped, and the pH of the system was 11. Add 1.5g of p-tert-butylphenol, continue to stir for 30min, separate the liquids, wash the organic phase with ...
Embodiment 2
[0020] In a 1L four-necked flask, add 200g of water, 450g of dichloromethane, 58g of bisphenol A, and 0.5g of tetrabutylammonium bromide to prepare 100g of 28% (mass percentage) NaOH solution for subsequent use. stage, control the temperature of the system at about 15°C, pass phosgene and drop the prepared NaOH solution at the same time. After reacting for 20 minutes, the temperature was raised rapidly to 25°C, and the reaction entered the second stage. Simultaneously pass phosgene and drip the unfinished NaOH solution, the speed of light passing is stable at 0.4-0.6L / min, adjust the speed control system of dropping NaOH solution The pH is 10-13, and the reaction temperature is controlled between 25-40°C. After 25 minutes, the lye is added dropwise, and the phosgene is stopped. The pH of the system is 11. Add 1.5g of p-tert-butylphenol, continue to stir for 30 minutes, and separate the liquid. The organic phase was first washed with 2% (mass percent) HCl solution, then washed ...
Embodiment 3
[0022] In a 1L four-necked flask, add 200g of water, 450g of dichloromethane, 58g of bisphenol A, and 0.5g of tetrabutylammonium bromide to prepare 100g of 28% (mass percentage) NaOH solution for subsequent use. stage, control the temperature of the system at about 15°C, pass phosgene and drop the prepared NaOH solution at the same time. After reacting for 30 minutes, the temperature was raised rapidly to 25°C, and the reaction entered the second stage. At the same time, the phosgene was passed and the unfinished NaOH solution was added dropwise. The light passing speed was stabilized at 0.4-0.6L / min. The pH is 10-13, the reaction temperature is between 25-40°C, the lye is added dropwise in 18 minutes, the phosgene is stopped, the pH of the system is 11, 1.5g of p-tert-butylphenol is added, and the stirring is continued for 30 minutes, liquid separation, organic The phase was first washed with 2% (mass percent) HCl solution, then washed with 300 g of deionized water until neut...
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