反应 #59223

反应方程式

4,4′-dihydroxydiphenyl ether

phosgene

sodium hydroxide

p-tert.-butylphenol

sodium hydroxide

n-ethylpiperidine

bisphenol A

→

bisphenol A 4,4′-dihydroxydiphenyl ether

溶剂

methylene chloride

water

反应条件

后处理

1. 1
   workup.ADDITIONwas added during the phosgenation
2. 2
   workup.ADDITIONis added as catalyst
3. 3
   其他The aqueous phase is separated off
4. 4
   洗涤washed with distilled water until neutral and free of salt
5. 5
   其他Precipitation of the polymer in methanol
6. 6
   干燥drying yield 5.76 g of polycarbonate

实验过程

126 ml of methylene chloride are added to a solution, rendered inert with nitrogen, of 8.088 g (0.04 mol.) of 4,4′-dihydroxydiphenyl ether and 9.132 g (0.04 mol.) of bisphenol A as well as 7.04 g (0.176 mol.) of sodium hydroxide in 126 ml of water. In a one-step procedure, 0.42 g (0.0028 mol. or 3.5 mol. % relative to bisphenol) of p-tert.-butylphenol (BUP) are added as chain terminator. At a pH value of 14 and at room temperature, 11 ml (15.8 g, 0.16 mol.) of phosgene are added in the course of 10 minutes. In order to prevent the pH value from falling below 12, 25% sodium hydroxide solution was added during the phosgenation. When the phosgenation is complete, and after rinsing with nitrogen, 0.11 ml (0.0008 mol., 1 mol. % relative to bisphenol) of n-ethylpiperidine is added as catalyst, and stirring is then carried out for one hour. The aqueous phase is separated off, and the organic phase is acidified with phosphoric acid and washed with distilled water until neutral and free of salt. Precipitation of the polymer in methanol and drying yield 5.76 g of polycarbonate.

来源