تفاعل #59229

معادلة التفاعل

4,4′-dihydroxydiphenyl ether

phosgene

sodium hydroxide

p-tert.-butylphenol

sodium hydroxide

n-ethylpiperidine

4,4′-dihydroxybiphenyl

→

4,4′-dihydroxydiphenyl ether 4,4′-dihydroxybiphenyl

المذيبات

methylene chloride

water

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas added during the phosgenation
2. 2
   workup.ADDITIONis added as catalyst
3. 3
   أخرىThe aqueous phase is separated off
4. 4
   غسيلwashed with distilled water until neutral and free of salt
5. 5
   أخرىPrecipitation of the polymer in methanol
6. 6
   تجفيفdrying yield 8.7 g of polycarbonate

الإجراء التجريبي

220 ml of methylene chloride are added to a solution, rendered inert with nitrogen, of 7.077 g (0.035 mol.) of 4,4′-dihydroxydiphenyl ether and 2.793 g (0.015 mol.) of 4,4′-dihydroxybiphenyl (DOD) as well as 4.4 g (0.111 mol.) of sodium hydroxide in 220 ml of water. In a one-step procedure, 0.263 g (0.00175 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, 6.9 ml (9.88 g, 0.099 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, 0.07 ml (0.0005 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 8.7 g of polycarbonate.

المصدر