CAS号 [135-12-6] 生产工艺 4,4’-二氯-2-硝基二苯醚
CAS名: Benzene, 4-chloro-1-(4-chlorophenoxy)-2-nitro-参考文献: Beil. 6. E2, 227.
用途: 有机合成。冰染重氮组分33。
生产工艺文献:
BIOS 1149, 37-40. (PB 80376) Fast Red FR Base. 4,4’-Dichloro-2-nitrodiphenyl ether. 英国人译自德文。抄录如下。
反应式: 本人有加注。暂未找到德文原件。 Plant: 1 2000 l. C.I. vessel, agitated, heating and cooling coils. 1 2000 l. enameled vessel. 1 Nutsche.
Materials: Chlorobenzene 900 kg. Sodium p-chlorophenate 421 kg. (=193 kg. NaNO2)
2,5-Dichloronitrobenzene 550 kg. (= 192 kg. NaNO2)
Process:
The reaction vessel is charged with 900 kg. of chlorobenzene followed by 421 kg. of the sodium salt of p-chlorophenol. The mixture is well stirred and heated to 950. 550 kg. of molten 2,5-dichloronitrobenzene are blown in from a pressure vessel during 8 hours with the temperature not higher than 1000 (cooling). Heating at 1000 is cpntinued until condensation is complete; this is shown by a constant caustic alkalinity figure equivalent to reaction of 100% of the dichloronitrobenzene. Total time approx. 5 days.
The molten batch is then blown into the second 2000 l. vessel, neutralized with mineral acid, and the chlorobenzene steam distilled off. The batch is filtered and washed free from sodium chloride. Yield; 96% theory.
张澍声 《精细化工中间体工业生产技术》 1996年。 P. 22. 译自BIOS 1149. 4,4’-二氯-2-硝基二苯醚。抄录如下。
在铸铁锅中加入900 kg氯苯,421 kg对氯苯酚钠盐,混合物很好搅拌,并加热到95℃。于8小时内加入熔融的2,5-二氯硝基苯,并冷却使温度不超过100℃。继续在100℃加热至缩合完全,这表现在恒定的氢氧化钠含量,以及全部二氯硝基苯缩合的消耗,总时间约为5天。
熔融的反应物在另一锅中用无机酸中和,水汽蒸馏出氯苯,过滤,水洗至不含氯化钠。收率96%。
陈忠源 2017年11月16日 本文地址:http://www.陈忠源化学文库.cn/Article.asp?ID=10000552