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| CAS号 [13663-59-7] 生产工艺。 4-硝基-N-环己基苯胺 |
CAS号 [13663-59-7] 生产工艺。 4-硝基-N-环己基苯胺
CAS名：Benzenamine, N-cyclohexyl-4-nitro- 历史参考文献：待检索。
用途：有机合成。酸性橙28. 酸性红157。 LookChem网登录生产与经营单位7家。 反应类别：缩合，脱磺酸基。
BIOS 1153, 135-136. 4-Nitro-N-cyclohexylaniline.
(Leverkusen). 英国人译自德文（无资料来源）。
反应式：本人有加注，暂未找到德文原件。
Material:
4-Chloronitrobenzene-3-sulphonic acid 520 kg. 100%
M.W. 237.5 (≈150 kg. nitrite)。
Cyclohexylamine 200 kg. 100%
M.W. 99 (≈ 140 kg. nitrite)。 Soda
ash 240 kg。
Sulphuric acid 400Be‘ 580 l.
Process:
The cast steel autoclave is charged with 1600
l. of water, 240 kg. of soda ash and 520 kg. of
4-chloronitrobenzene-3-sulphonic acid and finally with 200 kg. of
cyclohexylamine. The total volume is
2700 l. The autoclave is sealed, heated
to 1400C, and held for 9 hours; pressure 4-5 atm.
The batch is cooled to 1000C. diluted with
500 l. of water and blown into the lead-lined autoclave. Here it is diluted with a further 1300 l. of
water and 580 l. of 400Be’ sulphuric acid added. Approx. 1/4 of the acid neutralizes the
excess soda and the remainder is required for the hydrolysis. The vessel is closed and heated at 1400C for
9 hours (press. 7 atm.). The autoclave
contents are then blown into a vat containing 3000 l. of cold water and stirred
until cold. In this way the product is
obtained in a very good filterable form which can easily be washed free from
sulphuric acid with cold water.
It is finally dried at 50-600 in vacuo. Yield = 355 kg. 100% M.W. 220. = 88% theory on cyclohexylamine.
张澍声 《精细化工中间体工业生产技术》 1996年。 P. 54. 4-硝基-N-环己基苯胺。 译自BIOS 1153, 134.
在3500 L铸钢高压釜中加入1600 L水，240 kg 碳酸钠和520 kg 4-氯硝基苯-3-磺酸，最后加入200 kg 环己胺，总体积为2700 L。封闭高压釜，加热到1400C，保持9小时，压力4-5巴。
反应物冷却到1000C，用500 L水稀释，并加入580 L 50% 硫酸，约1/4 的酸用于中和过量的碳酸钠，其余的酸用于水解（抄注：指脱去磺酸基）。关闭压力釜。在1400C加热9小时，压力为7巴。在30000 L槽中预先加入3000 L冷水，将高压釜内物料压入，搅拌冷却，过滤，水洗至不含酸。于50-600C真空干燥。
得量355 kg 100% 4-硝基-N-环己基苯胺。 收率 88%。
抄注：本人手头资料不多，暂未见国内出版物有本产品的报导，当然，读者可从LookChem网找到本产品。
陈忠源 2018年11月17日星期六。（抄录资料上网免费共享，是自得其乐，谢谢各位读者的点读！）。
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