C.I. 冰染重氮组分26 (C.I. 37070) 生产工艺  CAS号 [93-67-4]

CAS名:Benzenamine, 5-Chloro-2-phenxy-, 参考文献:Beil. 13, E¹, 118. E², 183. E³, 843.

用途: C.I. 酸性红249. C.I. 酸性蓝128. 发明者: Montmollin, Bonhote, Spieler  1922年。

生产工艺文献:  FIAT 764 – Echtrot FG.  Echtrotsalz FG. 原版Colour Index 未作进一步说明，为什么？

BIOS 1149, 35-36.  (=胶卷 PB 80376)  Fast Red FG Base. 英国人译自德文。抄录如下。

反应式:  本人有加注。译者未注明译自哪个PB报告号。
 

Stage 2: 4-Chloro-2-aminidiphenyl ether.

Plant: 2000 l. C. I. reduction pan. 3000 l. C.I. extracter. 3000 l. Wrought iron still. 3000 l. Settling vessel.

Process:

The reducer is charged with 300 l. of water, 100 kg. of iron borings and 20 kg. of formic acid and the mixture boiled for 1 hour. Then 240 kg. molten 4-chloro-2-nitrodiphenyl ether are run in simultaneously with the addition of 280 kg. of iron borings over 3 hours. Heating with jacket steam is continued until reduction is complete – 16 hours total time including charging.

Test: The C. Pt. of a sample of the oil must be 40⁰ and it must give a clear solution in dilute hydrochloric acid.

The water is then distilled and the residue blown to the extractor.

Here the sludge is extracted with 6 lots of benzene, the total usage being 10000 l. The benzne extracts are blown to the still and the benzene recovered. Vacuum is applied to distil off any phenol arising from excess phenol contained in the crude nitro compound. The residual oil is blown to the purification still where several batches are accumulated and distilled together, b. p. 240 – 250⁰C at 25 mm.

Yield = 96% theory.  Quality:  C. Pt. ≤ 43⁰C.

Notes: If the water is not removed prior to extraction emulsification may occur. More benzene is then required for complete separation.

Stage 3:  Fast Red FG Base.  4-chloro-2-aminodiphenyl ether hydrochloride.

Plant:  3500 l. agitated vat, tiled with Hoechster tiles and cement.     Lead stirrer, lead piping, and acid-resisting tiled nutsche.

Process:

    1000 l. of water and 500 kg. of the base re heated to 70⁰ whereby the base melts. The air in the vessel is replaced by nitrogen to

Minimize oxidation.

    Hydrochloric acid (19.5⁰Be’. 1000 kg.) is then run in at 70⁰. The suspension is cooled to 15 - 20⁰ during 12 hours and then blown to

The nutsche, pulled dry and washed three times with saturated brine (500 l. each). The hydrochloride is dried at 60⁰ in vacuum, ground

and sieved through 40 mesh.

    The dry product has a strength of nearly 100% as hydrochloride (107 wt.% of base charged) and is standardized to 85 – 86% for sale

As Fast Red FG Base. Yield = 92% theory.

中文摘译文。张澍声。《精细化工中间体工业生产技术》 1996年。P. 137. 摘译自BIOS 1149,35. 请见原书。 

PB 70422, 1995-1996. Echtrotsalz FG. By Prosiegel. 1943年9月19日。生产工艺。1.5美元 未抄录。

国内研究动态：

4-氯-2-氨基二苯醚的合成。（铁粉还原法）[J]  上海染料 1974,2, 17-18.

邱 彬 孙喜成。2-硝基-4-氯二苯醚合成新工艺。（无还原）  [J]  染料工业. 1990,1, 14-17.

刘 杰  李树仁。弱酸艳红B 合成工艺的改进。（用硫化碱还原法）[J] 染料工业。1997,5, 24-26.

加注：

    产品生产技术的先进性，只有对比才有可能进行评述。

陈忠源  2016年11月16日       于 无锡   明辉国际。