CAS号 [4273-98-7] 生产工艺     2-氨基二苯砜

CAS名: Benzenamine, 2-(phenylsulfonyl)-     历史参考文献: Beil. 13, 339; E3, 905; E4, 913.

用途; 农药。医药。染料：酸性黄246。 酸性红42。冰染重氮组分18。  反应类别: 还原。

BIOS 1149, 18-19.（=胶卷PB 80376）。 o-Aminodiphenylsulphone. (Leverkusen).  英国人译自德文（无资料来源）。

反应式:  本人有加注。（Leverkusen = Bayer 公司），暂未找到德文原件。

Plant:  2000 l.  C.I. reducer.      3000 l.  C.I. extractor.      3000 l.  Wrought iron still.       3000 l.  C.I. settling vessel. 

Process:

The reducer is charged with 400 l. of water, 200 kg. of iron and 20 kg. of formic acid, and heated for 1 hour at 1000.  After cooling to 950, 100 l. toluene are added.

500 kg. 100% o-nitrodiphenylsulphone are charged in during 12 hours with simultaneous addition of 360 kg. iron.  The batch is then stirred at 950 until reduction is complete.

Test: A sample is dissolved in benzene and filtered and the solvent then removed; the residue should have a m. p. of 120-1210 and should give a clear solution in hydrochloric acid.

When reduction is complete, the batch is blown to the extractor and after addition of 10 kg. soda and 10 kg. Terrana is extracted 10 times with 1000 l. benzene..  Each extraction is stirred for only a short while to prevent too much base from being extracted; otherwise the gravity of the solvent layer becomes too great and emulsification may result.

The benzene extracts are blown to the distillation vessel and the solvent distilled off.  The remaining product can be further worked up if desired in one of three ways: by vacuum distillation, by solvent extraction or by sublimation.

Yield of crude = 95.5%.    Quality M. Pt. (dry) 117.5℃.

张澍声 《精细化工中间体工业生产技术》1996年。 P. 136, 邻氨基二苯砜。 译自BIOS 1149, 17.

在2000 L 铸铁还原锅中加入400 L水，200 kg铁粉和20 kg甲酸，在100℃加热1小时。冷却到95℃后，加入100 L甲苯。于12小时内加入500 kg邻硝基二苯砜，同时加入360 kg铁粉，反应物在95℃搅拌直至还原完全。

检验 – 取样溶解于苯，过滤，除去溶剂，熔点应为120-121℃。在盐酸中应为澄清溶液。

还原完成后，反应物压入萃取器中，加入10 kg Na2CO3和10 kg活性白土，用1000 L苯萃取10次。每次萃取只搅拌很短时间，以避免萃取更多的胺，否则胺溶剂层的比重变得过大，可造成乳化。苯萃取物在蒸馏锅中，，蒸馏出溶剂。留下的产品可采取三种方法之一加工：真空蒸馏，溶剂萃取或升华。粗品收率95.5%，熔点117.5℃。邻氨基二苯砜商品名Fast Orange LB Base.

抄注:

新时代应有新的动作，可惜本人老了（按退休时间计已过去25年多了，不去见上帝已算是最大的幸福！），只能做点力所能及的一点点小事，好在“奋斗是幸福的”。See you every day !

陈忠源 2018年2月24日