CAS号 [31515-43-2] 生产工艺      2-硝基二苯砜

CAS名: Benzene, 1-nitro-2-(phenylsulfonyl)-   历史参考文献: Beil. 6, 338; E1, 154; E3, 1059; E4, 1665.

用途: 医药，染料中间体（酸性黄246；酸性红42；冰染重氮组分18）。    反应类别: 脱硝缩合。

BIOS 1149, 17-18.（=胶卷PB 80376）。  o-Nitrodiphenylsulphone. (Leverkusen).  英国人译自德文（无资料来源）。

Plant:  1.  C.I., 6000 l. capacity, agitated autoclave.    2.  Distillation units.   1.  Blow-egg.   1.  Nutsche. 

Charge:  Ethanol 94%   4100 l.      o-Dinitrobenzene as 90% product = 250 kg.  NaNO2.         Benzenesulphinic acid = 254 kg.  NaNO2.

Process:

The autoclave is charged with 4100 l. of 94% alcohol and o-dinitrobenzene equivalent to 250 kg. NaNO2.  Then benzenesulphinic acid equivalent to 254 kg. NaNO2, is shoveled into the autoclave; this benzenesulphinic acid must be used immediately after delivery owing to its unstable nature.

The autoclave is sealed, heated to 700 with open steam and then to 130-135℃. with 2 atm. closed steam.  The temperature is held at 130-1350 for 15 hours and then cooled back to 50-600.  Residual pressure is released to atmosphere and the batch then blown to a separator.  Alcohol is distilled off during 5 hours, and the residue then heated with live steam to remove last traces.  The distilled alcohol is collected in a blow-egg and is then redistilled and re-used.

The product remaining is dropped to the nutsche at 60-700 and washed 2-3 times with hot water.    Yield = 85% theory.

The mother liquor is examined and if free from solid is blow to drain.  Quality: M. Pt. (dry)  142-146℃  (pure, 148℃.).

抄注：以上是英文译文。（因为未抄录德文原件，所以不好评述。）。应该是二次文献吧！

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

在6000 L高压釜中加入4100 L 94% 乙醇和相当于250 kg亚硝酸钠的90% 邻二硝基苯，再用铁锹加入相当于254 kg 亚硝酸钠的苯亚磺酸。由于苯亚磺酸不稳定，要现产现用。

关闭高压釜，用直接蒸汽加热到70℃，再用2巴间接蒸汽加热到130-135℃。在130-135℃保温15小时，然后冷却到50-60℃，剩余的压力释放到大气中，反应物压入分离器中。于5小时内蒸馏出乙醇，再用直接蒸汽除去最后残留的少量乙醇。蒸出的乙醇收集起来，经再蒸馏后复用。产品在60-70℃抽滤，用热水洗涤2-3次。干燥后的熔点142-146℃ （纯品148℃），收率 85%。

抄注：以上是译自英文，应该是三次文献吧！未见日人细田豊有译文。同时未见国内有那本化工手册有收录！

PB 25626, 1188.  Direction for technical production of o-nitro diphenyl sulfone. 1美元。美国人介绍如下。

Starting materials are benzene sulfinic acid and o-dinitrobenzene in alcohol.  The process is described.  Yield is about 85% of the theoretical.  In German.  德文。1940年2月。

抄注：PB 25626胶卷除北京有收藏，上海图书馆也有收藏。未知国内有多少人看过？当然这已是历史资料了！

奋斗是幸福的 ！只希望对读者有点参考价值，如果还有点用，欢迎读者参加讨论！

陈忠源 2018年2月20日（年初五）。