CAS号 [102-08-9] 生产工艺  二苯硫脲

CAS名: Thiourea, N,N’-diphenyl- 历史参考文献: Beil. 12, 394; E¹, 245; E², 227; E³, 856; E⁴, 810.

用途: 硫化促进剂，（以及合成二苯胍）。C.I.还原蓝1 =C.I.颜料蓝66.反应类别: 脱硫化氢缩合。

生产工艺文献: 本人按手头资料整理如下：

BIOS 986, 381-382.（=胶卷PB 77764）No. 185. Thiocarbanilide (Vulkacit CA) (I.G. Hoechst).  英国人译自德文。  抄录如下。

反应式: 本人有加注，译者未说明资料来源。本人暂未找到德文原件。
 

Materials charge per Batch:   每批投料量:  以下抄录不分项。

Aniline  300 kg. Carbon disulphite 180 kg.  Sulphur   0.4 kg.     

Leonil SB  0.4 kg. （Dispersing agent）。 Caustic soda 33%  200 kg. Nitrogen  25 cu.m.

Capacity:  9 Batches / week = 150 tones per year.

Process Description:

Charge into a 1,000 l. enameled kettle 500 l. water, 300 kg. aniline, 0.4 kg. sulphur and 0.4 kg. Leonil SB. Remove the air with nitrogen and charge 180 kg. carbon disulphide by nitrogen pressure. Heat slowly to 45-50⁰C and hold at that temperature for 16 hr. The distillate proceeds through a reflux, two small aniline receivers, two static washers containing 33% caustic soda, a small tower in which caustic soda circulates, and finally into a 2 cu.m. kettle containing potassium permanganate where the last traces of hydrogen sulphide and other sulphurous bodies are removed. The scrubbed gases then proceed to the atmosphere via a chimney. The recovered aniline is used up in the next batch. When the reaction is complete the excess carbon disulphide is distilled off into a 70 l. receiver. The batch is blown to a tile-lined filter with nitrogen and washed with 4 cu.m. water. Drying is carried out in a Venulith dryer at 60-70⁰C. For the manufacture of isatin-a-aniline the product is ground twice in a Kolloplex mill, but for normal sales purposes it is not ground. In summer the reflux and the carbon disulphide coolers are serviced with brine. The product is a white crystalline powder of M.P. 154⁰C and crystallizing point 148⁰C.

Remarks:

The gland of the condensation kettle is packed with asbestos string and graphite, and this is claimed to be very satisfactory.

The whole of the plant up to the recovered aniline receivers is of aluminium, but the Venulith is of iron.

Carbon disulphide handling is by means of nitrogen. Yield 340 kg. = 113% v.E.

Actual Yields: 1934 – 114.5%.  1935 – 114.6%. 1936 – 114%.   1937 – 114%.

张澍声  编译。《精细化工中间体工业生产技术》 1996年。P. 19. 二苯硫脲。译自BIOS 986,381. 抄录如下。

在1000 L搪瓷釜内加入500 L水，300 kg苯胺，0.4 kg硫和0.4 kg分散剂Leonil SB（抄注：为甲基萘磺酸甲醛缩合物分散剂）。用氮气赶出空气，加入180 kg二硫化碳。缓缓加热到45-50⁰C，在此温度保持16小时。馏出物经过一回流柱，两个小的苯胺接受器，两个静止的洗涤器（含33% 氢氧化钠溶液），一小塔，内有氢氧化钠溶液回流，最后进入2000 L锅中，锅内有高锰酸钾，以除去最后痕量的硫化氢和其它含硫物质，洗涤后的气体经烟道进入大气。回收的苯胺用于下批反应。反应完成后，过量的二硫化碳蒸馏出来。反应物用氮气压往过滤机过滤，用4000 L水洗涤，滤饼用耙式干燥器在60-70⁰C干燥。如果用于制备N-靛红-a-酰苯胺，产品需研磨两次；如果正常销售，无需研磨。（抄注: Venulith 为耙式干燥器，译者未译！）

产品为白色结晶粉末，熔点154⁰C，结晶温度148⁰C。得到340 kg 二苯硫脲。 

本人观点:  任何译文提供原文是每个技术人员应该做到的事。因为你不是完人。（抄注：是本人所加。）

如果读者对Lenonil商品品名感兴趣，可参见PB 74735.

陈忠源  2017年7月6日         于 无锡   明辉国际。