CAS号 [98-09-9] 生产工艺       苯磺酰氯

CAS名: Benzenesulfonyl chloride  历史参考文献: Beil. 11, 34; E1, 11; E2, 23; E3, 51; E4, 49.

用途: 医药。染料：冰染重氮组分41。 酸性黄65, 68。 酸性橙49。 酸性紫5。 酸性蓝264等。

生产工艺参考文献: 按本人手头资料整理如下。

BIOS 986, 56. （=胶卷PB 77764）  No. 21.   Benzenesulphonchloride. (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，暂未找到德文原件。

Plant Description:  设备: 以下抄录不再按原文分项。

1.  1 x 3.5 cu.m. reaction vessel of iron covered with Phenytal Resin and bottom tiled-lined. External cooling by means of a water spray.   2.  1 x 2 cu.m. intermediate vessel, tile-lined.   3.  1 x 6 cu.m. agitated vessel, tile-lined, with lead cooling coil.   4.  1 x 2 cu.m. homogeneously lead-lined separator.   5.  1 x 3.2 cu.m. receiver.   6.  1 x 4 cu..m. distillation vessel, iron, with jacket for heating with H.P. steam.   7.  1 x cu.m. stone-lined distillate receiver.   8.  1 x 2.5 cu.m. iron distillate receiver.   9.  2 x 7.5 cu.m. storage vessels for benzenesulphonchloride distillation.   10.  2 x 9 cu.m. iron storage vessels for benzenesulphonchloride distilled.

11.  1 x 10 cu.m. iron storage vessel for chlorsulphnic acid.   12.  1 x 7.5 cu.m. iron storage vessel for benzene.

Plant Capacity:  100 tons per month.

Process Description:

To 2,650 kg. chlorsulphonic acid in (1) charge at 30-330C. 600 kg. benzene, the hydrochloric acid being absorbed in a spray tower with water.  Stir for about 0.5 hr. and run the reaction mixture into (2).  From this run it at about 250C. into (3) condaining about 2,000 kg. drinking water with agitation.  The upper acid layer is removed and the oil washed twice with about 2 cu.m. water.  Separate the water in (4) and run the water-free oil to (5).  In this two batches are joined, and run into (6).  Distil under about 10 min. vacuum and at about 1600C.  The vacuum is produced by a steam ejector.  The residue from the distillation containing diphorylsulphone is run off molten to a wagon.  A water-containing fore-runnings fraction is received in (7) and the pure benzenesulphonchloride in (8).

Yield: 1,030 kg. benzenesulphonchloride.

The benzene used is pure and with setting point above + 50C.  The strength of the benzenesulphonchloride distilled is 98.99%.

张澍声  《精细化工中间体工业生产技术》 1996年。 P. 63.  苯磺酰氯。    译自BIOS 986, 56.         抄录如下。

在3.5 m3反应器中加入2650 kg氯磺酸，在30-330C加入600 kg苯，在喷淋塔中用水吸收盐酸。搅拌约0.5小时，在250C于搅拌下加入到2000 kg水中。去掉上层的酸，下层的油用约2 m3水洗涤2次。在约10 mmHg及1600C蒸馏，含砜的蒸馏残渣熔融取出。最初馏份含水另行接受，得到1030 kg苯磺酰氯，纯度98-99%。

PB 73377, 2386-2388.  Benzenesulfonyl chloride.           未抄录。

学习与思考：

以上抄录文，仅供共享参考。如何追踪和借鉴历史文献为我服务，是应该讨论的问题。

陈忠源  2018年4月30日