CAS号 [3453-84-7] 生产工艺      2,4,5-三甲基苯磺酸

CAS名: Benzenesulfonic acid, 2,4,5-trimethyl-         历史参考文献: Beil. 11. 待检索。

用途: 医药。LookChem 网，生产与经营单位登录25家。

BIOS 1153, 65-66. （=胶卷PB 85687）。 Pseudocumene-5-sulfonic acid. (Höchst).  英国人摘译自德文（无资料来源）。

反应式: 本人有加注。

Plant:  One sulfonator, 1500 l., iron agitator,thermometer, blow-leg, reflux condenser, heating and cooling jacket. 

One monohydrate measure vessel, 540 l., iron.          One stone nutsche, 3300 l., rubber-covered iron.

One nutsche receiver, 7500 l., rubber-covered, rubber-covered agitator, rubber-covered blow-leg.

Procedure:

1300 kg. of 95% sulfuric acid are charged to the sulfonator and heated to 75℃.  At this temperature 400 kg. of pseudocumene are run in slowly at such a speed that the temperature remains at 75-80℃. (finally with cooling water on).  The batch is agitated at 80℃. for 1 hour and a sample taken.

Test: A few cc. of the sample are mixed with just sufficient water to redissolve the precipitate which forms.  The solution must then contain no oily droplets of unchanged pseudocumene and must be only slightly turbid.

If the test is satisfactory 120 l. of water are slowly run into the completed sulphonation during which time the temperature must not rise above 80℃.  The pseudomene sulphonic acid crystallizes out with evolution of heat.  Final concentration of the mother liquor = 82% H2SO4.  The batch is now cooled to 20℃. with agitation and allowed to stand 12 hours.  It is then blown to the stone nutsche and filtered by suction.  The sulphonator is rinsed out with mother-liquor and the filtrates are run to drain.

The well-dried, filtered, crystalline batch is dug out into a rubber lined truck and weighed.

Yield = Approx. 900 kg., at ca. 70% strength = approx. 630 kg. 100% = 94% of theory.

The analysis by barium salt or organic sulphur is not accurate; the yield of sulphotrimellitic acid (obtained by further processing) is calculated back to the pseudocumene charged.

张澍声 《精细化工中间体工业生产技术》 1996年。P. 91.  1,2,4-三甲苯-5-磺酸。 译自BIOS 1153, 65.

在1500 L铸铁磺化釜中加入1300 kg 95% 硫酸，并加热至75℃。在此温度将400 kg 1,2,4-三甲苯缓缓加入，加入速度要使温度保持75-80℃，最后可用冷水冷却。反应物在80℃搅拌1小时，取样检验。

检验：取几毫升样品，加水使形成的沉淀重新溶解，溶液必须不含未反应的1,2,4-三甲苯的油滴，并且只能是稍有浑浊。

如果检验是满意的，向磺化反应物中缓缓加入120 L水，加入温度不可超过80℃，1,2,4-三甲苯-5-磺酸结晶出来，并释放出结晶热。母液的最后那段为82% 硫酸。反应物搅拌冷却到20℃,并放置12小时，在抽滤机上过滤。磺化物用母液洗涤，滤液弃去（抄注：当时无三废处理，是排入下水道。 To drain!）。干燥后得约900 kg产品，含量70%，相当于630 kg 100% 产品，为理论量的94%。

该收率是不精确的，因为用钡盐分析或分析有机硫是不准确的。

PB 70254, 7088-7089.  Pseudomene-5-sulfonic acid.  德文原件，未抄录。

学习与思考:

如何了解和利用历史文献，看来已不太重要，但本人坚信有总比没有好！再次谢谢读者的点读！

陈忠源 2018年5月23日。