CAS号 [97-06-3] 生产工艺  4-甲基-3-硝基苯磺酸

CAS名: Benzenesulfonic acid, 4-methyl-3-nitro-  参考文献: Beil. 11, 110; E², 68; E³, 323; E⁴, 481.

用途: 硫化棕54。活性染料染色助剂。农药。有机合成等。（通过CA可以看到有关资料。）

生产工艺文献: 按手头资料整理如下：

BIOS 1153, 34-36.（=胶卷PB 85687）2-Nitrotoluene-4-sulphonic acid. (Na salt) (Leverkusen).英国人译自德文. 抄录如下。

反应式: 本人有加注，译者未说明译自哪个德文原件。本人未抄录德文原件（PB 25624,1078-1080.）
 

Outline: o-Nitrotoluene is sulphonated with 26% oleum.

Plant: 1 Container for 26% oleum. 800 l. 1 Cast iron sulphonation vessel. 1 Vat. 10,000 l.

1  Nutsche. 6 cu.m. rubber-lined. Montejus. 2 Salt bins of 16 cu.m. 1 Centrifugal pump for salt solution.

Materials: 700 kg. o-Nitroroluene ≌ 352 kg. Nitrite. 1920 kg.  26% oleum. Approx. 4000 kg.salt.

Process:

The sulphonation vessel is charged with 700 kg. of o-nitrotoluene and at 20-25⁰C., 1920 kg. of 26% oleum are run slowly in as a thin stream. When this addition is completed, the temperature is raised by means of the jacket to 60-65⁰C. for 6 hours.

Test: A sample in water must be completely soluble and not show the presence of o-nitrotoluene. The solution however is usually slightly milky and opalescent.

The sulphonation is now cooled to 20⁰C. and blown into two separate vats (10,000 l.), into each of which has been charged 2,500 l. of water. The temperature rises to about 45⁰C.

3,000 l. of saturated brine are then added to each vat. By the addition of the cold brine the temperature drops to 25-30⁰C. By salting in this manner, the product separates in a more crystalline manner than would otherwise be the case. A further addition of 750 kg. of rock salt is then made to each of the vats.  The vats are stirred overnight until cold.

Test: A test of a filtered portion is taken to ensure that no further precipitation takes place with salt and that a reduced portion, when titrated, does not show more than 30 kg. NaNO₂ left in the mother liquors.

If these tests are satisfactory and the temperature is down to 20⁰C., the product is filtered. It is washed twice with brine solution and well pressed to remove the excess.

Yield: Paste – about 1,500 kg. (100 g. ≌ 21 g NaNO₂) ≌ 320 kg. NaNO₂ = 91% theory.

张澍声《精细化工中间体工业生产技术》 1996年。P. 69. 2-硝基甲苯-4-磺酸钠。译自BIOS 1153,34. 抄录如下。

在铸铁磺化釜中加入700 kg 邻硝基甲苯，在20-25⁰C以细流缓缓加入1920 kg 26% 发烟硫酸，加完后温度升至60-65⁰C,反应6小时。检验: 取样放入水中必须完全溶解，不显示邻硝基甲苯的存在。但是溶液通常微呈乳浊和不透明。

磺化液冷却到20⁰C,分别放入2个10000 L的槽中，每个槽中预先加有2500 L水，温度上升至45⁰C，然后加入3000 L饱和食盐水，由于食盐水的加入，温度降至25-30⁰C。在这种方式下盐析，与其他方式比较，产品更多以结晶方式分出，再加入750 kg 岩盐，搅拌过夜直至冷却。  检验; 取样过滤，滤液加盐确保不再有沉淀产生。另取样还原，用NaNO₂标液滴定，确保留在母液中的硝基甲苯磺酸消耗NaNO₂不大于30 kg。

检验满意后，温度降至20⁰C，产品过滤，用盐水洗涤二次，很好压滤。得到1500 kg滤饼，每100 kg滤饼相当于21 kg NaNO₂,

1500 kg滤饼相当于320 kg NaNO₂,收率91%。

PB 25624, 1078-1080. o-Nitrotoluolsaeure. 2-硝基甲苯-4-磺酸德文生产工艺原件。未抄录。

PB 70188, 6000. o-Nitrotoluolsaeure. 德文分析方法。 编号：71. 未抄录。

耐还原助剂BD试制成功。[J]化工技术资料（染料及中间体专业分册）1965, 3, 46-47. 摘录如下。

耐还原助剂BD= Albetex BD (Ciba.). 本资料未引用上述文献，硝化，磺化和成盐为实验室方法。不再抄录。以下为印花浆的配制和具体的应用例，请看原刊物。加注: 由此可以看到老产品的新应用开发！

陈忠源  2017年5月17日              于 无锡  明辉国际。