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| CAS号 [97-06-3] 生产工艺 4-甲基-3-硝基苯磺酸 |
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。
文章作者：陈忠源 |
