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| CAS号 [6086-29-9] 生产工艺 3-硝基-4-氨基乙酰苯胺 |
CAS号 [6086-29-9] 生产工艺 3-硝基-4-氨基乙酰苯胺
CAS名: Acetamide, N-(4-amino-3-nitrophenyl)- 历史参考文献: Beil. 13, 121; E1, 38; E4, 231.
用途: 酸性蓝6。 碱性棕17。 颜料紫17。
BIOS 1153, 131-134.
（=胶卷PB 85687）。 3-Nitro-4-aminoacetanilide. (Leverkusen). 英国人摘译自德文（无资料来源）。
反应式: 本人有加注，暂未找到德文原件。
Materials: 417 kg. 100% Diacetyl-p-phenylenediamine
(M.W. 192) ≈ 150 kg. Nitrite. 1500
kg. 98%
H2SO4 . 430 kg. Oleum 26%.
350 kg. Mixed
acid A (40% HNO3) ≈ 140 kg. HNO3 .
530 kg. Caustic soda 30%. 50
kg. Caustic soda 30%.
(a) Nitration: Into a 2,500 l. cast iron vessel, with water
cooling and gate-type agitator, are run 1500 kg. of 98% H2SO4 and 430 kg. of
26% oleum. After cooling to 15℃., 417 kg. of 100%
diacetyl-p-phenylenediamine (M.W. 192) (≈150 kg. nitrite) are added during 2
hours and agitated until all in solution.
This is run into the 2,500 l. nitration vessel, cooled to 0℃. and nitrated with 350 kg. of mixed acid “A”
(40% HNO3, 48% H2SO4, 12% H2O).
Test: A
portion of the nitration mass is diluted in ice water, reduced under 30℃. with zinc dust and titrated with sodium
nitrite solution.
If the test
is passed by the laboratory, dilute the mass into 5000 l. of water, keeping
under 10℃. with brine
cooling. After dilution, blow to the two
filter presses and wash acid-free with cold water. The resulting nitroacetyl-p-phenylenediamine
is charged into another vat with 3,000 l. of water and neutralized with approx.
50 kg. of caustic soda liwuor.
(b) Hydrolysis: The neutralized suspension is made up to
10,000 l. with water (in the iron vessel), 530 kg. of 30% caustic soda liquor
are run in and the mixture heated in approx. 1/2 hour to 95-100℃. The
mass must be alkaline to phenol phthalein throughout.
Test: A
sample is cooled to 20℃., filtered, acidified with hydrochloric acid and diazotized; a clear
diazo solution should result.
When passed
by laboratory the batch is cooled to 20-25℃., filtered on a nutsche, and washed clear
with water.
Yield: 395
kg. paste = 127 kg. Nitrite (100/32.2) = 85% of theory.
张澍声 《精细化工中间体工业生产技术》 1996年。 P. 53-54. 3-硝基-4-氨基乙酰苯胺。 译自BIOS 1153,131.
（1）硝化: 在一2500 L带水冷和框式搅拌器的铸铁溶剂釜中，加入1500 kg 98% H2SO4 和430 kg 26% 发烟硫酸，冷却到15℃后，于2小时内加入417 kg 100% 二乙酰基对苯二胺，相当于150 kg亚硝酸钠，并搅拌至完全溶解。将此溶液流入2500 L铸铁硝化釜中，冷却到0℃，并用350 kg混酸（40%硝酸，48%硫酸，12%水）硝化。
检验: 部分硝化物用冰水稀释，在30℃用锌粉还原，用亚硝酸钠溶液滴定。
如果检验通过，将硝化物稀释到5000 L水中，用冰盐水冷却到10℃以下，压滤，用冰水洗涤至不含酸。生成的硝基二乙酰基对苯二胺与3000 L水一起加入10000 L衬砖水解槽中，用约50 kg 30% 氢氧化钠溶液中和。
（2）水解: 中和的悬浮体加水至10000 L，加入530 kg 30% 氢氧化钠溶液，在约0.5小时内将混合物加热至95-100℃，在整个过程中反应物必须对酚酞为碱性。
检验: 取样冷却到20℃，过滤，用盐酸酸化，重氮化，应生成清晰的重氮化溶液。合格后，反应物冷却到20-25℃，抽滤，冷水洗涤。
得395 kg 膏状物，相对应127 kg NaNO2 。 收率85%。
学习与思考：
本资料作为历史资料，供无上述资料原件的读者参考！其中 [5345-53-9] 不再另列，请见以后要编写的CAS号总目录！
记得2004年，由《中国化工信息中心， 全国精细化工原料及中间体行业协作组》出版的《精细化工原料及中间体分册》，已使用“CAS登记号索引”。可惜！当时仍未利用好进口的历史资料，本人仍坚持上网只能说“吃饱了没事干”！
陈忠源 2018年5月17日。
文章作者：陈忠源 |
