| [打印本页][打印选项] |
| CAS号 [99-98-9] 生产工艺。 N,N-二甲基对苯二胺 |
CAS号 [99-98-9] 生产工艺。 N,N-二甲基对苯二胺
CAS名：1,4-Benzenediamine, N,N-dimethyl- 历史参考文献：Beil. 13, 72; E1, 21; E2, 39; E3, 109; E4, 106.
用途：酸性蓝4。碱性红5。碱性紫5, 8。碱性蓝9, 10, 17, 25。 碱性黑1。媒介蓝35, 51。 溶剂蓝8, 51。
塑料助剂，医药等。LookChem网登录生产与经营单位52家。
BIOS 1155, 7-8.
（=胶卷PB 79309）。 p-Aminodimethylaniline solution. (Mainkur). 英国人译自德文（Mainkur厂）。
反应式：本人有加注，暂未找到德文原件。（含单，双盐酸盐及其LookChem网登录数。）。
Materials: p-Nitrosodimethylaniline (100%) M.W. 150.
218 kg. Iron powder 200 kg.
Soda ash 130 kg.
Procedure:
The reducer
(standard C.I. vessel) is charged with 5000 l. water and 200 kg. iron powder,
and the temperature adjusted to 35-40℃. At
this temperature is added during 1 hour, 218 kg. p-nitrosodimethylaniline
hydrochloride (as 100% M.W. 150). After
stirring 1 hour reduction is complete giving a colourless solution.
Soda ash (130
kg.) is added to neutralize and precipitate iron oxide, the batch is filtered
and the oxide washed with cold water.
Final volume
of filtrate = 8000 l. Yield (as total
liquor) 8000 l. containing 173 kg. p-aminodimethylaniline at 100%. = 89%
theory.
细田豊 《理论制造染料化学》 1957年。 P. 468. p-Aminodimethylaniline. 译自BIOS 1155.
铸铁还原釜に水5 t と铁粉200 kgを装入，35-400でニトロソジメチルアニリン盐酸盐218 kgを1 hで加え1 h搅拌すれば还原して無色の溶液となる。ソ- ダ灰130 kgでアルカリ性にし酸化铁と滤别，水洗する。8 m3, p-アミノジメチルアニリン173 kg含有，收率89%。
张澍声 《精细化工中间体及产品生产工艺》2006年。 P. 445. 对氨基-N,N-二甲基苯胺。 译自BIOS 1155, 7.
在铸铁还原锅中加入5000 L水和200 kg铁粉，在35-40℃于1小时内加入218 kg对亚硝基二甲基苯胺盐酸盐，搅拌1小时后，还原为无色的溶液。用130 kg碳酸钠中和至析出氧化铁，过滤除去氧化铁，水洗。得到的8000 L溶液中含有173 kg对氨基二甲基苯胺，收率89%。
BIOS 1433, 12.
（=胶卷PB 81029）。 p-Aminodimethylaniline. (Hoeschst). 英国人译自德文 （Hoeschst厂）。
Plant: 1 x 500 litre lead lined vessel for H2SO4 and
ice. 1 x 4000 litre tile lined
pressure vessel.
1 x 7000 litre iron pressure vessel for
reduction liquor. 1 x washing type
press.
Process: Reduction.
（抄注： nitroso 见CAS号 [138-89-6]）。
The
equivalent in 600Be’ strength of 101.4 kg. H2SO4 100% is added to the nitroso
mixture and the volume made up to 3000 litres at 0℃. with ice.
This is reduced in four or five portions. For reduction of the first portion, 1300 kg.
iron borings and 800 litres water are brought to 26℃. in the reducer, and the nitroso mixture
blown inthrough an 8 mm. spray. The
temperature rises to 40℃. After 21/2 hours the
reduction is filtered, the filtrate running to the “Thio acid” plant. 100-150 kg. iron are added to the reducer,
with 800 litres water, and the second portion of nitroso reduced, and so
on. After each reduction, the tile lined
vessel is washed out with 250 litres water.
The
temperature of reduction must not exceed 40-42℃. and ice is added if necessary. The iron residue is finally washed with 800 litres
water and the sludge press is given six water washes of 150 litres each.
FIAT 1313,II,
372. （=胶卷PB 85172）。 p-Aminodimethylaniline. (Hoeschst). 美国人译自德文。 （Hoeschst厂）。
In the
jacketed 2600 l. iron reducer containing 1300 kg. iron filings reduce the nitrosation
charge in 4-5 parts at 25-40℃. After each reduction add
100-150 kg, iron filings to replace that consumed. Filter into 16,000 l. wooden tub with iron
agitator and brine coil.
国内出版物：
侯乐山 主编 《中国精细化工产品集 – 原料及中间体10396种》 2006年。 P. 238. 对氨基二甲基苯胺。
生产方法：还原：将亚硝化粗品有水搅拌成糊状，再加工业浓盐酸，外面用冰水冷却，慢慢加入锌粉，加入温度不宜超过45℃。
提取：加氢氧化钠溶液至碱性后，再用苯提取，苯溶液用无水碳酸钾干燥，用水浴回收苯，再减压蒸馏收集成品。
其它制法：略。 （抄注： 无资料来源！ 用锌粉还原和苯萃取方法好吗？）。
陈忠源 2018年8月22日。
文章作者：陈忠源 |
