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| CAS号 [27428-84-8] 生产工艺。 间三氯甲基苯甲酰氯 |
CAS号 [27428-84-8] 生产工艺。 间三氯甲基苯甲酰氯
CAS名：Benzoyl chloride, 3-(trichloromethyl)- 历史参考文献：Beil. 9. E2, 326.
用途：有机合成。C.I. 还原蓝30.
LookChem网登录生产与经营单位3家。
FIAT 1313, I, 265-266.（=胶卷PB 85172）。 m-Trichloromethyl-benzoyl
chloride. (I.G. Hoechst). 美国人译自德文（无资料来源）
(For m-trifluoromethyl benzoyl fluoride, an intermediate for
Indanthrene CLB.). 美国人未说明有德文原件，德文原件本人未抄录。
Plant capacity: 5 tons.
Equipment: 1) 1 leaded reaction
vessel, 1 cu. m., with leaded stirrer and bottom outlet. 2) 1 absorption system for hydrogen chloride.
Materials used per ton:
m-Xylenehexachloride 1250
kg. Iron chloride 130 kg.
Service requirements per ton of product:
Electricity 250 kwh. Steam
9 tons. Water 400 cu.m.
Air 400 cu.m.
Procedure:
In (1) 764 kg of m-xylene hexachloride are heated at 130℃ and 40 g of sublimed iron chloride are added. Within 5 – 6 hours a solution of 40 g of iron
chloride in 45 l of water is run in (2).
The evolved hydrogen chloride is absorbed in (2). After further stirring for several hours a
dried feeble air current is conducted through the product until the HCl has
been removed to a large extent. The
batch is discharged into leaded drums. Yield:
613 kg as is.
Control:
Determination of the freezing point of m-xylenehexachloride. Determination of the specific gravity and of
the boiling point of the trichloromethyl benzoyl chloride. Determination of the percentsge of
trichloromethyl benzoyl chloride: 18.6 g of aniline in 200 g of benzene and
25.8 g of trichloromethyl benzoyl chloride are mixed at room temperature and
200 cc. of benzene are slowly added.
After stirring for 1 hour the precipitate is sucked off and washed at
first with benzene, then with water, until aniline is no longer
detectable. The crude product shall melt
at 122-123℃.
Yield: About 25 g of aniline.
Quality: m-xylenehexachloride:
freezing point 30-35℃. d 35℃ =1.564. Trichloromethyl
benzoyl chloride: d 20℃ =1.51.
boiling point 285-286℃.
张澍声 《精细化工中间体工业生产技术》1996年。 P. 150-151. 间三氯甲基苯甲酰氯。 译自FIAT 1313,I, 265.
在1000 L铅反应器中加入764 kg 1,3-双(三氯甲基)苯，加热至130℃，加入40 g升华的三氯化铁。于5-6小时内加入40 g 三氯化铁在45 L水的溶液，释放的氯化氢吸收。再搅拌数小时后，通入干的空气流经过产品直至氯化氢在很大的程度上已经除去。反应物装入铅制的桶中。得到613 kg 产品。
1,3-双(三氯甲基)苯凝固点30-35℃。 d 35℃ =1.546。 三氯甲基苯甲酰氯沸点285-286℃。 d 20℃ = 1.51.
PB 70361. Reports on the
preparation of intermediates and inorganic chemicals. Machine shop pamphletis.
1929-1946年。6美元。
PB 70361, 7079. Trichloromethyl-m-benzoylchloride.
By Schuuhmacher. 1941年1月28日。 1.5美元。 本人未抄录。
加注：美国人出售的整卷为6美元，单个项目是1.5美元。它也有放大本。整卷95美元（国内未单独进口放大本）。
如何看待进口的科技历史资料，而且是实用性的参考资料，请读者看吧！本人是否有点多余？
国内染料专业出版物。
何岩彬 主编 《染料品种大全》沈阳出版社 出版。 P. 1851-2038. 染料中间体及可合成的染料。
按分子式应该列入p. 1895。未见列入，读者可以补充。
陈忠源 2019年5月18日星期六。
文章作者：陈忠源 |
