Method for synthesizing 4-nitro diphenylamine and 4-nitroso diphenylamine or/and their salts

A technology for nitrosodiphenylamine and nitrodiphenylamine, which is applied in the field of organic synthesis, can solve the problems of high moisture control requirements, difficult to effectively control, small processing capacity, etc., and achieves accelerated dehydration rate, low production cost, and increased The effect of forced heat exchangers

Inactive Publication Date: 2004-01-28
JIANGSU SINORGCHEM TECH CO LTD
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  • Abstract
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Problems solved by technology

Dehydration has a great influence on the parallel reaction of condensation. Generally, strong base catalysts need to be dehydrated in advance, and the requirements for water control are high, that is, the ratio of water to alkali at the beginning of the condensation reaction is required to be not less than 4:1 and not less than 0.6: at the end of the reaction. 1 o'clock (CN1307556A), in the specific embodiment, adopt first dehydration and then enter the reactor to carry out condensation reaction, the operation is complicated, it is difficult to effectively control, and the processing capacity is not large

Method used

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  • Method for synthesizing 4-nitro diphenylamine and 4-nitroso diphenylamine or/and their salts

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Embodiment Construction

[0020] Simultaneously open composite catalyst, aniline and nitrobenzene delivery pumps, adjust the flow rate to 150 kg / hour of aniline, 30 kg / hour of nitrobenzene, composite alkali catalyst (its components are composed of tetramethylammonium hydroxide, sodium hydroxide and the aqueous solution composed of tetramethylammonium carbonate, the sum of the concentration of the three is 29.9%, and the molar ratio of the three is 1:1:0.5) 80 kg / hour, continuously enters the forced heat exchanger, and the heat medium of the forced heat exchanger Alcohol steam is used to force the condensed liquid in the heat exchanger into the primary reactor from the top, continue to dehydrate and react, then open the bottom valve of the primary reactor and the condensation circulation pump, and adjust the outlet valve of the condensation circulation pump to make the material return Into the forced heat exchanger, a local circulation system is formed, so that the material is continuously circulated, de...

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Abstract

The present invention relates to a method for making continuous condensation reaction to synthesize 4-nitrodiphenylamine and 4-nitrosodiphenylamine or/and their salts by using phenylamine and nitrobenzol as raw material in the presence of compound catalyst. Said invention selects and uses the cheap compound alkali catalyst, phenylamine and nitrobenzol, and places them into a reactor according to a certain proportion, and makes them pass throu gh one-stage or multistage reactor and forced heat exchanger at a certain pressure and temp., and utilizes forced circulation pump to make said materialimplement locak circulation and reaction while dewatering. Said invented reaction condition is moderate, conversion rate of nitrobenzol is greater than 99%, and its selectivity is greater than 97%.

Description

technical field [0001] The present invention relates to a kind of synthetic method of organic matter, be specifically related to use aniline and nitrobenzene as raw material, select a kind of compound type base catalyst and technological process, continuously synthesize 4-nitrodiphenylamine and 4-nitrosodiphenylamine or / and their methods of salt. Background technique [0002] At present, the method for synthesizing 4-nitrodiphenylamine and 4-nitrosodiphenylamine or / and their salts is to adopt the nucleophilic aromatic ring substitution hydrogen reaction (NASH), that is, the functionalized carbanion containing a leaving group is The reaction of substituting hydrogen on nitroarenes and aromatic heterocycles in the presence of a strong base. Most compounds are substituted on the ortho position, and the yield is generally between 5-65%. For example, in the presence of tetramethylammonium hydroxide, aniline and nitrobenzene undergo NASH reaction to synthesize 4-nitrodiphenylami...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07C209/60C07C211/56
Inventor 余瑞标
Owner JIANGSU SINORGCHEM TECH CO LTD
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