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A technology of p-aminodiphenylamine and nitrodiphenylamine, which is applied in the field of preparation of p-aminodiphenylamine, can solve the problems of unfavorable large-scale industrial production, low product yield, low product quality, etc., and achieve remarkable economic and social benefits, The effect of many times of application and high product conversion rate
Active Publication Date: 2009-03-11
张国柱
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The disadvantage of this method is that a large amount of hydrochloric acid and liquid caustic soda are used, the pollution of "three wastes" is serious, and nitroso compounds are also carcinogenic
[0005] 3) o-sulfonic acid method: produce p-aminodiphenylamine with o-sulfonic acid method, the quality is better, and the yield is relatively high, but this method has a long process flow, consumes a large amount of acid, seriously corrodes the equipment, and produces ...
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[0033] The preparation method of composite alkali catalyst is that tetraalkylammonium hydroxide, alkali metal hydroxide, tetraalkylammonium salt are (3~8):(1~4):(0.5~4) add Add a certain amount of water, control the temperature, and stir evenly, that is, to the composite alkali catalyst.
[0034] 2. Extraction process:
[0035]The main task of the extraction process is to separate the aqueous phase and the organic phase in the condensation liquid. The soft water extracted from the condensation process is used as the extract, and the ratio of the soft water to the condensation liquid is 1:2 to 1:6 (volume), such as 1:2, 1:3, 1:4, 1:5, 1:6, etc. Preferable 1:3~1:5, enter the multi-stage extraction tower of the second level or above for extraction, the extracted water phase enters the condensation reactor again, and participates in the condensation reaction, and the organic phase after extraction enters the reduction process, and is carried out with a palladium carbon catalyst. ...
Embodiment 1
[0065] Embodiment 1: Take by weighing 30 kilograms of tetraalkylammonium hydroxide, potassium hydroxide and tetraalkylammonium bicarbonate according to the ratio of 3:2:4 in molar ratio, add 70 kilograms of soft waters and stir, until all dissolve, form concentration It is a 30% composite base catalyst.
Embodiment 2
[0066] Embodiment 2: Take by weighing 20 kilograms of tetraalkylammonium hydroxide, sodium hydroxide and tetraalkylammonium sulfate according to the ratio of 5:4:0.5 in molar ratio, add 180 kilograms of demineralized waters and stir, until all dissolving, form concentration is 10% composite base catalyst.
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Abstract
The invention relates to a method for preparing p-aminodiphenylamine, which comprises the following: (1) a step of condensation, in which, nitrobenzene and aniline produce condensation reaction in the presence of a catalyst to generate condensation solution including 4-nitrodiphenylamine and 4-nitrosodiphenylamine; (2) a step of extraction, in which, water phase and organic phase in the condensation solution are separated by an extracting method; (3) a step of reduction, in which, hydrogen and the organic phase of the condensation solution produce reduction reaction in the presence of the catalyst to generate reduction solution including the p-aminodiphenylamine; (4) a step of separation, in which, the p-aminodiphenylamine is separated from the reduction solution to form crude p-aminodiphenylamine feed liquid; and (5) a step of rectification, in which, the p-aminodiphenylamine is separated from the crude p-aminodiphenylamine feed liquid in a rectification mode to form a p-aminodiphenylamine product. The method is suitable for serialized industrialized production in large scale, and has the advantages of low reduction reaction temperature, mild reaction condition, few side products, high conversion rate and selection, low labor intensity and no corrosive liquid, thereby reducing pollution to environment.
Description
technical field [0001] The invention relates to a method for preparing p-aminodiphenylamine, which uses nitrobenzene and aniline as raw materials, adopts two kinds of composite catalysts and a cyclic operation process flow, and continuously prepares p-aminodiphenylamine. Background technique [0002] p-Aminodiphenylamine is an intermediate product for the manufacture of p-phenylenediamine anti-aging agents and stabilizers, and is an important chemical product in the rubber industry and polymer industry. According to the different preparation raw materials, there are many ways to produce p-aminodiphenylamine at present , which includes: [0003] 1) Formanilide method: aniline reacts with formic acid to form formanilide, then condenses with p-nitrochlorobenzene to produce N-formyl dianiline, decarbonylates to form p-nitrodiphenylamine, and then reduces it with alkali sulfide to obtain p-Aminodiphenylamine. The advantage of the formanilide method is that the reaction temperat...
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