Preparation method of p-aminobenzene sulfonic acid

A technology of p-aminobenzenesulfonic acid and p-nitrobenzenesulfonic acid, which is applied to the preparation of sulfonic acid, preparation of organic compounds, chemical instruments and methods, etc., can solve the problem of low production efficiency, high energy consumption, and environment of sulfanilic acid pollution and other issues

Inactive Publication Date: 2018-05-18
YANTAI ANOKY FINE CHEM CO LTD +4
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The technical problem to be solved by the present invention is to overcome the problems of serious environmental pollution, cumbersome process operation, high energy consumption, low safety, high material and labor costs in the preparation process of p-aminobenzenesulfonic acid in the prior art , the problem of low production efficiency, thus a kind of preparation method of p-aminobenzenesulfonic acid is provided

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  • Preparation method of p-aminobenzene sulfonic acid

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Effect test

Embodiment 1

[0095] A kind of preparation method of p-aminobenzenesulfonic acid, take p-nitrobenzenesulfonic acid as raw material, adopt Pd / Al 2 o 3 The catalyst is used for continuous catalytic hydrogenation reaction in the reactor. After the catalyst is separated and recovered, the reducing solution is desolvated and purified to obtain the target product p-aminobenzenesulfonic acid.

[0096] Specific steps include:

[0097] (1) Put 5000kg of 50% methanol aqueous solution and 1250kg of p-nitrobenzenesulfonic acid into the chemical material tank, follow-up feeding is carried out according to the ratio, stir evenly, pump into the first-stage hydrogenation reactor, and add Pd / Al 2 o 3 Catalyst 125kg, the particle size of the catalyst is 10nm, pass through the nitrogen replacement system three times, then pass through the hydrogen replacement system three times, start stirring, raise the temperature to 90-100°C, and pump it into the first-stage hydrogenation tank at a flow rate of 6000L / h ...

Embodiment 2

[0101] (1) Put 5000kg of 50% methanol aqueous solution and 1250kg of p-nitrobenzenesulfonic acid into the chemical material tank, follow up the feeding according to the ratio, stir evenly, pump into the first-level hydrogenation reaction tank, and add Pd / Al 2 o 3 125kg of catalyst, the particle size of the catalyst is 500μm; pass through the nitrogen replacement system three times, then pass through the hydrogen replacement system three times, start stirring, raise the temperature to 80-90°C, and pump it into the first-stage hydrogenation tank at a flow rate of 5000L / h The raw material solution of p-nitrobenzenesulfonic acid is passed into H 2 , control the hydrogen pressure in the system to 3.0MPa, and add Pd / Al to the primary hydrogenation reactor every 3h 2 o 3 Catalyst 2.5kg, after the material in the primary hydrogenation kettle gradually increases, it flows into the secondary hydrogenation kettle through the overflow port, and the residence time of the material in the ...

Embodiment 3

[0105] (1) 12500kg of 50% methanol aqueous solution and 1250kg of p-nitrobenzenesulfonic acid are put into the chemical material tank, and the follow-up feeding is stirred evenly according to the ratio. al 2 o 3 Catalyst 125kg, the particle size of the catalyst is 10nm; pass through the nitrogen replacement system three times, then pass through the hydrogen replacement system three times, start stirring, raise the temperature to 90-100°C, and pump it into the first-stage hydrogenation tank at a flow rate of 6000L / h The raw material solution of p-nitrobenzenesulfonic acid is passed into H 2 , control the hydrogen pressure in the system to 3.0MPa, and add Pd / Al to the primary hydrogenation reactor every 3h 2 o 3 Catalyst 2.5kg, after the material in the primary hydrogenation kettle gradually increases, it flows into the secondary hydrogenation kettle through the overflow port, and the residence time of the material in the hydrogenation kettle is about 2-3h, and the reaction i...

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Abstract

The invention discloses a preparation method of p-aminobenzene sulfonic acid. According to the method, p-nitrobenzene sulfonic acid is continuously catalyzed and hydrogenated and then subjected to sedimentation and membrane filtration to obtain the p-aminobenzene sulfonic acid. The method has the advantages of being simple to operate, high in safety and capable of being constantly produced, effects of high production efficiency, good product quality, low labor intensity, environmental friendliness, and high catalyst utilization rate can be achieved, and the method facilitates industrializationof the p-aminobenzene sulfonic acid.

Description

technical field [0001] The invention belongs to the field of chemical product production, and in particular relates to a preparation method of p-aminobenzenesulfonic acid. Background technique [0002] P-aminobenzenesulfonic acid is an important reactive dye intermediate used in the production of reactive brilliant red K-2B, brilliant red K-2BP, brilliant red K-2G, brilliant red M-2B, brilliant red X-B, brilliant red X -10B, reactive violet K-3R, etc. Using p-nitrobenzenesulfonic acid as raw material, the existing production method in my country is mainly the traditional iron powder reduction method, which uses iron powder. After reduction, a large amount of iron sludge needs to be removed, the operation process is complicated, and a large amount of iron sludge The production of the environmental pollution is extremely serious, and the traditional production method is no longer suitable for chemical production in the form of increasingly severe environmental protection trend...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/22C07C303/44C07C309/46B01J8/00B01J8/10
CPCC07C303/22B01J8/0035B01J8/006B01J8/007B01J8/009B01J8/10C07C303/44C07C309/46
Inventor 张永明刘云龙曲美君杨勇贺晓丽
Owner YANTAI ANOKY FINE CHEM CO LTD
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