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Preparation method of 4,4'-diaminobenzenesulphonamide

A technology of diaminobenzenesulfonyl anilide and acetanilide, which is applied in 4 fields, can solve problems such as immaturity, and achieve the effects of reducing content, avoiding the generation of carbon dioxide, and reducing product accumulation

Inactive Publication Date: 2013-06-12
河北永泰柯瑞特化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a kind of preparation method of 4,4'-diaminobenzenesulfonanilide, which solves the problems such as the synthesis process of 4,4'-diaminobenzenesulfonanilide which is not mature in the prior art

Method used

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  • Preparation method of 4,4'-diaminobenzenesulphonamide

Examples

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Embodiment 1

[0059] Add 2,500 kg of chlorosulfonic acid to a 5,000-liter enamel reaction kettle, and slowly add 900 kg of acetanilide, during which the temperature is controlled at 35°C. After the addition, the temperature is raised to 45°C for 3 hours, and then 600 kg of thionyl chloride is slowly added. After the addition, react at 40-45°C for 2 hours. After the end of the reaction, slowly add the sulfonated material to 5000 kg of ice-water mixture, during which the temperature is controlled not to be higher than 20°C. , The resulting filter cake was added to 4000 kg of water evenly and then used.

[0060] Add 750 kg of p-phenylenediamine to 6000 liters of water and heat up to 60°C to dissolve. After dissolving, use ice cubes and open frozen brine to cool down to 15°C. Slowly add the ice precipitated material, and adjust the pH to 8.0 with 15% sodium hydroxide solution during the process. -8.5, keep the temperature at 15-20°C, add the condensation material, after 3 hours of reaction, tes...

Embodiment 2

[0065] Add 3000 kg of chlorosulfonic acid to a 5000 liter enamel reaction kettle, then slowly add 900 kg of acetanilide, open the jacket cooling water during the adding process to control the temperature in the kettle not to exceed 40 ° C, after adding chlorosulfonic acid, adjust the temperature at 50 Incubate at -55°C for 3 hours, then slowly add 700 kg of thionyl chloride dropwise, control the temperature at 55-60°C during the addition, keep the reaction for 3 hours after adding, cool down to 25°C to prepare for ice crystallization.

[0066] Put 4000 kg of water in the dilution tank, open the coil tube to cool the frozen brine to 0 °C, then add 1000 kg of ice, slowly add the sulfonated material, control the temperature in the tank not higher than 10 °C, and beat the sulfonated material after adding the sulfonated material Into the filter press filter. The filter cake is ready for condensation.

[0067] Put 8,000 kg of water in the condensation kettle, raise the temperature ...

Embodiment 3

[0072] Except that the chlorosulfonic acid consumption of sulfonation becomes 3000 kilograms by 2500 kilograms, sulfur oxychloride becomes 500 kilograms by 600 kilograms, and all the other are identical with embodiment 1 except that neutralization reductive agent changes hydrosulfite into. The product yield is 92%, the content is 98.2%, the purity is 98.7%, and the product is light in color.

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Abstract

The invention discloses a preparation method of 4,4'-diaminobenzenesulphonamide. The method comprises the following steps of: based on acetanilide, chlorosulfonic acid, thionyl chloride, water, liquid caustic soda, p-phenylenediamine and the like as raw materials, implementing chlorosulfonation, ice separation, condensation, hydrolysis, neutralization, filter pressing and other processes to obtain the target product 4,4'-diaminobenzenesulphonamide. 4,4'-diaminobenzenesulphonamide prepared by the method disclosed by the invention is good in stability, quite stable, high in yield, and low in production cost.

Description

technical field [0001] The invention belongs to the technical field of intermediate development, in particular to a preparation method related to 4,4'-diaminobenzenesulfonanilide. Background technique [0002] 4,4'-diaminobenzenesulfonanilide is a very important acid dye intermediate, the compound's CAS Number: 16803-97-7, and its structural formula is: The dye intermediate is mainly used as a substitute for the banned dye intermediate benzidine and its derivatives. Acid Black 210 and Acid Black 234 prepared from this dye intermediate play an important role in dye products. [0003] Although 4,4'-diaminobenzenesulfonanilide is a very important raw material for dyes, there are few reports on its preparation. The present invention thus comes. Contents of the invention [0004] The purpose of the present invention is to provide a kind of preparation method of 4,4'-diaminobenzenesulfonanilide, which solves the problems such as the synthetic technique of 4,4'-diaminobenzene...

Claims

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Application Information

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IPC IPC(8): C07C311/44C07C303/40
Inventor 房永法
Owner 河北永泰柯瑞特化工有限公司
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