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Production method of 3,4-dichloroaniline-6-sulfonic acid

The technology of a dichloroaniline and a production method is applied in the directions of sulfonic acid preparation, sulfonate preparation, organic chemistry, etc., can solve the problems of large solvent loss, good labor conditions, large heat energy consumption, etc., and achieves improved yield and quality, The effect of reducing solid waste and three wastes

Active Publication Date: 2016-09-28
JIAXING ZHENGDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the working conditions are poor, the heat energy consumption is large, the temperature is not uniform, carbide is easy to form, and the yield is low.
2) Baking sulfonation method in roller milling reactor: the advantage of this method is that the working conditions are good, and the disadvantages are that the volume of the drum should not be too large, less charging, low production capacity, poor mixing effect of materials, and easy formation of carbides
The disadvantage is that there is a large loss of solvent, and the solvent needs to be distilled. The main reason is that the product contains a small amount of solvent, and the application of the pigment prepared by it is limited.

Method used

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  • Production method of 3,4-dichloroaniline-6-sulfonic acid
  • Production method of 3,4-dichloroaniline-6-sulfonic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 400kg of 3,4-dichloroaniline with a content of 99.20% is put into a stirred reactor and the temperature is raised to 75°C; 247.5kg of 98.03% concentrated sulfuric acid is added dropwise, vacuumed, and the vacuum degree is maintained at 0.03-0.04Mpa, and the reaction temperature is maintained at 200-210°C Between, the vacuum degree is 0.10 MPa; After the reaction is completed, put it into the hydrolysis kettle, adjust the pH value to 8, the temperature is 90°C, stir for 2.5 hours until it is completely dissolved; add 20kg of activated carbon, filter; add sulfuric acid to the clear liquid to PH = 1, filter pressure 0.4 MPa, press filter, rinse for 30min, and dry. Obtain 570.4kg of 6B acid solid, the amino acid content is 98.36%, and 3,4-dichloroaniline is used as the raw material, and the product yield is 96.25%.

Embodiment 2

[0034]300kg of 3,4-dichloroaniline with a content of 99.20% is put into a stirred reactor and the temperature is raised to 78°C; 187.3kg of 98.03% concentrated sulfuric acid is added dropwise, and vacuum is maintained to maintain a vacuum degree of 0.02-0.03Mpa and a reaction temperature of 190-195°C Between, the vacuum degree is 0.09 MPa; After the reaction is completed, put it into the hydrolysis kettle, adjust the pH value to 7.5, the temperature is 92 ° C, stir for 3 hours until it is completely dissolved; add 16 kg of activated carbon, filter; add sulfuric acid to the clear liquid to PH = 1, filter pressure 0.5 MPa, press filter, rinse for 30min, and dry. Obtain 426kg of 6B acid solids, the amino acid content is 98.22%, and the product yield is 95.85% with 3,4-dichloroaniline as the raw material.

Embodiment 3

[0036] 400kg of 3,4-dichloroaniline with a content of 99.20% is put into a stirred reactor and the temperature is raised to 76°C; 257kg of 98.02% concentrated sulfuric acid is added dropwise, vacuumed, and the vacuum degree is maintained at 0.01-0.02Mpa, and the reaction temperature is maintained between 200-205°C room, vacuum 0.085 MPa; after the reaction, put it into the hydrolysis kettle, adjust the pH value to 8, temperature 90 ℃, stir for 3 hours until completely dissolved; add 17kg of activated carbon, filter; add hydrochloric acid to the clear liquid until PH = 1, filter pressure 0.4 MPa , press filter and rinse for 40min, and dry. Obtain 565.6kg of 6B acid solid, the amino acid content is 98.19%, and 3,4-dichloroaniline is used as the raw material, and the product yield is 95.43%.

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Abstract

The invention provides a production method of 3,4-dichloroaniline-6-sulfonic acid and belongs to the technical field of chemical synthesis. The production method takes 3,4-dichloroaniline and sulfuric acid as raw materials and comprises the following steps: carrying out a sulfonation reaction in a reactor which has a jacket and is heated by carried heat-conducting oil to obtain a 3,4-dichloroaniline-6-sulfonic acid rough product; carrying out alkali dissolving, de-coloring and filtering, acid precipitation, filter pressing and rinsing and drying on the sulfonated product, namely the 3,4-dichloroaniline-6-sulfonic acid rough product, so as to obtain a 3,4-dichloroaniline-6-sulfonic acid finished product. After the raw material 3,4-dichloroaniline is completely melted, acid addition and sulfonation are controlled under a certain condition, so that the problem that the reaction is incomplete, caused by the fact that a reaction system is not uniform, is avoided; the salt formation time is controlled and waste dreg pollution caused by a process is reduced, so that the process is simpler and the yield is improved; the produced product can improve the flowability of pigments and adjust a color phase and transparency; the yield of the product is 95 percent or above and the content is 98 percent or above.

Description

technical field [0001] The invention belongs to the technical field of synthesis of 3,4-dichloroaniline-6-sulfonic acid (hereinafter referred to as 6B acid), and specifically relates to using 3,4-dichloroaniline and sulfuric acid as raw materials, using a heat-conducting In the oil-heated reactor, the sulfonation reaction is carried out under certain conditions to obtain the crude 6B acid. The crude 6B acid of the sulfonated product is subjected to alkali dissolution, decolorization and filtration, acid analysis, pressure filtration, rinsing, and drying to obtain the finished product of 6B acid. Background technique [0002] 3,4-Dichloroaniline-6-sulfonic acid (hereinafter referred to as 6B acid) is mainly used in the pigment industry to produce C.I. Pigment Yellow 183 series yellow pigments, which are widely used in plastics, coatings, color inks, rubber and paints coloring etc. According to the literature, the usual preparation method for the sulfonation of primary arylam...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/48C07C303/02
CPCC07C303/02C07C303/06C07C303/32C07C309/48
Inventor 杨丽艳吴国庆史沈明季金华史迎军邱艳慧陶明泉
Owner JIAXING ZHENGDA CHEM