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Preparation method of barium diphenylaminesulfonate

A technology of barium diphenylamine sulfonate and diphenylamine, applied in the direction of sulfonate preparation, organic chemistry, etc., can solve the problems of low content of barium diphenylamine sulfonate, reduced sensitivity, and affecting use, so as to improve sulfonation efficiency and reduce Operation steps, cost-saving effect

Inactive Publication Date: 2016-05-11
TIANJIN GUANGFU TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is a large amount of barium sulfate in the product, which makes the content of barium diphenylamine sulfonate low, which reduces its sensitivity and seriously affects the use
Barium carbonate can only precipitate impurity sulfate, and the acidity of the solution must be neutralized with a large amount of sodium carbonate, and finally converted into barium diphenylamine sulfonate. The process is complicated, the working hours are long, and the cost is high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A preparation method of barium diphenylamine sulfonate, the steps are as follows:

[0019] (1) In a 10L Erlenmeyer flask, add 5Kg of diphenylamine, add 4L of concentrated sulfuric acid (≥98%), add a stirring device and a decompression device, heat up to 155-160°C under stirring, start the decompression device, and steam out 500 -700ml of water, check the degree of sulfonation, if the sulfonation is not complete, increase the decompression, and quickly distill 100-300ml of water;

[0020] (2) After the sulfonation is completed, add 4L of water for hydrolysis reaction, keep warm at 120-125°C for 20 minutes, add stirring, then quickly pour into 50Kg boiling water, add 32Kg50wt% barium hydroxide hot solution, keep warm for 1-2 hours, Filter, collect filter residue and filtrate respectively;

[0021] (3) Soak the filter residue in 10L hot water for 10min, then suction filter, combine the filtrate with the previous filtrate, discard the precipitate, heat the filtrate to 60-9...

Embodiment 2

[0023] A preparation method of barium diphenylamine sulfonate, the steps are as follows:

[0024] (1) In a 20L conical flask, add 8Kg of diphenylamine, add 5-10L of concentrated sulfuric acid, heat to 160°C, evaporate 550ml of water under reduced pressure within 1 hour, take a sample for testing, and check the degree of sulfonation. If the sulfonation is not complete, Distill 200-300ml of water under reduced pressure;

[0025] (2) After the sulfonation is completed, add 5L of water to carry out the hydrolysis transposition reaction, keep it warm at 125°C for 20 minutes, then pour into 50-60Kg of water, heat to boiling, add 80-100Kg of 20wt% barium hydroxide solution, filter, and collect the filter residues separately and filtrate.

[0026] (3) Put the filter residue in 10L of water, heat and stir for 20min, then filter with suction, combine the filtrate with the previous filtrate, soak the filter residue in 10L of water for 20min, then filter with suction, combine the filtrat...

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Abstract

The invention relates to a preparation method of barium diphenylaminesulfonate. The preparation method comprises 1, adding 5kg of diphenylamine into a container, adding 4L of concentrated sulfuric acid into the container, installing a stirring device and a pressure reduction device, carrying out stirring heating to a temperature of 155-160 DEG C, starting the pressure reduction device and carrying out pressure reduction for water distillation, 2, after sulfonation, adding water into the sulfonation product, wherein the volume of the water is 1-2 times that of the sulfonation product, carrying out hydrolysis, keeping a temperature of 120-125 DEG C for 20-30min, carrying out stirring, fast pouring the mixture into boiling water of which the volume is 10-15 times that of the mixture, adding a barium hydroxide hot solution which has a concentration of 50wt% and has the weight is 5-7 times that of the mixed solution into the mixed solution, carrying out thermal insulation and precipitation for 1-2h, carrying out filtration and respectively collecting filter residues and filtrate, and 3, carrying out washing and drying to obtain a product. A diphenylamine sulfonation direct synthesis method is used and barium hydroxide is used as a SO4<2-> precipitating agent and an acid neutralizer so that deposition and neutralization are realized in one process and thus a cost is saved and work time is shortened.

Description

technical field [0001] The invention belongs to the field of indicators in chemical reagents, in particular to a preparation method of barium diphenylamine sulfonate. technical background [0002] Barium diphenylamine sulfonate is white or light gray fine flaky crystalline powder, sometimes with light blue. Slightly soluble in cold water, slightly soluble in hot water, decomposed by heating, but not melted, easily oxidized in air, mainly used as indicator of ferrous salt and redox indicator. The existing preparation method is obtained by sulfonating diphenylamine with concentrated sulfuric acid to obtain diphenylamine sulfonic acid, and then neutralizing it with barium carbonate. However, there is a large amount of barium sulfate in the product, which makes the content of barium diphenylamine sulfonate low, which leads to a decrease in its sensitivity and seriously affects its use. Barium carbonate can only precipitate impurity sulfate, and the acidity of the solution must...

Claims

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Application Information

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IPC IPC(8): C07C309/46C07C303/32
Inventor 赵鹏李倩
Owner TIANJIN GUANGFU TECH DEV
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