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Preparation method of barium diphenylamine sulfonate

A barium diphenylamine sulfonate, sulfonation technology, applied in the preparation of sulfonate, organic chemistry, etc.

Inactive Publication Date: 2015-11-04
TIANJIN GUANGFU TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In view of this, the main purpose of the present invention is to provide a kind of preparation method of barium diphenylamine sulfonate, which can solve the complex process of existing barium diphenylamine sulfonate preparation method , The cost is high, and the barium diphenylamine sulfonate produced contains a large amount of barium sulfate, which leads to the problem of reduced sensitivity

Method used

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specific Embodiment approach 1

[0020] Specific embodiment one: the preparation method of a kind of barium diphenylamine sulfonate described in this embodiment is realized through the following steps:

[0021] Step 1, add 5Kg diphenylamine and 4~5L concentrated sulfuric acid in 20L conical flask;

[0022] Step 2. Install a stirring device and a decompression device in the 20L Erlenmeyer flask, turn on the stirring device, and raise the temperature of the 20L Erlenmeyer flask to 155~160°C in the stirring state;

[0023] Step 3, start the decompression device, decompress and steam out 500~700ml of water;

[0024] Step 4. Check the degree of sulfonation of the mixed solution in the 20L Erlenmeyer flask. If the sulfonation is not complete, increase the pressure reduction and steam out 100~300mm of water again;

[0025] Step five, add 4 ~ 5L water in 20L conical flask and carry out hydrolysis reaction;

[0026] Step 6. Pour the mixed solution in the 20L Erlenmeyer flask into 50Kg boiling water, add 32~80Kg of 2...

specific Embodiment approach 2

[0031] Embodiment 2: The concentration of concentrated sulfuric acid in step 1 of the preparation method of barium diphenylamine sulfonate described in this embodiment is not less than 98%. Other components and connections are the same as those in the first embodiment.

specific Embodiment approach 3

[0032] Embodiment 3: The hydrolysis reaction in step 5 of the method for preparing barium diphenylamine sulfonate described in this embodiment is carried out at 120-125° C. and kept for 20 minutes. Other components and connections are the same as those in the first embodiment.

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Abstract

The invention provides a preparation method of barium diphenylamine sulfonate, aiming to solve the problems that existing barium diphenylamine sulfonate preparation methods are complex in processes and higher in costs, and produced barium diphenylamine sulfonate contains plenty of barium sulfate, thus reducing the sensitivity of barium diphenylamine sulfonate. The preparation method comprises the following specific steps: adding 5Kg of diphenylamine and 4-5L of concentrated sulfuric acid to a 20L conical flask; checking the sulfonation degree of a mixed solution in the 20L conical flask; adding 4-5L of water to the 20L conical flask to carry out hydrolysis reaction; pouring the mixed solution in the 20L conical flask into 50Kg of boiling water, adding 32-80Kg of 20-50% barium hydroxide hot solution while stirring the mixed solution, filtering the mixed solution after carrying out insulation and precipitation for two hours and respectively collecting filtrate and filter residues; heating the filtrate to 60-90 DEG C and adjusting the PH value of the filtrate to 6-7 with 10% of sodium carbonate solution; drying the filtrate in a vacuum drying oven. The preparation method is used in the field of chemical reagents.

Description

technical field [0001] The invention relates to a preparation method of barium diphenylamine sulfonate, which belongs to the field of chemical reagents. Background technique [0002] Barium diphenylamine sulfonate is white or light gray fine flaky crystalline powder, sometimes light blue, slightly soluble in water, slightly soluble in hot water, decomposed by heating, but does not melt, and is easily oxidized in air. It is mainly used as an indicator of ferrous salt and a redox indicator. The general preparation method is to obtain diphenylamine sulfonic acid by sulfonating diphenylamine with concentrated sulfuric acid, and then neutralize it with barium carbonate. However, there is a large amount of barium sulfate in the barium diphenylamine sulfonate produced by this method, which makes the barium diphenylamine sulfonate content lower, resulting in reduced sensitivity and seriously affecting the use. However, barium carbonate can only precipitate impurity sulfate, and the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/46C07C303/32
Inventor 赵鹏袁秋菊
Owner TIANJIN GUANGFU TECH DEV
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