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Method for preparing nitryl chlorine solution

A technology of concentrated nitric acid and nitroaniline, which is applied in the field of nitric chloride preparation, can solve problems such as incomplete precipitation of nitrates, difficult treatment of dilute sulfuric acid, complicated process operation, etc., shorten the production cycle, improve extraction and separation efficiency, and improve the efficiency of process water less effect

Inactive Publication Date: 2019-02-15
SHAOXING JIANG HUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this process is: the amount of water added is insufficient and the precipitation of nitrates is not complete. Adding a large amount of water will generate a large amount of dilute sulfuric acid.
The nitrates must be washed many times to be close to neutral, and the close to neutral nitrates are dissolved with organic solvents, so the whole process is complicated to operate, and the dilute sulfuric acid produced is difficult to handle

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] a) Add 300 kg of process water into the water analysis kettle, start stirring, slowly put in 1000 kg of nitrated nitrated products, and stir at room temperature for 5 hours;

[0023] b) 1300 kg of water analysis kettle material enters the slot of the screw distributor from the outer pipe inlet of the CA226 decanter, and enters the conical end through the extraction area in the opposite flow direction to the extractant, and is used as the waste sulfuric acid solution from the decanter 400 kg of dichloromethane enters the distributor from the inlet of the inner pipe, and passes through the extraction zone in the opposite flow direction to that of the water analysis tank material to the end of the reversing drum equipped with a variable control disc and enters the separation rotor. In the tympanic chamber, it is left as an extraction liquid with the help of a porous disc, and is discharged by the pressure of a centripetal pump to obtain nitric chloride liquid.

[0024] Tes...

Embodiment 2

[0026] a) Add 400 kg of process water into the water analysis kettle, start stirring, slowly put in 1000 kg of nitrated nitrated products, and stir at room temperature for 5 hours;

[0027] b) 1,400 kg of water analysis kettle material enters the slot of the screw distributor from the outer pipe inlet of the CA290 decanter, and enters the conical end through the extraction area in the opposite flow direction to the extractant, as the waste sulfuric acid solution from the decanter 450 kg of dichloromethane enters the distributor from the inlet of the inner pipe, and passes through the extraction area in the opposite flow direction to that of the water analysis tank material to reach the end of the reversing drum equipped with variable control discs and enters the separation rotor. In the tympanic chamber, it is left as an extraction liquid with the help of a porous disc, and is discharged by the pressure of a centripetal pump to obtain nitric chloride liquid.

[0028] Test resu...

Embodiment 3

[0030] a) Add 200 kg of process water to the water analysis kettle, start stirring, slowly put in 1000 kg of nitrated nitrated products, and stir at room temperature for 5 hours;

[0031] b) 1,200 kg of water analysis kettle material enters the slot of the screw distributor from the outer pipe inlet of the CA226 decanter, and enters the conical end through the extraction area in the opposite flow direction to the extractant, and is used as the waste sulfuric acid solution from the decanter 400 kg of dichloromethane enters the distributor from the inlet of the inner pipe, and passes through the extraction zone in the opposite flow direction to that of the water analysis tank material to the end of the reversing drum equipped with a variable control disc and enters the separation rotor. In the tympanic chamber, it is left as an extraction liquid with the help of a porous disc, and is discharged by the pressure of a centripetal pump to obtain nitric chloride liquid.

[0032] Test...

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Abstract

The invention relates to a method for preparing a nitryl chlorine solution. Methylene dichloride is taken as an extracting agent, extraction is carried out by adopting a decanter, the extraction and separation efficiency can be improved effectively, the using amounts of the extracting agent and process water are reduced, the obtained nitryl chlorine solution is high in purity and can be directly used for a next-step reaction, compared with a hydraulic analysis method, the concentration of the waste sulfuric acid prepared according to the method is high, and the method can be directly used in the preparation process of ferrous sulfate.

Description

technical field [0001] The invention relates to the technical field of chemical production, in particular to a method for preparing nitric chloride solution. Background technique [0002] As we all know, 2-cyano-4-nitroaniline is a very important intermediate of disperse dyes. However, due to the complex steps of the traditional synthesis process of 2-cyano-4-nitroaniline, there are many by-products and the yield is low. , low purity, unable to meet the requirements of this field for the annual output of 2-cyano-4-nitroaniline, also unable to meet increasingly stringent quality requirements and environmental protection requirements. In the production of 2-cyano-4-nitroaniline, after the nitrate 2-cyano-4-nitrochlorobenzene is formed, it must be separated from sulfuric acid containing a small amount of nitric acid. The traditional process is to use the different solubility of nitrates in water and concentrated sulfuric acid, add sulfuric acid containing nitrates to water to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/50C07C253/34
CPCC07C253/34C07C255/50
Inventor 李江华
Owner SHAOXING JIANG HUA CHEM
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