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New technology for separating nitride in production of 2-cyano-4-nitroaniline

A technology of nitroaniline and new process is applied in the new process field of nitrate separation in the production of 2-cyano-4-nitroaniline, and can solve the problems of incomplete precipitation of nitrates, difficult handling of dilute sulfuric acid, complicated process operation and the like , to achieve the effect of shortening the production cycle, small output and increasing production capacity

Inactive Publication Date: 2016-08-17
HEJIAN YINGZHOU CHEM IND CO LTD
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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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  • New technology for separating nitride in production of 2-cyano-4-nitroaniline
  • New technology for separating nitride in production of 2-cyano-4-nitroaniline
  • New technology for separating nitride in production of 2-cyano-4-nitroaniline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Major equipment:

[0020] serial number

device name

Specification

material

use

1.

Water analysis kettle

10000L

enamel

Dilute with water

2.

Extraction phase separation tank

15000L

enamel

Chlorinated benzene extraction

[0021] The amount and quality of extraction raw materials

[0022]

[0023]

[0024] Add 4,000 kg of process water into the water analysis kettle, start stirring, slowly put in the nitrated nitrated product, and control the temperature at 30-35°C. Add 5,000 kilograms of chlorinated benzene after feeding, stir for half an hour and let it stand for half an hour. By separation, the oil phase obtains a chlorinated benzene solution of 2-cyano-4-nitrochlorobenzene, and the water phase obtains a concentration-diluted benzene solution. sulfuric acid.

[0025] Test results: the acid concentration in the water phase is 60.5%, and does not contain 2-cyano-4-nitrochlorobenzene; the oil ...

Embodiment 2

[0027] Major equipment:

[0028] serial number

device name

Specification

material

use

1.

Water analysis kettle

10000L

enamel

Dilute with water

2.

Extraction phase separation tank

15000L

enamel

Chlorinated benzene extraction

[0029] The amount and quality of extraction raw materials

[0030] process

Material name

Weight (Kg)

Water analysis

process water

4000

extraction

Extractant: Chlorinated Benzene

6000

[0031] Add 4,000 kg of process water into the water analysis kettle, start stirring, slowly put in the nitrated nitrated product, and control the temperature at 30-35°C. Add 6,000 kilograms of chlorinated benzene after discharging the material, leave it to stand for half an hour after stirring for half an hour, and through separation, the oil phase obtains a chlorinated benzene solution of 2-cyano-4-nitrochlorinated benzene, and the water phase obta...

Embodiment 3

[0034] Major equipment:

[0035] serial number

device name

Specification

material

use

1.

Water analysis kettle

10000L

enamel

Dilute with water

2.

Extraction phase separation tank

15000L

enamel

Chlorinated benzene extraction

[0036] The amount and quality of extraction raw materials

[0037] process

Material name

Weight (Kg)

Water analysis

process water

3500

extraction

Extractant: Chlorinated Benzene

5000

[0038] Add 3,500 kg of process water into the water analysis tank, start stirring, slowly put in the nitrated nitrated product, and control the temperature at 30-35°C. Add 5,000 kilograms of chlorinated benzene after feeding, stir for half an hour and let it stand for half an hour. By separation, the oil phase obtains a chlorinated benzene solution of 2-cyano-4-nitrochlorobenzene, and the water phase obtains a concentration-diluted benzene solution....

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Abstract

The invention belongs to the field of chemical industry, and relates to a new technology for separating nitride in a technology of using concentrated sulfuric acid and concentrated nitric acid to nitrify o-chlorobenzonitrile so as to generate 2-cyano-4-nitro chlorobenzene. An extraction technology is used for extracting the 2-cyano-4-nitro chlorobenzene from waste acid of nitration, and then a product 2-cyano-4-nitroaniline is obtained by an ammonolysis reaction. After the new technology is adopted, the nitride is separated from the waste acid of nitration; the new technology is simple in operation, overcomes the defect that a great deal of waste acid is produced in the traditional technology, and omits the operations of washing the nitride for a plurality of times and dissolving the nitride again after the nitride is separated out; nitride-containing organic liquid is stirred and washed in water, so that a small amount of sulfuric acid and water-soluble organic impurities in an organic phase are removed, and the purity of the nitride-containing organic liquid is higher.

Description

technical field [0001] The invention relates to the technical field of chemical production, in particular to a new process for separating nitrates in the production of 2-cyano-4-nitroaniline. Background technique [0002] 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 precipitate (abbreviated as water analysis), then filter out dilute acid to obtain nitrates, and then wash and remove nitrates to near Neutral, then dissolved in the selected organic solvent, and then carry out the subsequent ammonolysis reaction to obtain the product 2-cyano-4-nitroaniline. The disadvantage of this process is: the amount of water added is insufficient and the precipitation of nitrates is incomplete...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/34C07C255/50
CPCC07C253/34C07C255/50
Inventor 陈泽海房永法雷明远孟铎万茂光
Owner HEJIAN YINGZHOU CHEM IND CO LTD
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