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Esterification and nitration process method of 2-chloro-5-nitrobenzene methyl acetate

A technology of methyl nitrophenylacetate and process method, which is applied in the field of esterification and nitration process of methyl 2-chloro-5-nitrophenylacetate, which can solve the problems of cumbersome dilution process steps, low discharge efficiency, and impact on production. , to achieve the effect of reducing process reaction process time, reducing labor costs, and reducing process costs

Pending Publication Date: 2019-02-22
YIXING XINYU CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Existing methyl 2-chloro-5-nitrophenylacetate first passes through the nitration process, then performs the dilution process, and then performs the esterification process. Because the dilution process steps are cumbersome, time-consuming and labor-intensive, the overall The output efficiency is low, seriously affecting the output

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A 2-chloro-5-nitrophenylacetic acid methyl ester esterification and nitration process, comprising the steps:

[0032] 1) Esterification process:

[0033] 1.1) First, put 160kg of o-chlorophenylacetic acid weighed into the esterification kettle, then suck the metered 300kg of methanol into the esterification kettle, close the vacuum system of the esterification kettle after the methanol is absorbed, and put the measured 4.5 kgcp sulfuric acid is dropped into the esterification kettle from the sampling port;

[0034] 1.2) Open the jacket steam valve and drain valve, drain the condensed water, and then switch to steam trap mode;

[0035] 1.3) Control the steam pressure in the esterification tank to 0.1MPa and raise the temperature to 40°C, then control the steam pressure to 0.05MPa and continue to raise the temperature to 66-68°C, start timing when there is reflux in the sight glass, and keep warm 2 hours;

[0036] 1.4) After the reflux heat preservation is over, confir...

Embodiment 2

[0051] A 2-chloro-5-nitrophenylacetic acid methyl ester esterification and nitration process, comprising the steps:

[0052] 1) Esterification process:

[0053] 1.1) First put 180kg of o-chlorophenylacetic acid weighed into the esterification kettle, then suck the metered 310kg of methanol into the esterification kettle, after the methanol is sucked, close the vacuum system of the esterification kettle, and put the metered 4.8 kgcp sulfuric acid is dropped into the esterification kettle from the sampling port;

[0054] 1.2) Open the jacket steam valve and drain valve, drain the condensed water, and then switch to steam trap mode;

[0055] 1.3) Control the steam pressure in the esterification tank to 0.1MPa and raise the temperature to 42°C, then control the steam pressure to 0.05MPa and continue to raise the temperature to 66-68°C, start timing when there is reflux in the sight glass, and keep warm 2.5 hours;

[0056] 1.4) After the reflux heat preservation is over, confirm...

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PUM

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Abstract

The invention discloses an esterification and nitration process method of 2-chloro-5-nitrobenzene methyl acetate. The esterification and nitration process method comprises the following steps: o-chlorophenylacetic acid and methyl alcohol are put into an esterification kettle to be subjected to an esterification reaction process; a discharged material subjected to the esterification reaction is struck into a nitration kettle, and nitric acid and chloroform are put into the nitration kettle to be subjected to a nitration reaction process; a discharged material subjected to the nitration reactionis layered; the layered discharged material is distilled and precipitated, and the chloroform is recovered; and finally, a precipitated material is cooled and dried and then extracted. According to the esterification and nitration process method, the process sequence of esterification first and then nitration is adopted, the original attenuation procedure after the nitration process is omitted, thus the overall process reaction procedure time is reduced greatly, the discharging efficiency is improved, the yield is increased, the labor intensity is lowered, and the manpower cost is reduced; and the chloroform used in the process procedure can be effectively recovered finally, thus the process cost is lowered greatly, and the higher productive profit is brought.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering, and in particular relates to a process method for esterification and nitration of methyl 2-chloro-5-nitrophenylacetate. Background technique [0002] Existing methyl 2-chloro-5-nitrophenylacetate first passes through the nitration process, then performs the dilution process, and then performs the esterification process. Because the dilution process steps are cumbersome, time-consuming and labor-intensive, the overall The output efficiency is low, which seriously affects the output. Contents of the invention [0003] Purpose of the invention: In order to overcome the deficiencies in the prior art, provide a process for the esterification and nitration of o-chlorophenylacetic acid with high discharge efficiency and reduced process cost. [0004] Technical solution: In order to achieve the above object, the present invention provides a process for the esterification and nitration of ...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/65C07C201/08C07C201/16C07C205/58
CPCC07C67/08C07C201/08C07C201/16C07C69/65C07C205/58
Inventor 袁顺福范洪振袁郡范琳许薇
Owner YIXING XINYU CHEM