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Production method for 2-chloro-4-methyl nitrobenzene

A technology of nitrotoluene and production methods, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as low product yield, environmental pollution, difficult to handle, etc., and achieve high product quality and high product yield. high rate effect

Inactive Publication Date: 2013-12-11
淮安嘉诚高新化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the present invention is to: provide a kind of production method of 2-chloro-4-nitrotoluene product, solve the waste water volume that exists in the production technology that adopts at present, be difficult to handle, serious to environmental pollution and product yield low, quality. Poor defects, realize the clean production of 2-chloro-4-nitrotoluene, improve the yield and quality of 2-chloro-4-nitrotoluene

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Example 1: Production of 2-chloro-4-nitrotoluene according to the following steps

[0011] 1) Put the molten p-nitrotoluene and 4A zeolite molecular sieve into the reactor, the mass ratio of p-nitrotoluene to 4A zeolite molecular sieve is 1:0.04, control the reaction temperature at 60 ℃, and pass it with p-nitrotoluene Equimolar amount of chlorine for chlorination reaction;

[0012] 2) Transfer the chlorinated liquid after the chlorination reaction to the rectification tower, rectify the chlorinated liquid under vacuum to obtain 2-chloro-4-nitrotoluene, and control the temperature at 160°C during the rectification process. The pressure is controlled at -0.095MPa;

[0013] 3) The light component hydrogen chloride absorbs the by-product hydrogen chloride with water, the unreacted raw material p-nitrotoluene is recycled back to the chlorinator, and the heavy component is sent to a qualified unit as solid waste for disposal.

[0014] Product yield: 95.1%, product content: 99.5%.

Embodiment 2

[0015] Example 2: Production of 2-chloro-4-nitrotoluene according to the following steps

[0016] 1) Put molten p-nitrotoluene and 13X type zeolite molecular sieve into the reactor, the mass ratio of p-nitrotoluene to 13X type zeolite molecular sieve is 1:0.04, control the reaction temperature at 80 ℃, and pass it into the reactor. Equimolar amount of chlorine for chlorination reaction;

[0017] 2) Transfer the chlorinated solution after the chlorination reaction to a rectification tower, rectify the chlorinated solution under vacuum to obtain 2-chloro-4-nitrotoluene, and control the temperature at 180°C during the rectification process. The pressure is controlled at -0.088MPa;

[0018] 3) The light component hydrogen chloride absorbs the by-product hydrogen chloride with water, the unreacted raw material p-nitrotoluene is recycled back to the chlorinator, and the heavy component is sent to a qualified unit as solid waste for disposal.

[0019] Product yield: 95.2%, product content: ...

Embodiment 3

[0020] Example 3: Production of 2-chloro-4-nitrotoluene according to the following steps

[0021] 1) Put the molten p-nitrotoluene and 13X type zeolite molecular sieve into the reactor, the mass ratio of p-nitrotoluene to 13X type zeolite molecular sieve is 1:0.04, control the temperature at 100℃, and pass into the p-nitrotoluene, etc. Molar amount of chlorine gas for chlorination reaction;

[0022] 2) Transfer the chlorinated solution after the chlorination reaction to the rectification tower, rectify the chlorinated solution under vacuum to obtain 2-chloro-4-nitrotoluene, and control the temperature at 200°C during the rectification process. The pressure is controlled at -0.08MPa;

[0023] 3) The light component hydrogen chloride absorbs the by-product hydrogen chloride with water, the unreacted raw material p-nitrotoluene is recycled back to the chlorinator, and the heavy component is sent to a qualified unit as solid waste for disposal.

[0024] Product yield: 95.4%, product cont...

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Abstract

The invention relates to a production method for 2-chloro-4-methyl nitrobenzene. The method comprises the following steps: using p-nitrotoluene as a raw material and 4A type or 13X type zeolite molecular sieve as a catalyst to perform chlorination reaction with chlorine gas of which molar weight is the same as those of the p-nitrotoluene and the 4A type or 13X type zeolite molecular sieve, and rectifying a chlorination solution by vacuum rectification to obtain a 2-chloro-4-methyl nitrobenzene product. According to the method, wastewater cannot be produced in a production process, so that the clean production of the 2-chloro-4-methyl nitrobenzene is achieved, the product yield is increased, the product quality is improved, the yield can reach more than 95%, and the content can reach more than 99%.

Description

Technical field [0001] The invention relates to a production method of 2-chloro-4-nitrotoluene. Background technique [0002] 2-Chloro-4-nitrotoluene is an important organic compound intermediate, mainly used in the production of pesticides and medicines. At present, the main method of producing 2-chloro-4-nitrotoluene is obtained by chlorination of p-nitrotoluene. The specific process is as follows: Put molten p-nitrotoluene into the reactor, add the catalyst ferric trichloride, and Pass in chlorine gas equal to p-nitrotoluene at 50~60℃, then wash with hot water, neutralize with sodium carbonate, put it in ice water, stir to precipitate crystals, filter, and dry in the shade to obtain 2-chloro-4-nitrate Base toluene products. The production process adopts water washing, neutralization, and cooling crystallization treatment methods for the post-treatment of the chlorinated liquid. The water washing and neutralization remove the catalyst ferric chloride and the hydrogen chloride...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/11C07C201/12C07C201/16
Inventor 石祖嘉马正杨陈雪琴
Owner 淮安嘉诚高新化工股份有限公司
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