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Method for preparing m-nitrochlorobenzene, o-nitrochlorobenzene and p-nitrochlorobenzene by using nitrochlorobenzene meta-position oil

A technology of nitrochlorobenzene meta-oil and p-nitroanisole, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., and can solve problems such as insufficient purity, pollution of the atmospheric environment, and difficulty in implementation

Inactive Publication Date: 2011-01-05
邵阳市申强化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Under the current technical conditions, it is feasible to continue to separate and purify the components in this part of the mixture by rectification-crystallization, but due to the similar physical properties, it is very difficult to implement
In order to obtain m-nitrochlorobenzene finished products, the m-nitrochlorobenzene in the material taken from the top of the rectification tower must be greater than 80% before crystallization, otherwise the purity of the m-nitrochlorobenzene product is insufficient or the yield is extremely low due to mutual solubility, and the intermediate The boiling points of nitrochlorobenzene and p-nitrochlorobenzene are 237°C and 239°C respectively, and the difference between the boiling points is only 2°C. During rectification, a high reflux ratio and a small amount taken from the top of the tower are required to meet the process requirements. High energy consumption and long production cycle
[0005] If it is incinerated as hazardous waste, it will produce a large amount of nitrogen oxides and pollute the atmosphere

Method used

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  • Method for preparing m-nitrochlorobenzene, o-nitrochlorobenzene and p-nitrochlorobenzene by using nitrochlorobenzene meta-position oil
  • Method for preparing m-nitrochlorobenzene, o-nitrochlorobenzene and p-nitrochlorobenzene by using nitrochlorobenzene meta-position oil
  • Method for preparing m-nitrochlorobenzene, o-nitrochlorobenzene and p-nitrochlorobenzene by using nitrochlorobenzene meta-position oil

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Experimental program
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Effect test

Embodiment 1

[0023] φ1400mm rectification tower, wire mesh corrugated packing, tower bottom temperature 172°C, tower top temperature 153°C, pressure 70mmHg, will contain m-nitrochlorobenzene 30.4%, p-nitrochlorobenzene 46.6%, o-nitrochlorobenzene 22.8% The nitrochlorobenzene meta-position oil is fed from the tower with a flow rate of 600kg / h, and the o-nitrochlorobenzene is extracted from the tower bottom with a flow rate of 460kg / h; Chlorobenzene-p-nitrochlorobenzene mixture, the composition of tower still and tower top is as follows with gas chromatography:

[0024]

Embodiment 2

[0026] 10m 3 Add 2200L of m-nitrochlorobenzene-p-nitrochlorobenzene mixture containing 39.5% of meta-position and 60.4% of para-position, and 2000L of methanol into the etherification reactor. 2800L of methanol solution with a concentration of 170.5g / L sodium hydroxide was added dropwise within the temperature range of 70°C to 90°C, and the addition time was 2 hours. Continue to heat up to 102°C and maintain for 4 hours. Rectify to remove excess methanol, wash and separate layers, and use gas chromatography to analyze the composition of the organic phase:

[0027] components

Embodiment 3

[0029] φ1200mm rectification tower, wire mesh corrugated packing, tower bottom temperature 200°C, tower top temperature 143°C, pressure 50mmHg, p-nitroanisole containing 59.2% p-nitroanisole and 40.1% m-nitrochlorobenzene -The m-nitrochlorobenzene mixture is fed from the tower with a flow rate of 500kg / h, and the p-nitroanisole crude product is extracted from the tower kettle with a flow rate of 300kg / h; Nitrochlorobenzene finished product, with gas chromatographic analysis tower still and tower top composition is as follows:

[0030]

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Abstract

The invention relates to a method for preparing m-nitrochlorobenzene, o-nitrochlorobenzene and p-nitrochlorobenzene by using nitrochlorobenzene meta-position oil. The method comprises the following steps of: separating the nitrochlorobenzene meta-position oil containing 20 to 45 percent of m-nitrochlorobenzene and produced in the conventional nitrochlorobenzene production process into an m-nitrochlorobenzene and p-nitrochlorobenzene mixture and an o-nitrochlorobenzene product by a rectification method, further converting the m-nitrochlorobenzene and p-nitrochlorobenzene mixture into an m-nitrochlorobenzene and p-nitroanisole mixture by methoxylation reaction, and performing rectification, separation and purification on the mixture to obtain m-nitrochlorobenzene and p-nitroanisole products. The method has the advantages of low energy consumption, short production period and capability of solving the atmospheric pollution problem of a burning treatment method for the nitrochlorobenzene meta-position oil.

Description

Technical field: [0001] The invention relates to a method for preparing m-nitrochlorobenzene, o-nitrochlorobenzene and p-nitroanisole from meta-nitrochlorobenzene oil. In particular, the method for preparing m-nitrochlorobenzene, o-nitrochlorobenzene and p-nitroanisole by using the nitrochlorobenzene meta-oil produced in the existing nitrochlorobenzene production process. Background technique: [0002] o-nitrochlorobenzene, p-nitrochlorobenzene and its derivative product p-nitroanisole are important intermediates for dyes, medicines, pesticides, and spices. The main production route is: nitration reaction of chlorobenzene at a certain temperature and pressure , to generate a nitrochlorobenzene mixture, including three isomers, of which p-nitrochlorobenzene accounts for 65%, o-nitrochlorobenzene accounts for 32%, m-nitrochlorobenzene accounts for 1%, and nitrochlorobenzene mixture O-nitrochlorobenzene and p-nitrochlorobenzene are separated and purified by means of rectificat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/12C07C205/37C07C201/16C07C201/12
Inventor 胡宏志王志强李成泽
Owner 邵阳市申强化工有限责任公司
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