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Method for preparing aromatic nitro compound using nitryl chloride as nitrating agent

A technology for aromatic nitro group and nitroxyl chloride is applied in the field of nitration of aromatic hydrocarbons and their derivatives, which can solve the problems of difficult treatment of nitroxyl chloride, and achieve the effects of saving funds, saving investment and reducing energy consumption.

Inactive Publication Date: 2009-03-11
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

[0007] The object of the present invention is to: provide a kind of method that uses nitroxyl chloride as nitrating agent to prepare aromatic nitro compound, to solve the difficult problem of handling when nitroxyl chloride is produced as tail gas

Method used

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  • Method for preparing aromatic nitro compound using nitryl chloride as nitrating agent
  • Method for preparing aromatic nitro compound using nitryl chloride as nitrating agent

Examples

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Effect test

example 1

[0020] Example 1: Preparation of nitrotoluene by nitration of toluene

[0021] Production according to the following specific steps: 1) Toluene, 69% sulfuric acid and nitroxyl chloride are respectively sent to the nitration reactor through a rotameter for nitration reaction, the mass ratio of toluene and 69% sulfuric acid is 1:2.9, and the reaction temperature is 20°C. Normal pressure, when the reaction finishes, the content of toluene in the feed liquid is less than 4%, and the content of dinitrotoluene is less than 0.2%;

[0022] 2) After the nitration reaction is finished, the feed liquid enters the separator, and the separated mononitrotoluene is washed with water, alkali washed, washed with water and distilled to obtain the industrial product mononitrotoluene; the separated concentration is 69% and waste acid is returned to the nitration The reactor is recycled; the molar ratio of the obtained mononitrotoluene mixture is: o-nitrotoluene: p-nitrotoluene: m-nitrotoluene=60:...

example 2

[0023] Example 2: Preparation of nitrochlorobenzene by nitration of chlorobenzene

[0024] Production according to the following specific steps: 1) Chlorobenzene, 70% sulfuric acid and nitroxyl chloride are respectively sent to the nitration reactor through the flow rate for nitration reaction, the mass ratio of chlorobenzene and 70% sulfuric acid is 1:2.3, and the reaction temperature is 55°C , normal pressure, the content of chlorobenzene in the feed liquid is not more than 3%, and the content of polynitrochlorides is not more than 0.2% when the reaction ends;

[0025] 2) After the nitration reaction is finished, the feed liquid enters the separator, and the organic matter in the upper layer enters the neutralization pot to add alkali for neutralization, water washing, and drying tower treatment; 70% of the waste acid in the lower layer of the separator is returned to the nitration reactor for recycling;

[0026] 3) The organic matter obtained by the reaction is mainly nitro...

example 3

[0027] Example 3: Preparation of nitrobenzene by nitration of benzene

[0028] Production according to the following specific steps: 1) Send benzene, 71% sulfuric acid and nitroxyl chloride into the nitration reactor through a flow meter for nitration reaction, the mass ratio of benzene and 71% sulfuric acid is 1:3.3, and the reaction temperature is 60 ° C. When the reaction finishes, the content of benzene in the feed liquid is not more than 3%, and the content of dinitrobenzene is not more than 0.2%;

[0029] 2) After the nitration reaction is finished, the feed liquid enters the separator, and the separated nitrobenzene is washed with water, alkali washed, washed with water and distilled to obtain the industrial product nitrobenzene; the separated concentration is 71% and waste acid is returned to the nitration reactor recycle. The reaction yield can reach 99% in terms of benzene, and the product content is not less than 99.5%

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Abstract

The invention relates to a method for preparing an aromatic nitro compound by using nitryl chloride as a nitrating agent. In the method, the aromatic nitro compound is prepared by using tail gas of nitryl chloride as the nitrating agent, wherein a nitrated substance is aromatic hydrocarbon and benzene, chlorobenzene, nitrobenzene or toluene of derivatives of the aromatic hydrocarbon; the nitryl chloride is the nitrating agent and sulfuric acid is a medium; and the nitration is carried out on aromaticring at a temperature of between 20 and 90 DEG C at normal pressure. The method has the following advantages: (1) changing wastes to valuables, and providing economic benefit for companies; (2) saving water resource; and (3) having small investment on production devices and having smaller energy consumption compared with production devices in the same scale.

Description

technical field [0001] The invention belongs to the technical field of nitration of aromatic hydrocarbons and derivatives thereof, and in particular relates to a method for preparing aromatic nitro compounds by using nitroxyl chloride as a nitrating agent. Background technique [0002] Aromatic nitro compounds are a very important class of chemical products, which are widely used in industrial fields such as medicine, pesticides, dyes, spices, explosives, solvents and surfactants. Methods and processes undergo very intensive and persistent research and development. [0003] Commonly used nitrating agents include various concentrations of nitric acid, a mixture of nitric acid and sulfuric acid (ie mixed acid), a mixture of nitric acid and acetic anhydride, etc. Nitrogen oxides are sometimes used as nitrating agents. The nitration of aromatic hydrocarbons is widely used in industry, and the hydrogen on the aromatic ring (Ar) is replaced by a nitro group, which can be express...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C203/06C07C205/12C07C205/06
Inventor 王士玉
Owner 淮安嘉诚高新化工股份有限公司
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