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Preparation method of 6-chloro-2-nitrotoluene

A technology of nitrotoluene and o-nitrotoluene, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of long chlorination reaction cycle, high production cost, and low reaction yield, and achieve Good economic and social benefits, short reaction cycle, and reduced side effects

Inactive Publication Date: 2017-12-15
山东福尔有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The shortcoming of this preparation method: 1, the chlorination reaction cycle is long
2. The reaction yield is low and the production cost is high

Method used

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  • Preparation method of 6-chloro-2-nitrotoluene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1. Chlorination step: Add 3300kg of o-nitrotoluene and 32kg of thionyl chloride into the chlorination kettle, turn on the tail gas absorption device, and stir at 63r / min. Feed vaporized chlorine into the chlorination kettle at a flow rate of 85kg / h, control the reaction temperature to be 65°C, react for 27 hours, and take samples for analysis. When the o-nitrotoluene content is 10%, after the chlorination reaction ends, the Blow compressed air in the kettle for about two hours to reduce the chlorine content in the chlorination kettle to obtain the primary product of 6-chloro-2-nitrotoluene. In the next operation, add new materials according to the specified amount, and start the next batch of chlorination reaction.

[0019] 2. Washing step: Add the measured 6-chloro-2-nitrotoluene primary product into the washing kettle, start the washing kettle to stir, add hydrochloric acid in the metering tank to the washing kettle, stir, let stand for 20min, separate layers, and cle...

Embodiment 2

[0028] Prepare according to the preparation method of 6-chloro-2-nitrotoluene in Example 1, only change the following parameters in the following steps of Example 1:

[0029] 1. Chlorination step: add 3300kg of o-nitrotoluene and 85kg of thionyl chloride to the chlorination kettle, turn on the tail gas absorption device, and stir at 63r / min. With the flow rate of 85kg / h, the vaporized chlorine gas is passed into the chlorination kettle, the control reaction temperature is 70°C, and the reaction is carried out for 27 hours. Sampling and analysis, when the o-nitrotoluene content is 10%, after the chlorination reaction ends, the Blow compressed air in the kettle for about two hours to reduce the chlorine content in the chlorination kettle to obtain the primary product of 6-chloro-2-nitrotoluene. In the next operation, add new materials according to the specified amount, and start the next batch of chlorination reaction.

[0030] 2. Washing step: Add the measured 6-chloro-2-nitro...

Embodiment 3

[0034] Prepare according to the preparation method of 6-chloro-2-nitrotoluene in Example 1, only change the following parameters in the following steps of Example 1:

[0035] 1. Chlorination step: add 3300kg of o-nitrotoluene and 155kg of thionyl chloride to the chlorination kettle, turn on the tail gas absorption device, and stir at 63r / min. With the flow rate of 85kg / h, the vaporized chlorine gas is passed into the chlorination kettle, and the reaction temperature is controlled to be 75°C, reacted for 27 hours, and sampling analysis is performed. Blow compressed air in the kettle for about two hours to reduce the chlorine content in the chlorination kettle to obtain the primary product of 6-chloro-2-nitrotoluene. In the next operation, add new materials according to the specified amount, and start the next batch of chlorination reaction.

[0036] 2. Washing steps: Add the measured primary product of 6-chloro-2-nitrotoluene into the washing kettle, start the washing kettle t...

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Abstract

The invention discloses a preparation method of 6-chloro-2-nitrotoluene. The preparation method comprises steps as follows: (1) ortho-nitrotoluene and thionyl chloride are added to a chlorination kettle, stirred and heated, chlorine is introduced, the mixture reacts at the temperature of 65-75 DEG C, and an initial 6-chloro-2-nitrotoluene product is prepared; (2) the initial 6-chloro-2-nitrotoluene product obtained in the step (1) is transferred to a water washing kettle, thionyl chloride is washed out, the washed material is dewatered, and a crude 6-chloro-2-nitrotoluene product is prepared; (3) the crude 6-chloro-2-nitrotoluene product obtained in the step (2) is transferred to a rectifying column for purification, and a purified 6-chloro-2-nitrotoluene product is obtained; (4) the purified 6-chloro-2-nitrotoluene product obtained in the step (3) is crystalized at the temperature of 40-50 DEG C, and the high-purity 6-chloro-2-nitrotoluene product is obtained. The preparation method has the benefits as follows: the problems of long chlorination production cycle and short content are solved with the adoption of thionyl chloride as a catalyst, and a good foundation is laid for preparation of high-purity 6-chloro-2-nitrotoluene.

Description

technical field [0001] The invention belongs to the technical field of preparation of chlorine-containing compounds, and in particular relates to a preparation method of 6-chloro-2-nitrotoluene. Background technique [0002] 6-Chloro-2-nitrotoluene is an important intermediate of medicine, pesticide and dyestuff. Chloro-2-nitrotoluene, using ferric chloride as a catalyst, reacts with chlorine gas to synthesize crude 6-chloro-2-nitrotoluene. After washing with water, pickling, alkali washing, standing and layering. Separate 6-chloro-2-nitrotoluene for dehydration. After distillation and crystallization purification, 6-chloro-2-nitrotoluene can be obtained. The shortcoming of this preparation method: 1, the chlorination reaction period is long. 2. The reaction yield is low and the production cost is high. Contents of the invention [0003] According to the deficiencies in existing technology, the invention provides a kind of 6-chloro-2-nitrotoluene preparation method, c...

Claims

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Application Information

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IPC IPC(8): C07C201/12C07C201/16C07C205/12
CPCC07C201/12C07C201/16C07C205/12
Inventor 于俊田张玲
Owner 山东福尔有限公司
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