Method for preparing o-chlorotoluene

A technology of ortho-chlorotoluene and toluene, which is applied in the field of preparation of ortho-chlorotoluene, can solve problems such as difficulty in obtaining pure ortho-chlorotoluene, high content of middle sites in chlorinated liquid, and decreased proportion of ortho-chlorotoluene, achieving good industrial prospects and high activity , the effect of fast reaction rate

Inactive Publication Date: 2016-03-23
NANJING ZHONGTENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the molecular sieve lattice is easily broken by the acid produced by the reaction, the catalyst life is short, and the proportion of o-chlorotoluene in the chlorination product is significantly reduced when it is reused after regeneration. toluene

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The method for preparing o-chlorotoluene, the steps are as follows: N 2 Under protection, the FeCl 3 and macroporous silica gel were added to absolute ethanol, FeCl 3 The ratio of the amount and mass of the macroporous silica gel to the substance is: 0.5mmol: 10g; the mass volume ratio of the macroporous silica gel to absolute ethanol is: 1g: 10ml; the temperature is raised to 60°C, refluxed and stirred for 2h, and after the reaction is completed, the The filtered sample was dried at 80°C for 12 hours, and the obtained sample was FeCl 3 Loaded macroporous metal silica gel catalyst; toluene raw material and catalyzer are added in the reactor, and the add-on of catalyst is 0.1% of toluene quality; Pass into chlorine in the reactor, make toluene and chlorine carry out liquid phase ring chlorination reaction, The chlorination reaction temperature is 50°C; the chlorination reaction time is 6h. The chlorination reaction is carried out by means of tower-type ring chlorinati...

Embodiment 2

[0021] The method for preparing o-chlorotoluene, the steps are as follows: N 2 Under protection, the FeCl 3 and macroporous silica gel were added to absolute ethanol, FeCl 3 The ratio of the amount and mass of the macroporous silica gel to the substance is: 5mmol: 10g; the mass volume ratio of the macroporous silica gel to absolute ethanol is: 1g: 15ml; the temperature is raised to 90°C, refluxed and stirred for 4h, and after the reaction is completed, filter The final sample was dried at 80°C for 12 hours, and the obtained sample was FeCl 3 The macroporous metal silica gel catalyst of load; Toluene raw material and catalyzer are joined in the reactor, and the add-on of catalyzer is 2% of toluene quality; Pass into chlorine in the reactor, make toluene and chlorine carry out liquid phase ring chlorination reaction, The chlorination reaction temperature is 80°C; the chlorination reaction time is 12h. The chlorination reaction is carried out by means of tower-type ring chlori...

Embodiment 3

[0024] The method for preparing o-chlorotoluene, the steps are as follows: N 2 Under protection, the FeCl 3 and macroporous silica gel were added to absolute ethanol, FeCl 3 The ratio of the amount and mass of the macroporous silica gel to the substance is: 3mmol: 10g; the mass volume ratio of the macroporous silica gel to absolute ethanol is: 1g: 12ml; the temperature is raised to 80°C, refluxed and stirred for 3h, and after the reaction is completed, filter The final sample was dried at 80°C for 12 hours, and the obtained sample was FeCl 3 Loaded macroporous metal silica gel catalyst; toluene raw material and catalyzer are added in the reactor, and the add-on of catalyzer is 1% of the toluene quality; Pass into chlorine in the reactor, make toluene and chlorine carry out liquid phase ring chlorination reaction, The chlorination reaction temperature is 60°C; the chlorination reaction time is 8h. The chlorination reaction is carried out by means of tower-type ring chlorinat...

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Abstract

The invention discloses a method for preparing o-chlorotoluene. The method comprises the following steps: adding a raw material toluene and a FeCl3-loaded macroporous metal silica gel catalyst into a reaction kettle; introducing chlorine into the reaction kettle for a liquid-phase ring chlorination reaction between the toluene and chlorine; after the reaction is complete, aerating to remove residual chlorine and hydrogen chloride gas in the reaction liquid; rectifying the reaction liquid to separate out unreacted toluene and a little dichlorotoluene to obtain mixed chlorotoluene; and then, separating high-purity p-chlorotoluene from the mixed chlorotoluene by using a melt crystallization process. According to the method disclosed by the invention, the FeCl3-loaded macroporous metal silica gel catalyst is adopted for catalyzing the selective chlorination of toluene, the reaction is fast, the catalytic activity is high, the o-chlorotoluene selectivity is good, the requirements for the technological conditions are low, the catalyst consumption is low, the catalyst has high activity and can be recycled, and the method has a good industrial prospect.

Description

technical field [0001] The invention belongs to the field of organic chemical industry, in particular to a method for preparing o-chlorotoluene. Background technique [0002] O-chlorotoluene is an important chemical raw material intermediate, widely used in pesticides, medicines, dyes and paints. It is also a medium-boiling organic solvent with good performance; at present, o-chlorotoluene is increasingly widely used in organic synthesis. [0003] Using o-chlorotoluene as raw material and aluminum chloride as a catalyst, thiazole pesticides and fungicides can be directly synthesized; the condensation reaction product of o-chlorotoluene and dichloroalkane can be used as high-pressure grease and oil; Under the condition of sodium oxide alkaline hydrolysis to synthesize m-cresol and o-cresol, the yield can reach more than 80%; o-chlorotoluene can be further chlorinated under the condition of Lewis acid catalyst to prepare 2,6-dichlorotoluene, 2,4- Dichlorotoluene, etc. [00...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/12C07C25/02B01J27/128
CPCC07C17/12B01J27/128
Inventor 钟华陆敏山陈秀珍蔡伟忠
Owner NANJING ZHONGTENG CHEM
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