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Novel chlorination process of o-chlorobenzotrichloride

A technology of o-chlorotrichlorotoluene and o-chlorotoluene, which is applied in the fields of organic chemistry, chemical instruments and methods, preparation of halogenated hydrocarbons, etc., can solve the problem of low conversion rate and yield of target products, complicated and time-consuming separation and purification process, organic Problems such as large amount of three wastes, to achieve the effect of low cost, simplify the separation and purification process, and reduce the discharge of organic three wastes

Inactive Publication Date: 2020-01-07
JIANGSU FENGHUA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The yield of this traditional side chain chlorination method is about 90%, the production process is cumbersome, and a large amount of by-product hydrochloric acid and sodium hypochlorite solution are produced with waste gas emission
In addition, when the side chain is chlorinated, monochlorinated, dichlorinated, side chain and benzene ring chlorinated by-products are generated, resulting in low conversion rate and yield of the target product, tedious and time-consuming separation and purification process, and a large amount of organic waste

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Catalytic side chain chlorination: Put 800g of o-chlorotoluene into a 3L reactor, raise the temperature to 115°C, start adding catalyst, and start to feed dry chlorine gas with a flow rate of 40-80 m 3 / h, after that, add catalyst every 15 minutes, add 40g catalyst in total, control the temperature at 115-117°C, and the reaction time is 24 hours. Stop feeding chlorine gas when o-chlorodichlorotoluene content is less than 0.5%, change into dry air to discharge unreacted chlorine in the reaction kettle, hydrogen chloride gas and gas impurity that reaction produces, obtain o-chlorobenzotrichlorotoluene thick product;

[0026] (2) Rectification: The above crude product was rectified under reduced pressure at a vacuum degree of 0.095Mpa and a reflux ratio of 5:2, and the distillate with a gas phase temperature of 145-148°C at the top of the tower was collected and condensed to obtain ophthalmic acid with a purity of 99.1wt%. Chlorotrichlorotoluene;

[0027] (3) Neutrali...

Embodiment 2

[0029] (1) Catalytic side chain chlorination: Put 800g of o-chlorotoluene into a 3L reactor, raise the temperature to 115°C, start adding catalyst, and start to feed dry chlorine gas with a flow rate of 40-80 m 3 / h, then add the catalyst every 15 minutes, add 80g catalyst in total, control the temperature at 120-125°C, and the reaction time is 22 hours. Stop feeding chlorine gas when o-chlorodichlorotoluene content is less than 0.5%, change into dry air to discharge unreacted chlorine in the reaction kettle, hydrogen chloride gas and gas impurity that reaction produces, obtain o-chlorobenzotrichlorotoluene crude product;

[0030] (2) Rectification: The above crude product was rectified under reduced pressure at a vacuum degree of 0.095Mpa and a reflux ratio of 3:1, and the distillate with a gas phase temperature of 145-148°C at the top of the tower was collected and condensed to obtain ophthalmic acid with a purity of 99.3wt%. Chlorotrichlorotoluene;

[0031] (3) Neutralizat...

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PUM

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Abstract

The invention discloses a novel chlorination process of o-chlorobenzotrichloride, wherein o-chlorotoluene is used as a raw material, and side chain chlorination, pressure reducing rectification, neutralization, filtration and other steps are performed to obtain the target compound o-chlorobenzotrichloride. Compared with the process in the prior art, the process of the invention has the following characteristics that the step-by-step catalytic process is adopted, the reaction conditions are mild, no special equipment is added in the production process, the side chain trichlorination selectivityis high, the generation of monochlorides, dichlorocompounds, side chains and benzene ring chlorination byproducts is greatly reduced, the separation and purification process is simplified, the emission of three organic wastes is reduced, and the yield is about 99% and is about 10% higher than the yield of the common chlorination process.

Description

technical field [0001] The invention relates to a preparation method of a pesticide chemical intermediate product, in particular to a novel chlorination process of o-chlorotrichlorotoluene. This method is applicable to the occasion of synthesizing o-chlorobenzotrichloride by using o-chlorotoluene as raw material through catalytic side chain chlorination, rectification, neutralization and other processes. Background technique [0002] O-chlorobenzotrichloride is an important pharmaceutical intermediate. The side chain chlorine atoms in its molecular structure can be replaced by fluorine atoms to have special activity. It is widely used in fine organic synthesis fields such as medicine, pesticides, and dyes. [0003] At present, the known synthetic method uses o-chlorotoluene as a raw material to obtain o-chlorotrichlorotoluene through side chain photochlorination. [0004] The yield of this traditional side chain chlorination method is about 90%, and the production process i...

Claims

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Application Information

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IPC IPC(8): C07C17/14C07C17/383C07C25/02
CPCC07C17/14C07C17/383C07C25/02
Inventor 郑龙生方东张亮李付香
Owner JIANGSU FENGHUA CHEM IND
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