Production process of high-purity 2,4-dichlorotoluene

A technology for dichlorotoluene and production process, applied in the field of compound synthesis and purification, can solve the problems of difficult purification, low purity, low yield and the like, and achieve the effects of good alkali washing effect, high rectification yield and high product quality

Inactive Publication Date: 2019-06-07
JIANGSU QIHENG AGRI & CHEM TECHCO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the deficiencies in the prior art, provide a kind of high-purity 2, the production process of 4-dichlorotoluene, solve the low yield, low purity and difficult purification of 2,4-dichlorotoluene in the prior art problems, the prepared 2,4-dichlorotoluene has the advantages of high yield, high purity and recyclable materials

Method used

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Examples

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Comparison scheme
Effect test

Embodiment 1

[0030] A production process of high-purity 2,4-dichlorotoluene, comprising the steps of:

[0031] Step 1. Catalytic synthesis of 2,4-dichlorotoluene: Add p-chlorotoluene and NaKL zeolite into the reaction vessel, then feed chlorine gas at a temperature of 40°C, stop feeding chlorine gas and react for at least 30 minutes, then add purified water to absorb Stand still for at least 30 minutes after hydrogen chloride to obtain a hydrochloric acid solution, recover the hydrochloric acid solution through a hydrochloric acid recovery device, and obtain an organic mixture for use, wherein the molar ratio of p-chlorotoluene to chlorine is 1:1.3, and the molar ratio of purified water to p-chlorotoluene is 1 : 3.0, the rate of introduction of chlorine gas is 0.6L / min;

[0032] Step 2. Alkali washing: Add alkali slag to the organic mixture in step 1 for alkali washing, filter to remove the alkali slag, then add purified water and diethyl ether or dichloromethane, shake and shake for at le...

Embodiment 2

[0038] A production process of high-purity 2,4-dichlorotoluene, comprising the steps of:

[0039]Step 1. Catalytic synthesis of 2,4-dichlorotoluene: Add p-chlorotoluene and NaKL zeolite into the reaction vessel, then feed chlorine gas at a temperature of 41°C, stop feeding chlorine gas and react for at least 30 minutes, then add purified water to absorb Stand still for at least 30 minutes after hydrogen chloride to obtain a hydrochloric acid solution, recover the hydrochloric acid solution through a hydrochloric acid recovery device, and obtain an organic mixture for use, wherein the molar ratio of p-chlorotoluene and chlorine gas is 1:1.5, and the molar ratio of purified water to p-chlorotoluene is 1 : 4.0, the feed rate of chlorine gas is 0.8L / min;

[0040] Step 2. Alkali washing: Add alkali slag to the organic mixture in step 1 for alkali washing, filter to remove the alkali slag, then add purified water and diethyl ether or dichloromethane, shake and shake for at least 5 m...

Embodiment 3

[0046] A production process of high-purity 2,4-dichlorotoluene, comprising the steps of:

[0047] Step 1. Catalytic synthesis of 2,4-dichlorotoluene: Add p-chlorotoluene and NaKL zeolite into the reaction vessel, then feed chlorine gas at a temperature of 40°C, stop feeding chlorine gas and react for at least 30 minutes, then add purified water to absorb Stand still for at least 30 minutes after hydrogen chloride to obtain a hydrochloric acid solution, recover the hydrochloric acid solution through a hydrochloric acid recovery device, and obtain an organic mixture for use, wherein the molar ratio of p-chlorotoluene to chlorine is 1:1.4, and the molar ratio of purified water to p-chlorotoluene is 1 : 3.5, the feed rate of chlorine gas is 0.7L / min;

[0048] Step 2. Alkali washing: Add alkali slag to the organic mixture in step 1 for alkali washing, filter to remove the alkali slag, then add purified water and diethyl ether or dichloromethane, shake and shake for at least 5 minut...

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PUM

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Abstract

The invention relates to the technical field of compound synthesis and purification, and particularly relates to a production process of high-purity 2,4-dichlorotoluene. The method comprises the following steps: carrying out catalytic synthesis on 2,4-dichlorotoluene by using p-chlorotoluene and chlorine, carrying out alkali washing, recovering fractions by rectifying, and carrying out purifying crystallization to obtain the high-purity 2,4-dichlorotoluene. The method solves the problem that 2,4-dichlorotoluene is low in yield and purity and is not easy to purify in the prior art. The prepared2,4-dichlorotoluene has the advantages that the yield is high, purity is high and materials can be recycled.

Description

technical field [0001] The invention relates to the technical field of compound synthesis and purification, in particular to a production process of high-purity 2,4-dichlorotoluene. Background technique [0002] 2,4-dichlorotoluene is medicine or dye intermediate CAS No. 95-73-8, 2,4-dichlorotoluene is colorless transparent liquid; 2,4-dichlorotoluene is poisonous, rat oral LD50 is 4640mg / kg. The operating place should be well ventilated, the equipment should be airtight, and the operators should wear protective equipment. 2,4-Dichlorotoluene should be stored in a cool and ventilated place, away from fire and heat sources, and stored separately from oxidants, food, feed, and seeds, and keep the packaging intact. [0003] 2,4-dichlorotoluene is a very important organic synthesis fine chemical intermediate, which can be used to synthesize 2,4-dichlorobenzoic acid, 2,4-dichlorobenzyl chloride, 2,4-dichloroacyl chloride and 2,4 —Dichlorobenzaldehyde and other organic chemica...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C25/125C07C17/12C07C17/395C07C17/383C07C17/392
Inventor 王健吴明俊
Owner JIANGSU QIHENG AGRI & CHEM TECHCO
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