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Preparation method and device of aromatic chloride

A chloride and aromatic technology, which is applied in the field of devices for realizing the above-mentioned aromatic chloride preparation method, can solve the problems of shrinkage, high safety risk, poor heat transfer, etc.

Active Publication Date: 2017-08-08
LIANHE CHEM TECH TAIZHOU +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the defects of high safety risk, many wastes, large reaction volume and poor heat transfer which lead to long reaction time in oxidative chlorination reaction in the prior art process, and discloses a A method and corresponding device for preparing aromatic chlorides by continuous chlorination in a tubular reactor. This method utilizes the large heat transfer area of ​​the tubular reactor and high heat transfer efficiency. The continuous preparation method can strengthen the reaction temperature, increase the reaction concentration, and greatly shorten the reaction time. time, improve production efficiency, reduce reaction volume, reduce safety risks, and have the advantages of simple operation, safer, more environmentally friendly, and lower cost

Method used

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  • Preparation method and device of aromatic chloride
  • Preparation method and device of aromatic chloride
  • Preparation method and device of aromatic chloride

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Experimental program
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Effect test

Embodiment 1

[0089] This tubular reaction device, such as figure 1 As shown, it includes: raw material storage tanks 2, 3, 4, crystallization tanks 5, 6, feed pumps 11, 12, 13, tubular reactor 15, liquid storage tank 7, heat exchanger 8, circulation pump 9 , a heat exchange liquid tank 14, a raw material dissolution kettle 1, and a transfer pump 10.

[0090] The number of raw material storage tanks, feed pumps and corresponding material inlets can be set as required. Such as figure 2 As shown, when there are two materials in the reaction that are first added to the tubular reactor, and then react with another added material in the tubular reactor 15, ports 16, 17, 20 and ports 18, 19, 21 They are the ports of two three-way hollow pipes respectively; port 21 is connected with tubular reactor 15; ports 16, 17 and 18 are material inlets of tubular reactor 15; material inlets 16, 17 and 18 are respectively connected with feed pump 11 , 12 and 13 are hermetically connected; the feed pumps 1...

Embodiment 2

[0098]

[0099] 1. Raw material preparation: Compound A-1 and acetic acid were stirred at 60°C for 30 minutes to dissolve and be configured into a solution (mass fraction 35.7%) placed in raw material tank 2, hydrogen peroxide (mass fraction 50%) placed in raw material tank 3, hydrochloric acid (mass fraction Fraction 36%) is placed in raw material tank 4.

[0100] 2. Utilize the tubular reactor of embodiment 1, reactor pipe inner diameter 4mm and pipe length 40m, according to the following steps: (1) by metering pump control, the flow rate of compound A-1 solution is 76ml / min, the flow rate of hydrogen peroxide is 10ml / min mixed first, residence time 2s; (2) mixed with hydrochloric acid controlled by a metering pump at 28ml / min, and reacted at an external temperature of 70°C, residence time 4.3min; (3) adding the effluent of the tubular reactor into water, Adjust to non-oxidizing with sodium sulfite, filter, wash the filter cake with water, and dry to obtain product B-1. ...

Embodiment 3

[0103] 1. Raw material preparation: Compound A-1 and acetic acid were stirred at 60°C for 30 minutes to dissolve and be configured into a solution (35.7% by mass fraction) placed in raw material tank 2, hydrogen peroxide (35% by mass fraction) placed in raw material tank 3, hydrochloric acid (mass fraction 35%) Fraction 36%) is placed in raw material tank 4.

[0104] 2. Utilize the tubular reactor of embodiment 1, reactor pipe internal diameter 4mm and pipe length 32m, according to the following steps: (1) by metering pump control, the flow rate of compound A-1 solution 51ml / min, the flow rate of hydrogen peroxide 9.7 ml / min first mixed, residence time 2s; (2) mixed with hydrochloric acid controlled by a metering pump at 19ml / min, and reacted at an external temperature of 70°C, residence time 5min; (3) adding the effluent from the tubular reactor into water, Adjust to non-oxidizing with sodium sulfite, filter, wash the filter cake with water, and dry to obtain product B-1.

...

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Abstract

The invention discloses a preparation method and a device of aromatic chloride. The preparation method comprises the following step: performing chlorination on a mixed solution of a solution of a compound A, a hydrogen peroxide solution and a hydrogen chloride solution in a tubular reactor so as to obtain a compound B, wherein the mole ratio of the compound A to hydrogen peroxide and hydrogen chloride in the mixed solution is 1:(1-4):(1-4), and the retention time of the mixed solution in the tubular reactor is 30-600s. The invention further discloses a tubular reaction device. The preparation method disclosed by the invention is very short in reaction time, precise in reaction condition control, high in security, good in continuous production, high in product yield, high in purity and applicable to large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of aromatic chlorides. The present invention also relates to a device for realizing the above aromatic chloride preparation method. Background technique [0002] In the field of organic synthesis, chlorination on aromatic rings is a widely used reaction; commonly used methods include direct chlorine chlorination, N-chlorosuccinimide chlorination, and oxidative chlorination. However, chlorine gas is highly toxic and belongs to a dangerous chemical process, and the reaction is violent and difficult to control; the raw material cost of N-chlorosuccinimide is high, and the atom economy is poor; in these several methods, oxidative chlorination, that is, hydrochloric acid and hydrogen peroxide, is used to generate chlorine gas in situ. Chlorination is relatively environmentally friendly and meets the requirements of contemporary green synthesis, and the raw materials are cheap and easy to obtain. [0003] ...

Claims

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Application Information

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IPC IPC(8): C07C269/06C07C271/28C07D263/58C07C227/16C07C229/64C07C231/12C07C233/15C07C233/54B01J19/24
Inventor 潘强彪邹本立李永锋谢春辉
Owner LIANHE CHEM TECH TAIZHOU
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