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
View PDF10 Cites 6 Cited by
  • 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

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method and device of aromatic chloride
  • Preparation method and device of aromatic chloride
  • Preparation method and device of aromatic chloride

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0088] Example 1

[0089] This tubular reaction device, such as figure 1 As shown, it contains: 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, circulating pump 9 , Heat exchange liquid tank 14, raw material dissolving tank 1, transfer pump 10.

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

Example Embodiment

[0097] Example 2

[0098]

[0099] 1. Preparation of raw materials: compound A-1 and acetic acid are stirred at 60°C for 30 minutes to form a solution (35.7% by mass) placed in raw material tank 2, hydrogen peroxide (50% by mass) is placed in raw material tank 3, hydrochloric acid (mass fraction) 36%) placed in the raw material tank 4.

[0100] 2. Using the tubular reactor of Example 1, the reactor pipe inner diameter is 4mm and the pipe length is 40m, according to the following steps: (1) Controlled by a metering pump, the flow rate of compound A-1 solution is 76ml / min, and the flow rate of hydrogen peroxide is 10ml / min mixed first, with a residence time of 2s; (2) then mixed with 28ml / min hydrochloric acid controlled by a metering pump, reacted at an external temperature of 70℃, with a residence time of 4.3min; (3) added 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...

Example Embodiment

[0102] Example 3

[0103] 1. Preparation of raw materials: compound A-1 and acetic acid are stirred at 60°C for 30 minutes to form a solution (35.7% by mass) placed in raw material tank 2, hydrogen peroxide (35% by mass) is placed in raw material tank 3, hydrochloric acid (mass fraction) 36%) placed in the raw material tank 4.

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

[0105] 3...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap