Unlock instant, AI-driven research and patent intelligence for your innovation.

Preparation method of 2, 4, 6-tribromoaniline

A technology of tribromoaniline and bromine salt, applied in the field of organic compound preparation, can solve the problems of huge investment, pollution, expensive catalysts and the like of catalytic hydrogenation method, and achieve the effects of preventing environmental pollution, high current efficiency and reducing production cost

Active Publication Date: 2021-12-07
SHANDONG JINGBO PETROCHEM
View PDF8 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, iron powder reduction needs to consume a large amount of iron powder, and if it is not handled properly, it will cause serious pollution; catalytic hydrogenation method not only requires a huge investment, but also requires expensive catalysts

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 of 2, 4, 6-tribromoaniline
  • Preparation method of 2, 4, 6-tribromoaniline
  • Preparation method of 2, 4, 6-tribromoaniline

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0023] The invention provides a preparation method of 2,4,6-tribromoaniline, comprising: using benzene as a raw material, bromine salt as a bromine source, and nitric acid aqueous solution as an electrolyte in a diaphragmless electrolytic cell provided with an anode and a cathode. Electrolysis reaction to obtain 2,4,6-tribromoaniline; micro-mesoporous composite molecular sieve HY / HMS and organic solvent are also added into the electrolytic solution.

[0024] Among them, the present invention has no special limitation on the sources of all raw materials, which can be commercially available.

[0025] The present invention reacts in a diaphragmless electrolytic cell provided with an anode and a cathode; the anode and the cathode are independently preferably copper electrodes, graphite electrodes, glassy carbon electrodes, platinum electrodes or lead electrodes, more preferably copper electrodes or lead electrodes electrode.

[0026] An electrolytic solution is provided in the di...

Embodiment 1

[0033]Weigh 1.25 g of dodecylamine (DDA) into a three-necked flask, add solvent and stir in a water bath at 25° C. for 30 min at constant temperature. After it is completely dissolved, transfer it to a microwave reactor. Put the mixed solution of 5.6ml TEOS and 10ml ethanol in a constant pressure dropping funnel and mix well. Set the reaction temperature at 45°C, the rotation speed at 240r / min, dropwise at a constant speed (3d / s), and stir at a constant temperature of 45°C for 3h after the dropwise addition is complete. Add 0.7gHY zeolite and continue stirring for 3h. Stand at room temperature for 18 hours for aging, suction filter, dry, and calcine at 500°C for 5 hours to remove the template agent, and obtain the micro-mesoporous composite molecular sieve HY / HMS.

[0034] Utilize scanning electron microscope to analyze the micro-mesoporous composite molecular sieve HY / HMS that obtains in embodiment 1, obtain its scanning electron microscope picture, as figure 1 shown.

[0...

Embodiment 2

[0038] Add 0.32g benzene in the diaphragmless electrolyzer, 40mL mass fraction is the nitric acid of 20% and 0.42g sodium bromide, the micro-mesoporous composite molecular sieve HY / HMS that obtains in the embodiment 1 is catalyzer its addition is 0.032g, 20mL ethyl acetate, constant temperature 60°C, electrolyze both the anode and the cathode with lead electrodes for 3h, and keep the current at 0.2A. The yield of 2,4,6-tribromoaniline was 42.6% as detected by gas chromatography.

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 provides a preparation method of 2, 4, 6-tribromoaniline, which comprises the following steps: carrying out an electrolytic reaction in a diaphragm-free electrolytic bath provided with an anode and a cathode by taking benzene as a raw material, taking bromine salt as a bromine source and taking a nitric acid aqueous solution as an electrolyte to obtain the 2, 4, 6-tribromoaniline; wherein a micro-mesoporous composite molecular sieve HY / HMS and an organic solvent are also added into the electrolyte. Compared with the prior art, the method has the advantages that benzene is used as a main raw material, nitrobenzene is generated through nitration under the action of the catalyst, then nitrobenzene is reduced into aniline on the cathode, meanwhile, free bromide ions in the solution are oxidized into elemental bromine on the anode, finally, 2, 4, 6-tribromoaniline is generated through electrophilic substitution, the utilization rate of bromine atoms is close to 100%, the current efficiency is high, and the repeated use effect of the catalyst is good; and meanwhile, use of strong acid in the nitration process is avoided, pollution is almost avoided, the production cost is reduced, environmental pollution is prevented, and the method has a relatively strong market application prospect.

Description

technical field [0001] The invention belongs to the technical field of organic compound preparation, in particular to a preparation method of 2,4,6-tribromoaniline. Background technique [0002] 2,4,6-Tribromoaniline is an important chemical product and an important chemical intermediate widely used in analytical reagents, synthetic dyes, chemical flame retardants, etc. The conventional synthesis method is mainly to pass bromine into the mixed solution of aniline, hydrochloric acid and water, and react under the condition of 40 ° C. If there are literature reports, MgBr2 is used as a catalyst to directly brominate aniline with liquid bromine to prepare 2, 4, 6 -Tribromoaniline, yield 98% (Zheng Ping, Jin Dongxia. Synthesis of 2,4,6-tribromoaniline [J]. Dyestuff Industry, 1999,36(6):32-33.). However, conventional synthesis methods not only use a large amount of liquid bromine and the utilization rate of bromine atoms is low, but also the toxicity of aniline is very high, whi...

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): C25B3/09C25B3/11C25B3/20
CPCC25B3/09C25B3/11C25B3/20Y02P20/584
Inventor 郭虎菲李寿丽崔勇赵德明史会兵王耀伟栾波
Owner SHANDONG JINGBO PETROCHEM
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com