Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

A kind of preparation method of 4-bromodiphenyl ether

A technology of brominated diphenyl ether and diphenyl ether, which is applied in the field of preparation of 4-bromodiphenyl ether, can solve the problems of unsatisfactory yield and quality, too many post-processing steps, cumbersome operation, etc., and achieve low raw material cost, The effect of low cost and simple equipment requirements

Active Publication Date: 2019-07-02
内蒙古源宏精细化工有限公司
View PDF1 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] From the perspective of synthesis: the yield and quality are not ideal;
[0008] From an economic point of view: the cost is too high and the benefit is too low;
[0009] From the perspective of technology: too many post-processing steps and cumbersome operations

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
  • A kind of preparation method of 4-bromodiphenyl ether
  • A kind of preparation method of 4-bromodiphenyl ether
  • A kind of preparation method of 4-bromodiphenyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Put diphenyl ether (44.2g, 0.26mol) into a 250ml four-necked bottle, add (123.5g, (1.25mol) dichloroethane and stir for 1 hour, cool down to -5~0°C, and quickly drop (21g, 0.13mol) ) bromine, stirred for 1 hour, cooled down to -5~0°C, started to drop 30% hydrogen peroxide (15g, (0.13mol), and finished dropping in 0.5~1 hour, the temperature was controlled between 0~5°C, After the dropwise addition, the temperature was naturally raised to 25°C, kept at 27°C for 32 hours, quenched with 49g of 15% sodium bisulfite, after phase separation, washed with water to neutrality, and distilled to recover dichloroethane. Diphenyl ether was recovered by distillation under reduced pressure, and 51.7 g of 4-bromodiphenyl ether was finally collected, with a yield of 80.0% and a content of 98.2%.

Embodiment 2

[0033] Put diphenyl ether (44.2g, 0.26mol) into a 250ml four-necked bottle, add (109g, 1.1mol) dichloroethane and stir for 1 hour, cool down to -5 ~ 0°C, and quickly drop (25.6g, 0.16mol) Bromine, stir for 1 hour, cool down to -5~0°C, start to add 30% hydrogen peroxide (15g, 0.13mol) dropwise, and finish the dropwise addition in 0.5 hour, control the temperature between 0~5°C, after the dropwise addition Naturally heat up to 25°C, keep warm at 28°C for 30 hours, quench with 49g of 15% sodium bisulfite, separate phases, then wash with water to neutrality, de-distill and recover dichloroethane, and recover by vacuum distillation Before boiling diphenyl ether, 47.8 g of 4-bromodiphenyl ether was finally collected, with a yield of 74.0% and a content of 98.5%.

Embodiment 3

[0035] Put diphenyl ether (44.2g, 0.26mol) into a 250ml four-necked bottle, add (136g, 1.37mol) dichloroethane and stir for 1 hour, cool down to -5~0°C, and quickly drop in (17.3g, 0.11mol) Bromine, stir for 1 hour, cool down to -5~0°C, start to add 30% hydrogen peroxide (15g, 0.13mol) dropwise, and finish the dropwise addition in 0.6 hours, control the temperature between 0~5°C, after the dropwise addition Naturally raise the temperature to 25°C, keep warm at 25°C for 48 hours, quench with 49g of 15% sodium bisulfite, separate phases, then wash with water until neutral, distill and recover dichloroethane, and recover by vacuum distillation Before boiling diphenyl ether, 49.3 g of 4-bromodiphenyl ether was finally collected, with a yield of 76.3% and a content of 98.0%.

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 4-bromodiphenyl ether. The preparation method specifically comprises the following steps: adding a diphenyl ether-dichloroethane solution into a reaction container, dropwise adding bromine at a temperature of -5 DEG C to 0 DEG C, stirring at the controlled temperature of -5 DEG C to 0 DEG C for 1 to 2 hours, dropwise adding a hydrogen peroxide serving as a catalyst, controlling the dropwise adding to be completed within 0.5 to 1 hour, after the dropwise adding is completed, heating to 25 DEG C, controlling the temperature at 25 to 30 DEG C for reaction for 24 to 48 hours, and quenching with a sodium hydrogen sulfite aqueous solution with the mass concentration of 15 percent; washing with water for phase separation: recycling an inorganic phase, performing coarse steaming on an organic phase to recycling dichloroethane serving as a solvent, performing reduced pressure distillation on a coarse product, recycling and indiscriminately using a front distillate serving as a raw material, and recycling a middle distillate which is the 4-bromodiphenyl ether. The preparation method of the 4-bromodiphenyl ether is simple in process, and the product is high in purity, yield and quality and low in cost; the purity of the 4-bromodiphenyl ether is 98.0 percent, and the yield is 78 percent.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of 4-bromodiphenyl ether. Background technique [0002] 4-Bromodiphenyl ether, as a low-brominated product of polybrominated diphenyl ether, is a kind of chemical additive and can also be used as a solvent. Its brominated properties make it have similar characteristics to its homologues - polybrominated diphenyl ethers. 4-Bromodiphenyl ether can be used as an additive flame retardant and has good flame retardant effect. The preparation method of existing synthetic 4-bromodiphenyl ether has the following several: Synthesize 4-bromodiphenyl ether with iodobenzene and 4-bromophenol in alkaline solution, raw material cost is higher, raw material separation, recovery step simultaneously Too much, the economic benefit is not good, and the product yield is about 68% low. The reaction formula is as follows: [0003] [0004] Using bromobe...

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
Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/22C07C43/29
CPCC07C41/22C07C43/29
Inventor 巫辅才
Owner 内蒙古源宏精细化工有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com