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Environment-friendly method for synthesizing tetrabromo bisphenol A diene propyl ether

A technology of bisallyl ether and tetrabromobisphenol, applied in ether preparation, organic chemistry and other directions, can solve problems such as hidden safety hazards, complicated follow-up processes, residual liquid and slag discharge, etc.

Active Publication Date: 2008-11-12
LIHAI CHEM IND CO LTD OF JIANGSU JINQIAO SALT & CHEM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Tetrabromobisphenol A diallyl ether can be obtained by adding tetrabromobisphenol A and 3-chloropropene to lower aliphatic alcohols (referring to alkanols containing 1 to 3 carbon atoms) for etherification, but this method The solvent needs to be recovered and rectified, and the residual liquid and slag should be discharged
Due to incomplete desolventization, by-products are brought, which need to be further separated, making the follow-up process complicated
It is especially important that when tetrabromobisphenol A diallyl ether is synthesized as a solvent with lower aliphatic alcohols, because the existence of lower aliphatic alcohols brings great potential safety hazards to each process operation in the process

Method used

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  • Environment-friendly method for synthesizing tetrabromo bisphenol A diene propyl ether
  • Environment-friendly method for synthesizing tetrabromo bisphenol A diene propyl ether
  • Environment-friendly method for synthesizing tetrabromo bisphenol A diene propyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 90g of tetrabromobisphenol A, 12g of NaOH, and 0.38g of triethylbenzyl ammonium chloride into a 500ml reactor equipped with a reflux tube, a thermometer, an agitator and a pressure balance dripping device, and add 90ml of water at the same time, and heat up to 95 ℃, began to drop 40g of 3-chloropropene, and the dropwise addition was completed in 1.5h. The reaction temperature is about 70°C, after reflux reaction for 3 hours, add 2gNOH, and then reflux reaction for 2h, steam off excess 3-chloropropene, cool down to below 40°C, centrifuge, wash the filter cake with deionized water, and wash the After the filter cake was dried at 85°C to constant weight, 98.68 g of tetrabromobisphenol A diallyl ether was obtained, with a yield of 95.5%. The purity of the product was 98.7% through liquid chromatography analysis.

Embodiment 2

[0033] Add 90g tetrabromobisphenol A, 12gNaOH, cetyltributylphosphonium bromide 0.84g in the 500ml reactor that reflux tube, thermometer, stirring and pressure balance dripping device are housed, add 84ml water simultaneously, heat up to At 95°C, 40g of 3-chloropropene was added dropwise, and the dropwise addition was completed in 1.5 hours. The reaction temperature was maintained at about 74°C. After reflux for 3 hours, 2g of NaOH was added and then refluxed. After 2 hours, the excess 3-chloropropene was evaporated and the temperature was lowered to below 40°C, centrifuged, the filter cake was washed with deionized water, and the washed filter cake was dried at 85°C to constant weight to obtain tetrabromobisphenol A diene Propyl ether 97.5g, yield 94.4%. The temperature of the product analyzed by liquid chromatography is 98.3%.

Embodiment 3

[0035] Add 80g of tetrabromobisphenol A, 10.1g of NaOH, and 1.62g of tetra-n-butylphosphonium bromide into a 500ml reactor equipped with a reflux tube, thermometer, stirring and pressure balance dripping device, and add 80ml of water at the same time, heat up to 95°C , began to add 34g of 3-chloropropene dropwise, and the dropwise addition was completed in 1h. The reaction temperature was maintained at about 66°C. After reflux for 2h, add 1.7g of NaOH and then reflux for 1.5h. Evaporate excess 3-chloropropene and lower the temperature to below 40°C, centrifuge, wash the filter cake with deionized water, and dry the washed filter cake at 85°C to constant weight to obtain tetrabromobisphenol A diallyl Ether 87.26g, yield 95.09%. The temperature of the product analyzed by liquid chromatography is 97.9%.

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Abstract

This invention relates to good environment synthesizing tetrabromo bisphenol A diolefine propyl ether method, the tetrabromo bisphenol A is material, phase transfer catalyst is added into NaOH water solution, and 3-chloropropene is added for reaction, then etrabromo bisphenol A diolefine propyl ether is generated, and product is got after separating, washing and drying. Only water is added as reaction solvent, and no organic solvent is added else, organic solvent post processing is reduced in technique, it is mild to environment and is easy for industrial manufacture. The reaction can be heated to higher temperature, so reaction speed is greatly accelerated.

Description

technical field [0001] The invention relates to a chemical synthesis method, in particular to an environment-friendly method for synthesizing tetrabromobisphenol A diallyl ether. Background technique [0002] Tetrabromobisphenol A diallyl ether can be obtained by adding tetrabromobisphenol A and 3-chloropropene to lower aliphatic alcohols (referring to alkanols containing 1 to 3 carbon atoms) for etherification, but this method The solvent needs to be recovered and rectified, and the residual liquid and slag should be discharged. At the same time, after the reaction is finished, a large amount of organic solvents are discharged indiscriminately during centrifugation to bring environmental pollution. Due to the incomplete desolventization and the by-products, further separation is required, which makes the follow-up process complicated. It is especially important that when carrying out tetrabromobisphenol A diallyl ether synthesis with lower aliphatic alcohol as solvent, be...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/01C07C43/225
Inventor 章庚柱李戈华
Owner LIHAI CHEM IND CO LTD OF JIANGSU JINQIAO SALT & CHEM GRP