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Environment-friendly method for preparing high thermal decomposition temperature octobromo ether

An environment-friendly, decomposition temperature technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as easy agglomeration, low thermal decomposition temperature of finished products, and potential safety hazards

Active Publication Date: 2006-10-25
LIHAI CHEM IND CO LTD OF JIANGSU JINQIAO SALT & CHEM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] The existing industrial preparation method of octabromoether is to dissolve tetrabromobisphenol A diallyl ether in a chlorinated hydrocarbon solvent, then carry out bromine addition reaction with bromine, neutralize and reduce reaction with sodium sulfite and NaOH after the reaction Excessive amount of bromine, and then washed with water to obtain octabromoether chlorinated hydrocarbon organic solution, this organic solution is moved to a crystallization kettle filled with lower aliphatic alcohols (referring to alkanols containing 1 to 3 carbon atoms), octabromoether It will be crystallized and precipitated in alcohol, and the finished product will be obtained by centrifugal separation, drying and crushing; however, the resulting product has a low thermal decomposition temperature and poor thermal stability, which will cause coloring of the material during material processing; it is easy to agglomerate when stored for a long time. need to be crushed before
When reducing and neutralizing excess bromine, bromine cannot be reused, resulting in waste of resources and certain environmental impacts. At the same time, in the process of crystallization and precipitation of octabromoether, a large amount of methanol or ethanol is used for subsequent centrifugation, drying and other operating units. It brings great safety hazards, and the solvent entrained in the octabromoether filter cake volatilizes without organization during centrifugation, causing environmental pollution

Method used

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  • Environment-friendly method for preparing high thermal decomposition temperature octobromo ether

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Experimental program
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Effect test

Embodiment 1

[0013] In a 500ml glass flask equipped with an anchor stirrer, a dropping funnel, and a condenser, add 80 g of tetrabromobisphenol A diallyl ether and 180 g of chloroform with a purity greater than 98%, until tetrabromobisphenol A diallyl After the base ether is completely dissolved, add 43g of dry bromine dropwise to the flask. After the dropwise addition of bromine is completed within 2h, continue the reaction for 2.5h. 2.25g~2.5g of 80% hydrazine hydrate makes the pH value of the mother liquor in the flask 6~7. Move all the mother liquor in the flask to a separatory funnel and let it stand, move the organic solution of chloroform and octabromoether in the lower layer to a 500ml glass flask equipped with an anchor stirrer, add a substantially equal volume of deionized water and stir for 3 to 5 minutes Then stop stirring; the upper layer of the aqueous solution of hydrazine bromide in the separatory funnel was moved to a special container for containing hydrazine bromide.

...

Embodiment 2

[0016] Except using 200g methylene chloride as the reaction solvent, 0.1g sorbitol instead of glycidyl isocyanurate, and adopting atmospheric distillation during crystallization, the others are the same as in Example 1. When the temperature in the crystallization bottle reached 60°C, the material in the crystallization bottle became viscous, and when the recovery of dichloromethane reached 93%, the viscosity of the viscous material in the crystallization bottle decreased, and octabromoether crystallized out, and continued to heat up to At 75°C, the remaining dichloromethane is basically recovered by distillation, cooled to below 40°C, and the mixture of octabromoether and water in the crystallization bottle is suction filtered and washed with deionized water, and the filter cake is dried at about 80°C until it weighs constant 117.8 g of octabromoether was recovered, with a yield of 97.3%, a purity of 98.1% by liquid chromatography, and a thermal decomposition temperature of 274...

Embodiment 3

[0018] Except that 210g of benzene was used instead of chloroform as the reaction solvent, and 0.02g of alkylphenol polyglycol ether phosphate was used instead of polyoxyethylene propylene ether, the others were the same as in Example 1, and the obtained octabromoether weighed 116.1g, with a yield of 96%. The purity by liquid chromatography analysis is 97.4%, and the thermal decomposition temperature is 269°C to 273°C.

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Abstract

This invention relates to good environment preparing high thermal decomposition temperature eight bromo ether methods. Tetrabromo bisphenol A diolefine propyl ether is dissolved in organic solvent, bromine is added for reaction, hydrazine hydrate is used to revert excess bromine after reaction, then standing, eight bromo ether solution at low player is washed and emulsifying agent, auxiliary agent, seed crystaland deionized water are added, then temperature sing and exsolution, the eight bromo ether is separated, washed and dried. Auxiliary agent is used in this invention; the product thermal decomposition temperature is risen near 50 degrees centigrade compare to normal sale. There is no need of solvent carrier of the product, and it is hard agglomeration for long time storage, special reducer is used and excess bromine is used again. Water is used as crystal decant precipitator of eight bromo ether crystallization, post processing unit safety after crystallization is ensured.

Description

technical field [0001] The invention relates to a chemical synthesis method, in particular to an environmentally friendly method for preparing octabromoether with high thermal decomposition temperature. Background technique [0002] The scientific name of octabromoether is tetrabromobisphenol A bis(2,3-dibromopropyl) ether, and its structural formula is: [0003] [0004] The existing industrial preparation method of octabromoether is to dissolve tetrabromobisphenol A diallyl ether in a chlorinated hydrocarbon solvent, then carry out bromine addition reaction with bromine, neutralize and reduce reaction with sodium sulfite and NaOH after the reaction Excessive amount of bromine, and then washed with water to obtain octabromoether chlorinated hydrocarbon organic solution, this organic solution is moved to a crystallization kettle filled with lower aliphatic alcohols (referring to alkanols containing 1 to 3 carbon atoms), octabromoether It will be crystallized and precipit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/22C07C43/225
Inventor 章庚柱李戈华
Owner LIHAI CHEM IND CO LTD OF JIANGSU JINQIAO SALT & CHEM GRP
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