Flame retardant chlorobromopropyl trisilicate compound and preparation method thereof

A flame retardant, chlorobromopropoxy technology is applied in the field of flame retardant tris[2-trisilyloxyethyl]isocyanurate compound and its preparation, and can solve the problems of difficulty in finding substitutes and the like , to achieve the effect of overcoming the volatile reaction, good plasticity and low production cost

Active Publication Date: 2015-12-30
SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high cost performance of halogenated flame retardants, the application technology is very mature, and it is still difficult to find suitable substitutes in many application fields.

Method used

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  • Flame retardant chlorobromopropyl trisilicate compound and preparation method thereof
  • Flame retardant chlorobromopropyl trisilicate compound and preparation method thereof
  • Flame retardant chlorobromopropyl trisilicate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condensing tube, and a drying tube at the top of the condensing tube, replace the air in the bottle with nitrogen, add 20ml of dioxane and 8.5 g (5.67ml, 0.05mol) of silicon tetrachloride, under stirring, cooled with a cold water bath to lower the temperature of the reaction system below 30°C, dropwise added 13.70g (8.56ml, 0.1mol) of epibromohydrin, and added dropwise The process control reaction temperature is not higher than 40°C. After the dripping is completed, the temperature is raised to 50°C, and the heat preservation reaction is carried out for 2 hours; the solution of 4.358g (0.0167mol) Cycla dissolved in 50ml of dioxane is dropped into the four-necked flask to The rate of addition controls the reaction temperature not to be higher than 65°C. After the drop is completed, the temperature is raised to 95°C and reacted for 9 hours. After the HCl gas is released...

Embodiment 2

[0029]Example 2 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and a drying tube at the top of the condenser, replace the air in the bottle with nitrogen, add 20ml of dichloroethane and 8.5 g (5.67ml, 0.05mol) of silicon tetrachloride, under stirring, cooled with a cold water bath to lower the temperature of the reaction system below 30°C, dropwise added 13.70g (8.56ml, 0.1mol) of epibromohydrin, and added dropwise The process control reaction temperature is not higher than 40°C. After the drop is completed, the temperature is raised to 50°C, and the heat preservation reaction is carried out for 2 hours; the solution of 4.358g (0.0167mol) Cycla dissolved in 50ml of dichloroethane is dropped into the four-necked flask to The rate of addition controls the reaction temperature not to be higher than 65°C. After the drop is completed, the temperature is raised to 80°C and reacted for 13 hours. After the HCl gas is released, ...

Embodiment 3

[0030] Example 3 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and a drying tube on the upper mouth of the condenser, replace the air in the bottle with nitrogen, and add 20ml of diethylene glycol dimethyl Ether and 8.5g (5.67ml, 0.05mol) silicon tetrachloride, under stirring, cool with cold water bath, make reaction system temperature drop below 30 ℃, dropwise add 13.70g (8.56ml, 0.1mol) epibromohydrin , the dropping process controls the reaction temperature not to be higher than 40°C. After the dropping, the temperature is raised to 50°C, and the heat preservation reaction is carried out for 2 hours; a solution of 4.358g (0.0167mol) of Saike dissolved in 50ml of diethylene glycol dimethyl ether is dropped into the In the four-necked flask, the reaction temperature was controlled by the dropping rate to not be higher than 65°C. After the dropping, the temperature was raised to 90°C and reacted for 10 hours. After the ...

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Abstract

The invention relates to a flame retardant tris(hydroxyethyl) isocyanurate trisilicate propyl chloride-bromine compound and a preparation method thereof. The compound has a structure shown in the specification, wherein m is an integer from 0 to 3. The preparation method comprises the following steps: dropwise adding epibromohydrin into an organic solution of silicon tetrachloride at a temperature being below 30 DEG C and reacting for 2 hours at 50 DEG C, wherein the molar mass of the epibromohydrin is 2 times that of the silicon tetrachloride; dropwise adding an organic solution of tris(hydroxyethyl) isocyanurate and reacting for 9-13 hours at 80-95 DEG C, wherein the molar mass of the organic solution of the tris(hydroxyethyl) isocyanurate is 1 / 3 that of the silicon tetrachloride; dropwise adding the epibromohydrin and reacting for 4-7 hours at 70-90 DEG C, wherein the molar mass of the epibromohydrin is 1-1.5 times that of the silicon tetrachloride; performing purification treatment to obtain the tris(hydroxyethyl) isocyanurate trisilicate propyl chloride-bromine. The flame retardant contains four flame retardant elements including silicon, nitrogen, chlorine and bromine, is suitable to be used as flame retardants of the materials such as polyvinyl chloride, polyurethane, epoxy resin and unsaturated resin, is high in synergistic flame retardant performance, simple in preparation process and low in cost, and can be put into industrial production.

Description

technical field [0001] The invention relates to a flame retardant chlorobromopropyl trisilicate compound and a preparation method thereof, in particular to a flame retardant tris[2-tris(chlorobromopropoxy)silyloxyethyl]iso The invention relates to a cyanurate compound and a preparation method thereof. The four elements of the compound silicon, nitrogen, chlorine and bromine have high synergistic flame retardant performance, and are suitable for use as a flame retardant for materials such as polyvinyl chloride, polyurethane, epoxy resin and unsaturated resin. Background technique [0002] With the successive promulgation of national flame retardant legislation, industry directives and the increase in international trade, the consumption of flame retardants has grown rapidly, especially the more urgent demand for new, efficient and environmentally friendly flame retardants. Halogenated flame retardants are the most widely used organic flame retardants with the highest comprehe...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C07F7/04C08L27/06C08K5/544
Inventor王彦林王玉霞董信
OwnerSHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD