Flame retardant Cyke bromopropyl trisilicate compound and preparation method thereof

A technology of flame retardant and bromopropanol, which is applied in the field of flame retardant bromopropyl trisilicate compound and its preparation, can solve the problems such as difficult to find substitutes, achieve good symmetry, low volatility, prevent The effect of secondary combustion

Active Publication Date: 2015-11-25
山东产研中科高端化工产业技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the increasing awareness of environmental protection, halogenated flame retardants are under pressure. However, in some fields where halogenated flame retardants are used, it is difficult to find suitable substitutes recently.

Method used

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  • Flame retardant Cyke bromopropyl trisilicate compound and preparation method thereof
  • Flame retardant Cyke bromopropyl trisilicate compound and preparation method thereof
  • Flame retardant Cyke bromopropyl trisilicate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034]Example 1 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, 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 25°C, and dropwise added 6.95g (4.46ml, 0.05mol) of bromopropanol, and the dropwise addition process Control the reaction temperature not to be higher than 30°C. After dripping, raise the temperature to 45°C and keep it warm for 2 hours; after the HCl gas is released, dissolve 4.358g (0.0167mol) Cycla in 50ml of dichloroethane dropwise into the In the four-necked flask, the reaction temperature was controlled by the dropping rate not to be higher than 65°C, and after the dropping was completed, the temperature was raised to 80°C, and the reaction was carried out for 12 hours; ml, 0...

Embodiment 2

[0035] Example 2 In a 250ml four-necked flask equipped with a stirrer, a thermometer and a high-efficiency reflux condensing tube, and a drying tube on the condensing tube, replace the air in the bottle with nitrogen, and 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 25°C, and dropwise added 6.95g (4.46ml, 0.05mol) of bromopropanol, and the dropwise addition process Control the reaction temperature not to be higher than 30°C. After dripping, raise the temperature to 45°C, and keep it warm for 2 hours; after the HCl gas is released, dissolve 4.358g (0.0167mol) Cycla in 50ml of dioxane dropwise 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 the reaction was carried out for 9 hours. ml, 0.11mol) of bromopropanol, the re...

Embodiment 3

[0036] Embodiment 3 In the 250ml four-necked flask that stirrer, thermometer and high-efficiency reflux condenser are equipped with, and drying tube is housed on the condenser upper mouth, replace the air in the bottle with nitrogen, add 20ml acetonitrile and 8.5g (5.67 ml, 0.05mol) of silicon tetrachloride, under stirring, cooled with a cold water bath to reduce the temperature of the reaction system to below 25°C, add 6.95g (4.46ml, 0.05mol) of bromopropanol dropwise, and control the reaction temperature during the dropwise addition Not higher than 30°C, after dropping, raise the temperature to 45°C, and keep it warm for 2 hours; after the HCl gas is released, drop 4.358g (0.0167mol) of Cycla in 50ml of acetonitrile 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 11 hours; after the HCl gas is released, the temperature of the system i...

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Abstract

The invention relates to a flame retardant tris(hydroxyethyl) isocyanurate trisilicate propyl bromide compound and a preparation method thereof. The compound has a structure shown in the specification, wherein -OC3H6Br is 2-bromo-1-propoxy or 1-bromo-2-propoxy or a mixture of the 2-bromo-1-propoxy and the 1-bromo-2-propoxy. The preparation method comprises the following steps: dropwise adding bromopropanol into an organic solution of silicon tetrachloride at a temperature being below 25 DEG C and reacting for 2 hours at 45 DEG C, wherein the molar mass of the bromopropanol is equal to that of the silicon tetrachloride; dropwise adding an organic solution of tris(hydroxyethyl) isocyanurate and reacting for 9-12 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; cooling to the temperature being below 55 DEG C, dropwise adding the bromopropanol, and reacting for 8-10 hours at 80-90 DEG C, wherein the molar mass of bromopropanol is 2-3 times that of the silicon tetrachloride; adding an acid binding agent, preserving heat and stirring for 1 hour; performing purification to obtain the flame retardant tris(hydroxyethyl) isocyanurate trisilicate propyl bromide. The compound disclosed by the invention is suitable to be as the flame retardants of the materials such as polyvinyl chloride, polyurethane, epoxy resin and unsaturated resin, is simple in preparation process and low in cost, and can be put into industrial production easily.

Description

technical field [0001] The present invention relates to a kind of flame retardant Sike bromopropyl trisilicate compound and its preparation method, in particular to a kind of flame retardant tris[2-tris(bromopropoxy)silyloxyethyl]isocyanurate An ester compound and a preparation method thereof, the compound can be used as a flame retardant for materials such as polyvinyl chloride, unsaturated polyester, polyurethane and epoxy resin. Background technique [0002] At present, organic synthetic polymer materials are widely used, and most of them are flammable. According to statistics, most of the fires that have occurred over the years are directly or indirectly related to flammable materials, thus promoting the research of flame retardants or flame retardant materials. Adding flame retardants to materials is an effective way to achieve flame retardancy and fire protection. Traditional halogen-based flame retardants will release harmful gases when materials are burned. With th...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C07F7/04C08K5/5455C08L27/06
Inventor王彦林董信万家明
Owner山东产研中科高端化工产业技术研究院有限公司