Flame retardant cyclo-bromoethyl trisilicate compound and preparation method thereof

A flame retardant and compound technology, which is applied in the field of flame retardant Seike trisilicate bromoethyl ester compound and its preparation field, can solve the problems of flammability, fire, life and property safety threats of synthetic polymer materials, etc., and it is difficult to improve The effect of low dispersion and activity, low production cost and high synergistic flame retardant efficiency

Active Publication Date: 2014-02-05
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

[0002] Organic polymer synthetic materials are more and more widely used in daily life, but most synthetic polymer materials are flammable, often cause fires, and pose a serious threat to people's life and property safety. development of fuel technology

Method used

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  • Flame retardant cyclo-bromoethyl trisilicate compound and preparation method thereof
  • Flame retardant cyclo-bromoethyl trisilicate compound and preparation method thereof
  • Flame retardant cyclo-bromoethyl trisilicate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 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 20°C, add 6.25g (3.55ml, 0.05mol) of bromoethanol dropwise, and the dropwise addition process is controlled The reaction temperature is not higher than 30°C. After dripping, raise the temperature to 40°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 to not be higher than 60°C. After the dropping, the temperature was raised to 80°C, and the reaction was carried out for 9 hours; ml, 0.101mol) of bromoetha...

Embodiment 2

[0031]Embodiment 2 In the 25Oml four-neck flask that agitator, thermometer and high-efficiency reflux condensation tube are equipped with, and drying tube is housed on the top of condensation tube, replace the air in the bottle with nitrogen, add 2Oml 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 20°C, add 6.25g (3.55ml, 0.05mol) of bromoethanol dropwise, and the dropwise addition process is controlled The reaction temperature is not higher than 30°C. After dripping, raise the temperature to 40°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 four In the open flask, the reaction temperature is controlled by the dropping rate not to be higher than 60°C. After the drop, the temperature is raised to 85°C and reacted for 8 hours; after the HCl gas is released, the system is cooled to...

Embodiment 3

[0032] 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, cool with a cold water bath to reduce the temperature of the reaction system to below 20°C, add 6.25g (3.55ml, 0.05mol) of bromoethanol dropwise, and control the reaction temperature during the dropwise addition Not higher than 30°C. After dropping, raise the temperature to 40°C, and keep it warm for 2 hours; after the HCl gas is released, dissolve 4.358g (0.0167mol) Cycla in 50ml of acetonitrile into the four-necked flask, Control the reaction temperature not higher than 60°C with the dropping speed, raise the temperature to 80°C after dropping, react for 9 hours, after the HCl gas is released, cool the system down to below 40°C, add dropwise 15.0g (8.51ml,...

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Abstract

The invention relates to a flame retardant cyclo-bromoethyl trisilicate compound and a preparation method thereof. The structure of the compound is represented by a formula shown in a drawing. The preparation method comprises the steps of reacting silicon tetrachloride with bromoethanol of a mole which is equal to that of silicon tetrachloride in an organic solvent at the temperature below 20 DEG C, then, dropwise adding an organic solution of trishydroxyethyl isocyanurate of a mole which is 1 / 3 that of silicon tetrachloride, heating to the temperature of 75-85 DEG C after completing dripping, and reacting for 8-10 hours; then, dropwise adding bromoethanol of a mole which is 2-3 times that of silicon tetrachloride, and carrying out heat-preservation reaction for 7-9 hours at the temperature of 75-85 DEG C; then, adding an acid binding agent, and carrying out heat preservation for 1 hour while stirring; purifying, thereby obtaining the flame retardant cyclo-bromoethyl trisilicate. The compound disclosed by the invention has high flame retarding efficacy and is suitable for serving as a flame retardant for materials, such as polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin and the like, and the preparation method is simple and is low in cost, so that the industrial production is easy to realize.

Description

technical field [0001] The present invention relates to a kind of flame retardant saike bromoethyl trisilicate compound and preparation method thereof, in particular to a kind of flame retardant tris[2-tris(bromoethoxy)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] Organic polymer synthetic materials are more and more widely used in daily life, but most synthetic polymer materials are flammable, often cause fires, and pose a serious threat to people's life and property safety. development of fuel technology. With the improvement of people's living standards and the increasing awareness of environmental protection, more stringent requirements have been put forward for halogenated flame retardants in recent years, that is, they are developing in the direction of high efficienc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/04C08K5/5455C08L27/06
Inventor 王彦林董信
Owner SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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