Flame retardant ethylenedioxy dual-silicate propyl bromide and preparation method thereof

A flame retardant and compound technology, which is applied in the field of flame retardant bis[trisilyloxy]ethane compound and its preparation, can solve the problems such as difficulty in finding substitutes, and achieve good symmetry, low volatility, and relative good capacitive effect

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

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 ethylenedioxy dual-silicate propyl bromide and preparation method thereof
  • Flame retardant ethylenedioxy dual-silicate propyl bromide and preparation method thereof
  • Flame retardant ethylenedioxy dual-silicate propyl bromide and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033]Embodiment 1 In the 250ml four-necked flask that stirrer, thermometer and high-efficiency reflux condenser are housed, and drying tube is housed on the condenser upper mouth, replace the air in the bottle with nitrogen, add 60ml carbon tetrachloride and 17g (11.47ml, 0.1mol) silicon tetrachloride, under stirring, cool with cold water bath, make reaction system temperature drop below 25 ℃, dropwise add 13.9g (8.92ml, 0.1mol) bromopropanol, dropwise process control The reaction temperature is not higher than 30°C. After dropping, raise the temperature to 45°C and keep the temperature for 2 hours; The dropping rate controls the reaction temperature not to be higher than 50°C. After the dropping, the temperature is raised to 55°C and reacted for 10 hours; after the HCl gas is released, the temperature of the system is lowered to below 40°C, and 27.939g (17.93ml, 0.201mol) of bromine is added dropwise Propanol, control the reaction temperature not higher than 55°C with the dr...

Embodiment 2

[0034] Example 2 In a 250ml four-necked flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and a drying tube on the condenser, replace the air in the bottle with nitrogen, add 60ml of acetonitrile and 17g (11.47ml , 0.1mol) silicon tetrachloride, under stirring, cool with a cold water bath, make the reaction system temperature drop below 25 ℃, dropwise add 13.9g (8.92ml, 0.1mol) bromopropanol, dropwise process control reaction temperature not If the temperature is 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 3.1g (2.78ml, 0.05mol) of ethylene glycol into the four-necked flask, controlled by the dropping rate The reaction temperature was not higher than 50°C. After the dropwise addition, the temperature was raised to 60°C and reacted for 9 hours; after the HCl gas was released, the temperature of the system was lowered to below 40°C, and 29.19g (18.73ml, 0.21mo...

Embodiment 3

[0035] 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, add 60ml of dioxane and 17g (11.47ml, 0.1mol) silicon tetrachloride, under stirring, cool with cold water bath, make reaction system temperature drop below 25 ℃, dropwise add 13.9g (8.92ml, 0.1mol) bromopropanol, dropwise process control The reaction temperature is not higher than 30°C. After dropping, raise the temperature to 45°C and keep the temperature for 2 hours; The dropping rate controls the reaction temperature not to be higher than 50°C. After the dropping, the temperature is raised to 70°C and reacted for 7 hours; after the HCl gas is released, the system is cooled down to below 40°C, and 30.58g (19.62ml, 0.22mol) of bromine is added dropwise For propanol, the reaction temperature should not be higher than 55°C at the rate of addition. After the d...

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Abstract

The invention relates to a flame retardant ethylenedioxy dual-silicate propyl bromide compound and a preparation method thereof. The compound has the structure shown as the formula specified 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 ethylene glycol and reacting for 6-10 hours at 55-75 DEG C, wherein the molar mass of the ethylene glycol is 0.5 time that of the silicon tetrachloride; cooling to the temperature being below 40 DEG C, dropwise adding the bromopropanol, and reacting for 6-10 hours at 65-85 DEG C, wherein the bromopropanol is 2-3 times that of the silicon tetrachloride; adding a small amount of acid binding agent, preserving heat and stirring for 1 hour; performing purification to obtain the flame retardant ethylenedioxy dual-silicate 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 invention relates to a flame retardant ethylenedioxyethylene disilicate bromopropyl ester compound and a preparation method thereof, in particular to a flame retardant bis[tris(bromopropoxy)silyloxy]ethane compound and its preparation method. The preparation method, 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 the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/04C08K5/5415C08L27/06
Inventor 王彦林董信刘芳
Owner SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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