2-(3-broMopropoxy)-2(2-dicholoropropoxy) silane compound used as fire retardant and preparation method thereof
A technology of tribromophenoxy and dichloropropoxy, which is applied in the direction of silicon organic compounds, can solve problems such as difficulty in finding substitutes, and achieve the effects of easy purification and separation, low production cost, and stable physical and chemical properties
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[0032] Example 1 In a 500ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel, a high-efficiency reflux condenser, and a hydrogen chloride absorption device connected in series with a drying tube at the top of the condenser, the air in the flask was replaced with nitrogen , Add 150ml diethylene glycol dimethyl ether and 16.99g (0.1mol) silicon tetrachloride, while stirring, cool with an ice-water bath to reduce the temperature of the reaction system to 0℃, and add drops to the organic solution of silicon tetrachloride Add 12.90g (0.1mol) 2,3-dichloro-1-propanol, and control the temperature under 8℃ during the dripping process. After dripping, the temperature is raised to 35℃ for 1h, and the reaction is kept for 1h. After the hydrogen chloride is released, add again 66.16g (0.2mol) tribromophenol, heat up to 90℃, keep for 4h, after the hydrogen chloride is released, cool down to below 40℃, then add 12.90g (0.1mol) 2,3-dichloro-1-propanol dropwise , Use ...
Example Embodiment
[0033] Example 2 In a 500ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel, a high-efficiency reflux condenser and a hydrogen chloride absorption device connected in series with a drying tube at the top of the condenser, the air in the flask was replaced with nitrogen , Add 150ml of ethylene glycol dimethyl ether and 16.99g (0.1mol) of silicon tetrachloride, while stirring, cool with an ice water bath to reduce the temperature of the reaction system to 0℃, and add dropwise to the organic solution of silicon tetrachloride 12.90g (0.1mol) 2,3-dichloro-1-propanol, the temperature of the dripping process is controlled below 8℃, after dripping, the temperature is raised to 35℃ for 1h, and the reaction is kept for 1h. After the hydrogen chloride is released, 66.16 is added. g(0.2mol) tribromophenol, heat up to 75℃, keep reaction for 5.5h, after the hydrogen chloride is released, cool to below 40℃, then add 12.90g(0.1mol) 2,3-dichloro-1-propanol dropwise ,...
Example Embodiment
[0034] Example 3 In a 500ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel and a high-efficiency reflux condenser, and a hydrogen chloride absorption device connected in series with a drying tube at the top of the condenser, the air in the flask was replaced with nitrogen , Add 150ml dioxane and 16.99g (0.1mol) silicon tetrachloride, cool with an ice-water bath while stirring, reduce the temperature of the reaction system to 0°C, add 12.90g dropwise to the organic solution of silicon tetrachloride (0.1mol) 2,3-Dichloro-1-propanol, the temperature of the dripping process is controlled below 8℃, after dripping, the temperature is raised to 35℃ for 1h, and the reaction is kept for 1h. After the hydrogen chloride is released, add 66.16g ( 0.2mol) tribromophenol, heat up to 80℃, keep the temperature for 5h, after the hydrogen chloride is released, cool down to below 40℃, then add 12.90g (0.1mol) 2,3-dichloro-1-propanol dropwise to The acceleration contro...
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