DECPP preparation method
A technology of diethylene glycol chloropropyl phosphate and diethylene glycol phosphoryl, applied in the direction of phosphorus organic compounds, etc., can solve problems such as not mentioned
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Embodiment 1
[0036] 1) Add 1.75mol (268.5g) phosphorus oxychloride to a four-neck flask equipped with a thermometer, a constant pressure dropping funnel, a mechanical stirrer, a reflux condenser and a drying tube (connected to a hydrogen chloride suction device), and cool down To 15°C, add 2mol (202g) triethylamine dropwise with a constant pressure dropping funnel, after the dropwise addition, control the temperature at 15-20°C, then add 1mol (106g) diethylene glycol dropwise with a constant pressure dropping funnel, A large amount of white triethylamine hydrochloride solid was produced, and the dripping was completed in about 1.5 hours. After the addition was completed, the reaction was completed by keeping the temperature for 1 hour.
[0037] 2) Use a Buchner funnel to fully filter out the above-mentioned white solid under vacuum conditions to obtain a clear liquid. During the filtration process, the temperature is controlled between 15 and 20°C. Add the above-mentioned filtrate into the...
Embodiment 2
[0042] 1) Add 1.6mol (245g) phosphorus oxychloride to a four-necked flask equipped with a thermometer, a constant pressure dropping funnel, a mechanical stirrer, a reflux condenser and a drying tube (connected to a hydrogen chloride suction device), and cool down to 10°C, use a constant pressure dropping funnel to add 1.8mol triethylamine dropwise, after the dropwise addition, control the temperature at 10-15°C, then add 1mol diethylene glycol dropwise with a constant pressure dropping funnel, there will be a large amount of white triethylamine The hydrochloride solid was produced, and the drop was completed in about 1.5 hours. After the addition was completed, the reaction was completed by keeping the temperature for 1 hour.
[0043] 2) Use a Buchner funnel to fully filter out the above-mentioned white solid under vacuum conditions to obtain a clear liquid. During the filtration process, the temperature is controlled between 16 and 18°C. Add the above-mentioned filtrate into ...
Embodiment 3
[0048] 1) Add 1.9mol (291g) phosphorus oxychloride to a four-necked flask equipped with a thermometer, a constant pressure dropping funnel, a mechanical stirrer, a reflux condenser and a drying tube (connected to a hydrogen chloride suction device), and cool down to 0°C, use a constant pressure dropping funnel to add 3.0mol triethylamine dropwise, after the dropping, control the temperature at 0-5°C, then use a constant pressure dropping funnel to drop 1mol diethylene glycol, there will be a lot of white triethylamine The hydrochloride solid was produced, and the drop was completed in about 1.5 hours. After the addition was completed, the reaction was completed by keeping the temperature for 1 hour.
[0049] 2) Use a Buchner funnel to fully filter out the above-mentioned white solid under vacuum conditions to obtain a clear liquid. During the filtration process, the temperature is controlled between 15 and 20°C. Add the above-mentioned filtrate into the bottle, and feed nitrog...
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