Synthetic method of biquaternary ammonium salt intermediate
A technology of a double quaternary ammonium salt and a synthesis method is applied in the field of synthesis of a double quaternary ammonium salt intermediate, which can solve the problems of active chemical properties, great harm to human health, easy to cause fire and explosion, etc. effect used
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Embodiment 1
[0018] Step 1: Add 129g of 1,3-dichloropropanol into the reactor, start stirring, and add trimethylamine aqueous solution dropwise at a flow rate of 65.5g / h, and keep the temperature of the reactor at 31±1°C during the dropping process.
[0019] Step 2: After 3.02 hours, the dropwise addition is completed, continue to keep the temperature of the reactor at 31±1°C and stir for 1 hour, then steam the reaction solution under reduced pressure at -0.1MPa to obtain the solid bisquaternary ammonium salt intermediate 3-chloro - 180.0 g of 2-hydroxypropyltrimethylammonium chloride.
[0020] After testing, the conversion rate (calculated as trimethylamine) of the product is 94.95%, the content of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride is 99.17%; the content of ammonium salt is 0.15%.
Embodiment 2
[0022] Step 1: Add 130g of 1,3-dichloropropanol into the reactor, start stirring, and add trimethylamine aqueous solution dropwise at a flow rate of 65.5g / h, and keep the temperature of the reactor at 39±1°C during the dropping process.
[0023] Step 2: After 3.02 hours, the dropwise addition is completed, continue to keep the temperature of the reactor at 31±1°C and stir for 1 hour, then steam the reaction solution under reduced pressure at -0.1MPa to obtain the solid bisquaternary ammonium salt intermediate 3-chloro - 180.9 g of 2-hydroxypropyltrimethylammonium chloride.
[0024] After testing, the conversion rate (calculated as trimethylamine) of the product is 95.58%, the content of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride is 99.33%; the content of ammonium salt is 0.10%.
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