Superbranched polyquaternary ammonium salt and its preparation method
A technology of hyperbranched poly and quaternary ammonium salts, applied in the field of polymer materials, can solve the problems of complicated synthesis process and harsh reaction conditions, and achieve the effects of simple synthesis process, low synthesis cost and high yield
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Embodiment 1
[0021] 1. Synthesis of the hydrochloride salt of N-methylbis(2-chloroethyl)amine: the molar ratio of raw materials is N-methyldiethanolamine:thionyl chloride=1:3. First add 14.4ml of N-methyldiethanolamine into a dry three-necked flask, and then add 80ml of solvent to dry benzene. Cool in an ice water bath. In the case of stirring, use a constant pressure dropping funnel to dissolve 36.6ml of thionyl chloride SOCl 2 Slowly drop into cold N-methyldiethanolamine, in order to prevent SO in the reaction 2 The thionyl chloride escapes too violently, and continuous and effective cooling must be maintained. When thionyl chloride SOCl 2 After dropping completely, remove the ice-water bath, and then heat to reflux for five hours. During the heating process, it can be observed that the reaction solution gradually turns yellow and stratification occurs. After the reaction, the reaction mixture was poured into a beaker, allowed to cool slowly to room temperature, and it was observed t...
Embodiment 2
[0025] 1. Synthesis of the hydrochloride salt of N-methylbis(2-bromoethyl)amine: the molar ratio of raw materials is N-methyldiethanolamine:phosphorus tribromide=1:0.83. First add 20ml of N-methyldiethanolamine into a dry three-necked flask, then add solvent to dry 70ml of benzene. Cool in an ice water bath. While stirring, slowly drop 13.8ml of phosphorus tribromide into cold N-methyldiethanolamine with a constant pressure dropping funnel, and continuous and effective cooling must be maintained during the dropping. When the phosphorus tribromide was completely dropped, the ice-water bath was removed, and the reaction was heated under reflux for seven hours. During the heating process, it was observed that the reaction solution gradually turned yellow and stratified. After the reaction, the reaction mixture was poured into a beaker, allowed to cool slowly to room temperature, and it was observed that white crystals began to precipitate in the solution, and then stood still fo...
Embodiment 3
[0029] 1. Synthesis of the hydrochloride salt of N-tris(2-chloroethyl)amine: the molar ratio of raw materials is triethanolamine:thionyl chloride=1:4. First add 15ml of N-methyldiethanolamine into a dry three-necked flask, then add solvent to dry 90ml of benzene. Cool in an ice water bath. In the case of stirring, use a constant pressure dropping funnel to dissolve 33ml of thionyl chloride SOCl 2 Slowly drop into cold triethanolamine, in order to prevent SO in the reaction 2 The thionyl chloride escapes too violently, and continuous and effective cooling must be maintained. When thionyl chloride SOCl 2 After dropping completely, remove the ice-water bath, and then heat to reflux for six hours. During the heating process, it can be observed that the reaction solution gradually turns yellow and stratification occurs. After the reaction, the reaction mixture was poured into a beaker, allowed to cool slowly to room temperature, and it was observed that white crystals began to ...
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