Quaternary amination organic phosphine surfactant and synthetic method thereof
A surfactant and organic phosphine technology, applied in the field of quaternized organic phosphine cationic surfactants and their synthesis, can solve the problems of complicated separation procedures
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[0085] The present invention also provides the synthetic method of described quaternized organic phosphine surfactant, adopts two-step method, concrete steps are as follows:
[0086] 1. Synthesis of Halogenated Organophosphine
[0087] After mixing the alkyl phosphite and the dihaloalkane uniformly according to the molar ratio of 1: (0.1-50), react at a temperature of 50-200° C. for 1-48 hours, and cool to room temperature after the reaction is completed. Then the product is distilled at a relative pressure of 0.2-50mmHg, and the halogenated organic phosphine is isolated;
[0088] 2. Synthesis of quaternized organic phosphine surfactant
[0089] The halogenated organic phosphine obtained in step (1), tertiary ammonia reagent, organic solvent, catalyst are mixed according to the molar ratio of 1: (0.1~10): (5~50): (0.01~4), at a temperature of React at 40-200°C for 1-72 hours, and cool to room temperature after the reaction. Then the product is distilled under reduced pressu...
Embodiment 1
[0093] Embodiment 1: the synthesis of the compound of following structural formula:
[0094]
[0095] Weigh 20 g of trimethyl phosphite and 125.3 g of ethylene dichloride in a round bottom flask. The reaction is carried out under the constant temperature control of an oil bath. The reaction system is continuously fed with nitrogen protection, and the temperature is raised to 100 ° C. The reaction is stirred for 24 hours. Then cool to room temperature. Then the product was distilled under reduced pressure at 85° C. under a pressure of 10 mmHg to remove unreacted ethylene dichloride to obtain 17.8 g of a reddish-brown liquid intermediate product chloroethyl phosphate (molecular weight: 172.55 g / mol).
[0096] Weigh 12g dimethyl chloroethyl phosphate, 41.4g N, N-dimethyloctadecylamine, 0.5g NaI, and 64g ethanol in a round-bottomed flask, protect the reaction system with nitrogen, and control the temperature in an oil bath The reaction was stirred at 80° C. for 48 h, and coole...
Embodiment 2
[0098] Weigh 2 g of trimethyl phosphite and 79.8 g of dichloroethane in a round-bottomed flask. The reaction is carried out under constant temperature control of an oil bath. The temperature is raised to 50 ° C, and the reaction is stirred for 48 hours. The reaction system is continuously fed with nitrogen protection. Then cool to room temperature. Then the product was distilled under reduced pressure at 85° C. under a pressure of 50 mmHg to remove unreacted dichloroethane to obtain 1.34 g of an intermediate product, dimethyl chloroethyl phosphate.
[0099] Weigh 1.2g dimethyl chloroethyl phosphate, 4.14g N,N-dimethyloctadecylamine, 1.62g NaCl, and 6g ethanol in a round bottom flask, protect the reaction system with nitrogen, and keep the temperature in an oil bath The reaction was stirred at 80° C. for 48 h, and then cooled to room temperature. Then the product was distilled under normal pressure at 80°C, further heated to 150°C, and subjected to vacuum distillation under 2m...
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