Gemini surfactant containing selenium atom in space group and preparation method thereof
A technology of gemini surface and active agent, which is applied in the field of gemini surfactant containing selenium atom in the spacer and its preparation, and achieves the effects of short process, good compatibility and strong biodegradation performance.
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Embodiment 1
[0031] 5.2 g of 1,2-dibromoethane and 30 mL of acetonitrile were added to the flask, and heated to 90°C. After fully stirring, slowly add the acetonitrile solution containing 4.0g N,N-dimethyldodecyl tertiary amine through the constant pressure dropping funnel, control the pH of the system at 10.0 by sodium hydroxide, and continue to react at this temperature for 8 hours . The solvent was removed to obtain intermediate M in 89% yield. Weigh 3.9g of intermediate M, dissolve 0.6g of sodium selenide in 20mL of deionized water, heat to 60°C and stir for reaction for 12 hours. After removing the solvent, the gemini surfactant 12-2-Se-2-12 containing a single selenium atom in the spacer can be obtained by recrystallization with ether, and the yield reaches 90%.
Embodiment 2
[0033] Add 9.5 g of 1-bromo-3-chloropropane and 50 mL of acetonitrile into the flask, and heat to 75°C. After fully stirring, the acetonitrile solution containing 5.4g N, N-dimethyldodecylamidopropyl tertiary amine was slowly added through a constant pressure dropping funnel, and the pH of the system was controlled at 9.6 by potassium hydroxide, and continued at this temperature. The reaction was carried out for 12 hours. The solvent was removed to obtain intermediate M in a yield of 93%. Weigh 6.5g of intermediate M, dissolve 1.0g of disodium diselenide in 40mL of deionized water, heat to 70°C and stir for 18 hours. After removing the solvent, recrystallize with ether / ethyl acetate mixture solvent to obtain the gemini surfactant 12N-3-SeSe-3-12N containing diselenium in the spacer, and the yield reaches 91%.
Embodiment 3
[0035] 2.6 g of 1,4-dichlorobutane and 20 mL of acetonitrile were added to the flask, and heated to 100°C. After fully stirring, slowly add the acetonitrile solution containing 2.8g N,N-diethylhexadecyl tertiary amine through the constant pressure dropping funnel, control the pH of the system at 8.8 by potassium bicarbonate, and continue to react at this temperature for 12 hours . The solvent was removed to obtain intermediate M in 83% yield. Weigh 3.3g of intermediate M, dissolve 0.38g of sodium selenide in 30mL of deionized water, heat to 70°C and stir for reaction for 20 hours. After removing the solvent, the gemini surfactant 16-4-Se-4-16 containing monoselenium in the spacer can be obtained by recrystallization with acetone / ethyl acetate mixture solvent, and the yield reaches 86%.
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