双十四直链烷基二苯甲烷双磺酸盐的合成及性能

实验以二苯甲烷和酰氯为原料,在催化剂作用下,合成双酰基二苯甲烷,经克莱门森还原成双烷基二苯甲烷,以氯磺酸磺化得到双烷基二苯甲烷双磺酸,再以NaOH溶液中和,制成双直链烷基二苯甲烷双磺酸钠Gemini表面活性剂。在酰基化反应中,n(二苯甲烷):n(酰氯):n(无水氯化铝):n(硝基甲烷)=1:2.5:3.2:6.5,首先在常温下反应24 h,然后在70℃反应6 h,收率93.4%;在克莱门森还原反应中,n(酰基二苯甲烷):n(锌粉):n(浓盐酸)=1:10:50,反应温度105℃,反应时间8 h,收率91%;在磺化反应中,n(烷基二苯甲烷):n(氯磺酸):n(氯仿)=1:2:14,反应时间6 h,收率90%。对中间体进行了红外光谱、核磁共振氢谱分析,对最终产物进行了红外光谱、质谱分析.同时还测定了其水溶液的油水界面张力、表面张力及临界胶束浓度、泡沫性和乳化力。结果表明,产物具有7.22×10~(-3)mN/m的超低界面张力。

SYNTHESIS AND PROPERTIES OF 4,4'-DI(N-TETRADECYL) DIPHENYLMETHANE DISULFATE SALT

The Gemini surfactant,4,4'-di(n-tetradecyl) diphenyl methane disulfate salt,has been obtained through four steps.First,diacyl diphenylmethane was produced by using diphenylmethane and acyl chloride as raw materials in a Friedel-Crafts acylation reaction in the presence of a catalyst.Then by means of Clemmensen reduction,sulfonation with chlorosulfuric acid and neutralization with NaOH aqueous solution,the final product was synthesized.In the acylation reaction,diphenyl methane, chloride,anhydrous aluminum chloride and nitromethane (molar ratio 1:2.5:3.2:6.5) first reacted for 24 h at room temperature and then heated to 70℃ for 6 h(yield 93.4%).In the Clemmensen reduction reaction,acyl-diphenylmethane,zinc and HCl (molar ratio 1:10:50) reacted for 8 h at 105℃ (yield 91%).In the sulfonation reaction,alkyldiphenylmethane,acid chloride and chloroform (molar ratio 1:2:14) reacted for 6 h (yield 90%).The structures of the intermediate products were analyzed by ~1H NMR and IR spectrometry.The final product was analyzed by IR spectrometry and mass spectrometry.The oil-water interfacial tension,surface tension and cmc of the aqueous solution, foam property and the emulsifying power were also measured.The results indicated that the Gemini surfactant exhibits an ultra-low interfacial tension of 7.22×10~(-3) mN/m.