以α,ω-二溴代烷、丁基咪唑和三丁基膦为原料经过二步反应合成了3种Bola型非对称阳离子表面活性剂。中间体1-(12-溴十二烷基)-3-丁基咪唑溴盐的较佳合成工艺条件为:n(丁基咪唑)∶n(1,12-二溴十二烷)∶n(四丁基碘化铵)=1∶1.5∶0.005,异丙醇作溶剂,反应温度65℃,反应时间6 h;Bola型表面活性剂的合成工艺条件为:n(1-(12-溴十二烷基)-3-丁基咪唑溴盐)∶n(三丁基膦)=1.05∶1,微波辅助反应,反应温度80℃,反应时间12 h。所合成的Bola型表面活性剂表现出了优良的表面活性,30℃时cmc在5.7×10^-3~8.7×10^-2mol·L^-1之间、γcmc在30~36 m N·m^-1之间;随着碳链长度的增长,其cmc,γ_cmc及分子最小横截面积(A_min)逐渐减小,饱和吸附量(Γ_max)和吸附效率(pc_20)逐渐增大。
The structure of a room temperature asymmetrical dicationic ionic liquid(ADIL), 1-(pyridinium-1-yl) propane-(1-methylpiperidinium) bi[bis(trifluoromethanesulfonyl)imide]([PyC 3Pi][NTf2]2), was studied by the X-ray diffraction method. Meanwhile, thermal analysis of [Py C3Pi][NTf2]2was also studied using non-isothermal thermogravimetric analysis(TGA). The title crystal belongs to the triclinic with space group Pī and unit-cell parameters a = 0.95217(8) nm, b = 1.05129(11) nm, c = 1.70523(14) nm, α = 89.759(8)°, β = 80.657(7)°, γ = 68.007(9)°, and F(000) = 792. Thermal stability and thermal decomposition kinetics of the title compound were also investigated using TGA under the atmosphere of highly pure nitrogen. Heating curves at different rates were correlated with kinetic equations Friedman and ASTM(also called iso-conversion method). The values of average activation E(k J·mol-1) and pre-exponential constant lg A are 149.58 k J·mol-1and 8.83, respectively, which were obtained by the two methods. The kinetic model function, activation energy and pre-exponential constant of this reaction using the multivariate non-linear-regression method were f(α) =(1- α)(1 + 4.1870α), 151.04 k J·mol-1and 8.81, respectively, which were basically consistent with iso-conversion methods.
Jun WangManman WangXuzhao YangWenyuan ZouXiang Chen