利用带有巯基的硅烷偶联剂对Fe3O4@SiO2 粒子进行表面巯基修饰.采用Frens法制备纳米金胶体,通过纳米金与巯基之间的配位作用,将纳米金附着在磁性纳米粒子的表面,制得磁性纳米催化剂.采用激光粒度仪检测Fe3O4 粒子、Fe3O4@SiO2 粒子及磁性纳米催化剂的粒径.用5,5′-二硫基-双(二硝基苯甲酸)试剂检测纳米粒子表面的巯基密度,并研究了温度对磁性纳米催化剂的催化活性的影响.结果表明:Fe3O4 粒子的粒径约为 251 nm,被SiO2 包覆的Fe3O4 粒子粒径约为 300 nm,而磁性纳米催化剂的粒径约为336 nm.巯基化磁性纳米粒子的表面巯基密度为3.54×10-6 mol/m2.升高温度对催化反应有促进作用,室温下对硝基苯酚的催化还原反应在35 min内完成,而70℃下5 min内即可完成.
以罗丹明B(RhB)、水合肼、苯甲醛为原料,通过两步反应合成了一种新型罗丹明B类荧光探针RhB-P,并利用傅里叶红外变换光谱与核磁共振氢谱对RhB-P的分子结构进行表征.紫外-可见光谱和荧光光谱表明:在V(乙腈):V(水)=1:1溶液中,RhB-P对Fe3+具有良好的选择性,溶液可从无色转变至粉色.荧光滴定实验以及Job's实验结果表明:络合物中n(RhB-P):n(Fe3+)=1:1,且络合物的荧光强度在c(Fe3+)为0.1μmol/L~20μmol/L区间范围内,与其呈正线性关系,检出限为0.193μmol/L.
Iron oxide nanoparticles were prepared by hydrothermal method,and were coated with silica layer by a St?ber process. The silica-coated magnetic nanoparticles were modified with thiol groups with 3-mercaptopropyltrimethoxysilane,and gold nanoparticles were then immobilized on the surface to fabricate the magnetic nanocatalyst. The prepared magnetic catalyst was characterized by X-ray diffraction,transmission electron microscopy and Fourier transform infrared spectroscopy,and its catalytic performance was investigated through the reduction of p-nitrophenol. The results showed that the average diameter of magnetic nanocatalyst was about 323 nm. The reduction of p-nitrophenol was completed in 6 min under the optimal experimental conditions. The catalyst was easily recycled with a magnet,and its catalytic efficiency kept higher than 92% after 8 times of recycling use.
Magnesium hydroxide was prepared by using di-n-butylamine as a precipitating agent instead of the traditional inorganic basic precursor. The reaction conditions were optimized by employing the single variable method. The morphology and particle size of the obtained magnesium hydroxide were characterized, and its anti?flaming mechanism was investigated. The results show that the optimal experimental conditions for the prepara?tion of magnesium hydroxide are as follows:reaction temperature of 70℃, reaction time of 50 minutes, and stir?ring rate of 400 r/min. The magnesium hydroxide has a form of lamellar crystal with an average diameter of 1.8μm, and its performances meet the industrial requirements. The precipitant can be recovered and recycled, thus this method is expected to improve the traditional technology for magnesium hydroxide preparation. The results of thermal gravimetric analysis and simulated combustion test suggest that the antiflaming mechanism of magne?sium hydroxide can be ascribed to:it improves the thermal decomposition temperature of the used materials, and the magnesium oxide produced by the decomposition of magnesium hydroxide with the carbon forms a layer to achieve thermal insulation and oxygen exclusion.
采用对苯二胺和丙烯酸甲酯为原料经迈克尔加成反应合成了多官能团化合物N,N,N ',N'-四丙酸甲酯-1,4-苯二胺.以该化合物和乙二胺为单体,通过熔融聚合-溶液聚合联用的方法,制备了耐热性好、水溶性高的芳香族超支化聚酰胺胺材料.利用傅立叶变换红外光谱和核磁共振氢谱对所合成的产物进行结构表征.以布洛芬为客体小分子,研究了芳香族超支化聚酰胺胺化合物对其在水中的增溶效果.结果表明,布洛芬的溶解度随超支化聚合物浓度增加而增加,2mg/mL聚合物可提升布洛芬溶解度20倍.