Long Alkyl Chain Organophosphorus Coupling Agents for in Situ Surface Functionalization by Reactive Milling
Long Alkyl Chain Organophosphorus Coupling Agents for in Situ Surface Functionalization by Reactive Milling
复制标题
DOI：
10.3390/inorganics2030410
复制
发表时间：
2014-09-01
期刊：
影响因子：
2.9
通讯作者：
Kickelbick, Guido
中科院分区：
文献类型：
--
作者：
Betke, Annika;Kickelbick, Guido
创新的合成方法应当简单和无害环境。在这里，我们提出了表面改性的无机亚微米粒子与长烷基链有机磷偶联剂，而不需要一个溶剂，这使得该技术环境友好。此外，在一个步骤中实现两个目标是非常有益的：尺寸减小，同时，表面功能化。采用自上而下的原位表面功能化方法合成了金属氧化物颗粒，并用长烷基链有机磷偶联剂对二氧化钛进行了改性。以二氧化钛为无机颜料，长烷基有机磷偶联剂十二烷基膦酸和十八烷基膦酸为偶联剂，采用高能行星式球磨机进行反应球磨。通过红外光谱、核磁共振谱、X射线荧光光谱、热分析、元素分析、X射线粉末衍射和扫描电子显微镜对产物进行了表征。该过程需要从起始材料的摩擦化学相转化为高压改性的二氧化钛和结晶更稳定的金红石，这取决于工艺参数。此外，颗粒显示出100 nm至300 nm的尺寸和高达0.8 mmol膦酸盐/g的表面覆盖度。
Innovative synthetic approaches should be simple and environmentally friendly. Here, we present the surface modification of inorganic submicrometer particles with long alkyl chain organophosphorus coupling agents without the need of a solvent, which makes the technique environmentally friendly. In addition, it is of great benefit to realize two goals in one step: size reduction and, simultaneously, surface functionalization. A top-down approach for the synthesis of metal oxide particles with in situ surface functionalization is used to modify titania with long alkyl chain organophosphorus coupling agents. A high energy planetary ball mill was used to perform reactive milling using titania as inorganic pigment and long alkyl chain organophosphorus coupling agents like dodecyl and octadecyl phosphonic acid. The final products were characterized by IR, NMR and X-ray fluorescence spectroscopy, thermal and elemental analysis as well as by X-ray powder diffraction and scanning electron microscopy. The process entailed a tribochemical phase transformation from the starting material anatase to a high-pressure modification of titania and the thermodynamically more stable rutile depending on the process parameters. Furthermore, the particles show sizes between 100 nm and 300 nm and a degree of surface coverage up to 0.8 mmol phosphonate per gram.