Silylation of saponite with 3-aminopropyltriethoxysilane
Silylation of saponite with 3-aminopropyltriethoxysilane
复制标题
皂石与 3-氨基丙基三乙氧基硅烷的硅烷化
DOI：
10.1016/j.clay.2016.05.026
复制
发表时间：
2016-11
影响因子：
5.6
通讯作者：
Noh Young Dong
中科院分区：
文献类型：
--
作者：
Tao Qi;Fang Yan;Li Tian;Zhang Dan;Chen Manyou;Ji Shichao;He Hongping;Komarneni Sridhar;Zhang Huaibin;Dong Yan;Noh Young Dong
采用水热法合成了一系列Si/Mg比固定、Al含量变化的皂矿（Sap）。采用XRD、FTIR、TG-DTG、TEM、29Si MAS NMR、13C NMR等手段对3-氨基丙基三乙氧基硅烷（APTES）接枝前后的光谱、结构和形貌特征进行了表征。XRD谱图表明，初始Si/Al比分别为5.43和7.89时，得到了有序的Sap。在APTES用量下，硅基化反应对Sap的层状结构几乎没有影响。在2937 cm−1的红外光谱中- 2伸展带的存在清楚地表明接枝样品中掺杂了硅烷。TG-DTG曲线显示，结晶度越高的样品脱羟基温度越高。硅烷化液在420℃左右出现了新的质量损失，这是由于硅烷中烷基的挥发造成的。29si核磁共振光谱显示了一系列的T结构信号，这归因于硅烷和Sap之间不同的硅化模式。此外，硅化过程导致信号强度在约- 84 ppm时下降，而q3信号强度增加。硅烷浓度的进一步增加没有进一步降低−84 ppm下的共振。这一现象证实了q2si （2Al）结构与Q3Si（2Al）结构的共存，这是由于合成Sap边缘表面的键断裂造成的。
A series of saponites (Sap) with a fixed Si/Mg ratio and varied Al contents were synthesized by using hydrothermal methods. The spectral, structural and morphology characters of the obtained products were characterized by a combination of XRD, FTIR, TG-DTG, TEM,29Si MAS NMR,13C NMR etc.before and after 3-aminopropyltriethoxysilane (APTES) grafting. XRD patterns showed that well-ordered Sap were obtained with starting Si/Al ratios of 5.43 and 7.89. Silylation reactions have little or no effect on the layered structure of Sap at the used dosage of APTES. The existence of the –CH2stretching bands at around 2937 cm− 1in IR spectra clearly showed the incorporation of silane in the grafted samples. TG–DTG curves revealed that the samples with higher crystallinity displayed higher dehydroxylation temperature, as expected. A new mass loss located at around 420 °C in silylated Sap was ascribed to the volatilization of the alkyl group in silane. The29Si NMR spectroscopy showed a series of signals of T structures, ascribed to the different silylation modes between silane and Sap. Furthermore, silylation procedures led to a decrease of the intensity of the signals at ca. − 84 ppm along with an increase of the intensity of Q3signals. A further increase in the silane concentration did not decrease the resonance at − 84 ppm any further. This phenomenon confirmed the coexistence of Q2structure with Q3Si(2Al) structure, which resulted from the broken bonds at the edge surfaces of the synthesized Sap.
登录
查看更多内容
DOI：
10.1016/j.msea.2009.07.023
发表时间：
2009-11-25
影响因子：
6.4
作者：
Park, Soo-Jin;Kim, Byung-Joo;Lyu, Yi-Yeol
通讯作者：
Lyu, Yi-Yeol
影响因子：
3.7
作者：
M. Casagrande;L. Storaro;M. Lenarda;S. Rossini
通讯作者：
M. Casagrande;L. Storaro;M. Lenarda;S. Rossini
DOI：
10.1016/s1572-4352(05)x0100-3
发表时间：
2006
期刊：
--
影响因子：
--
作者：
F. Bergaya;B. Theng;G. Lagaly
通讯作者：
F. Bergaya;B. Theng;G. Lagaly
影响因子：
1.7
作者：
Sun Ha Kim;O. Han;Jong Kil Kim;K. Lee
通讯作者：
Sun Ha Kim;O. Han;Jong Kil Kim;K. Lee
影响因子：
2.1
作者：
O. Grauby;S. Petit;A. Decarreau;A. Baronnet
通讯作者：
O. Grauby;S. Petit;A. Decarreau;A. Baronnet