苯基化纳米MCM-41材料的制备与表征
Preparation and Characterization of Phenylated Nanometer MCM-41 Material
作者单位
翟庆洲 长春理工大学纳米技术研究中心长春 130022 
刘 磊 长春理工大学纳米技术研究中心长春 130022 
李晓东 长春理工大学纳米技术研究中心长春 130022 
胡伟华 长春理工大学纳米技术研究中心长春 130022 
摘要: 以苯基三甲氧基硅烷为偶联剂对纳米MCM-41分子筛进行了有机改性,制备了苯基改性的纳米MCM-41分子筛MCM-41(m)。利用元素分析、粉末XRD、傅里叶变换红外光谱、氮气吸附-解吸附、扫描电镜和差热-热重分析对制备产物进行了表征。粉末XRD结果表明,改性过程中,分子筛骨架未被破坏,并且所制备MCM-41(m)分子筛结晶度依然很高;傅里叶变换红外光谱表明苯官能团已经成功地接枝到了分子筛的孔道表面,且所得产物的骨架依然完好;低温氮气吸附-解吸附分析结果表明,MCM-41(m)分子筛孔道具有高度有序性,改性的纳米MCM-41分子筛孔道内的硅羟基与苯基三甲氧基硅烷发生了硅烷化反应,苯基成功地接枝到了分子筛的孔道表面。扫描电镜结果表明, 制得的苯基改性纳米MCM-41平均尺寸为110 nm。差热-热重分析结果说明了所制备的苯基化的纳米MCM-41样品具有良好的热稳定性,骨架稳定温度为823 ℃。苯基化的纳米MCM-41材料具有作为催化剂材料的潜在应用前景。
关键词: 纳米MCM-41分子筛  苯基三甲氧基硅烷  苯基化  表征
基金项目: 
Abstract: Nanometer molecular sieve MCM-41 was modified by using phenyltrimethoxysilane as a coupling agent and phenylated nanometer molecular sieve MCM-41(m) was prepared. The prepared product was characterized by means of element analysis, powder X-ray diffraction(XRD), Fourier transform infrared (FTIR) spectroscopy, low-temperature nitrogen adsorption-desorption technique, scanning electron microscopy(SEM) and thermogravimetry-differential thermal analysis(TG-DTA) methods. The powder XRD results showed that during the process of modification the frameworks of the molecular sieve were not destroyed. The crystallinity of the prepared MCM-41(m) is still very high. FTIR spectra showed that phenyl functional group was successfully grafted to the surface of channels of the molecular sieve and the framework of the obtained product is still full and good. The low-temperature nitrogen adsorption-desorption analytical results showed that the channels of the MCM-41(m) has a high ordered property. The reaction of silanization between the silanols in the channels of the modified nanometer MCM-41 molecular sieve and the phenyltrimethoxysilane occurs. The phenyl group was successfully grafted to the surface of channels of the molecular sieve. The SEM results showed that the average size of the prepared phenyl group modified nanometer MCM-41 was 110 nm. The TG-DTA analytical results showed that the prepared phenylated nanometer MCM-41 sample has a good thermal stability. The stable temperature of the framework is 823 ℃. The phenylated nanometer MCM-41 material has a potential application foreground as a catalyst.
Keywords: nanometer MCM-41 molecular sieve  phenyltrimethoxysilane  phenylation  characterization
 
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翟庆洲,刘 磊,李晓东,胡伟华.苯基化纳米MCM-41材料的制备与表征[J].无机化学学报,2009,25(4):679-684.
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