埃洛石纳米管碱活化改性探究本文导读：这是一篇关于埃洛石纳米管碱活化改性探究的文章,近年来，随着硅酸盐矿物资源在功能材料和环境保护领域的广泛应用，以硅铝酸盐矿物为原料制备功能矿物材料已成为无机非金属材料加工领域的研究热点 摘 要 硅酸盐矿物种类多、分布广，拥有独特的结构和性质，享有"万能土";的美誉将天然粘土矿物进行改性加工处理，改变其晶体结构和表面化学性质，从而产生具有新型结构和性能的改性材料，是制备新型材料的一个重要途径埃洛石纳米管（HNTs）是一种天然的 1:1 型硅酸盐粘土矿物，具有成本低廉、高强度、耐腐蚀性的天然优势将其改性处理后，可制备出低成本，高性能的 HNTs复合材料，其开发与应用成为当今研究的热点 本论文通过对 HNTs 进行碱活化改性，改变 HNTs 的晶体结构，增加纳米管的比表面积、孔体积和羟基活性位点，同时在活性位点处嫁接有机硅烷，使其表面由亲水性变为亲有机性，并通过 X 射线衍射（XRD）、电感耦合等离子体质谱（ICP）、透射电子显微镜（TEM）、扫描电子显微镜（SEM）、原位傅里叶变换红外光谱（FTIR）、热失重（TG-DSC）分析、氮气等温吸附脱附测试、核磁共振（MAS NMR）等技术，对改性后样品的物质组成、物相转变、结构特征以及矿物活化后铝、硅在碱溶液中的溶解行为做了相应的研究。
探讨了 HNTs在不同溶剂体系和相同溶剂体系不同比例溶剂下的嫁接效果和影响机制本文主要研究成果如下： （1）HNTs 碱活化过程中，内径逐渐增大，管壁变薄在保留较完整的管状形貌并得到较多羟基活性位点的前提下，4 天为最佳的活化时间，并通过XRD、TEM、SEM、FTIR 等表征手段发现埃洛石在碱活化后形成了新的物相沸石 （2）甲苯嫁接体系下，在埃洛石上嫁接有机硅烷或称硅烷偶联剂（3-氨基丙基三乙氧基硅烷，APTES），并从红外光谱图中发现 APTES 官能团，表明APTES 已成功的嫁接到埃洛石上通过热失重分析计算，发现 4 天的碱活化嫁接样在 250-475oC 之间的失重量最大，失重率达到 8.88%通过氮气等温吸脱附、核磁共振等分析，结果进一步表明，埃洛石 4 天的活化样嫁接量最多 （3）对活化 2 天、4 天、6 天、8 天、10 天、13 天的埃洛石样品进行了在乙醇/水（浓度（V/V））分别为 10/0、9/1、8/2、7/3、6/4、5/5 体系下嫁接 APTES的实验，发现 4 天活化样并在 9/1 比例条件下，样品的嫁接量最多，嫁接后的SBET由嫁接前的 40.8 m2/g 降至 36.18 m2/g，Vpore由嫁接前的 0.124 cm3/g 降至0.096 cm3/g。
说明体系中有适量水的存在可加速 APTES 的水解，更加有利于嫁接反应的进行 （4）无水甲苯体系与乙醇/水体系相比，无水甲苯体系的嫁接量更高说明在非极性溶剂中，更加有助于有机硅烷的嫁接 关键字：埃洛石纳米管；晶体结构；表面活性基团；有机硅烷；碱活化；嫁接改性 ABSTRACT Silicate minerals have wide variety and distribution，with unique structure and character, enjoying the reputation of "universal soil";. It is an important way to prepare new materials by modifying and processing natural clay minerals and change their crystal structure and surface chemistry further producing modified materials with novel structure and properties. Halloysite nanotubes (HNTs) are natural 1:1 type silicate clay mineral with the natural advantage of low cost, high strength and corrosion resistance. After modification and treatment, the composite materials with low-cost and high-performance can be prepared, and its development and application have become hotspots in current research. In this paper, the HNTs were modified by alkali to change the crystal structure of HNTs, increase the specific surface area, pore volume and hydroxyl active sites of nanotubes, organic modification will change the surface of halloysite from hydrophilic to hydrophobic and by X-ray diffraction (XRD), inductively coupled plasma mass spectrometry (ICP), transmission electron microscopy (TEM), scanning electron microscopy (SEM), in situ fourier transform infrared spectroscopy (FTIR),heat weight loss analysis, nitrogen isotherm adsorption desorption test, nuclear magnetic resonance (MAS NMR) and other techniques were used to investigate the material composition, phase transformation, structural characteristics of the modified sample. the material composition, phase transformation, structural characteristics of the modified sample, the dissolution behavior of aluminum and silicon in alkaline solution after mineral activation and the corresponding research about the grafting effect and influence mechanism of HNTs in different solvents systems and the same solvent system different solvent ratios were discussed. The main research results of this paper are as follows: (1) During the activation of HNTs, the inner diameter gradually increased and the tube wall became thinner. Under the premise of retaining a more complete tubular morphology and obtaining more hydroxyl active sites, 4 days is the best activation time, and halloysite forms a new phase, zeolite, after alkali activation. (2) Under the toluene grafting system, APTES was grafted on the halloysite, and the signal of APTES was found in the FTIR spectra, indicating that the APTES was grafted into halloysite successfully. According to the weight loss analysis, it was found that the 4-day alkali-activated grafting sample had the largest weight loss between 250 and 475C, and the weight loss rate reached 8.88%. By TG, nitrogen isothermal adsorption and desorption, nuclear magnetic resonance and other analyses,the results further showed that the activation of the hallucination of the halloysite for 4 days was the most. (3) The halloysite samples of activation for 2 days, 4 days, 6 days, 8 days, 10 days, and 13 days were carried out in ethanol/water (concentration (V/V)) of 10/0, 9/1, 8/2, 7/3, 6/4, 5/5 system grafted APTES experiments, found that 4 days of activation and in the case of 9/1 ratio, the sample grafted the most, after grafting SBET by grafting The 40.8 m2 /g was reduced to 36.18 m 2 /g, and the V Porewas reduced from 0.124 cm 3 /g before grafting to 0.096 cm 3 /g. It indicates that the presence of proper amount of water in the system can accelerate the hydrolysis of APTES, which is more conducive to the grafting reaction. (4) Compared with the ethanol/water system, the anhydrous toluene system has a higher grafting amount of the anhydrous toluene system. It shows that in non-polar solvents, i。