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1、密级保密期限： （涉密论文须标注） Z S T UZhejiang Sci-Tech University硕士专业学位论文Professional Masters Thesis中文论文题目:介孔二氧化硅的改性及其调湿性能的研究 英文论文题目：Modification of Mesoporous Silica Materials and their Humidity Control Properties 专业学位类别：工程专业学位 专业学位领域：材料工程 作者姓名：姚清清 指导教师：胡智文、彭志勤 完成日期：2014 年 12 月 10 日 摘要湿度和人们的生产生活密切相关，对人体舒适度、产品生
2、产过程与质量以及物品保存 等都有重要意义。环境湿度的波动会对文物、药品、高端珠宝等造成严重的破坏。特别是 像纺织品文物这样的有机质文物，对湿度的变化更为敏感。过去对调湿材料的研究主要着 眼于材料的调湿速率和湿容量上，目标是制备出调湿速率快，湿容量大的高效调湿材料。 课题组经过几年的研究，制备了包括调湿纸板、调湿球等 8 种不同成分的不同类型的高效 调湿材料。但随着对调湿材料的应用研究的深入，我们发现相比于调湿速率和湿容量，保 证调试性能的稳定性才是至关重要的。因此，本课题旨在保证调湿材料具有相对较优的调 湿速率和湿容量的前提下，制备出一种具有稳定调湿性能的材料。本课题根据纺织品文物存放环境的特
3、殊要求，通过对介孔二氧化硅金属离子掺杂和扩 孔等改性，测试其调湿性能，得到一种最适宜纺织品文物保护馆藏应用的调湿材料，得出 孔道结构对调湿性能的关系。本课题在常规调湿性能测试方法的基础上，测试不同吸湿率 情况下的平衡湿度，通过分析两者的关系，得出了不同材料的调控湿度精确度，以期更全 面地对材料调湿性能进行评估。主要研究结果如下：（1）选用三嵌段共聚物 P123 作为模板剂在酸性介质下制备的 SBA-15，是具有排布 规整的六边形孔道结构的介孔材料，平均孔径 6.03nm，具有较高比表面积和孔容，目标湿 度为 59.7%，符合纺织品文物存放环境湿度范围 40%-60%，但略高于最佳湿度 50%的
4、要求。 通过一步法和后处理法对其进行金属掺杂改性，研究发现只有一步法 Si/Al=10 和后处理法 Si/Al=50 的两种样品目标湿度存在细微下降，因此，金属改性对材料目标湿度的影响较小， 通过金属改性大幅度降低目标湿度的方法无法实现。（2）选用离子型表面活性剂 CTAB 在碱性介质中制备 MCM-41，碱性介质、温度的 选择以及模板剂和硅源的用量都会对其表面形貌、介孔的有序性、粒径大小和分散性产生 影响。加入辅助剂 TMB 对其进行扩孔改性，得到一系列不同孔径的 MCM-41，几种样品 的氮气吸附-脱附等温线都属于 Langmuir型。随着辅助剂用量的增加，孔径逐步增大，孔 径分布先变窄后
5、变宽，晶胞参数和衍射强度均呈现出先增大后减小的变化趋势。（3）选用离子型表面活性剂 CTAB 在碱性介质中制备 MCM-41，当 TMB/CTAB=2.5 和TMB/CTAB=5，孔径分别是 3.64nm 和 4.01nm，目标湿度分别是 49.3%和 50.1%，且 调湿精确度较高，最符合纺织品文物湿度范围要求，这主要和其孔径大小和孔径分布情况 有关。I本文制备的调湿材料具有工艺简单、调湿性能优异、调湿稳定性和重复性好等特点。 对于湿度敏感性强的有机质文物具有积极地保护作用，可为文物创造一个恒湿干净的存放环境，对我国文物的预防性保护工作具有积极的意义。 关键词：调湿；介孔；二氧化硅；文物环境
6、；孔径；吸附IIAbtractEnvironment relative humidity is important for our daily life and industry. The changes of environment relative humidity cause the negative consequences and difficulty regulation to cultural relics, drugs, jewelries and so on. Organic cultural relics are more sensitive to environment
7、relative humidity, such as fabrics. Formerly, more attention was paid to absorption (desorption) rate and amount. We hope to prepare a kind of humidity control materials, which has a high level of absorption rate and amount. In previous years, our group has prepared 8 different kinds of humidity con
8、trol materials, such as composite humidity control paper, composite humidity control paperboard, the porous composite resin and so on. However, after application, we have an knowledge that the stability and repeatability of materials are more important than absorption (desorption) rate and amount. B
9、ecause polymer materials, inorganic mineral materials and inorganic/organic composite materials have characters of poor stability and controllability of structure, the stability of humidity control properties are impossibleAccording to the special requirements of f textile cultural relics, a mesopor
10、ous silica with hexagon pore structure was made. The modification methods were metal doping and pore bearizing. The effect of pore structure on humidity control properties was discussed. Besides, by discuss the relationship between absorption amount and equilibrium humidity as a reference of humidit
11、y control accuracy, we can evaluate humidity control properties comprehensively. The conclusions are as following.（1）SBA-15 is prepared in acidic medium, with P123 as template. It has hexagon porestructure, with high specific surface area and entrance. The average pore size is 6.03 nm. Equilibrium m
12、oisture is 59.7%, which in the humidity range of textile cultural relics. Al-SBA-15 is made by one step and post-treatment. The equilibrium moisture of most samples is more than 60%. However, the equilibrium moisture of samples of one-step Si/Al = 10 and after-treatment Si/Al = 50 is less than SBA-1
13、5.（2）MCM-41 is prepared in alkaline medium, with CTAB as template. The choice of alkalinemedium, temperature and reactant dosage would change surface morphology, mesoporous order, particle size and dispersion of samples. a series of MCM 41 with different pore diameters were made by addition of TMB.
14、The several samples of nitrogen isothermal adsorption-stripping belongIIIto Langmuir type. Nitrogen isothermal adsorption desorption curves of samples belong to Langmuir style. With the increase of TMB amount, pore diameters gradually increase, whilepore size distribution, crystal cell parameters an
15、d the intensity of the diffraction increase firstly, and then decrease.（3）Compared to other samples, when (TMB)/(CTAB) is 2.5 and 5.0 respectively, thesamples has good performance and humidity control accuracy. The equilibrium moisture is 49.3% and 50.1%, respectively.In this paper, the humidity control material has the characters of simple technology, good humidity control properties, stability and repeatability of humidity control properties. It can be used to create a clean and humidity storage environment for cultural r
