低成本合成介孔二氧化钛和共伴生明矾石矿综合利用新方法研究
文献类型：学位论文
| 作者 | 秦鸣 |
| 学位类别 | 硕士 |
| 答辩日期 | 2012-05-22 |
| 授予单位 | 中国科学院研究生院 |
| 导师 | 齐涛 ; 赵伟 |
| 关键词 | 介孔二氧化钛 介孔形成机理 元素掺杂 明矾矿 酸浸 |
| 其他题名 | New Methods of Lower Cost Synthesis of Mesoporous Titania and Integrated Utilization of Alunite Associated Ore |
| 学位专业 | 化学工程 |
| 中文摘要 | 本论文对有机钛源合成介孔二氧化钛的方法进行了改进和比较，并探索了用低成本无机工业钛源合成介孔二氧化钛的新方法，两条路线均得到了高比表面积、孔容大、孔径分布窄、具有锐钛矿型骨架的介孔二氧化钛材料，通过实验研究和XRD、TEM、SEM、FT-IR、低温氮吸附脱附、UV-vis等分析测试手段表征了所得产物的物化性质。实验研究和分析结果可归纳如下：（1）利用有机钛源通过三种方法合成了介孔二氧化钛，相对于传统方法，减少了溶剂用量。实验中发现，反应过程中混合溶液的流动性和热交换对于介孔结构的形成非常重要，还发现介孔的形成有助于提高产物的光催化性能。（2）以工业钛源为原料，混合表面活性剂为模板剂，水热合成了高孔道有序度的介孔二氧化钛，合成体系的工艺条件对产物介孔结构的形成至关重要。以十二烷基苯磺酸钠（SDBS）为主表面活性剂，十二胺（DDA）、十六烷基三甲基溴化铵（CTAB）、聚氧乙烯辛基苯基醚（OP10）等作副表面活性剂的混合体系均有良好的结构导向作用，其中，SL和CTAB形成的复合模板剂效果最好；保持体系的酸浓度在5%左右，可以很好地控制钛离子的水解缩聚速率及其与模版剂之间的界面组装；提高合成温度（120℃以上）和延长合成时间（48h），均能促进孔壁的晶化和孔道有序性的提高。在反应过程中掺杂某些金属盐类，可明显改善介孔特征。 本文还提出了一种新的拌酸焙烧结晶工艺处理伴生明矾石尾矿，经300℃拌酸焙烧，90℃水浸处理后，大幅提高了Al和K的浸取率，分别达到了94.6%和92.9%。该结果大大优于直接酸浸工艺，且降低了能耗和酸耗。同时，通过分步结晶法分别得到了高纯度的水合硫酸铝和明矾晶体，实现了铝、钾产品的初步分离。 |
| 英文摘要 | The method of mesoporous titania synthesis using organic titanium was improved and compared and a new method of synthesizing high performance mesoporous titania from cheap titanium source was explored. All of the products possess ordered mesostructure, high surface area, large pore volume, uniform pore size and anatase framework.The mesoporous titania were studied through systematic experiments and characterized by X-ray diffraction(XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier transform infrared test (FT-IR), nitrogen adsorption-desorption isothermos and so on. Experimental studies and analyze results can be concluded as follows: (1) Three ordered mesoporous TiO2 samples were successfully synthesized via three processes using organic titanium source and less solvent usage.Since the evaporation of ethanol and hydrolyzed butanol is conducive to the forming the stable inorganic-organic interface.The mesostructure of TiO2 can improve the photocatalysis activities. (2) The synthesis conditions have very important effect on formation of mesostructure when industrial TiOSO4 solution hydrolyzing is induced by self-assmebly template which orients the mesostructure.Using SL as main surfactant and CTAB, DDA, OP10 as vice surfactants have better structural directing ability than others,especially SL/CTAB.Keeping the acid concentration at about 5%,it is convenient for controlling hydrolysis and condensation rate of titanium ion and its interface assemble with template.Elevating synthesis temperature(120℃) and prolonging synthesis time are beneficial to crystallizing pore wall and enhancing pore order degree.Doping certain kinds of metal element during the synthesis can improve the mesoporous characteristic of TiO2. A new acid melting-water leaching method was introduced to treat the alunite associated ore considering its high massfraction of potassium and aluminum and its simple crystalline phase composition. Under the optimum process conditions: liquid-solid ratio 10:1, acid concentration 30%, calcine temperature 300℃, leaching temperature 90℃, the leaching ratio of aluminum and potassium was 94.6% and 92.9%, respectively. This result is much more superior to direct acid leaching method and also reduce the consumption of energy and acid. A multi-step crystallize method was taken to prepare the aluminium sulphate and alum crystal and separate potassium and aluminum product preliminarily. |
| 语种 | 中文 |
| 公开日期 | 2013-09-25 |
| 源URL | [http://ir.ipe.ac.cn/handle/122111/1849]  |
| 专题 | 过程工程研究所_研究所（批量导入） |
| 推荐引用方式 GB/T 7714 | 秦鸣. 低成本合成介孔二氧化钛和共伴生明矾石矿综合利用新方法研究[D]. 中国科学院研究生院. 2012. |
入库方式： OAI收割
来源：过程工程研究所
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