小分子CO_2，CH_4的活化和转化研究
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摘要
二氧化碳和甲烷分子的转化是—碳化学的重要新领域，这两种化学物质中最稳定分子的活化也是化学领域最富挑战性的理论课题。攻博期间，我有幸参加了与此相关的两个课题，取得了一些成绩。我的博士学位论文由两部分组成：一、有机改性SiO_2固载的Ru基催化剂上的scCO_2加H_2合成HCOOH反应(受到国家自然科学基金和高等学校博士学科点专项科研基金的资助)；二、HZSM-5负载的Mo基催化剂上的甲烷无氧脱氢芳构化(受到浙江省自然科学基金的资助)，其中第一部分是博士学习期间主要的攻关方向和研究工作。
第一部分、有机改性SiO_2固载的Ru基催化剂上的scCO_2加H_2合成HCOOH反应
从CO_2加氢直接合成甲酸，这不但是一个原子经济性反应，更符合当代绿色化学发展趋势。如果CO_2处于超临界状态，则对另一反应物H_2有很高的溶解性，另一方面，为了克服对此反应有效的均相催化剂难以从液相产物中分离、回收的缺点，我们将高活性和高选择性催化剂固载化与超临界CO_2技术结合起来，利用有较高的机械强度、耐热稳定性和化学稳定性的无机氧化物为载体，开发了固载于有机功能化的SiO_2上的Ru配合物催化剂，取得了比相应的均相Ru催化剂更高的活性，同时，此催化剂还具有良好的回收再用性能。并运用多种实验技术(元素分析、BET、FT-IR、ICP-AES、UV-VIS、XPS、量子化学理论计算)对SiO_2的有机功能化过程、Ru基催化剂的固载过程、不同催化体系的活性差异进行了表征，探讨了固载化的Ru基催化剂的可能结构、CO_2的活化方式以及可能的反应机理，得到的主要结果如下：
一、不同体系的固载Ru基催化剂上scCO_2加H_2合成HCOOH的研究
1．合成了文献未见报道的有机功能化的SiO_2固载Ru基催化剂，并首次用于超临界CO_2加H_2合成HCOOH反应，克服了均相催化剂难以从体系分离的缺点。该催化剂除了可以重复使用，具有较好的回收再用性能，还具有比相应的均
The conversions of carbon dioxide and methane are important and new regions in C_1 chemistry, the activations of these two stablest chemical substances are also the challengingest theoretic tasks in chemistry field. It's lucky for me to participate in two tasks correlative to the research of these two moleculars in the period of studying for my doctor's degree. My Ph. D. dissertation is made up of two parts: Part Ⅰ . Supercritical carbon dioxide hydrogenation to formic acid using functionalized silica supported ruthenium catalyst. Part Ⅱ . Methane dehydro-aromatization using HZSM-5 supported molybdenum catalyst under O_2-free condition. The first part is the main research work of my studying period.
Part Ⅰ . Supercritical carbon dioxide hydrogenation to formic acid using organic functionalized silica supported ruthenium catalyst
The synthesis of formic acid from carbon dioxide hydrogenation is not only an atom economic reaction, but also according with the developing trend of green chemistry. If carbon dioxide is in supercritical condition, it will increase the solubility of hydrogen in it. On the other hand, to overcome the disadvantage of difficult separation and recovery when using homogeneous catalyst effective to this reaction, we combine the immobilization of homogeneous catalyst bearing high activity and high selectivity with the technique of applying supercritical fluid. We developed ruthenium complexes supported on functionalized silica with mechanically, chemically and thermally stability, obtained higher activity than homogeneous counterparts. Simultaneously, the immobilized catalyst exhibited good recoverability and reusability. We also applied the techniques of element analysis, BET, FT-IR, ICP-AES, UV-VIS, XPS and quantum chemistry theoretic calculation to characterize
第一部分、有机改性SiO_2固载的Ru基催化剂上的scCO_2加H_2合成HCOOH反应
从CO_2加氢直接合成甲酸，这不但是一个原子经济性反应，更符合当代绿色化学发展趋势。如果CO_2处于超临界状态，则对另一反应物H_2有很高的溶解性，另一方面，为了克服对此反应有效的均相催化剂难以从液相产物中分离、回收的缺点，我们将高活性和高选择性催化剂固载化与超临界CO_2技术结合起来，利用有较高的机械强度、耐热稳定性和化学稳定性的无机氧化物为载体，开发了固载于有机功能化的SiO_2上的Ru配合物催化剂，取得了比相应的均相Ru催化剂更高的活性，同时，此催化剂还具有良好的回收再用性能。并运用多种实验技术(元素分析、BET、FT-IR、ICP-AES、UV-VIS、XPS、量子化学理论计算)对SiO_2的有机功能化过程、Ru基催化剂的固载过程、不同催化体系的活性差异进行了表征，探讨了固载化的Ru基催化剂的可能结构、CO_2的活化方式以及可能的反应机理，得到的主要结果如下：
一、不同体系的固载Ru基催化剂上scCO_2加H_2合成HCOOH的研究
1．合成了文献未见报道的有机功能化的SiO_2固载Ru基催化剂，并首次用于超临界CO_2加H_2合成HCOOH反应，克服了均相催化剂难以从体系分离的缺点。该催化剂除了可以重复使用，具有较好的回收再用性能，还具有比相应的均
The conversions of carbon dioxide and methane are important and new regions in C_1 chemistry, the activations of these two stablest chemical substances are also the challengingest theoretic tasks in chemistry field. It's lucky for me to participate in two tasks correlative to the research of these two moleculars in the period of studying for my doctor's degree. My Ph. D. dissertation is made up of two parts: Part Ⅰ . Supercritical carbon dioxide hydrogenation to formic acid using functionalized silica supported ruthenium catalyst. Part Ⅱ . Methane dehydro-aromatization using HZSM-5 supported molybdenum catalyst under O_2-free condition. The first part is the main research work of my studying period.
Part Ⅰ . Supercritical carbon dioxide hydrogenation to formic acid using organic functionalized silica supported ruthenium catalyst
The synthesis of formic acid from carbon dioxide hydrogenation is not only an atom economic reaction, but also according with the developing trend of green chemistry. If carbon dioxide is in supercritical condition, it will increase the solubility of hydrogen in it. On the other hand, to overcome the disadvantage of difficult separation and recovery when using homogeneous catalyst effective to this reaction, we combine the immobilization of homogeneous catalyst bearing high activity and high selectivity with the technique of applying supercritical fluid. We developed ruthenium complexes supported on functionalized silica with mechanically, chemically and thermally stability, obtained higher activity than homogeneous counterparts. Simultaneously, the immobilized catalyst exhibited good recoverability and reusability. We also applied the techniques of element analysis, BET, FT-IR, ICP-AES, UV-VIS, XPS and quantum chemistry theoretic calculation to characterize
引文
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