摘要
磷酸铝(AlPO)分子筛经过30多年的发展已成为分子筛家族的一个重要组成部分。二价金属离子M~(2+)可以引入到AlPO分子筛的骨架中，形成含二价金属磷酸铝分子筛M(Ⅱ)APO。M~(2+)离子的引入，不仅赋予了AlPO分子筛优异的催化性质、光学性质，同时也能诱导产生新颖的分子筛拓扑结构。因此M(Ⅱ)APO分子筛的合成受到科研工作者的广泛关注。在本论文中，我们合成了一系列M(Ⅱ)APO分子筛，并对其进行了
结构分析与性质表征。在三乙烯二胺体系下，详细研究了M~(2+)(M=Co, Zn, Mg和Mn)对最终M(Ⅱ)APO分子筛的影响。本文取得的主要结果如下：
1.以N-甲基哌嗪为模板剂，在水热条件下合成出两个新颖的M(Ⅱ)APO分子筛M(Ⅱ)APO-CJ62(M=Co, Zn)。M(Ⅱ)APO-CJ62展现了一种新颖的分子筛拓扑结构，于2012年被国际分子筛协会收录，并命名为JSW。M(Ⅱ)APO-CJ62的骨架是由M/AlO4四面体与PO4四面体通过桥氧原子严格交替连接而成，并沿[010]方向具有一维8元环孔道。在M(Ⅱ)APO分子筛中，M~(2+)离子在骨架中大多是无序分布的，而在M(Ⅱ)APO-CJ62中，M~(2+)选择性的占据了结晶学不等价Al3+位置中的两个。ICP分析表明M/Al的摩尔比为1:2。结构优化与扭曲度分析表明，在假想的磷酸铝分子筛AlPO-CJ62中，以Al(1)、Al(2)为中心的AlO4以及AlP4四面体存在严重的扭曲，因此需要引入M~(2+)来释放由于扭曲所带来的张力，进而得到了稳定的M(Ⅱ)APO-CJ62骨架结构，反之仅由磷、铝组成的分子筛AlPO-CJ62无法在实验中被合成出来。
2.以三乙烯二胺为模板剂，在水热条件下合成了四种M(Ⅱ)APO分子筛：M(Ⅱ)APO-CGF与M(Ⅱ)APO-OSI (M=Co, Zn)。通过进一步调变初始凝胶中二价金属离子的种类与含量，我们详细的研究了M~(2+)在合成M(Ⅱ)APOs中的影响，经过大量实验获得了11种M(Ⅱ)APOs化合物，对应于6种不同的拓扑结构：CGF,OSI, AFN, SOD, LEV以及AFI。我们发现，不同种类金属离子的配位形式的差别对所得产物的结构起到了决定性作用。此外，初始凝胶中二价金属离子的含量也是重要的相选择因素，这与晶化产物的结构优化以及键角方差分析结果一致。
3.在水热条件下，以2,2’（乙烯二氧）双（乙胺）为模板剂，合成了三个含二价金属离子的开放骨架磷酸铝化合物M(Ⅱ)APO-CJ50(M=Mg, Mn和Fe)。M(Ⅱ)APO-CJ50具有三维交叉的10元环和8元环孔道。2,2’（乙烯二氧）双（乙胺）分子位于交叉孔道中，同时以两个醚氧原子与骨架上的金属杂原子形成双齿配位。这三种化合物与我们之前报道的以咪唑为模板剂合成的含三价金属杂原子的M(ⅡI)APO-CJ50具有类似的骨架拓扑结构。与M(ⅡI)APO-CJ50对比，醚胺模板剂的引入不仅改变了CJ50结构中金属杂原子的氧化态，形成了新颖的配位形式，更改变了金属中心电子的自旋态，从而影响了CJ50的磁学性质。
Over the course of the past30years, aluminophsphates molecular sieves(denoted as AlPOs) have become an important member of zeolite family. Metal ionscan be introduced into the frameworks of AlPOs to form a metal-containing AlPOs(named as M(Ⅱ)APOs). The introduction of the metal ions, not only gives theM(Ⅱ)APOs excellent catalytic and optical properties, but also can induce novelzeolite topologies. Therefore, the synthesis of M(Ⅱ)APOs has attracted extensiveattention. In this thesis, we have synthesized a series of M(Ⅱ)APOs, and theirstructures and properties have been characterized in detail. Meanwhile, we studiedthe effect of M~(2+)ions (M=Co, Zn, Mg and Mn) on the final products of M(Ⅱ)APOsin the triethylene diamine system. The main results in this thesis are as follows:
1. Two divalent-metal-containing aluminophosphates: M(Ⅱ)APO-CJ62;(M=Co,Zn), have been hydrothermally synthesized by using N-methylpiperazine as thestructure directing agent. Both of these compounds exhibit a new zeolite frameworktopology, which has been assigned a three-letter code JSW by international zeoliteassociation (IZA). All the M/Al and P atoms are tetrahedrally coordinated andalternately connected to each other through bridging O atoms. This new zeoliteframework contains1-dimensional8-ring channels running along the [010] direction.The M~(2+)ions in M(Ⅱ)APO-CJ62selectively occupy two of the three possiblecrystallographically distinct positions. Inductively coupled plasma (ICP) analysisshows that the molar ratio of M:Al in M(Ⅱ)APO-CJ62is1:2. Structural optimizationand distortion analysis reveal that serious distortions exist in Al(1) andAl(2)-centered tetrahedra in the hypothetical framework of AlPO-CJ62. To releasethe stress generated at these two sites, incorporation of M~(2+)ions appears to benecessary to form flexible M-centered tetrahedra instead of rigid Al-centeredtetrahedra. The introduction of M~(2+)becomes a favorable factor for the formation ofM(Ⅱ)APO-CJ62. A pure aluminophosphate analogue of M(Ⅱ)APO-CJ62, denoted as AlPO-CJ62, has not been obtained in experiment so far.
2. Four M~(2+)-containing aluminophosphate molecular sieves, M(Ⅱ)APO-CGFand M(Ⅱ)APO-OSI (M=Co and Zn) have been synthesized hydrothermally in thepresence of DABCO as the SDA. By varying the types and the amounts of M~(2+)ions,we have further studied the role of M~(2+)ions in the synthesis of M(Ⅱ)APOs. ElevenM(Ⅱ)APOs with the CGF, OSI, AFN, SOD, LEV and AFI topologies are obtained.The result shows that the types of M~(2+)ions play an important role in directing thefinal crystalline products, due to the different coordination geometry of M~(2+)ions. Inaddition, more than one structure can be produced by altering the amounts of M~(2+)ions. Structural optimization and bond angle variances analysis reveal that thedistortions of AlO4tetrahedra in the structures are AlPO-OSI
3. Three divalent-metal-containing open-framework aluminophosphates,designated M(Ⅱ)APO-CJ50,(M=Mg, Mn and Fe), have been hydrothermallysynthesized by using2,2’(Ethylenedioxy)bis(ethylamine) as the template. Singlecrystal and powder X-ray diffraction analyses show that their structures are similar tothose of trivalent-metal-containing aluminophosphates M(ⅡI)APO-CJ50synthesizedby imidazole. The differences between M(Ⅱ)APO-CJ50and M(ⅡI)APO-CJ50are:hetero-metal-atoms in M(Ⅱ)APO-CJ50have lower oxidation states owing to theusage of ether amine; in M(Ⅱ)APO-CJ50, hetero-metal-atoms are coordinated to thetwo O atoms in each ether amine molecule, whereas in M(ⅡI)APO-CJ50hetero-metal-atoms are coordinated to pairs of imidazole molecules through single Natoms. Moreover, magnetic measurements reveal that the hetero-metal-atoms inM(Ⅱ)APO-CJ50are high-spin whereas those in M(ⅡI)APO-CJ50are low-spin owingto the differences in oxidation states and ligand molecules.
引文
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