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以表面活性剂十六烷基三甲基溴化铵(CTABr)为模板剂,在水热体系对水蒸气处理后的超稳Y型(USY)沸石进行晶化处理,获得高酸量和高水热稳定性的USY-c-w样品。利用X射线衍射、扫描电子显微镜、透射电子显微镜、固态核磁共振、N2吸附-脱附、NH3-程序升温脱附、傅里叶变换红外光谱及吡啶红外对所制备催化剂的物化性质进行详细表征。选用1,3,5-三异丙苯(TIPB)催化裂化作为探针反应,研究制备的催化剂的催化性能,并与工业USY沸石进行对比。结果表明,再次水热晶化后,样品的硅铝骨架局部重构,非骨架铝重新进入沸石骨架,合成样品的硅铝比(nSiO2/nAl2O3)由10降至3.0;再晶化后的USY沸石,不仅具有丰富的介孔结构,并且具有更多的弱酸和中强酸位点。在TIPB裂解反应中,再晶化后的USY沸石表现出比原样品更优异的催化性能。 相似文献
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对NaY分子筛(nSi/nAl=2.65)进行了草酸脱铝处理并作为载体采用液相离子交换法制备CuY催化剂, 应用于常压甲醇氧化羰基化合成碳酸二甲酯(DMC)反应。NaY分子筛及其CuY催化剂通过N2低温吸附-脱附、透射电子显微镜、X射线衍射、29Si固体核磁共振、NH3吸附程序升温脱附、吡啶吸附红外光谱、H2程序升温还原、原子吸收等方法进行表征。研究结果表明, 酸处理NaY分子筛后, 骨架铝被脱除, 导致骨架nSi/nAl比增加、相对结晶度降低并产生介孔, 有利于产物分子的扩散, 从而影响催化活性。采用4 h、2 mol·L-1草酸处理NaY分子筛作为载体制备的CuY催化剂显示出较高的催化性能, DMC时空收率和甲醇转化率分别从103.6 mg·g-1·h-1和6.3%增加到184.9 mg·g-1·h-1和10.2%。产生的介孔能够促进催化剂中铜活性位的可接近性及反应物分子和产物分子的扩散。 相似文献
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对NaY分子筛(nSi/nAl=2.65)进行了草酸脱铝处理并作为载体采用液相离子交换法制备CuY催化剂,应用于常压甲醇氧化羰基化合成碳酸二甲酯(DMC)反应。NaY分子筛及其CuY催化剂通过N2低温吸附-脱附、透射电子显微镜、X射线衍射、29Si固体核磁共振、NH3吸附程序升温脱附、吡啶吸附红外光谱、H2程序升温还原、原子吸收等方法进行表征。研究结果表明,酸处理NaY分子筛后,骨架铝被脱除,导致骨架nSi/nAl比增加、相对结晶度降低并产生介孔,有利于产物分子的扩散,从而影响催化活性。采用4 h、2 mol·L-1草酸处理NaY分子筛作为载体制备的CuY催化剂显示出较高的催化性能,DMC时空收率和甲醇转化率分别从103.6 mg·g-1·h-1和6.3%增加到184.9 mg·g-1·h-1和10.2%。产生的介孔能够促进催化剂中铜活性位的可接近性及反应物分子和产物分子的扩散。 相似文献
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一种合成高水热稳定性微孔-介孔复合分子筛β沸石/MCM-41的新方法 总被引:10,自引:0,他引:10
首次以β沸石作为硅铝源制备了β沸石/MCM-41微孔-介孔复合分子筛材料,通过XRD、IR、N2吸附脱附、SEM和水热处理等手段对复合材料进行了表征,并与MCM-41和β沸石及二者的机械混合物的有关性能进行了对比研究。结果表明,复合分子筛明显不同于机械混合物,其水热稳定性远远高于普通方法合成的介孔分子筛,而且发现通过改变体系的nNa/nSi比,可以调变复合样品中的微孔、介孔相的相对含量。 相似文献
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采用并流共沉淀法制备了不同Zr/Cd原子比(nZr/nCd)的ZrCdOx金属氧化物,并与水热法制备的不同硅铝比(nSiO2/nAl2O3)的片状SAPO-18分子筛物理混合制得ZrCdOx/SAPO-18双功能催化剂,研究了其催化CO2加氢直接合成低碳烯烃性能。采用透射电子显微镜(TEM)、X射线衍射(XRD)、N2吸附-脱附、CO2程序升温脱附(CO2-TPD)、NH3程序升温脱附(NH3-TPD)和X射线光电子能谱(XPS)对催化剂进行了分析。与单一ZrO2相比,引入CdO使得ZrCdOx比表面积下降,当nZr/nCd=8时制备的Zr8Cd1氧化物呈现出无定形小颗粒状,Zr与Cd之间较强的协同作用使得ZrCdOx氧化物产生了更多的氧空位,有利于CO2的吸附活化。通过对Zr8Cd1金属氧化物与SAPO-18(硅铝比0.1)的质量比、工艺反应温度、压力和空速对催化性能影响的考察,获得了最佳反应条件。研究还发现,当SAPO-18的硅铝比从0.1降为0.01时,Brø;nsted酸含量降低,产物中烯烃/烷烃物质的量之比从18.6提高至37.2,但副产物CO含量迅速增加,低碳烯烃时空收率明显下降。 相似文献
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利用水热合成法,以三乙烯四胺(TETA)为模板剂,正硅酸乙酯、磷酸、氢氧化铝及乙酸钴为原料,合成了CoSAPO-34分子筛。通过扫描电子显微镜(SEM)、粉末X射线衍射(XRD)、热重(TG)、N2吸附-脱附和紫外-可见漫反射光谱(UV-Vis DRS)等方法对合成的分子筛进行表征。以吡啶-正辛烷体系为模拟油品对分子筛催化剂的脱氮效果进行评价,考察了样品的用量、光催化时间及循环催化次数对其脱氮性能的影响。结果表明:当合成原料的物质的量之比为nP2O5:nAL2O3:nSiO2:nCo:nTETA=1:0.26:0.82:0.81:2.05,在200 ℃晶化24 h,合成得到粒径约为50 μm、仍保持了SAPO-34分子筛的骨架结构、形貌为立方体的CoSAPO-34分子筛,而且该分子筛具有较好的热稳定性。在500 W氙灯光照条件下反应150 min,样品对质量分数为100 μg·g-1模拟油品的脱除率达到70%,循环3次光催化脱氮活性基本保持不变。 相似文献
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以廉价水玻璃为硅源,在晶种替代有机模板剂的条件下采用干胶法合成了ZSM-5分子筛。利用XRD、SEM、TEM、FTIR、N2吸附-脱附和NH3-TPD等分析方法对合成样品进行了表征和测试,考察了合成条件对ZSM-5分子筛晶化过程的影响。结果表明,在硅铝比(n/n)为30~70,钠硅比(n/n)为0.12~0.20时都可以得到结晶度良好的ZSM-5分子筛。研究发现,干胶法合成ZSM-5,在不引入外加水的情况下也可以得到ZSM-5样品,外加水的引入能够有效地提高晶化速率;与水热法合成ZSM-5分子筛相比,干胶法可以显著地缩短晶化时间,同时,合成样品的晶体尺寸也有所减小。 相似文献
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以松香基季铵盐(脱氢枞基三甲基溴化铵,标记为DTAB)为模板剂、正硅酸乙酯为硅源、氨水为碱性介质成功合成出具有纳米片状形貌的六方有序超微孔二氧化硅材料。采用X射线衍射、N2吸附-脱附、透射电镜、扫描电镜等手段对样品进行表征,结果表明,体系中模板剂添加量、硅源添加量、碱性介质添加量、晶化温度、搅拌时间对前驱体的有序度有着较大的影响。当物质的量之比为nSio2:nDTAB:nNH3·H2O:nH2O=1.0:0.1:11.3:924.0,晶化温度为373K,搅拌时间为24h,所得样品有序度最高。经煅烧后样品具有较大的比表面积(1024 m2·g-1)和孔容(0.56 cm3·g-1),以及狭窄的孔径分布(集中于1.80 nm)。 相似文献
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纳米Mn-Zn铁氧体的制备和研究 总被引:10,自引:0,他引:10
Nanosize manganese zinc ferrites were fabricated by hydrothermal precipitation route using Fe2(SO4)3, ZnSO4·7H2O, MnSO4·H2O as material, then some calcinated at 500 ℃ and studied by XRD, TEM, IR and VSM. The results showed that the products were spinel crystal structure and uniformly sized nanoparticles (15~25 nm) with little aggregation. The analysis of IR showed that the superficial water can be eliminated, but that was embedded in crystal lattice can not be removed by calcinating. The effect Zn content x on the lattice (a) of nanosize Mn1-xZnxFe2O4 was also discussed. The lattice of nanosize Mn1-xZnxFe2O4 decreases with x increasing; and its value deviated the standard lattice (a0) of normal size manganese zinc ferrites. A lot of water was absorbed during the hydrothermal process owing to the large surface of nanosize particles. The change of magnetic properties of MnxZn1-xFe2O4 with x increasing was studied: nanosize MnxZn1-xFe2O4 particles synthesized by us exhibited peculiar magnetic properties curve with Zn content (x) increasing, Superparamagnetic behaviors of the synthesized ZnFe2O4 samples were confirmed by magnetic characterization, which can be explained by the difference between the distribution of the metal ions (Mn2+, Zn2+ and Fe3+) among the tetrahedral (A) and the octahedral (B) sites of nanosize ferrite and that of bulk ferrite. 相似文献
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氧化锌纳米棒的制备和生长机理研究 总被引:12,自引:0,他引:12
ZnO nanorods are prepared by different assistants (cetyltrimethylammonium bromide,trisodium citrate and ethylene diamine anhydrous) favored hydrothermal synthesis with Zn(OH)2 colloid as the precursor. The samples are characterized by transmission electron microscopy (TEM) and X-ray diffraction (XRD). The results show that the as-synthesized ZnO nanorods are of uniform size with 25 nm in diameter and 200~300 nm in length. The effects of the different assistants to the morphology, size and mechanism of nano-ZnO are discussed. 相似文献
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WU Yanga JIANG Xiao-Yub ZHANG Quan-Zhengc CHEN Li-Juanc YU Ya-Qinc CHEN Shu-Meic HE Xiangc YANG Wen-Binc LU Can-Zhongc② a 《结构化学》2005,24(3):291-294
1 INTRODUCTION Current research interest is focused on the designof structures built up from octahedral and tetrahedralbuilding blocks[1]. During the wide investigations intransition-metal phosphates for many years, a num-ber of new mixed transition-metal phosphates havebeen reported[2]. A great number of manganese phos-phates were largely discovered as minerals[1]. On theother hand, many vanadium phosphates have alsobeen prepared recently partly because of their poten-tial applications … 相似文献
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A new metal-organic complex Mn2(cbba)4(phen)2 (Hcbba = 2-(4'-chlorine-benzoyl)-benzoic acid, phen = 1,10-phenanthroline) 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses and IR spectroscopy. The compound crystallizes in orthorhombic, space group Pbcn with a = 12.154(5), b = 18.166(7), c =31.197(13) (A°), V = 6887(5) (A°)3, C80H48C14Mn2N4O12, Mr= 1508.90, Dc = 1.455 g/cm3, μ(MoKa) =0.591 mm-1, F(000) = 3080, Z = 4, the final R = 0.0408 and wR = 0.0873 for 4033 observed reflections (I > 2σ(I)). In the crystal structure, the manganese atom is six-coordinated with four carboxylate oxygen atoms from three different cbba ligands and two nitrogen atoms from phen ligands, showing a distorted octahedral geometry. Furthermore, it exhibits a 3D supramolecular network through π-π interactions. 相似文献
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YU Ling-Ling 《结构化学》2011,30(12):1725-1730
Two new carboxylate coordination polymers [Ni(2,3'-oba)(bib)]n] and [Mn(2,4'-oba)(bib)0.5]n(2,3'-oba = 2-(3-carboxyphenoxy)benzoic acid,2,4'-oba = 2-(4-carboxyphenoxy) ben-zoic acid and bib = 1,4-bis(2-methyl-imidazol-yl)butane) have been synthesized and characterized by elemental analysis,IR and X-ray single-crystal diffraction studies.Compound 1 crystallizes in monoclinic,space group P21/c,while compound 2 in the triclinic space group P.Compound 1 displays a one-dimensional ladder-like chain.The dinuclear paddle-wheel secondary building units(SBUs) constructed by four 2,4'-oba2-ligands in compound 2 are linked by bib into a 2D(4,4) layer structure. 相似文献