汽相转移法合成不同硅源的MCM-22分子筛

采用汽相转移(VPT)法合成出结晶度较高的纯MCM-22分子筛,并首次将硅酸钠应用于VPT法合成MCM-22分子筛;合成过程模板剂和Na⁺ 用量与水热合成法相比明显减少。用X射线衍射仪、扫描电子显微镜及BET比表面测定对产物作了表征,并重点对不同硅源对结晶产物的影响作了讨论.     

干胶-水蒸汽辅助晶化法合成多级孔ZSM-5分子筛

采用干胶-水蒸汽辅助晶化法,通过优化制备条件,合成了粒径约80 nm的表面多孔纳米球形ZSM-5.考察了结构导向剂质量分数、硅源、铝源、沉淀剂种类、晶核形成时间及老化温度对纳米ZSM-5晶体形貌的影响.采用X射线衍射(XRD)、傅里叶变换红外光谱(FT-IR)、N_2物理吸附-脱附及透射电子显微镜(TEM)等表征手段对合成的分子筛进行了表征.结果表明:结构导向剂的质量分数、铝源的类型和晶核形成时间均能明显影响分子筛晶体形貌;结构导向剂质量分数的降低有助于提高ZSM-5微孔结构的长程有序性;优化合成条件可制备出具有约介孔2 nm、比表面积357.1 m~2/g、由80 nm的晶粒堆积形成的多级孔ZSM-5分子筛材料.     

AlMCM-41的水热合成及其孔结构表征

以水玻璃为硅源,铝酸钠为铝源,十六烷基三甲基溴化铵为模板剂,在100℃水热条件下合成高度有序的AIMCM-41介孔分子筛,并用小角X射线衍射（SAXRD）、N2吸附脱附、高分辨透射电镜（HRTEM）等方法对其性质及结构进行表征。研究硅铝比（摩尔比）与表面活性剂浓度对AIMCM-41合成及其孔结构的影响。研究结果表明：在低表面活性剂浓度下形成单一孔径分布的圆柱孔;在高表面活性剂浓度下,随着铝含量的增加,结晶程度降低。高表面活性剂浓度下的AIMCM-41形成双孔分布,在硅铝比小于25时形成二维孔径结构;而硅铝比大于25时形成膨胀孔。     

无晶种合成ZSM-5分子筛的研究

在无晶种条件下,以水玻璃为硅源,硫酸铝为铝源,无水乙醇为有机模板剂合成ZSM-5分子筛.从晶化温度、晶化时间、模板剂用量方面考察实验条件对ZSM-5合成的影响,用X射线衍射仪进行物化表征.研究结果表明:在180℃晶化温度下,晶化时间为35h,乙醇硅比为1时,水热合成的ZSM-5分子筛结晶度最高.     

合成条件对Silicalite-1沸石分子筛形貌的影响

以TPAOH为模板剂,TEOS为硅源,采用水热合成法制备Silicalite-1沸石分子筛。通过改变晶化方式、晶化温度、晶化时间、模板剂用量及乙醇用量等合成参数,调变分子筛的形貌。SEM和XRD检测结果表明,采用油浴晶化所得的Silicalite-1沸石分子筛比采用烘箱晶化所得沸石分子筛中的孪晶含量少;合成液中较低的模板剂、乙醇含量,较高的晶化温度,较短的晶化时间都有利于合成含较少孪晶的Silicalite-1分子筛。     

合成条件对偏高岭土水热合成Y型分子筛结构的影响

采用苏州高岭土作原料,在不同条件下水热合成Y型分子筛,考察合成条件对形成Y型分子筛结构和性能的影响.结果表明,各种合成条件(高岭土的煅烧温度、导向刺用量、碱用量、陈化条件、成胶温度、晶化温度)对合成分子筛复合材料的结晶度、硅铝比、颗粒度、形貌都有影响,最后提出了制备高活性分子筛复合材料的较佳合成条件:650℃偏高岭土,导向剂用量4%,碱用量3%,成胶温度60℃,陈化2 h,晶化温度90℃.     

Al-MCM-41介孔分子筛的合成与表征

在碱性条件下,采用水热晶化法,以水玻璃为硅源,偏铝酸钠为铝源,十六烷基三甲基溴化铵为结构模板剂,成功合成出了含铝介孔分子筛Al-MCM-41.采用XRD,TEM,IR及N2吸附等表征手段研究了合成条件对Al-MCM-41介孔分子筛的的影响.结果表明,在pH值为11~13、模板剂与SiO2之比为0.07~0.20,120℃下晶化72h,以2℃/min的速率升温至550℃焙烧5h得到结晶度和有序性高的Al-MCM-41.N2吸附结果表明:合成的Al-MCM-41的孔容为0.942cm3/g,比表面积为1190m2/g,平均孔径为3.16nm,该分子筛具有较大的孔容、比表面积和较窄的孔径分布.     

新型纳米双孔硅铝分子筛的溶胶——凝胶法合成及表征

以正硅酸乙酯（TEOS）和水合硝酸铝（ANN）为硅源和铝源，以离子型表面活性剂十六烷基三甲基溴化铵（CTAB）为模板剂通过溶胶－凝胶途径合成了具有双孔分布特征和纳米尺寸的硅铝复合分子筛，并通过XRD、HRTEM、^27A1 MASNMR和N2吸附－脱附等手段对其结构性质进行了表征，同时与单一孔的A1MCM－41和无定形硅铝材料进行了比较。     

TPABr—正丁胺体系中TS—1的合成与表征

采用水热晶化法，以ＴＰＡＢｒ为模板剂，正丁胺为碱源合成出钛硅分子筛ＴＳ－１，并探讨了合成过程中的影响因素，利用ＸＲＤ、ＩＲ、ＵＶ－Ｖｉｓ、ＳＥＭ等对合成的分子筛作了表征。     

酸性条件下合成纯硅六方介孔分子筛的条件探索

以十六烷基三甲基溴化铵为模板剂,正硅酸乙酯为硅源,在酸性条件下合成了纯硅六方介孔分子筛。对晶化温度、陈化时间、酸介质的用量和种类等合成条件进行了考察,发现合成条件对样品的结晶度、结构有序性、孔径、壁厚等有明显影响,讨论了这种影响产生的原因和酸性介质中合成纯硅介孔分子筛的适宜条件。     

Influence of deposition time on the morphology and optical properties of SiO<Subscript>2</Subscript>-ZnO composite photonic crystals

SiO2 photonic crystal were successfully prepared by vertical deposition and then used as a template to fabricate SiO2-ZnO composite photonic crystals on ITO substrates by electrodeposition and subsequent calcination. A number of different deposition times were used. The morphologies of the silica opals and SiO2-ZnO composite photonic crystals were investigated by scanning electron microscopy. It was found that ZnO particles grew randomly on the surfaces of the silica spheres when the deposition time was short. As the deposition time was increased, the ZnO particles grew evenly on the surfaces of the silica spheres so that the interstitial space of the silica template was filled with ZnO particles. Reflectance spectra of the SiO2-ZnO composite crystals revealed that all of the fabricated photonic crystals exhibit a photonic band gap in the normal direction.     

Effect of Na+ on xonotlite crystals in hydrothermal synthesis

The effect of Na⁺ ion concentration on the crystalline phase composition and morphology of xonotlite crystals prepared in a CaO-SiO₂-H₂O system via hydrothermal synthesis was analyzed. X-ray diffraction (XRD) and scanning electron microscopy (SEM) results indicate that Na⁺ ion concentration has a significant impact on the composition and morphology of crystalline phases in the products under the initial conditions of a molar ratio of CaO/SiO₂ of 1.0 and a reactant concentration of 0.05 mol·L^?1 at 225°C for 15 h. The main crystalline phase in the products has a phase transition from xonotlite to pectolite, and the morphology changes from fibrous to broomlike shape with the Na⁺ ion concentration increasing. Therefore, the content of Na₂O in the raw material should be less than 5wt% for preparing pure xonotlite crystals via hydrothermal synthesis in a CaO-SiO₂-H₂O system.     

Synthesis of 3-D ordered macroporous silicate using the template formed from monodispersed polystyrene latex

Based on the template formed from monodispersed polystyrene (PS) latex, a modified fast sol-gel process was employed to synthesize a three-dimensional (3-D) ordered macroporous silica material after removing the template by calcination at high temperature. It was indicated that there existed highly ordered packed pores within the whole silica material by SEM morphology observation. It was also found that the pores were interconnected. The pore size could be controlled mainly by varying the particle size of the latex ranging from 10¹ to 10² nm. The formation process of the ordered pores was also preliminarily discussed.     

纳米硅铝酸盐的水热制备及催化性能

采用水热法制备了一系列纳米硅铝酸盐材料,考察了晶化时间、模板剂、硅源、铝源、稀土离子掺杂等对材料制备的影响.发现以TEAOH为模板剂,白炭黑为硅源,硫酸铝为铝源,铈离子掺杂制备的硅铝酸盐在苯甲醛与吲哚的Friedel-Crafts烷基化反应中的催化活性最好.通过XRD,BET和SEM表征了该材料的结构特性.     

New evidence for microstructural evolution model of acid-activated montmorillonite

Ca-montmorillonite samples from Choushan treated at various acid concentrations were studied using chemical analysis, XRD, ²⁹Si and ²⁷Al MAS NMR, to investigate the microstructure of the activated montmorillonites. With the increase of acid concentration and dissolution of cations of montmorillonite, the intensity of d(001) decreased obviously and significant changes of the microstructure of Si and Al occurred. There were two new types of structural units of Si atoms formed: (SiO)₃SiOH units and Q⁴(0Al) units. For Al atoms, in the course of activation, the removal of one of a pair of octahedral aluminium atoms from montmorillonite removed two hydroxyl groups and left the other aluminum of the pair in the four-fold coordination. The ²⁷Al signal at δ 54.0 corresponding to Al^Ⅳ arose from the four- coordinated Al in the octahedral sheet. This study first con-firmed, by ²⁹Si and ²⁷Al MAS NMR spectra, that the model of microstructural evolution for activated montmorillonite postulated by Thomas et al. (1950) is correct.     

Synthesis and photo-responsive behaviors of hollow polyazobenzene micro-spheres

By means of distillation precipitation polymerization, the silica-hybrid particles with polyazobenzene shell (PAzo@SiO₂) micro-spheres were prepared with 6-(4-methoxy-4′-oxy-azobenzene) hexyl methacrylate (Azo-M) as monomer, divinylbenzene (DVB) as cross-linker, and ~250 nm vinylated sol-gel silica particles as template. Hollow polyazobenzene microspheres were further developed after selective removal of the silica cores with HF solution. When the content of DVB related to Azo-M is 20 wt%, the acetonitrile is 200 mL, and the polymerization time is 4.5 h, the hollow PAzo microspheres with about 20 nm shell are successfully fabricated. These hollow PAzo microspheres have excellent reversible photoisomerization, and their first-order rate constant of trans-cis isomerization only decreases 11.8% compared with homopolymer of azobenzene (Homo-PAzo).     

The synergistic effect of quaternary ammonium cations on the corrosion inhibition of Fe by inorganic anions

The synergistic effect of tetrabutylammonium cation (TBA⁺) or N-hexadecylpyridinium cation (HDP⁺) and SCN⁻ or I⁻ in 0.5 mol·L⁻¹ H₂SO₄ solution on the corrosion inhibition of Armco iron was investigated by potentiodynamic polarization and polarization resistance measurements. The results show that the synergistic effect of HDP⁺ containing π-electron and anion is stronger than that of TBA⁺ and anion. The joint adsorption models of cation and anion at electrode-solution interface are related to the structure and property of both ions by analyzing the desorption behaviours of both ions when the electrode is polarized anodically. Supported by the national scientific foundation of China Zou Jinyun: born in Aug. 1936. Prof.     

PbxNayYzF2x+y+3z+3m∶Erm3+上转换发光粉的低温燃烧合成及表征

采用低温燃烧合成（LCS）法一步合成了Pb_xNa_yY_zF_2x+y+3z+3m:Er_m3+氟化物体系1 550 nm响应的红外上转换发光材料. 通过正交实验研究了4种阳离子影响发光性能的主次关系及最佳配比,研究了燃料用量对晶相形成及上转换发光性能的影响. 采用X射线粉末衍射仪、透射电镜、荧光分光光度计（耦合1 550 nm激光器）等手段对样品的物相、形貌及发光性能进行了测试与表征. 结果表明:阳离子含量对红光发射强度影响的主次关系为Y3+,Pb2+,Na+,Er3+,最佳配比为Pb_0.004Na_0.003 Y_0.003 F_0.032:Er3+_0.004. 燃料取2.5倍理论用量时样品的结晶度和发光强度最高.      

Selective catalytic oxidation of ammonia to nitrogen over orderly mesoporous CuFe2O4 with high specific surface area

Orderly mesoporous CuFe2O4 spinel-type mixed oxide with high specific surface area was prepared successfully by a hard-template method in which KIT-6 mesoporous silica was selected as the hard template. The KIT-6 hard template and CuFe2O4 samples were charac- terized by X-ray diffraction, X-ray photoelectron spec- troscopy, X-ray fluorescence, transmission electron microscopy, scanning electron microscopy, nitrogen physisorption, and hydrogen-temperature programmed reduction. The KIT-6 hard template had perfect crystalli- zation and ordered mesoporous structure with a probable pore distribution of about 9.1 nm, large enough to be filled by the spinel precursor. The mesoporous CuFe2O4 spinel oxide synthesized inside the KIT-6 mesopores had a rela- tively small pore size （4.3 nm）, orderly arrangement, and high specific area （194 m2/g）. The catalytic activity of the mesoporous CuFe2O4 was tested for the selective oxidation of ammonia to nitrogen. The conversion of ammonia reached nearly 100 % at 300 ℃with a nitrogen selectivity as high as 96 %. The nitrogen selectivity remained high with increasing temperature and even maintained a value of 80 % at 600 ℃.     

酸碱度对分子筛吸附性能影响研究

以硅溶胶为硅源、六亚甲基亚胺(HMI)为模板剂,通过掺杂Ce合成了具有MWW层状结构的Ce-MCM-22分子筛;叠氮化钠为氮源、钛酸四丁酯为钛源,采用静态水热合成法合成了N-Ti-ZSM-5分子筛;叠氮化钠为氮源、钛酸四丁酯为钛源、按SiO2:0.03TiO2:(0-0.01)N:0.03HM:0.035Al2O3:0...