微波辐射法合成4A沸石及表征

本文主要是采用微波辐照的方法合成4A沸石分子筛,并先后以纯化学原料,工业用高岭土为原料等进行合成,结果表明4A沸石合成的质量与微波功率及辐照时间密切相关,用高岭土为原料能合成出与化学法具有同等质量的4A沸石。     

高铁高砂煤矸石合成4A沸石分子筛

以六盘水矿区的高铁高砂煤矸石为原料合成4A沸石分子筛,将煤矸石低温焙烧、盐酸酸浸除铁、高温焙烧后再碱融活化获得了活性原料,最后采用水热晶化的方法,合成了4A沸石分子筛产品.本研究采用单因素实验的方法,考察了合成条件对4A沸石分子筛性能的影响,并运用XRD和SEM对产品进行了表征,结果表明所得产品为4A沸石分子筛,粒度分...     

介孔分子筛Al-MCM-41的合成与催化异构化性能

采用正硅酸乙酯(TEOS)为硅源,九水硝酸铝为铝源,十六烷基三甲基溴化胺(CTMABr)为模板剂,在室温条件下合成了介孔Al-MCM-41分子筛.通过XRD、N2等温吸附、SEM、FTIR等分析测试手段表征了分子筛的介孔结构和表面性质.结果表明所合成的分子筛有良好的介孔结构和较高的有序度,并且有较高的比表面积(达到816 m2·g-1)和窄的孔径分布.采用程序升温的焙烧方式、凝胶Al/Si比最大范围控制在0.06～0.13有利于合成高度有序的介孔Al-MCM-41分子筛.评价结果表明,所合成的Al-MCM-41分子筛对桥式四氢双环戊二烯(endo-TCD)异构化反应合成挂式异构体exo-TCD及金刚烷具有较高的催化活性和极高的选择性.     

以MCM-22分子筛为前驱体制备MCM-36分子筛

以MCM-22分子筛为前驱体,对原料配比和合成步骤等参数进行调变,探索了MCM-36分子筛的合成规律。通过X射线衍射、扫描电镜和N2吸附-脱附等表征方法对所合成的MCM-36分子筛物理化学性质进行表征。结果表明,以MCM-22为前驱体,溶胀原料质量配比为1∶3∶1.2时,MCM-36分子筛介孔和微孔比表面积最大。     

微波谐振腔中电子与微波作用的非稳态过程研究

 在微波腔中微波场影响电子的运动，同时电子束作为电流源也产生辐射，影响微波场，这种相互作用包含线性和非线性过程。根据Maxwell理论，微波腔中的实际微波场可以按微波腔的模式展开，而且不同模式与电子束之间的相互作用不同。将电子束作为激励源，根据Maxwell方程和电子受到的洛伦兹力，建立不同模式在电子束作用下的激励方程和电子束电子在不同模式作用下的运动方程（即微波谐振腔中电子束与微波场相互作用的自洽方程组），并由此进一步分析一维情况下单间隙微波腔中微波建场、辐射场呈指数增长和饱和等非稳态作用过程，该过程涉及到电子束与微波作用的线性和非线性过程。     

微波辅助提取-紫外分光光度法检测土壤中的油脂总量

以合成土样为对象 ,研究了微波辅助提取油脂的条件及其提取效率 ,由此建立了土壤中油脂分析的快速光度检测方法。在中档微波场辐射 3× 10 s时 ,2次 15 m L丙酮 -正己烷 (体积比 1∶ 1)萃取 10 g合成土样中的油脂时所获收率最高。方法的平均回收率大于 97.3% ,RSD小于 2 .5 % ,其结果与索氏萃取 4 h的效果相当     

微波射频场调制下Λ型三能级原子系统的电磁感应光栅

研究了在微波射频场调制下的Λ 型三能级原子系统的电磁感应光栅现象. 结果表明: 微波场可以增强对探测场的相位调制和增益作用, 使得衍射强度、尤其是一阶衍射强度明显提高; 当系统参数取值适当时, 一阶衍射强度随微波场强度呈指数增长的趋势. 关键词： 电磁感应光栅 电磁感应透明 微波射频场     

用XRD法研究MCM-22分子筛的逐级放大合成

在100,250和1 000 mL高压釜静态成功合成MCM-22分子筛的基础上,在2,5和200 L高压釜中进行了MCM-22分子筛的动态合成试验,对合成的样品用XRD等技术进行了表征。结果表明,在静态和动态条件下合成的样品,全部为纯相MCM-22分子筛,且结晶度较高,从100 mL到200 L的放大试验是成功的。     

“无水”NiC_o_2O_4纳米棒在电化学无酶葡萄糖传感中的应用（英文）

本文介绍了棒状NiCo_2O_4的制备,并将其修饰玻碳电极作为无酶葡萄糖传感器.通过简单的水热反应合成了NiCo_2O_4,然后在商用微波炉中对NiCo_2O_4进行处理,以消除水热合成过程中可能引入的残存水.扫描电镜、透射电镜、X射线衍射谱和X射线光电子能谱分析表明,微波处理前后结构无变化.通过EDS对Ni,Co,O原子比例的分析,证明微波处理对残存水的消除作用.微波处理的NiCo_2O_4(MNiCo_2O_4)作为葡萄糖传感器的灵敏度高达431.29μA mM~(-1) cm~(-2).最后,将M-NiCo_2O_4在水中浸泡不同时间后,其对葡萄糖的感应性能下降.结果表明,水热过程中引入的残存水对其电化学性能有很强的影响,微波预处理对其电化学性能也有着重要的影响.     

溶胶-凝胶法和微波辐射法制备红色荧光粉及发光性质的研究

采用溶胶-凝胶法和微波辐射法制备了Mn2+,DY3+∶Mg2SiO4红色发光材料.研究了以Mg2SiO4为基质,在单一掺杂Mn2+的情况下,微波合成时间和Mn2+的掺杂浓度对材料发光性能的影响.选择最佳微波合成时间和Mn2+的掺杂浓度,研究了共掺Dy3+浓度对材料发光性能的影响.通过这种方法制备了在410 nm激发下,...     

一维取向LTL型分子筛荧光阵列的快速组装

通过有效控制合成液配比,合成出了形貌规则、结晶度高且具有不同长径比的LTL型分子筛晶粒。采用"瓶中造船法",在不同长径比的LTL型分子筛晶粒孔道中组装稀土有机配合物,制得LTL分子筛/Eu-TTA主-客体荧光材料。荧光光谱表征结果表明,在激发波长为350 nm时,长径比为0.2的LTL分子筛/Eu-TTA晶粒在617 nm处的5D0→7F2发光强度最大,而长径比为3的晶粒发光强度最小。最后,将长径比为0.2的LTL分子筛/Eu-TTA晶粒在PEI修饰的玻璃表面快速擦涂10 s后,就制得厘米尺寸的一维取向LTL型分子筛荧光阵列。SEM表征结果证实,该分子筛荧光阵列中几乎所有的LTL分子筛晶粒都沿着与底基表面垂直的c轴方向一维高密度、单层有序排列。在激发波长为365 nm时,该一维取向LTL分子筛荧光阵列发出鲜艳的红色荧光。     

Synthesis of zeolite A from coal fly ash using ultrasonic treatment – A replacement for fusion step

The synthesis of zeolites from fly ash has become an increasingly promising remedy to the crisis of coal fly ash production and disposal in South Africa. In recent studies, South African fly ash was proven to be a suitable feedstock for the synthesis of essential industrially used zeolite A. However, the process involves a costly energy intensive step whereby fly ash is fused at high temperatures, which may make the process economically unattractive on a large scale. The aim of this study is to investigate the possibility of replacing high temperature fusion with less energy intensive sonochemical treatment for the synthesis of zeolite A. Sonochemical treatment was first thought possible due to the violent cavitation caused by high intensity sonication. The results of the study showed that fusion can be replaced by 10 min of high intensity sonication. The incorporation of sonication also consequently reduced the crystallization temperature of the process making it possible to synthesize a pure phase zeolite A at lower temperatures and reduced times. This study effectively developed a novel process to replace the energy intensive fusion step with a short, easy and inexpensive treatment. Scale up of this synthesis approach may proffer a promising alternative option to the anticipated energy demand of the synthesis of fly ash-based zeolite with fusion method.     

Conversion of silica by-product into zeolites by thermo-sonochemical treatment

The fine powdered silica by-product of processing of aluminum fluoride (fertilizer plant, Lithuania) was used for zeolite synthesis as silica and aluminum source. The effect of sonication time and the time of hydrothermal synthesis on crystallinity of the synthesized zeolite were studied. This allowed the transformation of the by-product to the mixture of Na–P zeolite and Na–X zeolite. It was determined that ultrasonic-assisted hydrothermal action effected the “diamond” shape formation of Na–P zeolite with clear crystal edges. Na–P zeolite had the morphology of pseudo-spherical forms constituted by small plates when hydrothermal treatment (without sonication) was use for the preparation of zeolites. Moreover, it was determined that ultrasonic-assisted hydrothermal method effected a reduction in the crystal size compared with the zeolites which were synthesized only by using hydrothermal synthesis. The total amount of zeolites as high as 88–93% was achieved after 24 h of hydrothermal treatment followed or unfollowed by sonication. By using longer duration (20 min) of ultrasound pretreatment it is possible to reduce the duration of hydrothermal synthesis: from 24 h to 12 h of hydrothermal treatment. In this case, similar results of total amount of zeolites were detected. In the present work, low-cost raw materials, such as silica by-product have been investigated for the production of zeolites.     

Synthesis of nanocomposites based on nanotubes and silicates

In situ synthesis of nanocomposites based on carbon nanotubes and zeolite/montmorillonite was carried out in a hot filament CVD reactor where the precursors (methane and hydrogen) are activated by carbonized tungsten filaments heated up to 2200 °C. In nanocomposites formed both on zeolite and montmorillonite we observed cross-linking of the catalytic particles by nanotubes and creation of carbon nanotube bridges and three-dimensional networks. The length of nanotube bridges was in a range from several nm to nearly 10 μm. A high density of carbon nanotubes was observed in the whole volume of zeolite. The high catalytic efficiency of zeolite is most likely caused by its structure that allows anchoring of Fe³⁺ catalytic particles in the pores and prevents their migration from the sample. At the ends of the nanotubes grown on zeolite we observed particles of the catalyst. In montmorillonite, the particles catalyzing the growth of carbon nanotubes may be present not only on the external surface but also in the interlayer voids of the mineral. Its catalytic efficiency is enhanced as proved by the higher amount of CNTs and their bundles. In the course of CNTs synthesis probably also clumps of Fe³⁺ catalytic particles arise, which may be the reason for formation of bundles of nanotubes.     

(K,Mo)Y分子筛中钼组分的EXAFS研究

应用同步辐射Eextended X-ray Ab sorption Fine S tructure(EXAFS)技术研究固态法制备的KHMoY分子筛的氧化态和硫化态样品以及硫化态KHY／MoO3样品中钼组分的局域配位环境结构,并与KHMoY和KHY／MoO3 样品催化加氢活性结果进行对照。结果表明,随原子比（K＋2Mo）／Al的变化,钼原子周围的配位环境有显著的差异。当（K＋2Mo）／Al时,KHMoY和KHY/MoO3硫化后,钼组分主要以MoS2小原子簇分散在分子筛超笼中;（K＋2Mo)/Al>1时,钼组分则有两种存在环境,即分子筛超笼中的和分子筛外表的钼组分。分子筛超笼中的Mo S2原子簇的催化加氢合成醇选择性较高;分子筛外表面的MoS2微小颗粒的尺寸相对于超笼中的要大许多,其合成醇选择 性较低。     

Ultrasound-assisted rapid hydrothermal design of efficient nanostructured MFI-Type aluminosilicate catalyst for methanol to propylene reaction

The influence of ultrasound-assisted rapid hydrothermal synthesis of aluminosilicate ZSM-5 catalysts was examined in this work. A series of MFI-type nanostructured materials with sonochemical approach and conventional heating were synthesized and evaluated for conversion of methanol to propylene reaction. The prepared samples were tested by characterization analyses such as XRD, FESEM, BET-BJH, FTIR, TPD-NH₃ and TG/DTG. The obtained results confirmed that ultrasound treatment enhanced the nucleation process and crystal growth for ZSM-5 sample synthesized at moderate temperature of 250 °C. Therefore, it was found the formation of pure MFI zeolite with high crystallinity and improved textural, structural and acidic properties for ZSM-5(UH-250) sample compared with the other zeolites. This observation was attributed to the relationship between the perfect crystallization mechanism and catalytic properties, which led to producing an efficient MFI zeolite toward the optimal catalytic performance. In this manner, the methanol conversion and products selectivity of prepared materials were carried out in MTP reaction at 460 °C and atmospheric pressure. The ZSM-5(UH-250) zeolite with slower deactivation regime exhibited the constant level of methanol conversion (84%) and high propylene selectivity (78%) after 2100 min time on stream. Moreover, the synthesis pathway for MFI zeolite at moderate temperature and also deactivation mechanism of improved sample were proposed.     

Effects of ultrasonic treatment on zeolite NaA synthesized from by-product silica

The synthesis of zeolite NaA from silica by-product was carried out in the presence of 20 kHz ultrasound at room temperature. Zeolites obtained in this type of synthesis were compared to zeolites obtained by performing conventional static syntheses under similar conditions. The sonication effects on zeolite NaA synthesis were characterized by phase identification, crystallinity etc. The effects of different parameters such as crystallization time and initial materials preparation methods on the crystallinity and morphology of the synthesized zeolites were investigated. The final products were characterized by XRD and FT-IR. It was possible to obtain crystalline zeolite NaA from by-product silica in the presence of ultrasound.     

氢在A、X及ZSM-5型沸石上的高压物理吸附

采用常规体积吸附装置测定了77、195、293K和7MPa的条件下氢在A、X及ZSM-5沸石上的吸附特性和吸附容量．所有的氢吸附等温线基本符合Ⅰ型等温线,但在77K,压力为2-5MPa的等温线上观察到了超临界高压吸附所特有的最大吸附量．从等温线确定了等量吸附热并讨论了其影响因素．根据骨架结构和所含阳离子类型的差异,各种沸石表现出不同的氢吸附量．其中NaX沸石在77K/4MPa下的重量储氢分数为2．55％,是该实验中所测得的最高吸附量．CaA、NaX和ZSM-5沸石的氢吸附量与其比表面积成正比,这与沸石中的可用空穴容积有关．然而NaA和KA沸石不存在这种线性关系．实验中还观察到,NaA与KA沸石间出现氢吸附量的临界值是由KA沸石中较大的阳离子堵塞效应引起的．该实验将吸附质分了的动力学直径与沸石主晶孔的有效直径之比用于判断物理吸附中的堵塞效应．