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Synthesis Of Different Condensed Matter Zeolite Materials

Posted on:2012-02-01Degree:DoctorType:Dissertation
Country:ChinaCandidate:N L YueFull Text:PDF
GTID:1111330368478930Subject:Inorganic Chemistry
Abstract/Summary:PDF Full Text Request
Zeolite has been used in industrial production and real life widely because of the nano structure, ion-exchange, acid and alkali resistant and other special physical and chemical characteristics. With the progress of science and technology, people greatly expand the application range of zeolites, from the initial separation, catalysis and adsorption to the electronic components, optical materials, biological materials and other applications. In recent years the functionalized zeolite has been used in other field. Zeolite membrane, spheres and block have been synthesized. Therefore our research work focused on the synthesis of different condensed matter zeolite materials, and the investigation of the influence of the synthesis conditions on the zeolite.The main application of molecular sieve membrane is used in separation of gas and liquid, the actual application of molecular sieve can be used for separation technology have large order membrane and integrity, so how to synthesize high mechanical strength and high permeability zeolite membranes become the key factors. Zeolite Y membranes supported on stainless-steel-net were synthesized using a seed method coupled with a secondary hydrothermal treatment for the first time. The zeolite membrane is intergrowth well, continuous, high degree of crystallization. Because the nets hole of stainless-steel-net (about 40 x 40μm) is much bigger than the zeolite Y nanocrystalline (about 300nm), in experiments we used detergent to increase the hydrophobic of the stainless-steel-net. During the synthesis of zeolite FAU, the impurity phase of zeolite GIS usually appear, due to the size of holes of zeolite P (0.31*0.44nm[100], 0.26*0.49nm[010]) is less than zeolite Y (0.74*0.74nm) the membrane permeability and the mechanical strength become lower. In this paper, through controlling reaction time and the number of secondary growth got dense Y zeolite membranes, avoiding P type molecular sieve miscellaneous phase formation. We got pure zeolite Y membranes testified by the XRD measurement. The membranes we synthesized were compact and no remarkable defects according to the SEM measurement. The thickness of the membrane was about 1.0μm after a hydrothermal treatment and about 3μm after hydrothermal treatment twice. This kind of membrane can be used to separate some relevant gases and to catalyze some reactions. We used the same method to synthesis zeolite Y membrane on other substrates and we optimized the synthesis parameters.In recent years a series of solid particles have been used to preparation of emulsion (Pickering emulsion), including metal oxides, metal hydroxides, silica, clay and carbon particles. We prepared emulsion in which the zeolite as emulsifier, and inspected two important factors pH value of emulsion and ionic strength mainly. The emulsion can be stable over a year in room temperature and being static placed. Usually, most of stable hollow zeolite spheres are prepared by the combination of the layer-by-layer self-assembly technique and the sacrificial core-shell technique, which includes three steps: the formation of cores, zeolite shells and hydrothermal treatment.Up to now, the different templates including the polystyrene microsphere, mesoporous silica spheres, and fly ash cenosphere, etc. have been reported in the preparation of hollow zeolite spheres acting as cores, and these cores control the spherical morphology and the size of the composite. We have successfully fabricated hollow silicalite-1 spheres through the preparation of emulsion coupled with hydrothermal treatment stabilized by silicalite-1 crystals. We used different organisms (1-octanol and toluene) and different emulsification method (hand shake and mechanical agitation) to synthesis hollow zeolite spheres with millimeter and micron size. The XRD, SEM, nitrogen adsorption and thermogravimetric analysis shows that the zeolite spheres are uniform, complete and monolayered. The cross-sectional image of the spheres with millimeter indicates the crystal intergrowth process in the sphere shells obviously. The oil phase acts as a template in the formation of sphere, so the interiors can be functionalized by dissolving the guest molecules in the oil. This method will open up a new route for the preparation of hollow spheres, and can be applied to modify the sphere interior structures to prepare multi-functional materials. In addition, we prepared different shape with different sizes of zeolite SOD nanocrystalline in ethanol and water system, and obtained SOD nanocrystals in large scale of Si/Al. By XRD and SEM characterization found that as silica content of different got flower shape and granular disperses nanocrystalline. Inspects the feeding Si/Al, the influence of molecular sieve synthesis than in a certain range of silicon aluminium material than by adjusting the silicon aluminium can be pure phase than the LTA type and FAU type molecular sieve, inspects two control molecular sieve synthetic factors affecting the influence of aluminum than scope of silicon. Characterized by XRD found that other parameters under the condition of the same pure water system and the product of alcohol water system has been completely different, this is to further research the formation mechanism of the zeolite has very important significance.
Keywords/Search Tags:Zeolite membranes, Zeolite spheres, nanocrystals, Condensed matter
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