• Proceedings of the KSEEG Conference
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• 2007.04a
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• pp.523-523
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• 2007

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• Korean Chemical Engineering Research
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• v.49 no.5
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• pp.657-663
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• 2011

Structure directing agent(SDA) containing piperidine moiety such as piperidine(PI), 2-methylpiperidine (MPI), 2,6-dimethylpiperidine(DMPI) and 2,2,6,6,-tetramethylpiperidine(TMPI), respectively has been utilized to synthesize aluminophosphate zeolite using hydrothermal method. The gel composition was $1.0Al_2O_3:1.0P_2O_5:0.76SDA:45H_2O$ and the hydrothermal heating was performed in an oven at 443 K and for 7 days at static mode. The obtained zeolitic material contained a lamellar structure when PI was used as the SDA. With a progressive increase of the SDA size, various structures of aluminophosphate including AlPO-5 of AFI structure were obtained. The aluminophosphate of SAS structure was formed when the largest TMPI was utilized as the SDA, which was confirmed by the Rietveld refinement. The result of $^{27}Al$ and $^{31}P$ MAS NMR of the sample suggested that Al and P were incorporated into the framework of the aluminophosphate.

• Proceedings of the Korean Radioactive Waste Society Conference
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• 2012.05a
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• pp.265-266
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• 2012

• Korean Journal of Crystallography
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• v.15 no.2
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• pp.59-68
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• 2004

Three crystal structures of dehydrated partially $Co^{2+}-exchanged$ zeolite A treated with 0.6 Torr of K at $300^{\circ}C$ (for 12 hrs, 6 hrs, and 2 hrs) vapor have been determined by single-crystal X-ray diffraction techniques in the cubic space group Pm3m at 21(1)$^{\circ}C(a=12.181(1)\;{\AA},\;a=12.184(1)\;{\AA},\;and\;a=12.215(1)\;{\AA})\;respectively)$. Their structures were refined to the final error indices, R(weight) of 0.090 with 10 reflections, 0.091 with 82 reflections, and 0.090 with 80 reflections, respectively, for which $1>\sigma(I)$. In each structure, all four $Co^{2+}$ and four $Na^+$ ions to be reduced by K atoms. The cobalt and sodium atoms produced are no longer found in the zeolite. K species are found at five different crystallographic sites: three $K^+$ ions lie at the planes of 8-rings, filling that position, ca. 11.5 K^+$ ions lie on threefold axes, ca. 4.0 in the large cavity and ca. 4.0 in the sodalite cavity, and ca. 0.5 $K^+$ ion is found near a 4-ring. ca. three $K^0$ atoms are found deep into the large cavity on threefold axes. In these structures, crystallographic results show that cationic tetrahedral $K_4$ (and/or triangular $K_3$) clusters have formed in the sodalites of zeolite A. The $K_4$ and/or $K_3$ clusters coordinate trigonally to three oxygens of a six-oxygen ring. The partially reduced ions of these clusters interact primarily with oxygen atoms of the zeolite structure rather than with each other. ca. 14.5K species are found per unit cell, more than the twelve $K^+$ ions needed to balance the anionic charge of zeolite framework, indicating that sorption of $K^0$ has occurred. The three $K^0$ atoms in the large cavity are closely associated with three out of four $K^+$ ions in the large cavity to form $K_7^{4+}$ clusters. The $K_7^{4+}$ cluster not interacts primarily with framework oxygens.

• Journal of the Korean Chemical Society
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• v.51 no.2
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• pp.178-185
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• 2007

Intermediate pentasil borosilicate zeolite-like materials have been crystallized by a novel method named steam-assisted conversion, which involves vapor-phase transport of water. Indeed, amorphous powders obtained by drying Na2O.SiO2.B2O3.TBA2O gels of various compositions using different boron sources are transformed into crystalline borosilicate zeolite belonging to pentasil family structure by contact with vapors of water under hydrothermal conditions. Using a variant of this method, a new material which has an intermediate structure of MFI/MEL in the ratio 90:10 was crystallized. The results show that steam and sufficiently high pH in the reacting hydrous solid are necessary for the crystallization to proceed. Characterization of the products shows some specific structural aspects which may have its unique catalytic properties. X-ray diffraction patterns of these microporous crystalline borosilicates are subjected to investigation, then, it is shown that the product structure has good crystallinity and is interpreted in terms of regular stacking of pentasil layers correlated by inversion centers (MFI structure) but interrupted by faults consisting of mirror-related layers (MEL structure). The products are also characterized by nitrogen adsorption at 77 K that shows higher microporous volume (0.160 cc/g) than that of pure MFI phase (0.119 cc/g). The obtained materials revealed high surface area (~600 m2/g). The infrared spectrum reveals the presence of an absorption band at 900.75 cm-1 indicating the incorporation of boron in tetrahedral sites in the silicate matrix of the crystalline phase.

• Journal of the Korean Institute of Gas
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• v.9 no.4 s.29
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• pp.17-25
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• 2005

The dealuminated and alkali/alkaline-earth metal exchanged Y-zeolites were prepared as a catalyst. Elemental compositions and structures of the prepared catalysts were analyzed by the various spectroscopic techniques such as inductively coupled plasma-atomic emission spectroscopy(ICP-AES), X-ray fluorescence(XRF) and X-ray diffraction(XRD), and the desorption behaviors of adsorbed species on the catalyst surfaces were investigated via NO-TPD experiment. Comparing with the composition of the starting material of NaY zeolite, the magnitudes of Si/Al ratio in catalytic materials were increased after dealumination. The Si/Al ratio of catalytic materials after dealumination followed by Cs and Ba cation exchange were additionally decreased. Dealumination to catalysts induced a destruction of basic frame due to a detachment of aluminum, which results in reducing framework structure, while increasing non-framework structure. This phenomenon becomes more serious with increasing time of steam treatment and even more significant for the cation exchanged catalysts. In NO-TPD experiments, the desorption peaks of NO which indicates an activity point of catalysts shifted to the low temperature region after dealumination and cation exchange. The desorption peaks of the NO-TPD profiles taken after steam treatment also shifted to the low temperature region as the steam treatment time increased. In dealuminated and cation exchanged Y-zeolites, the catalytic activities were more influenced by exchanged cation and the formation of non-framework structure.

• Journal of the Korean Chemical Society
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• v.33 no.4
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• pp.357-365
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• 1989

The positional parameters of framework atoms, cations, and water molecules in hydrated and dehydrated $Mg_4Na_4-A$, $Ca_6-A$, $Zn_5Na_2-A$ and $Co_4Na_4-A$ were determined by the optimization technique using some potential energy functions and VAIOA optimization program. Upon dehydration, cations in hydrated states move toward the framework oxygens of 6 rings. Frameworks of fully dehydrated zeolite A are more stable than those of fully dehydrated divalent cation exchanged Zeolite A. There are three different kinds of water molecules in divalent cation exchanged Zeolite A; W(III) (water molecules having hydrogen bonds), W(II) (water molecules associated with $Na^+$ ions), and W(I) (water molecules associated with divalent cations). Three different DTA endothermic peaks were observed corresponding to the dehydration of three different kinds of water molecules in divalent cation exchanged Zeolite A.

• Membrane Journal
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• v.18 no.3
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• pp.198-205
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• 2008

A novel technology for homogeneous deposition of zeolite particles on a porous support was developed so that those particles played a seeding role for the growth of zeolite crystals. After the particles were dispersed in water, the aqueous solution was 134 through the bore of a porous tubular support. By keeping the other side of the support in a vacuum, the aqueous solution passed through the pores of the support, leading the particles to be homogeneously deposited on the support. The amount of the deposited particles was investigated by changing the following operating parameters: a particle concentration in the solution, a time for deposition, and the feeding rate of the solution. The amount of the deposited particles increased from 0.0019 g to 0.0208 g as the concentration of the particles was changed from 0.01 wt% to 0.3 wt%, while the feeding rate and the deposition time were kept to 100 mL/min and 4 min, respectively. As the deposition time was varied from 1 min to 4 min, the deposition amount increased from 0.0004g to 0.0019g at the typical condition of the rest parameters. Also, it was observed that the deposited weight increased from 0.0029 g to 0.01 g as the feeding rate increased from 100 mL/min to 300 mL/min. However, the total permeance of water and ethanol decreased through the zeolite membrane as the deposited weight increased.

• Korean Chemical Engineering Research
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• v.45 no.2
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• pp.160-165
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• 2007

The synthesis and the characterization of Low Silica X (LSX) zeolite for nitrogen adsorption have been studied. The performance of LSX zeolite for nitrogen adsorption was compared to that of the commercial zeolite. The $Na_2O/(Na_2O+K_2O)$ ratio in the gel and the crystallization time were fixed as the synthetic factor. The LSX zeolite was formed at the $Na_2O/(Na_2O+K_2O)$ ratio of 0.75. The formation of LSX zeolite was confirmed by XRD and SEM. The Si/Al ratio was investigated by using XRF and FT-IR. The synthesized LSX zeolite showed a lower Si/Al ratio than the NaY and NaX zeolites although they have a same faujasite structure. The Si/Al ratio of the LSX zeolite converged close to 1. 1A (Li, Na, K) and 2A (Mg, Ca, Ba) group elements were ion-exchanged to the LSX zeolite. As the charge density of cation rises, the amount of nitrogen adsorbed increased. $Li^+$ ion-exchanged LSX zeolite showed the highest nitrogen adsorption weight. When the Li/Al ratio was over 0.65, nitrogen adsorption increased remarkably. $Li^+$ ions located on the supercage (site III, III') in the LSX zeolite played a role as nitrogen adsorption sites. When the $Ca^{2+}$ ions were added to the LiLSX zeolite by ion-exchange method, the performance for nitrogen adsorption increased more. The performance for the nitrogen adsorption was the highest at the Ca/Al ratio of 0.26. Nitrogen adsorption capacity of LiCaLSX (Ca/Al=0.26) zeolite was superior to the commercial NaX zeolite.

• Korean Chemical Engineering Research
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• v.44 no.4
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• pp.329-339
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• 2006

The production of lower olefins from methanol becomes an attractive process because of the rapid increase in crude oil price. This paper reivews the conversion mechanisms of methanol to hydrocarbons over zeolite and SAPO molecular sieve catalysts to understand the formation steps of lower olefins from methanol. The feasibility of the conversion mechanisms such as the direct mechanism based on well-defined intermediates and the hydrocarbon pool mechanism involving hydrocarbon moieties as an active centers is discussed with reepect to the induction period, the selectivity for products and the deactivation phenomena of the methanol conversion. The literature appeered since 1999 for the structure of the hydrocarbon pool and its catalytic role in the methanol conversion are summariged, and the prospect for the methanol-to-olefins process is described.