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

• Korean Chemical Engineering Research
• /
• v.51 no.2
• /
• pp.203-207
• /
• 2013

Zeolites with different structures were synthesized from the hydrothermal synthesis condition employing simple structure directing agent (SDA) containing piperidine moiety. The gel containing $1.0SiO_2$:0.9SDA:$0.062NaAlO_2$:0.217NaOH:$20H_2O$ was subject to hydrothermal synthesis at 413~453 K for 7 days. FER type zeolite was obtained at 433 K when piperidine was employed as SDA, whereas TON and MFI type zeolites were also obtained at 433 K when 2,6-dimethylpiperidine and 2,2,6,6-tetramethylpiperidine were used, respectively. Further increase of hydrothermal synthesis temperature to 453 K resulted in the formation of TON type zeolite when 2-mtheylpiperidine was used. The structural analysis of powder X ray diffraction pattern over FER type zeolite suggested that the SDA, piperidine interacted intimately with the zeolite where it located close to the framework.

• Journal of radiological science and technology
• /
• v.29 no.3
• /
• pp.147-155
• /
• 2006

The crystal structures of fully dehydrated $K_3Na_8H-A(R_1=0.0478,\;R_2=0.0458\;and\;a=12.257(1){\AA})$ have been studied by single-crystal x-ray diffraction methods in the cubic space group. Pm3m in order to understand the structure of the zeolite as a gas storage medium and the mechanisms based on the encapsulation and decapsulation processes of gas molecules. In the crystal structures of dehydrated $K_3Na_8H-A$, three $K^+$ ions per unit cell are located on the 8-oxygen ring(0.0, 0.4531, 0.4531) and eight $Na^+$ ions per unit cell are located near the centers of 6-oxygen rings. Each $K^+$ ions on the 8-ring is $2.87(2){\AA}$ and $2.79(1){\AA}$ away from two kinds of framework oxygen atoms. These values are more realistic than previously known values in $K_{12}Na-A$. The exact positions of $K^+$ ions are ca. $0.8{\AA}$ away from the centers of the 8-rings which are previously reported as the preferred location of $K^+$ ions. Because the zeolites frameworks are stabilized as the results, more effective controls of gas molecules at encapsulation, decapsulation, and storage are achieved. Additionally, the available storage volumes are also maximized and more volume of gases can be stored in the materials. Therefore, oxygen storage bottles in hospital can be minimized and portable oxygen bottles for patients in emergency can be developed by using the materials.

• Korean Chemical Engineering Research
• /
• v.56 no.4
• /
• pp.600-606
• /
• 2018

The influence of acidity in MTT zeolite of different Si/Al molar ratio's on the catalyst activity in methanol-to-olefin (MTO) reaction has been investigated. The Si/Al ratio was controlled with the Al content in the gel when N,N,N',N'-tetramethyl-1,3-diaminopropane was used as a structure directing agent (SDA). The gel composition was controlled to $20SiO_2$ : 30SDA : x (=0.25~1.25)$NaAlO_2$ : 2NaOH : $624H_2O$, which was subject to the hydrothermal synthesis at 433 K for 4 days. As the composition of sodium aluminate decreased, the particle size of MTT zeolite increased, and also the amount of acid sites decreased. To investigate the catalytic performance, MTO reaction was carried out at 673 K with $1.2h^{-1}$ WHSV. It was found that the H-MTT (1.00Al) catalyst with a Si/Al molar ratio of 24 maintained the methanol conversion over 90% for 900 min.

• Journal of the Mineralogical Society of Korea
• /
• v.19 no.4 s.50
• /
• pp.301-310
• /
• 2006

Smectites were synthesized from Na-P type and Na-A type zeolites by the hydrothermal synthetic method, and their physicochemical properties were studied. The optimal synthetic conditions for producing smectite were $290^{\circ}C$, 72 hr and $75{\sim}100kgf/cm^2$ in autogenous pressure. pHs of initial reaction solutions for the synthesis of smectites from Na-P type and Na-A type zeolite s were pH 6 and pH 10, respectively. The synthetic smectite was confirmed as $12{\AA}$-beidellite by a series of analysis such as X-ray diffraction analysis with random and oriented mounts, ethylene glycol treatment, and Greene-Kelly test, and their several physicochemical properties were studied.

• Bulletin of the Korean Chemical Society
• /
• v.28 no.10
• /
• pp.1675-1682
• /
• 2007

Large colorless single crystals of faujasite-type zeolite with diameters up to 200 μm have been synthesized from gels with the composition of 3.58SiO2:2.08NaAlO2:7.59NaOH:455H2O:5.06TEA:1.23TCl. Two of these, colorless octahedron about 200 μm in cross-section have been treated with aqueous 0.1 M TlC2H3O2 and KNO3 in order to prepare Tl+- and K+-exchanged faujasite-type zeolites, respectively, and then determined the Si/Al ratio of the zeolite framework. The crystal structures of |Tl71|[Si121Al71O384]-FAU and |K53Na18|[Si121Al71O384]-FAU per unit cell, a = 24.9463(2) and 24.9211(16) A, respectively, dehydrated at 673 K and 1 × 10-6 Torr, have been determined by single-crystal X-ray diffraction techniques in the cubic space group Fd m at 294 K. The two single-crystal structures were refined using all intensities to the final error indices (using only the 905 and 429 reflections for which Fo > 4σ(Fo)) R1/R2 = 0.059/0.153 and 0.066/0.290, respectively. In the structure of fully Tl+-exchanged faujasite-type zeolite, 71 Tl+ ions per unit cell are located at four different crystallographic sites. Twenty-nine Tl+ ions fill site I' in the sodalite cavities on 3-fold axes opposite double 6-rings (Tl-O = 2.631(12) A and O-Tl-O = 93.8(4)o). Another 31 Tl+ ions fill site II opposite single 6-rings in the supercage (Tl-O = 2.782(12) A and O-Tl-O = 87.9(4)o). About 3 Tl+ ions are found at site III in the supercage (Tl-O = 2.91(6) and 3.44(3) A), and the remaining 8 occupy another site III (Tl-O = 2.49(5) and 3.06(3) A). In the structure of partially K+-exchanged faujasite-type zeolite, 53 K+ ions per unit cell are found at five different crystallographic sites and 18 Na+ ions per unit cell are found at two different crystallographic sites. The 4 K+ ions are located at site I, the center of the hexagonal prism (K-O = 2.796(8) A and O-K-O = 89.0(3)o). The 10 K+ ions are found at site I' in the sodalite cavity (K-O = 2.570(19) A and O-KO = 99.4(9)o). Twenty-two K+ ions are found at site II in the supercage (K-O = 2.711(9) A and O-K-O = 94.7(3)o). The 5 K+ ions are found at site III deep in the supercage (K-O = 2.90(5) and 3.36(3) A), and 12 K+ ions are found at another site III' (K-O = 2.55(3) and 2.968(18) A). Twelve Na+ ions also lie at site I' (Na-O = 2.292(10) and O-Na-O = 117.5(5)o). The 6 Na+ ions are found at site II in the supercage (Na-O = 2.390(17) A and O-Na-O = 113.1(11)o). The Si/Al ratio of synthetic faujasite-type zeolite is 1.70 determined by the occupations of cations, 71, in two single-crystal structures.

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

• Applied Chemistry for Engineering
• /
• v.30 no.6
• /
• pp.726-730
• /
• 2019

The removal of calcium ions using zeolite to solve problems of the CaCO₃ manufacturing process using cement kiln dust was investigated. To do so, a modified zeolite was employed and experiments were conducted to select the optimal zeolite type considered the binding cation and structure, evaluate the removal performance of calcium ions, the influence of the type and concentration of the modifying solution, and the removal selectivity when K coexists. Among five zeolites, 13X zeolite was found to have the best calcium ion removal performance, and it was confirmed that the removal performance was enhanced when KCl was used as a modifying solution instead of NaCl. This study is expected to be the basis for the solution of carbonation process and high concentration of KCl recovery technology.

• Clean Technology
• /
• v.26 no.4
• /
• pp.263-269
• /
• 2020

Zeolite was synthesized hydrothermally using the water-treatment sludge, and the effects of various synthesis parameters like reaction temperature, reaction time, and Na2O/SiO2 molar ratio on the crystallization of zeolite were investigated. Crystal structure, physical property, and thermal stability of zeolite crystals were characterized by X-ray powder diffraction, FTIR spectroscopy, BET nitrogen adsorption, and TGA measurements. The removal efficiencies of nitrogen in ammonia, heavy metal ions, and TOC were calculated to evaluate zeolite's adsorption capacity. The primary chemical composition of water-treatment sludge was 28.79% Al2O3 and 27.06% SiO2. The zeolites were synthesized by merely employing the water-treatment sludge as silica and alumina sources without additional chemicals. Zeolite crystals synthesized through the water-treatment sludge were confirmed as an A-type zeolite structure. Zeolite A had the highest crystallinity obtained from a gel with the molar composition 2.1Na2O-Al2O3-1.6SiO2-65H2O after 5 h at a temperature of 90 ℃. The specific surface area of zeolite obtained was 55 ㎡ g-1, which was higher than commercial zeolite A. The removal efficiency of nitrogen in ammonia was 68% after 3 h of reaction time, while the removal efficiencies of Pb2+ and Cd2+ ions were 99.1% and 99.3%, respectively. These results indicate active ion exchange between Pb2+ or Cd2+ ion and Na+ ion in the zeolite framework. The adsorption experiments on the different zeolite addition conditions were performed for 3 h with 300 ppm humic acid. Based on the results, TOC's highest efficiency was 83% when 5 g of zeolite was added.

• Applied Chemistry for Engineering
• /
• v.9 no.3
• /
• pp.317-321
• /
• 1998

X-type Zeolite for the gas separation was prepared by hydrothermal methods and the zeolite was ion-exchanged with KCl, $CaCl_2$, $YCl_3$ and $InCl_3$ in order to investigate the effect of ions on the properties of molecular sieves. Adsorption isotherms of $CO_2$ on ion exchanged X-type zeolites and those of $O_2$ and $N_2$ on the synthesized zeolite were measured at $25^{\circ}C$ using a volumetric method and the adsorption characteristics were compared with each other. Model parameters for the Langmuir, Freundlich and Toth equations were regressed for the measured adsorption isotherms. In order to confirm the applicability of the zeolite on $CO_2-PSA$ processes, breakthrough tests and process simulation were undertaken. It was found that the X-type zeolite could be a potential adsorbent in recovering $CO_2$ from flue gas.