• Journal of the Mineralogical Society of Korea
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• v.21 no.4
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• pp.341-347
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• 2008

The feasibility of commercializing the hydrothermal synthesis of Na-A type zeolite from siliceous mudstone has been conducted using a 50-liter bench-scale autoclave and the application of the zeolite as an environmental remediation agent. Siliceous mudstone, which is widely distributed around the Pohang area, was adopted as a precursor. The siliceous mudstone is favorable for the synthesis of zeolite because it contains 70.7% $SiO_2$ and 10.0% $Al_2O_3$, which are major ingredient of zeolite formation. The synthesis of zeolite was carried out under the following conditions that had been obtained from the previous laboratory-scale tests: 10hr reaction time, $80^{\circ}C$ reaction temperature, $Na_2O/SiO_2$ ratio = 0.6, $SiO_2/Al_2O_3$ ratio = 2.0 and $H_2O/Na_2O$ ratio= 98.6. The crystallinity and morphology of the zeolite formed were similar to those obtained from the laboratory-scale tests. The recovery and cation exchange ion capacity were 95% and 215 cmol/kg, respectively, which are slightly higher than those obtained in laboratory scale tests. To examine the feasibility of the zeolite as an environmental remediation agent, experiments for heavy metal adsorption to zeolite were conducted. Its removal efficiencies of heavy metals in simulated waste solutions decreased in the following sequences: Pb > Cd > Cu = Zn > Mn. In a solution of 1500 mg/L total impurity metals, the removal efficiencies for these impurity metals were near completion (> 99%) except for Mn whose efficiency was 98%. Therefore, the synthetic Na-A type zeolite was proven to be a strong absorbent effective for removing heavy metals.

• Korean Chemical Engineering Research
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• v.53 no.3
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• pp.339-349
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• 2015

In this work, DAY (Dealuminated Y-type) zeolites were prepared to be used as easily regenerable and thermally stable adsorbent substituting activated carbon. NaY zeolites were transformed into DAY zeolites through ion exchange, calcination, steaming, and acid leaching. Calcination temperature and time, and steaming time were changed to increase the Si/Al ratio and maintain crystallinity. Adsorption of VOCs were done for prepared DAY, commercial NaY and Hisiv 1000 in air with relative humidity of 50%. The DAY zeolite prepared by calcination at $520^{\circ}C$ for 4 hrs and steaming for 7 hrs had a same structure and a Si/Al ratio of 80.4. Its adsorption capacity for water vapor was 10% of NaY, indicating its hydrophobicity. Its adsorption capacity for MEK was 0.8 times of Hisiv 1000, that for toluene 1.6 times, and that for EA 1.3 times.

• Journal of the Mineralogical Society of Korea
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• v.19 no.1 s.47
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• pp.7-14
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• 2006

Melting slag generated from the lots of municipal incineration ash, which causes the one of big urban problems in modern industrial society, was used as starting material for the hydrothermal synthesis of zeolite. P-type zeolite has been successfully synthesized by the combined process of both 'hydrogelation' and 'clay conversion' method. Commercial sodium silicate was used as Si source, and $NaAlO_2$ was prepared by the reaction in a $Na_{2}O/Al_{2}O_{3}$ molar ratio of 1.2. The optimum conditions for zeolite synthesis was found to be the $SiO_{2}/Al_{2}O_{3}$ ratio in the 3.2 and 4.2 range, the $H_{2}O/Na_{2}O$ ratio in the 70.7 and 80.0 range, and more than 15-hour reaction time at $80^{\circ}C$, In the synthesized zeolite, inhomogeneous melting slag particles were disappeared and homogeneous P-type zeolite crystal was grown. The cation exchange capacity of the synthesized zeolite was determined to be approx. 240 cmol/kg.

• Bulletin of the Korean Chemical Society
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• v.28 no.10
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• pp.1675-1682
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• 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 Journal of Crystallography
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• v.12 no.2
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• pp.97-101
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• 2001

Phillipsite-type zeolite powders were synthesized from domestic coal fly ash by hydrothermal reaction with 2.0 M-3.5M NaOH solution at $80^{\circ}C{\sim}120^{\circ}C$ for 24 h. The properties of zeolite were investigated by XRD, SEM and IR spectroscopy. The effects of chemical composition of fly ash, reaction temperature and NaOH concentration on the zeolite synthesis were well appeared on IR spectra. It is found that the $TO_4$(T=Si, Al) tetrahedra have a well ordered structure as the $SiO_2$ content, synthesis temperature and NaOH concentration become high.

• Journal of the Mineralogical Society of Korea
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• v.21 no.1
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• pp.37-44
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• 2008

This study was performed to synthesize Na-A type zeolite with melting slag from the Mapo incineration site and recycle the zeolite as an environmental remediation agent. The melting slag used had a favorable composition containing 26.6% $SiO_2$, 10.9% $Al_2O_3$ and 2.7% $Na_2O$ for zeolite synthesis although there were high contents of iron oxides, including 19.6% $Fe_2O_3$ and 18.9% FeO, which had been used as a flux for the melting. It was confirmed that the Na-A type zeolite could be successfully synthesized at $80^{\circ}C$ and $SiO_2/Al_2O_3\;=\;0.80{\sim}1.96$. The cation exchange capacities (CEC) of the zeolites was determined to be about 220 cmol/kg leveled off at the synthetic time more than 10hrs. The adsorption capacities of zeolite to heavy metals (Cd, Cu, Mn and Pb) were high except for As arid Cr. It was also confirmed through the Eh and pH analysis that As and Cr existed in the forms of $HAsO_4^{2-}$ and $CrO_4^{2-}$. The low absorption rates of zeolite for As and Cr are attributed to the fact that the pore size ($4\;{\AA}$) of Na-A type is smaller than those of $HAsO_4^{2-}$ and $CrO_4^{2-}$ ions ($4\;{\AA}$ ionic radii and $8\;{\AA}$ diameter).

• Membrane Journal
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• v.18 no.3
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• pp.250-255
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• 2008

Zeolite A have been known to be chemically, mechanically and thermally quite stable. The ion-exchanged membranes were tested for the removal of water from ethanol/water mixtures by pervaporation. Since it is quite difficult to prepare the potassium form of zeolite A by a direct synthesis, it was obtained by the ion-exchange method from NaA zeolite. The effects of concentration of ethanol at the feed side and the temperature were studied on the permeation flux and the separation factor of water. After $Na^+$ ion was exchanged to $K^+$ ion, it was found that the total flux decreased and the separation factor increased.

• Journal of Environmental Science International
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• v.28 no.6
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• pp.561-570
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• 2019

A zeolitic material (Z-Y2) was synthesized from Coal Fly Ash (CFA) using a fusion/hydrothermal method under low-alkali condition (NaOH/CFA = 0.6). The adsorption performance of the prepared zeolite was evaluated by monitoring its removal efficiencies for Sr and Cs ions, which are well-known as significant radionuclides in liquid radioactive waste. The XRD (X-ray diffraction) patterns of the synthesized Z-Y2 indicated that a Na-A type zeolite was formed from raw coal fly ash. The SEM (scanning electron microscope) images also showed that a cubic crystal structure of size $1{\sim}3{\mu}m$ was formed on its surface. In the adsorption kinetic analysis, the adsorption of Sr and Cs ions on Z-Y2 fitted the pseudo-second-order kinetic model well, instead of the pseudo-first-order kinetic model. The second-order kinetic rate constant ($k_2$) was determined to be $0.0614g/mmol{\cdot}min$ for Sr and $1.8172g/mmol{\cdot}min$ for Cs. The adsorption equilibria of Sr and Cs ions on Z-Y2 were fitted successfully by Langmuir model. The maximum adsorption capacity ($q_m$) of Sr and Cs was calculated as 1.6846 mmol/g and 1.2055 mmol/g, respectively. The maximum desorption capacity ($q_{dm}$) of the Na ions estimated via the Langmuir desorption model was 2.4196 mmol/g for Sr and 2.1870 mmol/g for Cs. The molar ratio of the desorption/adsorption capacity ($q_{dm}/q_m$) was determined to be 1.44 for Na/Sr and 1.81 for Na/Cs, indicating that the amounts of desorbed Na ions and adsorbed Sr and Cs ions did not yield an equimolar ratio when using Z-Y2.

• Journal of the Korean Ceramic Society
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• v.25 no.6
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• pp.685-693
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• 1988

From leaching of Korean native halloysite with hot sulfuric acid, active species of siliceous aluminosilicate are obtained as residue, which gives the mole ratio of SiO2/Al2O3 10 and substantially removes most acid-soluble impurities. By dissolving the residue in sodium hydroxide at an ambient temperature sodium silicate solution is prepared, this is used for zeolite synthesis as one of starting materials. In order to prepare zeolite Type 4A thereform, addition of a proper aluminum source is made so that the composition of the reactant materials may be of the following mole ratios : Na2O/SiO2=1.2-1.5, SiO2/Al2O3=1.8-2.0 and H2O/Na2O=34-45 By careful control of ageing time and temperature, subsequent crystal growth is induced into microfine zeolite 4A, which gives optimum particle size distributjion being suitable for detergent builder. The zeolite products thus obtained and highly competitive with those from the use of the refined clay in comparison of their calcium exchange capacity, whiteness and particle size distribution. The present method shows a marginal advantage over the existing procedures requiring neitherseparate purification nor calcinating otherwise necessary for the raw clay ores in use.

• Journal of the Mineralogical Society of Korea
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• v.18 no.1
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• pp.11-17
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• 2005

Na-A zeolite were synthesized from melting slag of the incinerated ash by the alkaline activation processes. The experiments were performed in stainless steel vessels, with continuous stirring during the reaction periods. The silica-rich solution, a starting material, which was the waste of crystal growth factory, contains 5.7 wt% SiO₂ and 3.2 wt% Na₂O. And NaAlO₂ was made by the reaction of aluminium dross and NaOH solution and its molar ratios were Na₂O/Al₂O₃= 1.2 and H₂O/Na₂O=9. During the residence time of 7∼8 h at 80℃, the mixing of the silica-rich solution, NaAlO₂ and melting slag yields the production of homogeneous Na-A zeolite. The optimal reactant composition in molar ratio of Na₂O:Al₂O₃:SiO₂ was 1.3∼l.4 : 0.8∼0.9 : 2 and mixing ratio of solution and slag was 1/7∼10 (g/cc). Synthesized Na-A zeolite has cubic form uniformly and its size ranges about 1 ㎛. Ca/sup 2+/ ion exchange capacity of the Na-A was about 180∼210 meq/100g, corresponding approximately 80% to the commercial detergent builder.