• Korean Journal of Soil Science and Fertilizer
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• v.32 no.1
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• pp.39-46
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• 1999

This study was performed to examine the effect of initial composition ratio and various reaction conditions on CEC and crystallinity of the product in hydrothermal synthesis of zeolitic materials from fly ash. Na-P1 zeolite was formed from the mixture with $SiO_2/Al_2O_3$ ratio above 2.55, however from the mixture with $SiO_2/Al_2O_3$ ratio below 2.25 hydroxy sodalite was formed. The CEC of reaction product(Na-P1 zeolite) treated with 3N-NaOH, $Na_2O/Al_2O_3$ ratio 2.55 and $SiO_2/Al_2O_3$ ratio 2.0 for 12 hours at $103^{\circ}C$ was about $285cmol^+kg^{-1}$, which was higher than those of the products of other reaction condition. The crystallinity of Na-P1 zeolite as high as 45.1% was attained at the optimum reaction condition of 2N-NaOH, $SiO_2/Al_2O_3$ ratio 2.55, $Na_2O/Al_2O_3$ ratio 1.5 for 12 hours at $103^{\circ}C$. The XRD peak of the reaction product could be measured at 7.16, 5.04, 4.12, 3.18, $2.69{\AA}$ and tetragonal pillar shape observed by SEM image be characteristic for Na-P1 zeolite. Judging from the result, it should be considered the optimum synthesis condition for Na-P1 zeolite from fly ash was 2~3N NaOH, $SiO_2/Al_2O_3$ ratio 2.55 and $Na_2O/Al_2O_3$ ratio 1.5~2.0 for 12 hours at $80{\sim}103^{\circ}C$.

• The Journal of the Petrological Society of Korea
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• v.6 no.2
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• pp.123-132
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• 1997

In the system $MgO-SiO_2-H_2O$, Talc[$Mg_3Si_4O_{10}(OH)_2$] has been synthesized hydrothermally at 200 MPa, $600^{\circ}C$ from the oxide mixture of the bulk composition of talc. The oxide mixture of the bulk composition of anthophyllite$[Mg_7Si_8O_{22}(OH)2]$ converted to talc, enstatite $(MgSiO_3)$, quartz at 200 MPa, $750^{\circ}C$ with excess of $H_2O$. In low to medium pressure metramorphism, enstatite-talc assemblage is metastable relative to anthophyllite with the reaction talc + 4 enstatite=anthophyllite (Greenwood, 1963). The high temperature stability of talc is bounded with the dehydration reaction to anthophyllite rather than that to enstatite(Greenwood, 1963; Chernosky et al., 1985). Therefore our experiment result assemblage, enstatite-talc-quatz at 200 MPa, $750^{\circ}C$ from oxide mixture of bulk compostion of anthophyllite is metastable assemblage. The hydrothermal experiment performed at 41 to 243 MPa, 680 to $760^{\circ}C$ with the starting material composed of synthetic talc, enstatite and quartz. Talc or enstatite grows during the runs and no extra phases including anthophyllite nucleated. Based on the increase or decrease of the each phase from run products, one of the possible reactions is talc=3 enstatite+quartz+H_2O$. The reversal bracket of the reaction is 699 to $700^{\circ}C$ at 100 MPa. Talc is stable up to $740^{\circ}C$ at 200 MPa and enstatite grow at $680^{\circ}C$, 40 MPa and at $760^{\circ}C$, 250 MPa. Though the high temperature limit of talc around 200 MPa is bounded thermodynamically by the reaction, 7 talc=3 anthophyllite+4 quartz+4 H_2O$, talc persisted throughout the previous reaction up to the reaction, talc=3 enstatite+quartz+$H_2O$.

• Applied Chemistry for Engineering
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• v.30 no.6
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• pp.749-756
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• 2019

Na-X and Na-A zeolites that give high adsorption capacity for heavy metals in an aqueous system were synthesized from the coal fly ash obtained from a thermoelectric power plant using a fusion method. The characteristics and Cu(II) adsorption capacity of the synthetic zeolites were also compared to those of using a commercial zeolite. For the selection of optimum conditions of zeolite synthesis, the effects of major parameters in the fusion method such as a dosage ratio of NaOH, aging time, hydrothermal reaction time, and also the dosage ratio of NaAlO₂ (Na-A) on the characteristics and Cu(II) adsorption capacity of the synthetic zeolites were studied. For the analysis of characteristics of the synthetic zeolites, X-ray diffraction (XRD), cation exchange capacity (CEC), Brunaue-Emmett-Teller (BET) and scanning electron microscopy (SEM) were used. The optimum conditions for the synthesis of zeolites with a high adsorption capacity for cationic heavy metals including Cu(II) were the aging time of 6 h, hydrothermal reaction time of 6 h and NaOH and NaAlO₂ dosage ratio of 1.5 and 0.5 (Na-A), respectively. According to the Langmuir isotherm test, maximum Cu(II) adsorption capacities of the synthetic and commercial Na-X and Na-A zeolites were found to be 90.1, 105.26, 102.05, and 109.89 mg/g, respectively. This indicates that the adsorption capacity of synthetic zeolites was comparable to commercial ones. The results of this study also suggest that the coal fly ash can be potentially used as a raw material for the zeolite synthesis.

• Journal of the Mineralogical Society of Korea
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• v.20 no.3
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• pp.223-229
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• 2007

The mechanism of hydrothermally synthesizing Na-A zeolite from siliceous mudstone at a $Na_2O/SiO_2$ ratio of 0.6, a $SiO_2/Al_2O_3$ 2.0 and a $H_2O/Na_2O$ 119 has been observed by IR, DTA, XRD and SEM. This mudstone is a tertiary periodic sedimentary rock and widely spreads around the Pohang area. In the early hydrothermal synthesis at $80^{\circ}C$ in an autoclave, sodium silicate and sodium aluminate were found to be preferentially reacted to generate Na-A type zeolite. Gibbsite and bayerite were also formed due to the presence of extra aluminum oxide in the feedstock. As reaction time in-creased up to 50 h, residual sodium aluminatewas reacted with siliceous mudstone, causing the Na-A zeolite crystal to grow and the hydroxylsodalite to generate. Therefore, in the $14{\sim}50\;h$ synthetic time, Na-A zeolite and hydroxylsodalite were formed. Also, if reaction time passed over 50 h, a part of the Na-A zeolite was finally redissolved and reacted with hydroxylsodalite to synthesize Na-P zeolite, generating porous surface of Na-A zeolite and disappearing hydroxylsodalite.

• 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.

• Applied Chemistry for Engineering
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• v.22 no.5
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• pp.555-561
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• 2011

The objective of this study is the development of carbon recycle technology which converts $CO_2$ captured from flue gas to CO or carbon and reuse in industrial fields. Since $CO_2$ is very stable and difficult to decompose, metal oxide was used as an activation agent for the decomposition of $CO_2$ at low temperature. Metal oxides which convert $CO_2$ to CO or carbon at $500^{\circ}C$ were prepared using Zn-ferrite by the solid state reaction and hydrothermal synthesis. The behaviors of $CO_2$ decomposition were studied using temperature programmed reduction/oxidation (TPR/TPO) and thermogravimetric analyzer (TGA). Zn-ferrite containing 5 wt% ZnO showed the largest reduction and oxidation. Reduction by $H_2$ was 26.53 wt%, oxidation by $CO_2$ was 25.73 wt% and 96.98% of adsorbed $CO_2$ was decomposed to $CO_2$ and carbon with excellent oxidation-reduction behaviors.

• Journal of the Korea Concrete Institute
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• v.20 no.5
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• pp.543-548
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• 2008

Solid hydrated by hydro-thermal synthesis reaction is cured two times, the first curing is the steam curing at atmospheric pressure and the second one is a high-pressure steam curing, that is autoclaving. Steam curing is to acquire the proper strength for the resistance of treatment in the first curing process, it was not evaluated properly so far. Because of ignorance about curing, some engineers even think that the dry curing is better than the steam curing. The relation between compressive strength of solid hydrated by hydrothermal synthesis reaction and curing condition are presented in this paper. In order to investigate the effect of curing on the strength properties of specimen, the hydration behavior of solid hydrated by hydro-thermal synthesis reaction has been studied over curing condition using XRD, DT-TGA and porosimeter, SEM analysis technique. The results show that the specimens which are cured with blended method of dry and steam curing appear to have better strength properties than that of dry curing and steam curing. Also, there are significant difference of hydration behavior among curing condition in the solid hydrated by hydro-thermal synthesis reaction.

• Economic and Environmental Geology
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• v.28 no.2
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• pp.109-121
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• 1995

The hydrothermal vein type deposits which comprise the Kasihan, Jompong and Gempol mineralized areas are primarily copper and zinc deposits, but they are also associated with lead and/or gold mineralization. The deposits occur within the Tertiary sedimentary and volcanic rocks in the Southern Mountain zone of the eastern Java island, Indonesia. Mineralization can be separated into two or three distinct stages (pre-and/or post- ore mineralization stages and main ore mineralization stage) which took place mainly along pre-existing fault breccia zones. The main phase of mineralization (the main ore stage) can be usually classified into three substages (early, middle and late) according to ore mineral assemblages, paragenesis, textures and their chemical compositions. Ore mineralogy and paragenesis of the three areas in the district are different from each other. Pyrite, pyrrhotite (/arsenopyrite), iron-rich (up to 20.5 mole % FeS) sphalerite and (Cu-)Pb-Bi sulfosalts are characteristic of the deposits in the Kasihan (/Jompong) area. On the other hand, pyrite + hematite + magnetite + iron-poor (2.7 to 3.6 mole % FeS) sphalerite assemblage is restricted to the Gempol area. Fluid inclusion data suggest that fluids of the main ore stage evolved from initial high temperatures (near $350^{\circ}C$) to later lower temperatures (near $200^{\circ}C$) with salinities ranging from 0.8 to 10.1 equiv. wt. percent NaCl. Each area represents a separate hydrothermal system: the mineralization at Kasihan and Jompong were largely due to early fluid boiling coupled with later cooling and dilution, whereas the mineralization at Gempol was mainly resulted from cooling and dilution by an influx of cooler meteoric waters. Fluid inclusion evidence of boiling indicates that pressures of ${\geq}95$ to 255 bars (${\geq}95$ bars for the Gempol area: $\approx$ 120 to 170 bars for the Jompong area: $\approx$ 140 to 255 bars for the Kasihan area) during portions of main ore stage mineralization. Equilibrium thermodynamic interpretation indicates that the evolution trends of the temperature versus fS2 variation of ore stage fluids in the Pacitan district follow two fashions: ore fluids at Kasihan and Jompong changed from the pyrite-pyrrhotite sulfidation stage towards pyritehematite- magnetite state, whereas those at Gempol evolved nearly along pyrite-hematite-magnetite reaction curve with decreasing temperature. The sulfur isotope compositions of sulfide minerals are consistent with an igneous source of sulfur with a ${\delta}^{34}S_{{\Sigma}s}$ value of about 3.3 per mil. The oxygen and hydrogen isotopic compositions of the fluids in each area indicate a progressive shift from the dominance of highly exchanged meteoric water at early hydrothermal systems towards an un- or less-exchanged meteoric water at later hydrothermal systems.

• Korean Journal of Mineralogy and Petrology
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• v.36 no.3
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• pp.167-183
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• 2023

The Janggun Pb-Zn deposit consists of Mn orebody, Pb-Zn orebody and Fe orebody. The Mn orebody composed of manganese carbonate orebody and manganese oxide orebody on the basis of their mineralogy and genesis. The geology of this deposit consists of Precambrian Weonnam formation, Yulri group, Paleozoic Jangsan formation, Dueumri formation, Janggum limestone formation, Dongsugok formation, Jaesan formation and Mesozoic Dongwhachi formation and Chungyang granite. This manganese carbonate orebody is hydrothermal replacement orebody formed by reaction of lead and zinc-bearing hydrothermal fluid and Paleozoic Janggum limestone formation. The wallrock alteration that is remarkably recognized with Pb-Zn mineralization at this hydrothermal replacement orebody consists of mainly rhodochrositization with minor of dolomitization, pyritization, sericitization and chloritization. Carbonates formed during wallrock alteration on the basis of paragenetic sequence are as followed : Ca-dolomite (Co type, wallrock) → ankerite and Ferroan ankerite (C1 type, early stage) → ankerite (C2 type) → sideroplesite (C3 type) → sideroplesite and pistomesite (C4 type, late stage). This means that Fe and Mn elements were enriched during evolution of hydrothermal fluid. Therefore, The substitution of elements during wallrock alteration beween dolomitic marble (Mg, Ca) and lead and zinc-bearing hydrothermal fluid (Fe, Mn) with paragenetic sequence is as followed : 1)Fe ↔ Mn and Mn ↔ Mg, Ca, Fe elements substitution (ankerite and Ferroan ankerite, C1 type, early stage), 2)Fe ↔ Mn, Mn ↔ Mg, Ca and Mg ↔ Ca elements substitution (ankerite, C2 type), 3)Fe ↔ Mn, Fe ↔ Ca and Mn ↔ Mg, Ca elements substitution (sideroplesite, C3 type), and 4)Fe ↔ Mg, Fe ↔ Mn and Mn ↔ Mg, Ca elements substitution (sideroplesite and pistomesite, C4 type, late stage)

• Journal of Korean Society of Environmental Engineers
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• v.30 no.6
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• pp.659-665
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• 2008

This study is about zeolite synthesis from the sewage sludge incinerator fly ash of "S" sewage treatment center located in Seoul. For this purpose, the properties of raw fly ash as starting material, the hydrothermal conditions for zeolite synthesis and the environmental applicabilities of synthesized zeolites were examined. Fly ash from sewage sludge incinerator has large quantities of SiO$_2$ and Al$_2$O$_3$ and their contents are 42.8 wt.% and 21.2 wt.% respectively. So fly ash is considered to be possible starting material for zeolite synthesis. The results from leaching test of fly ash showed that the concentration of hazardous metals were very low as compared with the Korea leaching standard of the Waste Management Law. But the concentration from total recoverable test of fly ash were higher than the fertilizer standard of Fertilizer Management Law. Major zeolite products synthesized by hydrothermal reaction are analcime in teflon vessel and zeolite P1 in borosilicate flask. Optimum conditions for the synthesis of analcime were 1 N of NaOH concentration, 16 hour of reaction time and 135$^{\circ}C$ of reaction temperature. For the zeolite P1 formation, the proper conditions were demonstrated to be 5 N of NaOH concentration, 16 hour reaction time and 130$^{\circ}C$ of reaction temperature in this study. Hazardous metal contents in the analcime product are similar with those in raw fly ash. In case of the zeolite P1, the contents are reduced to nearly a half. Raw fly ash and the analcime product showed NH$_4{^+}$ ion exchange capacity of 0$\sim$1.0 mg of NH$_4{^+}$g$^{-1}$ and 3.0$\sim$7.4 mg of NH$_4{^+}$g$^{-1}$, respectively. However, the zeolite P1 product reached exchange capacity to 14.6$\sim$17.8 mg of NH$_4{^+}$g$^{-1}$. This values are in the range of those of natural clinoptilolite and phillipsite. From this point of view, zeolite synthesis from sewage treatment sludge incinerator fly ash is a good alternative for solid waste recycling.