Reaction, Mechanism and Application of Various Zeolite Syntheses from Coal Fly Ash

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1 Materials Transactions, Vol. 44, No. 12 (23) pp to 248 Special Issue on New Systems and Processes in Recycling and High Performance Waste Treatments #23 The Japan Institute of Metals Reaction, Mechanism and Application of Various Zeolite Syntheses from Coal Fly Ash Norihiro Murayama, Mitsuaki Tanabe*, Hideki Yamamoto and Junji Shibata Department of Chemical Engineering, Faculty of Engineering, Kansai University, Suita , Japan The hydrothermal syntheses of zeolites from coal fly ash were carried out using NaOH and KOH as an alkali source in order to clarify the reaction mechanism of zeolitization. The physical properties such as surface structure, crystal structure and cation exchange capacity (CEC), and the ion exchange properties were measured for the zeolites synthesized by hydrothermal treatment. From these results, the effective usage was investigated for various zeolites derived from coal fly ash. Zeolite P, HS (hydroxysodalite) and K-CHA (potassium-chabazite) are mainly formed as zeolite species in NaOH or KOH solution at 393 K. The zeolite P and K-CHA have a large exchange capacity as a cation exchanger. There are three reaction steps; the dissolution, deposition and crystallization reactions in a series of conversion process from coal fly ash to zeolitic materials. The selectivity of cation exchange of various zeolites is explained by the Coulomb s attractive force between the ionic charge of metal ions and the surface charge of zeolites. The obtained zeolites can be used as a cation exchanger and a soil improvement agent. The usage of the synthesized zeolites as soil improvement makes a contribution to return coal residue to soil environmentally friendly. (Received June 3, 23; Accepted August 4, 23) Keywords: zeolite, coal fly ash, inorganic materials, ion exchange, recycle 1. Introduction The exhaustion of petroleum resources has been warned in recent years. Atomic energy, natural gas, coal and so on are being reconsidered as alternative energy sources. It is very difficult, however, to establish a new atomic energy power plant in Japan. Coal has been reassessed as an energy source from the viewpoints of low cost, large deposits and provision stability. The transition from oil to coal as an energy source is planed in the large electric power plants. 1) A large amount of coal ash is discharged from electric power plants and many other factories using coal. The amount of discharged coal fly ash in Japan steeply increases every year. For example, the amount of coal fly ash discharged from electric power plants was about 7.6 million tons in ) The law of promotion of the ash usage states that coal fly ash emitted by electric power plants should be effectively recycled. About 4% of the coal fly ash is reused as raw materials in the manufacture of cement and concrete, but the rest is mainly used as landfill. The development of a new usage method, by which a large amount of coal fly ash is consumed, is needed because of difficulty to increase the potential demand of coal fly ash in the field of cement and concrete engineering. 1) The conversion of coal fly ash to zeolite is investigated all around the world as one of the effective usages. Many researchers 2 1) have reported that the zeolite synthesized from coal fly ash is applied to the various fields such as water purification, soil improvement, adsorption of heavy metal ions, catalyst and so on. The authors have reported the production methods of zeolite from coal fly ash 11 13) and incineration ashes 14) using a hydrothermal reaction, and the effective usage of the obtained zeolite in the field of environmental protection. 15,16) The above technologies have not led to the commercial scale yet. This is caused by the high cost for zeolite production and the small market of synthetic and natural zeolites. The present market scale of synthetic *Graduate Student, Kansai University zeolite is estimated to be about 1,t/y in Japan. 17) Therefore, it is important to produce the zeolite effectively and to develop the new usage of the zeolite, in other word, to clarify the reaction mechanism of zeolitization and the various natures of the obtained zeolite. The objective of this study is to investigate the zeolite synthesis from coal fly ash, the reaction mechanism of zeolitization and the suitable usage of the obtained product. The hydrothermal synthesis of zeolite from coal fly ash was carried out using NaOH and KOH as an alkali source. The physical properties such as surface structure, crystal structure and cation exchange capacity (CEC), and the ion exchange properties are measured for the various products obtained by hydrothermal treatment. The formation mechanism of zeolitic materials was investigated from these experimental results. The new concept for zeolite usage, which is used in large quantity and has many advantages compared with the other methods, was discussed in this study in order to establish a more effective and environmentally friendly method for the treatment of coal fly ash. 2. Experimental 2.1 Zeolite synthesis from coal fly ash Coal fly ash made by Denpatsu Coal Tech. Co., Ltd. was used as a raw material for zeolite synthesis. The coal fly ash had been discharged from a coal power plant. Coal fly ash and NaOH or KOH solution were put into an 8 cm 3 autoclave and a hydrothermal reaction was initiated. The solid-liquid ratio was 1 g/4 cm 3. The reaction temperature and agitation speed were 393 K and 5 rpm, respectively. The reaction product was washed with distilled water, and the solid-liquid separation was carried out by a vacuum filtration. The obtained solid cake was dried in an oven at 353 K for 12 h. In order to make Ca type zeolite by the cation exchange reaction with Ca 2þ, 1. g of the obtained Na type zeolite and 4 cm 3 of 1. mol/dm 3 CaCl 2 solution were mixed and

2 2476 N. Murayama, M. Tanabe, H. Yamamoto and J. Shibata Table 1 Physical properties of coal fly ash and obtained zeolites. Sample Coal fly ash S-1 S-2 S-3 S-4 Alkali source - 2. mol/dm 3 NaOH 5. mol/dm 3 NaOH 2. mol/dm 3 NaOH 3. mol/dm 3 KOH Reaction condition Temp., Time K, 3 h 393 K, 3 h 393 K, 3 h 393 K, 24 h Substitution 5 times of Ca treatment substitution - Zeolite species - Na-P Na-HS Ca-P K-CHA Total capacity (mmol/1 g) Cation exchange capacity Substitution ratio - 1%, Na þ 1%, Na þ 94%, Ca 2þ 1%, K þ Index ion for CEC mesurment Ca 2þ Ca 2þ Ca 2þ Na þ,ca 2þ Na þ Si Al Chemical Na composition [wt%] Ca K Others shaken by using a vertical type shaker. The cation exchange reaction between Na þ in zeolite and Ca 2þ in aqueous solution was carried out at around ph7. The zeolite and aqueous solution being separated, then the zeolite was contacted with fresh CaCl 2 solution. A series of ion exchange operations were repeated 5 times. 2.2 Physical properties of synthesized zeolite The chemical compositions of the coal fly ash and the reaction products obtained by hydrothermal reaction were analyzed by X-ray fluorescence analysis (JED-211, Nihon Denshi Co., Ltd.). An X-ray diffraction analyzer (JDX-353, Nihon Denshi Co., Ltd.) was used to identify the crystal structures of the coal fly ash and the products. The surface structure of the products was observed by using a scanning electron microscope (JSM-541, Nihon Denshi Co., Ltd.). The cation exchange capacity (CEC) of the Na type zeolite and K type zeolite was measured by the modified Harada- Aomine method. 18) In case of CEC measurement of Na type zeolite and K type zeolite, Ca 2þ and Na þ were used as an index ion, respectively. In order to substitute Na þ or K þ in the product by Na þ or Ca 2þ in the solution, 2 g of the product and 2 cm 3 of 1. mol/dm 3 CH 3 COONa or (CH 3 COO) 2 Ca solution were contacted for 1 min. The above substitution operation was repeated 6 times, by which saturation substitution was achieved. The product was washed 5 times with 2 cm 3 of 8 wt% ethanol solution to remove the excess Na þ or Ca 2þ adhering to the surface of the product. NH 4 þ substitution operations were also carried out 6 times by using 2 cm 3 of 1. mol/dm 3 NH 4 Cl solution. The amount of Na þ or Ca 2þ released from the product was determined in order to evaluate the CEC value (mmol per 1 g of product). The cation exchange test was conducted for various zeolites. One gram of dried zeolite was contacted with 4 cm 3 of various metal chloride solutions by a vertical type shaker. The concentration of various ions in aqueous solution was determined by inductively coupled plasma atomic emission spectrometry (ICP-1III, Shimadzu Co., Ltd.) and atomic absorption spectrometry (AA-68, Shimadzu Co., Ltd.). The concentration of NH 4 þ in solution was measured by an ion chromatograph (DX-5, Nihon Dionex Co., Ltd.). 3. Results and Discussion 3.1 Zeolite synthesis from coal fly ash Generally, the main component of coal fly ash is amorphous aluminosilicate, quartz (SiO 2 ) and mullite (3Al 2 O 3 2SiO 2 ) existing as a crystalline substance in coal fly ash. 13) The amorphous materials of Si and Al can be changed into zeolite crystals by hydrothermal treatment. The reaction conditions and physical properties of various zeolites obtained from coal fly ash are shown in Table 1. Four kinds of zeolites, that is, Na type zeolite P (Na-P, sample #S-1), Na type hydroxysodalite (Na-HS, sample #S- 2), Ca type zeolite P (Ca-P, sample #S-3) and potassium chabazite (K-CHA, sample #S-4), are synthesized in NaOH or KOH solutions under various reaction conditions. The cation exchange capacities of Na-P, Na-HS, Ca-P and K- CHA zeolites are about 31, 13, 3 and 26 mmol/1 g, respectively, which are a large value as a cation exchanger except for the Na-HS. The Na-P and Na-HS mainly consist of Si, Al and Na, and the sums of three components in the Na-P and Na-HS are about 75.8% and 78.2% to all metal components, respectively. The other components are Fe, Ti, Mg, Zn and so on. The content of Si and Al is caused by zeolite structure, whereas Na is based on an exchangeable Na þ in the Na-P. The Na-HS contains 14.7% of Na component, but the CEC value is very low compared with Na-P zeolite because of the pore size of Na-HS smaller than that of Na-P zeolite. 13) In cases of Ca-P and K-CHA, the same results are obtained each other, that is, about 6% of Si and Al, and Ca or K based on an exchangeable cation contained in the zeolite products. The Ca substitution ratio of Ca-P is about 94%, and the rest is exchangeable Na þ. The formation behavior of zeolites is investigated to clarify the reaction mechanism of zeolitization. The hydro-

3 Reaction, Mechanism and Application of Various Zeolite Syntheses from Coal Fly Ash 2477 Intensity (cps) Heating Temp., T / K Reaction Time, t / h Fig. 1 Change in X-ray diffraction intensities of K-CHA products obtained in 3. mol/dm 3 KOH solution as a function of reaction temperature and time. Si 4+, Al 3+ and K + Concn. In Liquid Phase, C / g. m -3 Heating Temp., T / K Reaction Time, t / h Fig. 3 Change in Al 3þ,Si 4þ and K þ concentrations in 3. mol/dm 3 KOH solution as a function of reaction temperature and time. thermal reaction of coal fly ash was carried out measuring the time courses of surface structure, the X-ray diffraction intensity of the reaction products and the concentrations of K þ,si 4þ and Al 3þ in aqueous solution through a series of hydrothermal reactions. Zeolites are produced from amorphous materials in coal fly ash. As a typical example, the change in X-ray diffraction intensity of the K-CHA product obtained in 3. mol/dm 3 KOH solution is shown in Fig. 1. The X-ray diffraction intensity of K-CHA first appears in a reaction time of 5 h, and the intensity of K-CHA remarkably increases due to K-CHA crystal growth in the reaction time from 5 to 2 h. The X-ray diffraction intensity becomes almost constant in the reaction time over 2 h. The X-ray diffraction intensity of quartz, which is originally present in coal fly ash, decreases as the reaction proceeds, whereas that of mullite gradually decreases. These decreases in XRD intensity are caused by K-CHA formation on the fly ash surface. The surface structure of the K-CHA is shown in Fig. 2. Coal fly ash comprises spherical particles (Fig. 2(a)), whereas fine deposit generates newly on the particle surface in the subsequent heating process (Figs. 2(b)-(d)). From the results shown in Fig. 1, these fine materials are confirmed to be amorphous materials. In the reaction time of 2.5 h, the surface structure of the product (Fig. 2(e)) is almost the same as that in Fig. 2(d). In a reaction time of 5 h, the particle surface is rendered elliptic by produced K-CHA crystals (Fig. 2(f)). The particle surface is completely covered with K-CHA crystals during further reaction time (Figs. 2(g),(h)). The obtained K- CHA is confirmed to be such complex material as coal fly ash (a) Coal fly ash (b) 353K,.8h (c) 373K, 1.3h (d) 393K, h (e) 393K, 2.5h (f) 393K, 5h (g)393k, 24h (h)393k, 5h Fig. 2 Change in surface structure of reaction products obtained in 3. mol/dm 3 KOH solution as a function of reaction temperature and time.

4 2478 N. Murayama, M. Tanabe, H. Yamamoto and J. Shibata particles covered with K-CHA crystal. The changes in Si 4þ, Al 3þ and K þ concentrations in 3. mol/dm 3 KOH solution are shown in Fig. 3. The Si component in the coal fly ash is dissolved with a temperature rise in the heating process, while the Al ingredient rapidly increases in the beginning of the heating process, and then decreases after 353 K in the heating process. The amounts of Si 4þ and Al 3þ dissolved in alkali solution approach to constant values of about 6 kg/m 3 and 1 g/m 3, respectively, after reaching to 393 K. On the other hand, the K þ concentration is about 4 kg/m 3 in a reaction time of 5 h, which indicates that 76.2% of K þ has been consumed to the initial KOH solution. Consequently, the change in the amounts of Si 4þ,Al 3þ and K þ in alkali solution mainly depends on the formation of K-CHA. The formation mechanism of K-CHA is considered to be the three steps composed of dissolution, deposition and crystallization from the above results. The dissolution reaction of coal fly ash takes place in the heating process from 293 to 393 K as a first step, and then the particle surface changes from sphere to something like unevenness. At the same time, the amorphous aluminosilicate gradually deposits on the particle surface of coal fly ash in the heating process, whereas the K-CHA is not formed yet in the reaction temperature below 393 K. In the reaction process at 393 K, the zeolite crystal is conspicuously formed in the reaction time from 5 h to 2 h after the reaction temperature reaches 393 K. As the zeolite crystallization progresses, the surface of coal fly ash is covered with the deposited K-CHA, as well as the Al 3þ concentration in the alkali solution substantially decreases. The crystallization process of K-CHA takes place very slowly after all dissolved aluminate ions is consumed to form aluminosilicates. In the reaction time over 2 h, the growth of K-CHA crystals is not recognized, and then the zeolitization reaction attains the saturation state. The formation of Na-P can be explained by the similar reaction mechanism, 13) though the reaction time is different for that of K-CHA. 3.2 Cation exchange property of zeolite The cation exchange reaction of Na-P zeolite for various monovalent and divalent cations is shown in Fig. 4. The initial concentrations for monovalent and divalent cations and ph of solution are 3. kg/m 3 (monovalent), 1.5 kg/m 3 (divalent) and about 7, respectively. For all monovalent cations in Fig. 4(a), the amount of exchanged cation reaches to an equilibrium in about 2 min. The amount of cation exchanged by Na-P is remarkably different among NH þ 4,K þ and Li þ, and that of NH þ 4 is the largest of all. The exchanged amounts of NH þ 4, K þ and Li þ are about 23, 185 and 5 mmol/1 g, respectively, in an equilibrium state. The order of selectivity of Na-P for monovalent cations is as follows; NH þ 4 >K þ >Li þ. For the divalent cations in Fig. 4(b), the amount of exchanged cation leads to an equilibrium in about 3 min. The exchanged amount of Ca 2þ is the largest, which is smaller compared with that of monovalent cation, NH þ 4 and K þ. The exchanged amounts of Ca 2þ, Cd 2þ,Pb 2þ,Mg 2þ and Ni 2þ are about 7, 43, 25, 8 and 8 mmol/1 g, respectively, in an equilibrium state. The order of selectivity for divalent cations is as follows; Cation Exchange Amount, E / mmol/1g Cation Exchange Amount, E / mmol/1g Fig Time, t / min (a) Monovalent cation Time, t / min (b) Divalent cation Cation exchange rate of various ions with Na-P zeolite. Ca 2þ >Cd 2þ >Pb 2þ >Mg 2þ >Ni 2þ. The cation exchange isotherms of various monovalent and divalent cations with K-CHA are shown in Figs. 5, 6. In Fig. 5, the high exchange amount more than 1 mmol/1 g is confirmed for NH 4 þ in the low equilibrium concentration. The exchange amounts of Na þ and Li þ are about 8 and 4 mmol/1 g. The order of selectivity of K-CHA indicates NH 4 þ >K þ >Li þ. For the divalent cation in Fig. 6, the exchange amount of Co 2þ shows the largest value that is about 75 mmol/1 g. The amounts of Cd 2þ and Ca 2þ are about 48 and 2 mmol/1 g, and the amounts of Mg 2þ and Ni 2þ shows low values below 1 mmol/1 g. On the other hand, the removal amount of 13 mmol/1 g is obtained for Pb 2þ in the low equilibrium concentrations below.2 mmol/ dm 3. The same phenomena are confirmed in case of Na-P. 19) The order of selectivity of K-CHA in low concentration is expressed in the following order; Pb 2þ >Co 2þ >Cd 2þ > Ca 2þ >Mg 2þ >Ni 2þ. The selectivity of ion exchange of zeolite can be considered from the viewpoint of ionic charge and ionic

5 Reaction, Mechanism and Application of Various Zeolite Syntheses from Coal Fly Ash 2479 Cation Exchange Amount, E / mmol/1g Cation Exchange Amount, E / mmol/1g Fig Co 2+ Cd 2+ Ca 2+ Mg 2+ Ni Fig. 6 NH 4 + Na + Pb Equilibrium cation concentration, C / mol. m -3 Ion exchange of divalent cations with K-CHA. radius. The crystal ionic radius (r c ) and Stokes hydration ionic radius (r s ) of various monovalent and divalent cations are shown in Table 2. The Stokes hydration ionic radius is calculated by the following equation; u i ¼ jz ije ð1þ 6 r s where u i,, Z i and e are mobility, viscosity of solvent, electric charge of ion and elementary electric charge, respectively. The selectivity of K-CHA for monovalent cation shown in Fig. 5 is corresponding to the order of r s.in case of divalent cation, the selectivity of K-CHA in Fig. 6 is Li Equilibrium cation concentration, C / mol. m -3 Ion exchange of monovalent cations with K-CHA. Table 2 Crystal ionic radius (r c ) and Stokes hydration ionic radius (r s )of various monovalent and divalent cations. Monovalent Diavalent Cation r c (nm) r s (nm) r s =r c K þ þ NH Na þ Li þ Pb 2þ Co 2þ Ni 2þ Ca 2þ Cd 2þ Mg 2þ similar to the order of r s, though there are some exceptions such as Ni 2þ,Cd 2þ. The cation exchange properties of Na-P and K-CHA are consider to mainly relate to the Coulomb s attractive force determined by the balance between ionic charge and hydration ionic radius. 3.3 Application of various zeolites In order to develop the new usage of the zeolitic materials derived from coal fly ash, the characterization as an ion exchanger and an adsorbent are considered for the obtained Na-P zeolite, Ca-P zeolite and K-CHA. The Na-P has a large cation exchange capacity of 3 mmol/1 g and high exchange amount for NH þ 4, K þ and Ca 2þ. In the low concentration region of Pb 2þ, the large amount of Pb 2þ is removed from aqueous solution. Therefore, the Na-P can be used as water purification agents such as eutrophication and removal of heavy metal ions, and as an ion exchanger to make soft water. The Ca-P as an ion exchanger has the similar properties to Na-P, 15) and the Ca-P can also be used as a water purification agent. The range of Ca-P usage is wide compared with Na-P. Because Na þ is hardly contained in the Ca-P, it is possible to use the Ca-P as soil improvement agents to keep fertilizer components and to remove various heavy metal ions in soil. The K-CHA has also both water purification and soil improvement abilities. As the advantages of K-CHA, the cation exchange sites of zeolite are occupied perfectly by K þ, and K þ tends to be selectively taken in the K-CHA compared with Na þ and Ca 2þ in the presence of these cations. The K-CHA can be used as a slowacting fertilizer of K component in addition to the original ion exchange function of zeolite. The activities of natural zeolite for soil improvement are mainly to keep soil moisture and fertilizer components such as NH þ 4 and K þ. In the ordinary method, both fertilizer and zeolite is needed to add to soil at the same time. On the other hand, the obtained K-CHA not only contains the adequate amount of K component, but also has the moisture and fertilizer keeping abilities. The method in which the obtained zeolites are used as a soil improvement is essentially a technology to return coal residue to soil. It is very important not only to be safe, but also to be more effective in order to exceed other materials, especially natural zeolite. Generally, there is no problem on safety of zeolite for the practical use such as soil improvement, because coal fly ash itself has the

6 248 N. Murayama, M. Tanabe, H. Yamamoto and J. Shibata soil improvement ability, and the safety of coal fly ash has already been confirmed. 1) According to the above consideration, the zeolite produced from coal fly ash should be finally returned to the soil with contribution to many environmental problems. This concept is very intelligent as the environmentally friendly technology of coal fly ash treatment to satisfy the factors mentioned above. 4. Conclusion The hydrothermal syntheses of zeolite from coal fly ash were conducted using NaOH and KOH as alkali sources. The change in surface structure, zeolite crystals, chemical composition, concentrations of Si 4þ,Al 3þ and K þ in alkali solution were investigated for the reaction products through a series of zeolitization reactions to clarify the reaction, mechanism and application of synthesized zeolite. Zeolite P, HS and K-CHA are mainly formed as zeolite species in NaOH or KOH solution at 393 K. The zeolite P (Na-P, Ca-P) and K-CHA have a large exchange capacity as a cation exchanger. There are three reaction steps; the dissolution, deposition and crystallization reactions in a series of conversion process from coal fly ash to zeolitic materials. The selectivity of cation exchange of various zeolites is explained by the Coulomb s attractive force between the ionic charge of metal ions and the surface charge of zeolites. The metal ions to be strongly captured in the zeolite have high positive charge and small hydration ionic radius. The obtained zeolites can be used as a cation exchanger and a soil improvement agent in the field of environmental protection. The usage of the synthesized zeolites as soil improvement makes a contribution to return coal residue to soil environmentally friendly. Acknowledgment This work was supported by MEXT, Grant-in-Aid (Young Scientist (B), ), Espec Foundation for Earth Environmental Research and Technologies and the Kansai University Grant-in-Aid for Promotion of Advanced Research in Graduate Course, 23. REFERENCES 1) Japan Fly Ash Association: Coal Ash Hand Book (second edition), (1995) pp. II ) T. Henmi: Sangyohaikibutu no Zeoraitotenkanniyoru Saisigenka Yukoriyougijyutukaihatu, (New Technology and Science, Tokyo, 1994), pp ) X. Querol, F. Plana, A. Alastuey and A. Lopez-Soler: Fuel 76 (1997) ) N. Shigemoto, H. Hayashi and K. Miyake: J. Mater. Sci. 28 (1993) ) Chen-Fang Lin and Hsing-Cheng His: Environ. Sci. and Technol. 29 (1995) ) C. Poole, H. Prijatama and N. M. Rice: Min. Eng. 13 (2) ) M. Park and J. Choi: Clay Science 9 (1995) ) B. Biserka and S. Boris: Sep. Sci. Technol. 33 (1998) ) A. Sultan, C. Shiraz and M. A. Keane: Sep. Purif. Technol. 13 (1998) ) D. B. Lee, K. B. Lee, S. S. Han and T. Henmi: J. Korean Soc. Soil Sci. 31 (1998) ) N. Murayama, Y. Yamakawa, K. Ogawa and J. Shibata: Shigen-to- Sozai 116 (2) ) N. Murayama, K. Ogawa, Y. Nishikawa, H. Yamamoto and J. Shibata: Shigen-to-Sozai 116 (2) ) N. Murayama, H. Yamamoto and J. Shibata: Int. J. Min. Process. 64 (22) ) N. Murayama, H. Ishimoto and J. Shibata: Shigen-to-Sozai 116 (2) ) N. Murayama, S. Yoshida, Y. Takami, H. Yamamoto and J. Shibata: Sep. Sci. Technol. 38 (23) ) J. Shibata, N. Murayama, and H. Yamamoto: Proc. EPD Congress 22, (TMS, 22) pp ) T. Tatsumi: Kinousei Zeoraito no Gosei to Oyo, (CMC, Tokyo, 1995) pp ) Y. Nishikawa, N. Murayama, H. Yamamoto, J. Shibata and K. Ogawa: Shigen-to-Sozai 115 (1999) ) Y. Takami, J. Shibata, H. Yamamoto, N. Murayama and K. Ogawa: Shigen-to-Sozai 117 (21)

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