(Shigen to Sozai) Vol.116 p (2000) 石炭灰フライアッシュからのゼオライトのアルカリ水熱合成と生成物の陽イオン交換特性 * 1 1 村山憲弘山川洋亮 2 3 小川和男芝田隼次 Alkali Hydrothermal Synthesis of Zeol

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石炭灰フライアッシュからのゼオライトのアルカリ水 Title 熱合成と生成物の陽イオン交換特性 Author(s) 村山, 憲弘, 山川, 洋亮, 小川, 和男, 芝田, 隼次 Citation 資源と素材 : 資源素材学会誌, 116(4): 279-284 Issue Date 2000 URL http://hdl.handle.

1 石炭灰フライアッシュからのゼオライトのアルカリ水 Title 熱合成と生成物の陽イオン交換特性 Author(s) 村山, 憲弘, 山川, 洋亮, 小川, 和男, 芝田, 隼次 Citation 資源と素材 : 資源素材学会誌, 116(4): Issue Date 2000 URL 資源素材学会 ( Rights se/shigentosozai/_vols/-char/ja) Type Journal Article Textversion publisher Kansai University

2 (Shigen to Sozai) Vol.116 p (2000) 石炭灰フライアッシュからのゼオライトのアルカリ水熱合成と生成物の陽イオン交換特性 * 1 1 村山憲弘山川洋亮 2 3 小川和男芝田隼次 Alkali Hydrothermal Synthesis of Zeolite from Coal Fly Ash and its Cation Exchange Property by Norihiro MURAYAMA 1, Yousuke YAMAKAWA 1 Kazuo OGAWA 1 and Junji SHIBATA 2 1. R&D Department, Kimura Chemical Plants Co., Ltd., Amagasaki-shi Department of Chemical Engineering, Faculty of Engineering, Kansai University, Suita-shi The synthesis of zeolite from coal fly ash by alkali hydrothemal reaction with NaOH was investigated under various conditions and the physical properties of the products were measured in this study. The reaction rate of cation exchange and substitution ratio of calcium ion were examined with some solutions containing calcium ion. Also, some physical properties of calcium type zeolite were measured. Zeolite P which had large cation exchange capacity (about 500 meq / 100 g as CEC) was synthesized from coal fly ash under the particular synthesis condition; reaction temperature of 393 K, reaction time of 5 hrs, NaOH concentration of 1.5 mol / dm 3 and solid-liquid ratio of 200 g / 800 cm 3. The crystal type of synthesized zeolite changed from zeolite P to hydroxysodalite with an increase in concentration of NaOH. The reaction rate was obviously increased when the reaction temperature was over boiling point of water. It was confirmed that the cation exchange reaction of zeolite synthesized in this study could be almost reversible between calcium ion and sodium ion. Optimum condition for zeolite synthesis with high CEC and calcium substitution, and some factors affecting zeolite synthesis and cation exchange reaction were discussed. KEY WORDSCoal Fly Ash, Calcium Ion, Sodium Ion, Zeolite, Alkali Hydrothermal Reaction, Ion Exchange % t ( ) 1) () 2. () 3. [ ]FAX ( ) 2) 6) wt% 2) Na Ca 2 NH 4 Ca 2 279

2 21 () JIS X (EMAX 3770 ) (S 2400 ) SEM (LA 90 ) (JDX 3530S ) 22 1.5 5.

5 mol / dm 3 50 cm 3 Na Ca 2 3 Ca 2 80 wt% Ca 2 1.0 mol / dm 3 50 cm 3 NH 4 5 Ca 2 (AA 880 Jarrell Ash ) 100 g CEC 23 22 1.

5 20 cm 3 ph 3 31 Fig.1SEM photograph of coal fly ash.

3 2 21 () JIS X (EMAX 3770 ) (S 2400 ) SEM (LA 90 ) (JDX 3530S ) mol / dm g / 800 cm g / 700 cm cm K 650 rpm X (Cation Exchange Capacity CEC) 2 g 0.5 mol / dm 3 50 cm 3 Na Ca 2 3 Ca 2 80 wt% Ca mol / dm 3 50 cm 3 NH 4 5 Ca 2 (AA 880 Jarrell Ash ) 100 g CEC g mol / dm 3 20 cm 3 Na Ca 2 NH 4 Na Ca g Na Ca 2 Na Ca 2 Ca 2 (Ca 2 / Na Ca 2 ) a 24 Ca g cm 3 ph 3 31 Fig.1SEM photograph of coal fly ash. Table 1Chemical composition of coal fly ash and synthesized zeolites. Fig.2Particle size distributions of coal fly ash, Na and Ca type zeolites. SEM Fig.1 Fig.1 Table 1 70 wt% CEC 18 meq / 100 g Ca 2 Fig mm ( mm ) 32 Fig mm Fig.3 280

P P Table 1 SEM Fig.4 P (CEC) Fig.5 1.5 mol / dm 3 CEC 500 meq / 100 g 2.

$3X-ray diffraction of coal fly ash and synthesized zeolites. Fig.$ 5Relationship between reaction time and cation exchange capacity at various NaOH

5Relationship between reaction time and cation exchange capacity at various NaOH

4 P P Table 1 SEM Fig.4 P (CEC) Fig mol / dm 3 CEC 500 meq / 100 g 2.5 mol / dm 3 CEC 340 meq / 100 g CEC 5 CEC CEC P P CEC ( 3 4 A) P ( 4 5 A) 7)8) CEC P 33 CEC Fig.6 CEC 200 g / 800 cm g / 700 cm 3 8 Fig.3X-ray diffraction of coal fly ash and synthesized zeolites. Fig.5Relationship between reaction time and cation exchange capacity at various NaOH concentrations. Fig.4SEM photographs of zeolites synthesized from coal fly ash at the different NaOH concentrations (reaction temperature, time:393k, 5hrs) 281

5 CEC CEC 300 g / 700 cm 3 Na OH CEC CEC Fig K CEC 8) 393 K CEC 393 K CEC Fig.5 7 (NaOH[g] / Fly Ash[g]) Fig.6Effect of ratio of solid and liquid on cation exchange capacity. Fig.7Relationship between reaction time and cation exchange capacity at various reaction temperatures. Fig.8Relationship between amount of NaOH to fly ash and cation exchange capacity. CEC Fig.8 CEC CEC 4)10) Na OH Na OH OH Na 3)4) Na OH 34 Fig min Ca 2 Ca 2 Na Fig.10 Ca 2 P 11) Ca 2 282

Fig.11Change in ph of Na and Ca type zeolite slurries at

9Time course of calcium substitution reaction of Na type

Table 2Amount of exchangeable cations, calcium substitution

10Behavior of cation exchange reaction on calcium substitution

6 Fig.11Change in ph of Na and Ca type zeolite slurries at various initial ph. Fig.9Time course of calcium substitution reaction of Na type zeolite by using CaCl 2 solution. Table 2Amount of exchangeable cations, calcium substitution ratio a and ph for various zeolites. Fig.10Behavior of cation exchange reaction on calcium substitution and sodium reverse substitution. Na Ca 2 Ca 2 35 Fig.2 SEM Na Ca 2 ph Fig.11 ph H H OH NH 4 CEC ph Na CEC Ca 2 ph ph Table 2 a ph a CEC(Na + Ca 2 ) 4 Ca 2 Ca 2 1) CEC P 283

7 2) Na OH CEC OH Na 3)Na Ca 2 Ca 2 Na 4) CEC 1) ( 2 ), (1995) 2), &, (1994) 3) 1998,, p , (1999) 4), Vol. 115, p , (1999) 5) )Lin, C. F and His, H-CEnviron. Sci. Technol., Vol. 29, p , (1995) 7) ), No. 2, p , (1996) 9) ),, (1987) 11)Shibue, Y.Clays and Clay Minerals, Vol. 29, No. 5, p , (1981) 284

31 5 pp x 0 40 mol% Ohe and Yokoyama, wt% 50 wt% 5 mol/dm 3 14 mol/dm % % 69% 6% Pauling Ni

31 5 pp x 0 40 mol% Ohe and Yokoyama, wt% 50 wt% 5 mol/dm 3 14 mol/dm % % 69% 6% Pauling Ni 硝酸 - 水系の低濃度域における気液平衡に及ぼす塩効 Title 果を利用した硝酸の濃縮山本, 秀樹, 前田, 領平, 山口, 修平, 北口, 剛司, Author(s) 芝田, 隼次 Citation 化学工学論文集, 31(5): 331-337 Issue Date 2005 URL http://hdl.handle.net/10112/5537 Rights Type Journal Article