資源と素材

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1 (Shigen to Sozai) Vol.116 p (2000) 共存硫酸塩を含む強酸性 MnSO 4 溶液中のオゾン酸化によって生成した沈殿の X 線回折および放電特性 * 西村忠久 1 梅津良昭 2 X-ray Diffraction and Discharge Behavior of Precipitates Produced by Ozone Oxidation in Acidified MnSO 4 Solutions with Addition of Other Sulfate by Tadahisa NISHIMURA 1 and Yoshiaki UMETSU 1 1. Institute for Advanced Materials Processing, Tohoku University, Aoba-ku, Sendai The incorporation of coexisting metal ion in the precipitates produced by ozone oxidation-precipitation in acidified MnSO 4 solutions with an added sulfate was investigated for 15 elements (18 ionic species) by chemical analysis, X-ray diffraction and discharge curve measurement of the precipitates.the precipitates were formed in the stream of O 3 O 2 gas mixture with ozone partial pressure of atm at 70 C in the solutions of 1.0 M sulfuric acid, 0.1 M MnSO 4 and other metal sulfate. A little incorporation in the g MnO 2 based precipitate was detected for alkali metal ions, Mg, Cu, Co and Ni ions. Both Fe ( ) and Fe ( ) ions were captured in the precipitate and affected significantly the discharge curve of the precipitate. The precipitates formed in the presence of Ti, V or As showed a fairly high content of the coexisting element, X-ray diffraction peaks remarkably differing from those for g MnO 2 and poor discharge behavior. These suggest possibility for Ti, V or As to be precipitated as some compounds with Mn rather than to be incorporated into the MnO 2 -based precipitate. KEY WORDS Ozone, Oxidative Precipitation, Manganese Dioxide, Coexisting Sulfate, Incorporation, Discharge Curve 1 (Merz and Gaia 1989) MnSO 4 Mn 2 MnSO 4 ( OMD ) ( a 1992b 1992c) (ORP) MnSO 4 OMD 25 C 4.0 mol / l ( mol / l M ) 70 C 5.0 M Fe As V Ti ( 1995) [ ] FAX ( ),,,,, Mn 15 Mn X H ( 1992c Kozawa et al, 1988 Ruetsch 1988 Ruetsch Giovanoli 1988) 9.0 MKOH MnSO 4 2 MnSO 4 MnSO 4 ( 1992) Mn M 1.0 M 0.1 M O 3 O 2 25 C KI Na 2 S 2 O 3 O atm 70 C O 3 O 2 ( 1992) Cu-Ka X Fe Ti V ICP EDTA 285

2 ( 1995) 0.10 g (IBA IC No.10)1.0 g 25 C ( 0.10 g 2.0 ma) 9.0 KOH Hg / HgO (9.0 KOH) ( 1992c) X 1.0 M MnSO 4 OMD ( "nil" ) MnSO 4 Mn Table 1 mass% ( 1992c) ( M / Mn ) Li Na K Mn Mg MnSO 4 Mg / Mn Al ( ) Al / Mn B (12 ) Zn Cd M / Mn Table 1 Chemical analyses of precipitates produced from 0.1 M MnSO 4-1 M H 2 SO 4 solutions with added metal ion at 70 C by ozonation Cd Hg HgSO 4 Hg M Hg( ) Hg( ) Hg Hg 0.5 % Hg 70 % Hg Fe( ) Fe( ) 0.1 M Fe Fe 4 % Fe( ) Fe / Mn A ( ) Co Ni 1.0 M (Nishimura and Umetsu 1992) Fe As As ( ) As ( ) As 0.02 M As 4 % (As / Mn ) As ( ) As As As Ti V % (M / Mn ) 3 2 X MnSO 4 X MnO 2 MnOOH (Kozawa et al Ruetsch 1988 Ruetsch and Giovalino 1988) MnSO 4 OMD ( "nil" ) mass% ( ) X g MnO 2 (De Wolff a) Fig.1 Li ( ) Na ( ) K ( ) g MnO 2 (EMD) K ( ) K ( ) a MnO g MnO 2 X OMD Mn 2 g MnO 2 286

3 MnSO 4 X Fig.1 X-ray diffraction patterns (a) and discharge curves (b) for precipitates containing Li ( ), Na ( ) or K ( ) produced by ozonation. Fig.2 X-ray diffraction patterns (a) and discharge curves (b) for precipitates containing Mg ( ) or Al ( ) produced by ozonation. Fig.3 X-ray diffraction patterns (a) and discharge curves (b) for precipitates containing Zn ( ), Cd ( ) or Hg ( ) produced by ozonation. Fig.2 Mg ( ) Al ( ) X OMD Fig.3 Zn ( ) Cd ( ) Hg ( ) X X g MnO 2 5 MnO 2 OMD Cd ( ) Hg ( ) MnO 2 Hg ( ) X Hg ( ) MnSO 4 OMD Zn Cd OMD ph ( 2000) 1.0 Zn Cd OMD Fig.4 Co ( ) Ni ( ) Cu ( ) X 1.0 M Co ( ) Ni ( ) (Nishimura and Umetsu 1992) g MnO Fe ( ) Fe Fig.4 X-ray diffraction patterns (a) and discharge curves (b) for precipitates containing Co ( ), Ni ( ) or Cu ( ) produced by ozonation. ( ) 0.1 M Fig.5 Fe 4 % Fe X g MnO g MnO 2 Fe OMD Fe ( ) X Fe ( ) Fe ( ) Fe ( ) Fe ( ) Fe ( ) Fe ( ) 287

4 Fig.5 X-ray diffraction patterns (a) and discharge curves (b) for precipitates produced in the presence of Fe ( ) or Fe ( ) by ozonation. Fig.6 X-ray diffraction patterns (a) and discharge curves of Fe ( ) by ozonation. Fig.7 X-ray diffraction patterns (a) and discharge curves (b) for precipitates produced in the presence of As ( ) or As ( ) by ozonation. Fe ( ) Mn ( ) ORP Fe ( ) OMD ( 1995) Fe ( ) M 0.01 M 0.1 M X Fig.6 Fe ( ) Fe ( ) 0.01 M (0.056 g Fe ( ) / l) Fe Fe ( ) Fe Fe 0.90 % Fe Fe As Fig.7 As 0.02 M As ( ) As ( ) As 4 % (As / Mn ) X As ( 1995) ORP As ( ) As ( ) Mn 2 As X g MnO As (open circuit voltage) 2 As ( ) X Fig.8 As ( ) As As ( ) M As Fig.8 X-ray diffraction patterns (a) and discharge curves of As ( ) by ozonation. As As As ( ) As ( ) 1.0 M As Mn ( ) As(V) Mn Table 1 Ti V Ti(SO 4 ) 2 MnSO 4 Fig.9 Ti Ti 0.1 M Ti 10.4 % (Ti / Mn 0.29) X Ti g MnO % Ti 288

5 MnSO 4 X Fig.9 X-ray diffraction patterns (a) and discharge curves of Ti ( ) by ozonation. Fig.10 X-ray diffraction patterns (a) and discharge curves of V ( ) by ozonation. Ti 0.27 % % Ti OMD Fig.10 VOSO 4 V ( ) V ( ) (Nishimura and Umetsu 1996) Ti As V V ( ) V X V 6.9 % V 0.5 % Fig.11 Discharge capacity of precipitate samples containing added metal element (1) nil (2) % Li ( ) (3) % Na ( ) (4) 0.67 % K ( ) (5) % Mg ( ) (6) % Al ( ) (7) 0.48 % Zn ( ) (8) 1.6 % Cd ( ) (9) 0.49 % Hg ( )* (10) 0.45 % Hg ( ) (11) 1.7 % Co ( ) (12) 0.41 % Ni ( ) (13) 0.81 % Cu ( ) (14) 0.14 % Fe ( )* (15) 0.90 % Fe ( )* (16) 4.5 % Fe ( )* (17) 3.9 % Fe ( ) (18) 0.14 % As ( )* (19) 1.2 % As ( )* (20) 3.8 % As ( )* (21) 4.0 % As ( ) (22) 0.27 % Ti ( ) (23) 2.0 % Ti ( ) (24) 10.4 % Ti ( ) (25) 0.50 % V ( )* (26) 3.0 % V ( )* (27) 6.9 % V ( )* (28) EMD (IC No-20) (29) CMD(IC No-5) * valence after ozonation V 6.9 % V OCV As Ti V MnSO 4 X g MnO 2 g MnO 2 As Ti V Mn g MnO 2 (Kozawa et al Ruetsch 1988 Ruetsch and Giovalino 1988) g MnO 2 X MnVO 3 Mn 2 (AsO 4 ) Fig.1 10 ( ma h volt (mw h)) MnO 2 HgO / Hg9.0 KOH V Fig.11 Ti V As Fe Fe M Fe 4.5 % (No.16 Fe ( ) ) 3.9 % (No.17 Fe ( ) ) Fe 289

6 4 Mn 15 MnSO 4 ( 1.0 M) X 1 2 Zn Cd Cu Co Ni Mg 2 X 3 Fe X 4 Hg 70 % 5 As V Ti X De Wolff, P. M. (1959) Acta Crystallogr.,Vol. 12, p Kozawa, A., Kano, G., Horita, K. and Takeuchi, K. (1988) Progress in Batteries and Solar Cells, Vol. 7, p. 2 Merz, E. and Gaia, F. (1989) OZONE SCIENCE AND ENGINEERING, Vol. 11, p (1991), Vol. 107, p (1992 ), Vol. 108, p (1992b), Vol. 108, p (1992c), Vol. 108, p (1995), Vol. 111, p Nishimura, T. and Umetsu, Y.(1992) Hydrometall., Vol. 30, p Nishimura, T. and Umetsu, Y.(1996) Down Under '96 OZONE AND ITS APPLICATIONS, (G. Landers and Greg Peters, eds), Proc.of the First Australasian Conference of the International Ozone Assoc., (Sydney), p (1969), Vol. 37, p Ruetsch, P. (1988) J. Electrochem. Soc., Vol. 125, p Ruetsch, P. Giovanoli, R. (1988) : J. Electrochem. Soc., Vol. 135, p. 2663, Bustos, R. C., 290

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