PH12016501165B1 - Process for suppressing elution of manganese - Google Patents
Process for suppressing elution of manganese Download PDFInfo
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- PH12016501165B1 PH12016501165B1 PH12016501165A PH12016501165A PH12016501165B1 PH 12016501165 B1 PH12016501165 B1 PH 12016501165B1 PH 12016501165 A PH12016501165 A PH 12016501165A PH 12016501165 A PH12016501165 A PH 12016501165A PH 12016501165 B1 PH12016501165 B1 PH 12016501165B1
- Authority
- PH
- Philippines
- Prior art keywords
- manganese
- slurry
- settling pond
- precipitate
- elution
- Prior art date
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- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 86
- 239000011572 manganese Substances 0.000 title claims abstract description 86
- 238000010828 elution Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims description 23
- 239000002002 slurry Substances 0.000 claims abstract description 63
- 239000002244 precipitate Substances 0.000 claims description 32
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 26
- 229910052759 nickel Inorganic materials 0.000 claims description 13
- 229910017052 cobalt Inorganic materials 0.000 claims description 11
- 239000010941 cobalt Substances 0.000 claims description 11
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 11
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 10
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 10
- 239000002351 wastewater Substances 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- 238000002386 leaching Methods 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 7
- 235000019738 Limestone Nutrition 0.000 claims description 5
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 5
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 5
- 239000000920 calcium hydroxide Substances 0.000 claims description 5
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 5
- 239000006028 limestone Substances 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 235000002908 manganese Nutrition 0.000 claims description 2
- 239000013049 sediment Substances 0.000 abstract 2
- 238000004062 sedimentation Methods 0.000 abstract 2
- 238000006386 neutralization reaction Methods 0.000 description 15
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- 230000007423 decrease Effects 0.000 description 8
- 239000000843 powder Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000001569 carbon dioxide Substances 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 238000009854 hydrometallurgy Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- NAIXASFEPQPICN-UHFFFAOYSA-O p-nitrophenylphosphocholine Chemical compound C[N+](C)(C)CCOP(O)(=O)OC1=CC=C([N+]([O-])=O)C=C1 NAIXASFEPQPICN-UHFFFAOYSA-O 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 238000009853 pyrometallurgy Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
- C02F1/004—Processes for the treatment of water whereby the filtration technique is of importance using large scale industrial sized filters
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/206—Manganese or manganese compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/10—Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities
Abstract
The present invention suppresses elution of manganese from manganese sediment in slurry accumulated in a sedimentation tank. The present invention sets the pH of the slurry including manganese sediment accumulated in the sedimentation tank to 8.0-9.0 and suppresses the elution of manganese.
Description
] ye Oe Pra Copy 10 Foe a . ) .
PROCESS FOR SUPPRESSING ELUTION OF MANGANESE
The present invention relates to a process for suppressing elution of manganese which suppresses elution of manganese from manganese precipitate in slurry containing manganese precipitate stored in a settling pond.
The present application claims priority on the basis of
Japanese Patent Application No. JP 2013-259175 filed on
December 16, 2013 in Japan.
In recent years, high pressure acid leach using sulfuric acid is attracting attention as a hydrometallurgical process of nickel oxide ore. This process is different from pyrometallurgical process which is a conventional general smelting process of nickel oxide ore, and it comprises consistent hydrometallurgical step and does not include pryometallurgical step such as reducing step and drying step, so it 1s advantageous in terms of energy and cost. Also, the high pressure acid leach is having an advantage that it is possible to obtain a sulfide containing cobalt and nickel in which a nickel grade is increased to the extent of 50% by mass (Hereinafter, referred to as nickel-cobalt mixed sulfide.).
A hydrometallurgical process of nickel oxide ore using this high pressure acid leach comprises: an ore treatment step for grinding nickel oxide ore to a predetermined size to be slurry; a (high pressure acid) leaching step for performing a leaching treatment under high temperature and high pressure by adding sulfuric acid to ore slurry; a preliminary neutralization step for performing a neutralization (Hereinafter, referred to as preliminary neutralization.) treatment to leached slurry before multistage washing of the leached slurry; a solid-liquid separation step (Hereinafter, referred to as “CCD step”.) for solid-liquid separating the leached slurry obtained by performing the preliminary neutralization step into a leached residue and a leachate containing impurity elements together with nickel and cobalt while multistage washing of the leached slurry; a neutralization step for obtaining a neutralization final solution containing zinc together with nickel and cobalt by separating a neutralized precipitate containing impurity elements by adjusting pH of the obtained leachate; a dezincification step for obtaining a mother liquor for nickel recovery by forming and separating zinc sulfide by adding sulfurizing agent to this kind of problem, for example in Patent Document 2, a process for precipitating manganese selectively and efficiently is described.
However, there is no useful knowledge about the change of manganese concentration at the time of solid-liquid separation in the settling pond after the neutralization treatment, namely, after the precipitation of manganese.
In Patent Document 3, a process for expediting coagulative precipitation by adding heavy metal inorganic compound at the time of neutralization treatment is described. However, in Patent Document 3, it is not mentioned about the behavior of concentration of heavy metal at the time of solid-liquid separation after the precipitation.
In the settling pond, the manganese concentration is normally controlled to the concentration that will not affect the environment. However, in the settling pond, there is a case that the manganese concentration will fluctuate suddenly, especially the concentration will rise suddenly, and its cause has not been found yet. Therefore, the control of the manganese concentration will be difficult. Therefore, in the settling pond, it is required to control the manganese concentration based on the knowledge about the change of manganese concentration at the time of solid-liquid separation.
Patent Document 1: Japanese Patent Application
Laid-Open No. 2005-350766
Patent Document 2: Japanese Patent Application
Laid-Open No. H9-248576
Patent Document 3: Japanese Patent Application
Laid-Open No. 2012-250226
The present invention has been proposed by considering such actual circumstances, and an object of the present invention is to provide a process for suppressing elution of manganese which suppresses elution of manganese from manganese precipitate in a settling pond.
A process for suppressing elution of manganese according to the present invention is a process for suppressing elution of manganese which suppresses elution of manganese from a manganese precipitate in slurry containing the manganese precipitate, an aluminum precipitate, nickel and cobalt stored in a settling pond, wherein pH of slurry in the settling pond is adjusted to 8.0 to 9.0, the slurry is a waste water generated by high pressure acid leach for leaching nickel and cobalt from nickel oxide ore, the waste water contains the manganese precipitate and the aluminum precipitate generated by a precipitating agent of limestone and slaked lime, and manganese concentration in the obtained slurry is less than 1 mg/L.
In the present invention, by adjusting the pH of slurry containing manganese precipitate stored in the settling pond to 8.0 to 9.0, it is possible to suppress elution of manganese from the manganese precipitate, so it is possible to decrease the manganese concentration of a supernatant obtained by depositing manganese precipitate.
Fig. 1 is illustrating a relation of change of pH and manganese concentration of slurry stored in a settling pond.
Fig. 2 is illustrating a relation of change of pH and manganese concentration of slurry after removing a solid content from a settling pond.
Hereinafter, a process for suppressing elution of manganese according to the present invention will be described in detail with reference to the drawings. In addition, the present invention should not be limited to the following embodiments, and various changes can be made within the scope not deviating from the gist of the present er ——————————————————— eee reer ____ invention
A process for suppressing elution of manganese is a process for suppressing elution of manganese from a manganese precipitate by adjusting pH of slurry containing the manganese precipitate stored in a settling pond to 8.0 to 9.0.
For slurry stored in the settling pond, it is the slurry containing precipitate formed by subjecting filtrate after recovering nickel and cobalt from leaching residue or leachate generated when high pressure acid leaching nickel and cobalt, for example from nickel oxide ore to neutralization treatment with limestone powder and slaked lime powder in neutralization treatment facilities. Namely, the process for suppressing elution of manganese can be applied to suppress elution of manganese for preventing the increase of manganese concentration of waste water stored in the settling pond, after the neutralization treatment of waste water containing leaching residue or filtrate generated in hydrometallurgy of, for example nickel oxide ore.
In nickel oxide ore, manganese, aluminum and else are contained as impurities other than nickel and cobalt.
Therefore, when the leached residue or filtrate is subjected to neutralization treatment by limestone powder or slaked lime powder, a precipitate of manganese, aluminum and else will be generated.
At the time of neutralization treatment, pH of waste water containing leached residue or filtrate is preferably adjusted to 8.0 to 10.0. When pH of waste water is too low, precipitation of manganese will be deteriorated. When pH is too high, it is not preferable as the used amount of neutralizing agent will be large.
The slurry containing the precipitate of manganese, aluminum and else is stored once at the settling pond before discharging into sea or river. Here, the settling pond includes dam. At the settling pond, the slurry containing the manganese precipitate is stored for a while and precipitates of manganese precipitate and else will be deposited. And, after the precipitates have deposited, a detoxified supernatant will be discharged to the outside such as sea or river by pumping up.
In the settling pond, it is necessary to discharge the detoxified supernatant into sea, river and else, in order to inhibit the burden on the environment. In the settling pond, it is preferable that, for example manganese is deposited as a precipitate and that manganese is not dissolved in the supernatant, but manganese concentration in the supernatant is increasing.
The increase of manganese concentration is related to pH of slurry. The manganese concentration increases when the pH of slurry decreases. It is considered that the pH of slurry decreases by the occurrence of proton when carbon dioxide in the air dissolves into slurry.
When the pH of slurry decreases, manganese will be eluted from the precipitate. The relation of the pH of slurry and the manganese concentration can be understood from the measurement result of the pH of slurry and the manganese concentration indicated in Fig. 1.
Fig. 1 is a result of measuring pH of slurry and manganese concentration in the settling pond for about 70 days. The pH achieved by the dissolution of carbon dioxide is in the order of 7.7. As indicated in Fig. 1, the elution of manganese begins when the pH of slurry becomes lower than 8.5, and the manganese concentration is over 1 mg/L when the pH of slurry becomes lower than 8.0. The value of 1 mg/L is a prescribed value defined, for example by National
Pollution Control Commission (NPCC) of Philippine.
Therefore, it is necessary to inhibit the manganese concentration in slurry to less than 1 mg/L.
Also, from the result indicated in Fig. 1, it can be understood that the time for the pH of slurry to reach 8.5 is about 20 days, and after 20 days, the elution of manganese caused by the decrease of pH will begin sharply, and at 30 days the manganese concentration will reach 1 mg/L.
Therefore, the discharge from the settling pond is performed before the pH of the stored slurry becomes lower than8.0, preferably 8.25. Inother words, if the pH of slurry could be maintained in the range of 8.0 to 9.0, preferably in the range of 8.25 to 8.75, the elution of the manganese is inhibited, and it is possible to discharge in the condition satisfying the prescribed value of NPCC, i.e. in the condition that the manganese concentration is less than 1 mg/L.
In the settling pond, the stored time of slurry should be 30 days or less, preferably 20 days or less, as the process for maintaining the pH of slurry below 8.0, preferably below 8.25. If the stored time is 30 days or less, the elution of manganese is inhibited, so it is possible to satisfy the condition that the manganese concentration is less than 1 mg/L.
Here, it is searched separately about the relation between the decrease of pH and carbon dioxide by measuring the pH in the state without a solid content (precipitates).
The result thereof is illustrated in Fig. 2. In addition, the precipitates are removed from slurry, but it was not possible to remove all of them, so small amount of manganese was detected.
From the result indicated in Fig. 2, it can be understood that pH will be decreased until 7.7 as well as the case including the solid content, even if it is held in the atmosphere, after removing the solid content (precipitates) from slurry. In other words, it can be understood that pH will be decreased to the extent of 7.7 when the slurry is held in the atmosphere, regardless of the existence of the solid content. The decrease of pH will be accelerated when there is no solid content as there is no substance to be eluted. Therefore, it can be understood that the decrease of pH is caused by the dissolution of carbon dioxide of acidic gas contained in the atmosphere into the slurry.
In the process for suppressing elution of manganese, it is preferable that the pH of slurry is 8.0 to 10.0 when discharging slurry into the settling pond. In the process for suppressing elution of manganese, it is possible to discharge slurry into the settling pond in the state that manganese is not eluted and that the manganese concentration is very low, by adjusting the pH of slurry to 8.0 to 10.0.
From the above, the process for suppressing elution of manganese can suppress the increase of manganese concentration even the slurry before discharging into sea or river is stored in the settling pond exposed to outside air. Thereby, the process for suppressing elution of manganese can suppress the environmental influences and its effect is very significant.
Explaining about the examples applying the present invention. In addition, the present invention should not be limited in any way to the examples below. <Example>
In the example, at first, slurry including a manganese precipitate was obtained by performing a neutralization treatment to add limestone powder and slaked lime powder to a waste water including manganese generated in a high pressure acid leach for leaching nickel and cobalt from nickel oxide ore.
Next, in the example, the slurry was discharged into a settling pond. The pH of the slurry at the time of discharge of the slurry into the settling pond was 9.10, and manganese concentration was 0.3 mg/L.
Next, in the example, the slurry was rested for 15 days in the settling pond in the air atmosphere. Then, a supernatant was discharged into sea by pumping up. The pH of the slurry at this time was 8.5, and the manganese concentration was 0.1 mg/L
Therefore, in the example, the elution of manganese was suppressed. <Comparative Example>
In the comparative example, a neutralization treatment was performed to a waste water including manganese generated by a high pressure acid leach as well as the example. Next, in the comparative example, slurry was discharged into a settling pond in the state that the pH of the slurry was 9.15.
Next, in the comparative example, the slurry was rested for 40 days in the settling pond in the air atmosphere. The manganese concentration of the slurry was 2.5 mg/L.
Claims (1)
1. A process for suppressing elution of manganese which suppresses elution of manganese from a manganese precipitate in slurry containing the manganese precipitate, an aluminum precipitate, nickel and cobalt stored in a settling pond, wherein pH of the slurry in the settling pond is adjusted to 8.0 to 9.0, the slurry is a waste water generated by high pressure acid leach for leaching nickel and cobalt from nickel oxide ore, the waste water contains the manganese precipitate and the aluminum precipitate generated by a precipitating agent of limestone and slaked lime, and manganese concentration in the obtained slurry is less than 1 mg/L.
2. The process for suppressing elution of manganese according to claim 1, wherein the stored time of the slurry in the settling pond is 30 day or less.
3. The process for suppressing elution of manganese according to claim 1, wherein a supernatant is discharged from the settling pond to outside by pumping up.
4. The process for suppressing elution of manganese according to claim 1, wherein pH of the slurry is 8.0 to
10.0 when discharging the slurry into the settling pond.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2013259175A JP5861694B2 (en) | 2013-12-16 | 2013-12-16 | Method for suppressing manganese elution |
| PCT/JP2014/082647 WO2015093363A1 (en) | 2013-12-16 | 2014-12-10 | Method for suppressing elution of manganese |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| PH12016501165B1 true PH12016501165B1 (en) | 2016-08-15 |
| PH12016501165A1 PH12016501165A1 (en) | 2016-08-15 |
Family
ID=53402712
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PH12016501165A PH12016501165A1 (en) | 2013-12-16 | 2016-06-16 | Process for suppressing elution of manganese |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP5861694B2 (en) |
| PH (1) | PH12016501165A1 (en) |
| WO (1) | WO2015093363A1 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6358570B2 (en) * | 2016-12-01 | 2018-07-18 | 住友金属鉱山株式会社 | Leaching residue slurry discharge facility |
| CN109626461A (en) * | 2018-11-13 | 2019-04-16 | 核工业北京化工冶金研究院 | A kind of in-situ acid uranium leaching evaporation tank waste liquid accelerates the device and method of evaporation |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3225836B2 (en) * | 1996-03-14 | 2001-11-05 | 大平洋金属株式会社 | Preferential removal of manganese from magnesium-containing manganese acidic solutions. |
| JP4207479B2 (en) * | 2002-07-16 | 2009-01-14 | 株式会社大林組 | How to treat dredged mud |
| JP4525428B2 (en) * | 2004-05-13 | 2010-08-18 | 住友金属鉱山株式会社 | Method for hydrometallizing nickel oxide ore |
| JP5359392B2 (en) * | 2009-03-09 | 2013-12-04 | 住友金属鉱山株式会社 | Method for removing manganese from wastewater |
| JP5749461B2 (en) * | 2010-03-10 | 2015-07-15 | 住友金属鉱山株式会社 | Wastewater treatment method for wastewater containing aluminum, magnesium and manganese |
| JP2012250226A (en) * | 2011-06-01 | 2012-12-20 | Nippon Filter Kk | Water-treating solid-liquid separation method |
-
2013
- 2013-12-16 JP JP2013259175A patent/JP5861694B2/en active Active
-
2014
- 2014-12-10 WO PCT/JP2014/082647 patent/WO2015093363A1/en active Application Filing
-
2016
- 2016-06-16 PH PH12016501165A patent/PH12016501165A1/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| WO2015093363A1 (en) | 2015-06-25 |
| PH12016501165A1 (en) | 2016-08-15 |
| JP2015112590A (en) | 2015-06-22 |
| JP5861694B2 (en) | 2016-02-16 |
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