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WO2012081896A2 - Procédé pour récupérer le nickel à partir de matières premières contenant du nickel - Google Patents

Procédé pour récupérer le nickel à partir de matières premières contenant du nickel Download PDF

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Publication number
WO2012081896A2
WO2012081896A2 PCT/KR2011/009601 KR2011009601W WO2012081896A2 WO 2012081896 A2 WO2012081896 A2 WO 2012081896A2 KR 2011009601 W KR2011009601 W KR 2011009601W WO 2012081896 A2 WO2012081896 A2 WO 2012081896A2
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WO
WIPO (PCT)
Prior art keywords
nickel
raw material
containing raw
hydrogen
leaching
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/KR2011/009601
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English (en)
Korean (ko)
Other versions
WO2012081896A3 (fr
Inventor
이재영
정형준
권오준
손진군
김기홍
정명채
김용래
강신명
이종섭
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Research Institute of Industrial Science and Technology RIST
Original Assignee
Research Institute of Industrial Science and Technology RIST
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Research Institute of Industrial Science and Technology RIST filed Critical Research Institute of Industrial Science and Technology RIST
Priority to PH1/2013/501376A priority Critical patent/PH12013501376A1/en
Priority to AU2011341871A priority patent/AU2011341871B2/en
Priority to CN201180067348.7A priority patent/CN103443303B/zh
Publication of WO2012081896A2 publication Critical patent/WO2012081896A2/fr
Publication of WO2012081896A3 publication Critical patent/WO2012081896A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/005—Preliminary treatment of ores, e.g. by roasting or by the Krupp-Renn process
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0407—Leaching processes
    • C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching

Definitions

  • the present invention relates to a method for effectively recovering nickel from a raw material containing nickel, and more particularly, to a method for effectively acid leaching and recovering nickel from a nickel ore having a high metal content.
  • Nickel-containing ores include ore such as limonite and saprolite, and these ores have passivation properties, which are slow in acid dissolution because of their resistance to acids. Therefore, as a method for effectively leaching nickel, a method of recovering nickel by dissolving acid in an autoclave under high temperature and high pressure has been proposed, which is called 'HPAL (High Pressure Acid Leaching)'.
  • 'HPAL High Pressure Acid Leaching
  • Nickel leaching at room temperature does not exceed 85% of nickel recovery even after leaching for several months or more.However, the HPAL method can be used to leach more than 90% of nickel within 2 hours. Can be.
  • Korean Patent Publication No. 2007-7020915, Japanese Patent Publication No. 2010-031341 and the like can be given.
  • HPAL method should be carried out under the high temperature and high pressure of the autoclave, and it is known that only titanium material can be used mainly because of its strong acidity, and thus has the disadvantage of high facility cost and high maintenance cost.
  • the present inventors have proposed a method of recovering nickel by acid leaching after the hydrogen reduction of the nickel-containing raw material in Korea Patent Publication No. 2009-0031321.
  • the technique of the patent document the step of recovering V, Mo in the petrochemical desulfurization waste catalyst and treating the remaining residue with an acid to remove alkali elements in the residue; Drying the residue from which the alkaline elements have been removed, and then heat-treating at a temperature range of 600-1300 ° C.
  • Disclosed is a method for producing an iron nickel-containing raw material from a petrochemical desulfurization waste catalyst recycling residue comprising the step of filtering and drying the product obtained in the above step to obtain Fe and Ni-containing raw materials.
  • the waste catalyst residue usually contains reduced metal (Fe + Ni) in a content of 15% by weight or less, but in the case of nickel ore, the content of metal (Fe + Ni) is 15-65% by weight, which is very high. You must do it.
  • the present invention provides a more improved method for recovering nickel compared to the conventional method in which Ni recovery can be carried out at a relatively low temperature (25-80 ° C.) and atmospheric pressure, which can be applied to a facility of a general material. To provide.
  • the present invention is to provide a method for effectively solving the stability problem due to oxidation during sampling after reduction caused by the high iron content of nickel oxide ore.
  • the present invention seeks to provide a method of recycling hydrogen to minimize the use of hydrogen in recovering Ni.
  • the present invention relates to a method for recovering nickel from a nickel-containing raw material, the nickel at a temperature of 550-950 °C using a reducing gas containing at least two times the number of moles of hydrogen relative to the (Fe + Ni) mole of the nickel-containing raw material
  • a reducing step of reducing the containing raw material A slurrying step of slurrying the reduced nickel-containing raw material; Leaching step of leaching nickel by dissolving the nickel-containing raw material by adding a slurry-containing raw material and acid to the reactor in an oxygen-free state;
  • the nickel-containing raw material may be dust obtained in the process of dry smelting nickel ore, or nickel ore, when the nickel-containing raw material is nickel ore, the nickel ore is dried, pulverized to a particle size of 1 mm or less, and What is obtained by baking at 250-850 degreeC can be used.
  • the reducing gas containing hydrogen may be a gas containing only hydrogen or a mixed gas of nitrogen and hydrogen.
  • the slurrying step is preferably carried out by immersing the reduced nickel-containing raw material in a tank containing oxygen-blocked water.
  • the acid may be sulfuric acid or hydrochloric acid, and in the case of sulfuric acid, at least one mole of the number of moles of (Fe + Ni) of the nickel-containing raw material, and in case of hydrochloric acid, at least two times the number of moles of (Fe + Ni). It is preferable to add.
  • the leaching step is preferably stopped when the pH of the solution is in the range of 0.1-1.0, it is preferably carried out for 0.5 to 2 hours at a reaction temperature of 25-80 °C.
  • the iron removing step may be performed by blowing the oxygen-containing gas to adjust the pH of the nickel-containing solution in the range of 2.5-5.5 to produce iron hydroxide, filtering the generated iron hydroxide, or by solvent extraction.
  • the collection of hydrogen from the exhaust gas may be done by cooling the exhaust gas containing water vapor and hydrogen to remove dust containing water produced by the condensation of the water vapor.
  • the hydrogen generated in the leaching step may be collected and re-supplied to the reduction step, using a scrubber from the exhaust gas containing hydrochloric acid mist and hydrogen discharged in the leaching step to remove the dust containing hydrochloric acid mist, Hydrogen can be resupplied to the reduction step by capture.
  • the present invention in recovering Ni, unlike in the prior art, it is not necessary to perform Ni at a high temperature and high pressure in order to leach nickel from a nickel-containing raw material, so that high-speed acid leaching is possible at low temperature and normal pressure, and thus the reactor is maintained at high temperature and high pressure. There is no need to use expensive titanium to withstand it.
  • the amount of hydrogen used in recovering Ni from nickel ore can be reduced and economical.
  • the present invention relates to a method for effectively recovering nickel from a nickel-containing raw material, and in particular, to a method for recovering nickel by effectively acid leaching nickel from a nickel ore having a high metal content.
  • the nickel ore to which the present invention is applied is not particularly limited as long as it contains nickel, and examples thereof include ore such as limonite and sapolite.
  • drying, grinding, and firing steps which are pretreatment steps, will be described in detail.
  • nickel when nickel is recovered from nickel-containing ore, it has been leached by the wet method, and for this purpose, it is usually pulverized in a state containing water.
  • it is necessary to uniformly control the ore particle size required for the reduction and leaching reactions it is possible to easily classify the particles by particle size using the wind speed of the dust collector, so that the uniform particle size required for the reduction and leaching reactions can be achieved. It is possible to obtain a powder having
  • an ore powder having a particle size of 1 mm or less it is preferable to use an ore powder having a particle size of 1 mm or less.
  • the particle size of the ore powder is larger than 1 mm, the reduction / leaching rate is slow, and in particular, the acid and leaching reactions are not preferable because of large clogging of the pump and pipes and poor workability.
  • the particle size of the powder is 1 mm or less, the lower limit thereof is not particularly limited, but in order to obtain a powder having a particle size smaller than 10 ⁇ m, the grinding process must be performed for a long time or more than several times. It is more preferable to do.
  • nickel ore contains crystal water, and if it is not subjected to calcination, crystal water contained in the ore is released as water in a subsequent reduction process to slow down the reduction reaction, and therefore, it is preferable to undergo a calcination process.
  • limonite emits crystal water at about 250-350 ° C and sapprite at around 650-750 ° C. Therefore, the ore powder obtained in the grinding process is in the range of 250-850 ° C. It is preferable to remove the crystal water contained in nickel ore by baking.
  • saprolite having a high nickel content is mainly used as a raw material for dry smelting, and nickel can be recovered by applying the present invention to rotary kiln dust generated in the dry smelting process.
  • the dust is included in a range suitable for applying the present invention and exposed to high temperature during the dry smelting process, the grinding and calcining process as in nickel-containing ore is not required.
  • the particle size is out of the range required by the present invention, for example, because the dust is exposed to air and contains moisture, it may be subjected to a pulverization or firing treatment as necessary.
  • Nickel ore is different depending on the type of ore, but usually contains 1-2.5% by weight of Ni and 15-55% by weight of Fe. Nickel can be recovered by reducing nickel from such a nickel ore.
  • the reduction is performed using a reducing gas.
  • Hydrogen is preferably used as the reducing gas used in reducing nickel.
  • excess hydrogen in the reduction reaction and hydrogen generated in the leaching reaction can be recovered and reused, thereby reducing the cost associated with the use of the reducing gas.
  • a reducing gas containing two or more moles of hydrogen relative to the number of moles of (Fe + Ni) contained in the nickel-containing raw material.
  • the upper limit is not particularly limited, it may cause an increase in cost due to an increase in the amount of hydrogen used, preferably not more than five times the number of moles of (Fe + Ni) contained in the nickel-containing raw material.
  • the temperature of the reduction furnace is preferably in the range of 550-950 °C. This is because the reduction rate does not sufficiently occur at the reduction temperature of 550 ° C. or lower, and the recovery rate is lowered during subsequent leaching. The reduction rate does not increase any more than 950 ° C. and only sinters between particles, which adversely affects workability.
  • the reducing gas may include an inert gas, and the inert gas may include nitrogen and the like, and the inert gas may also be recovered and reused.
  • Excess hydrogen and water vapor are generated by the reduction reaction as in Equation (2), which requires separation of water vapor and hydrogen to recycle hydrogen. Separation of water vapor and hydrogen can be separated from excess hydrogen by cooling the exhaust gas discharged after the reaction to change the water vapor into water. That is, when the exhaust gas is cooled, water vapor condenses to become water, whereby it can be separated and recovered from hydrogen through separation and recovery of gas and liquid.
  • the reduced nickel-containing raw material obtained in the reduction process is dust having a particle size of 1 mm or less, these must be separated from the exhaust gas. Therefore, it is necessary to separate both the liquid water and the hydrogen gas and the solid dust.
  • a scrubber can be used. When the exhaust gas is cooled in the scrubber, dust and water vapor are discharged to the lower part, hydrogen is discharged to the upper part, and hydrogen can be recovered by separating and collecting the compressed hydrogen gas and compressing the recovered hydrogen gas. It can be reloaded into the furnace.
  • the reduced nickel-containing raw material may be discharged into a tank containing oxygen-blocked water to slurry the reduced nickel-containing raw material to prevent oxidation of the iron component.
  • the slurry obtained is transferred to a pump and subjected to a subsequent leaching step.
  • the leaching step the slurried nickel-containing raw material is introduced into an oxygen-free reactor, and acid is added to dissolve the nickel by dissolving the nickel-containing raw material.
  • the acid used in the leaching step is not limited thereto, and hydrochloric acid, sulfuric acid and nitric acid, as well as various other acids may be used. However, it is more preferable to use hydrochloric acid and sulfuric acid in terms of wastewater treatment and cost.
  • metal acid reactions such as the following formulas (3) and (4) proceed to generate hydrogen gas.
  • the reduced nickel-containing raw material is leached with an acid
  • nickel and iron are selectively dissolved as ions by the reactions of the formulas (3) and (4), and Al 2 O 3 and SiO 2 contained in the nickel-containing raw material , Cr 2 O 3 and the like hardly occur due to acid dissolution and are obtained as a solid residue. Therefore, the nickel-containing solution obtained by the leaching step and the residue of the solid phase are very easy to be separated by filtration, so that the nickel-containing solution can be separated by a solid-liquid separator such as a filter press or a decanter.
  • the leaching step may be carried out at a temperature of 25-80 °C. Leaching of nickel by acid can be completed within 2 hours even if the present invention is applied at room temperature.
  • the leaching step is faster as the reaction temperature is higher, but the energy cost is higher as the reaction temperature is higher, especially when the leaching reaction is carried out at 80 °C or more, the generation of hydrogen gas exploded, it is difficult to control the pressure of hydrogen Hydrogen recovery and reuse becomes difficult. Therefore, it is preferable to carry out the leaching reaction in the above temperature range.
  • Termination of the leaching reaction can be confirmed by changing the pH.
  • the pH of the solution in the reactor rises. It is preferable to terminate the leaching reaction when the pH is in the range of 0.1-1. If the pH is lower than 0.1, free acid must be removed in a subsequent process, which increases the alkali consumption.
  • the pH is higher than 1 because hydrochloric acid is less than the equivalent ratio, substitution substitution of Ni occurs by the unreacted Fe metal, resulting in a problem that the nickel recovery rate decreases. Therefore, when the pH of the solution in the reactor reaches the range of 0.1-1, the leaching reaction is terminated and filtered to separate the solution containing nickel ions and the residue sludge.
  • the leaching step is performed in the same manner as above, leaching is terminated within 2 hours. At this time, 90% or more nickel leaching rate can be secured. More preferably, if the leaching step is performed in less than 30 minutes, since the nickel is not sufficiently leached from the nickel-containing raw material, the leaching step is preferably performed for 30 minutes or more.
  • Hydrogen used in the reaction of formula (1) is generated in the leaching step as shown in formulas (3) and (4). Therefore, the hydrogen demand can be greatly reduced by recovering and reusing hydrogen generated in the formulas (3) and (4).
  • the recovery of the hydrogen may be recovered by removing the dust containing hydrochloric acid mist using a scrubber from the exhaust gas containing hydrochloric acid mist and hydrogen discharged in the leaching step, by collecting the hydrogen, the recovered hydrogen is reduced Can be reused by resupplying
  • Hydrogen generated in the leaching step was recovered according to the method of the present invention and the hydrogen generation amount and recovery amount were measured. As a result, 95% of the theoretical hydrogen generation amount could be recovered.
  • the reason for not reaching the recovery rate of 100% is that the leaching rate is rapidly slowed at the end of the reaction, so that the leaching rate of the metals of nickel and iron does not reach 100% and the reduction rate of iron and nickel does not reach 100%. .
  • the method for recovering nickel from the nickel-containing raw material of the present invention includes the step of removing iron from the nickel-containing solution in the leaching step after separating the nickel-containing solution from the nickel-containing solution with the solid residue. .
  • the content unit of each component is weight percent, the balance is oxygen, and includes a trace amount of Mn.
  • the nickel ore of Table 1 was ground and calcined under the pretreatment conditions as shown in Table 2 to prepare a sample.
  • Ni-containing raw materials were reduced at a temperature of 700 ° C. by using twice the number of moles of hydrogen as the reducing gas with respect to the number of moles of (Fe + Ni) included in each of the samples. Water vapor and excess hydrogen produced in the reduction reaction were discharged as exhaust gas.
  • the reduced nickel-containing raw material was slurried by feeding to a tank containing oxygen and containing water.
  • Hydrochloric acid was added to the obtained slurry at a molar number of 1 times the number of moles of (Fe + Ni) contained in the sample, and the sample was dissolved at a temperature of 30 ° C. to leach nickel.
  • the leaching reaction was performed until the pH of the solution was 0.5, the time required for this time was 1 hour 45 minutes. Hydrogen gas produced in the leaching reaction was discharged as exhaust gas.
  • the solid residue sludge was removed using a solid-liquid separator to obtain a nickel-containing solution.
  • Oxygen was added while adjusting the obtained nickel-containing solution to pH 3 to convert iron in the solution to iron hydroxide, and iron hydroxide was filtered to recover nickel.
  • the content unit of each component is weight percent, the balance is oxygen, and includes a trace amount of Mn.
  • limonite was prepared by pretreatment as inventive example 1 of Example 1
  • saprolite was prepared by pretreatment as inventive example 3 of Example 1 to prepare a sample.
  • the reduction rate of the sample obtained by the reduction step was collected by cooling the steam generated by the reaction of the formula (1) and calculating the amount of steam generated relative to the FeNi input equivalent. The results are shown in Table 4.
  • the reduced sample was fed to a tank containing oxygen and contained water, and slurried or extracted into air. Accordingly, it is observed whether or not the sample is ignited by the exothermic due to Fe oxidation and the flame propagation due to the exotherm during extraction outside the reduction furnace, and the results are shown in Table 4.
  • Comparative Example 10 raising the reduction temperature prevents the ignition problem occurring during extraction in the air, but causes the sintering of the sample, causing a problem of sticking in a facility such as a rotary kiln. Furthermore, there exists a possibility that it may have a bad influence also in a subsequent leaching process.
  • Reference Example 1 when the kiln dust is reduced at 825-850 ° C., the iron content in the dust is low, so even if extracted into the air, no problem of ignition of the sample occurs, but it is applied to a sample having a high iron content. There is also a risk of fire.
  • Inventive Examples 4 to 7 performed a reduction reaction within the temperature range defined by the present invention, and showed a high reduction rate. Also, by extracting the reduced sample into a tank filled with oxygen-blocked water, The reduced iron content prevented the sample from igniting. The reduced sample deposited in water is limited in oxidation due to the small oxygen in the water. It may also be supplied in the form of a slurry in a subsequent leaching process.
  • the water storage tank in the reduction furnace extraction unit as a barrier to prevent out-of-hydrogen discharge and ingress of oxygen in the furnace, can provide a so-called water sealing effect to provide a base for hydrogen recycling.
  • NiFe + 4HCl NiCl 2 + FeCl 2 + 2H 2 (7)

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

La présente invention concerne un procédé pour récupérer efficacement le nickel à partir de matières premières contenant du nickel et comprend les stades suivants: un stade de réduction visant à réduire les matières premières contenant du nickel à une température entre 550 et 950℃ en utilisant un gaz réducteur qui contient le double ou plus de moles d'hydrogène que de moles de matières premières contenant du nickel (Fe+Ni); un stade de transformation en boue pour transformer en boue les matières premières réduites contenant du nickel; une stade de lixiviation pour lixivier le nickel en versant les matières premières contenant du nickel transformées en boues et de l'acide dans un réacteur exempt d'oxygène et en dissolvant les matières premières contenant du nickel; un stade de séparation solides / liquides visant à obtenir une solution contenant du nickel par le filtrage et l'élimination de boues résiduelles, au moyen d'un séparateur solides / liquides, à partir de la solution qui a été obtenue lors du stade de lixiviation; et un stade d'élimination de fer visant à éliminer le fer de la solution contenant du nickel.
PCT/KR2011/009601 2010-12-13 2011-12-13 Procédé pour récupérer le nickel à partir de matières premières contenant du nickel Ceased WO2012081896A2 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
PH1/2013/501376A PH12013501376A1 (en) 2010-12-13 2011-12-13 Method for recovering nickel from raw material containing nickel
AU2011341871A AU2011341871B2 (en) 2010-12-13 2011-12-13 Method for recovering nickel from raw material containing nickel
CN201180067348.7A CN103443303B (zh) 2010-12-13 2011-12-13 从含镍原材料回收镍的方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR10-2010-0127208 2010-12-13
KR1020100127208A KR101172897B1 (ko) 2010-12-13 2010-12-13 니켈 함유 원료로부터 니켈을 회수하는 방법

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WO2012081896A2 true WO2012081896A2 (fr) 2012-06-21
WO2012081896A3 WO2012081896A3 (fr) 2012-10-04

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KR (1) KR101172897B1 (fr)
CN (1) CN103443303B (fr)
AU (1) AU2011341871B2 (fr)
PH (1) PH12013501376A1 (fr)
WO (1) WO2012081896A2 (fr)

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KR101449195B1 (ko) * 2012-12-24 2014-10-13 주식회사 포스코 습식 제련 공정 중 침출단계에서 발생하는 수소 가스의 회수 방법 및 회수된 수소 가스의 재활용 장치
KR20150062254A (ko) * 2013-11-28 2015-06-08 주식회사 포스코 제련 공정 부산물의 리사이클링 장치 및 방법
KR101995458B1 (ko) * 2017-12-22 2019-07-02 주식회사 포스코 니켈 습식 제련을 위한 니켈광의 건식 장치
CN110257630A (zh) * 2019-05-31 2019-09-20 荆门德威格林美钨资源循环利用有限公司 一种从提钨废料中综合回收钴镍的方法
KR102503805B1 (ko) * 2021-10-18 2023-02-24 도담케미칼 주식회사 석유탈황용 폐촉매로부터의 Ni, Al 및 NaOH 추출 및 회수 방법

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AUPS201902A0 (en) * 2002-04-29 2002-06-06 Qni Technology Pty Ltd Modified atmospheric leach process for laterite ores
WO2006029499A1 (fr) * 2004-08-02 2006-03-23 Skye Resources Inc. Procede permettant de recuperer du nickel et du cobalt a partir de minerais de laterite par combinaison de lixiviation a pression atmospherique et a pression moderee
FR2905383B1 (fr) * 2006-09-06 2008-11-07 Eramet Sa Procede de traitement hydrometallurgique d'un minerai de nickel et de cobalt lateritique,et procede de preparation de concentres intermediaires ou de produits commerciaux de nickel et/ou de cobalt l'utilisant.
CN100503848C (zh) * 2006-12-20 2009-06-24 潘继红 氧化镍矿的硫酸强化浸出提取法
JP5143232B2 (ja) 2007-09-21 2013-02-13 リサーチ インスティチュート オブ インダストリアル サイエンス アンド テクノロジー 石油化学脱硫触媒リサイクル残渣からの鉄ニッケル含有原料及びコバルト含有原料の製造方法、及び鉄ニッケル含有原料を用いたステンレス原料の製造方法、及びフェロニッケルの製造方法

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Publication number Publication date
KR101172897B1 (ko) 2012-08-10
CN103443303A (zh) 2013-12-11
KR20120065874A (ko) 2012-06-21
AU2011341871A1 (en) 2013-07-18
AU2011341871B2 (en) 2015-07-02
PH12013501376A1 (en) 2013-08-28
WO2012081896A3 (fr) 2012-10-04
CN103443303B (zh) 2015-06-17

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