WO2015159846A1 - 炭素及び硫黄の濃度が低いニッケル粉の製造方法 - Google Patents
炭素及び硫黄の濃度が低いニッケル粉の製造方法 Download PDFInfo
- Publication number
- WO2015159846A1 WO2015159846A1 PCT/JP2015/061358 JP2015061358W WO2015159846A1 WO 2015159846 A1 WO2015159846 A1 WO 2015159846A1 JP 2015061358 W JP2015061358 W JP 2015061358W WO 2015159846 A1 WO2015159846 A1 WO 2015159846A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- nickel powder
- nickel
- sulfur
- carbon
- powder
- Prior art date
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F9/26—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions using gaseous reductors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F2009/245—Reduction reaction in an Ionic Liquid [IL]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/15—Nickel or cobalt
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Definitions
- the present invention relates to a method for producing nickel powder with reduced impurities, particularly carbon and sulfur, from nickel powder produced from a nickel solution by a complex reduction method.
- iron ore is roasted to reduce the form of sulfides and oxides to obtain ferronickel, which is an alloy with iron, and used as a raw material for stainless steel.
- ferronickel which is an alloy with iron
- impurities are separated from an acid solution dissolved with hydrochloric acid or sulfuric acid, and electrolytic nickel is collected to obtain electric nickel.
- the acid-dissolved solution may be recovered as nickel salts such as nickel sulfate and nickel chloride and used for plating or battery materials.
- Non-Patent Document 1 As a method for producing powdered nickel from the nickel salts, for example, there is a wet process shown in Non-Patent Document 1.
- a complexing agent is mixed in a nickel sulfate aqueous solution and complexed to form a nickel ammine complex solution.
- the solution is placed in a pressure vessel and sealed, and about 150 to 250 ° C.
- the nickel ammine complex is reduced by hydrogen to produce nickel powder by a so-called complexing reduction method in which the temperature is raised and maintained and hydrogen gas is blown into it.
- nickel powder is used as a positive electrode active material such as a paste or a nickel metal hydride battery
- impurity elements such as carbon and sulfur cause gas generation, and thus reduction thereof is required.
- Patent Document 1 discloses nickel sulfide ore obtained from wet refining of nickel oxide ore, scrap, or work-in-process. A method for providing a production method for producing a ferronickel raw material from a mixed sulfide containing benzene is shown.
- Nickel sulfide or a mixed sulfide of nickel sulfide and cobalt sulfide is made into a slurry, and when nickel sulfide is dissolved by adding an oxidizing agent to the slurry, nickel is contained.
- a deironing step in which an alkali is added to the concentrate obtained in the redissolving step to obtain a neutralized starch and a neutralized solution.
- the present invention provides a production method for reducing the content of sulfur and carbon, which are impurities in nickel powder, in order to further improve the quality of nickel powder produced using a complexing reduction method.
- the present invention separates sulfur and carbon by washing and roasting nickel powder produced from a nickel solution using a complex reduction method.
- 1st invention of this invention is a manufacturing method of nickel powder with low carbon and sulfur concentration, Comprising: The complexation which produces the solution containing the nickel complex ion formed by adding a complexing agent to nickel sulfate aqueous solution The solution containing the nickel complex ions charged in the pressurized container is maintained at a liquid temperature of 150 to 250 ° C., and hydrogen gas is blown into the solution containing the nickel complex ions to perform hydrogen reduction.
- This is a method for producing nickel powder having a low carbon and sulfur concentration.
- a second invention of the present invention is a method for producing nickel powder having a low carbon and sulfur concentration, characterized in that the hydrogen concentration of the mixed gas in the roasting treatment of the first invention is 2 to 4% by weight. is there.
- the third invention of the present invention is a method for producing nickel powder having a low carbon and sulfur concentration, characterized in that the temperature in the roasting treatment of the first and second inventions is 700 ° C. or higher and 1250 ° C. or lower. is there.
- a fourth invention of the present invention is characterized in that the amount of water in the water washing treatment of the first to third inventions is 1 to 5 times the weight of the nickel powder. This is a method for producing nickel powder having a low concentration.
- sulfur and carbon of impurity elements can be effectively removed from nickel powder produced using a complexing reduction method, and the quality of nickel powder can be greatly improved. It is.
- nickel powder of the present invention It is a manufacturing flow figure of nickel powder of the present invention. It is a figure which shows the quantity of the sprinkling water in the washing
- the present invention reduces the impurity concentration of nickel powder, which has been difficult until now, by making the atmosphere of roasting a mixed gas of hydrogen and nitrogen, maintaining the specific surface area of particles, and providing a cleaning process. It is possible.
- the production method of the present invention will be described with reference to the drawings.
- FIG. 1 is a production flow diagram showing a method for producing nickel powder of the present invention.
- the present invention is characterized by the removal of impurities, particularly carbon and sulfur, contained in the nickel powder produced using the complex reduction method.
- impurities particularly carbon and sulfur
- the sample powder was prepared by adding ammonia and a dispersing agent as a complexing agent to a nickel-containing solution and complexing it to form a slurry containing nickel complex ions such as “nickel sulfate ammine complex”.
- a slurry containing nickel complex ions such as “nickel sulfate ammine complex”.
- hydrogen gas is blown into the slurry, and nickel complex ions in the slurry are reduced to produce a test powder of nickel powder by hydrogen reduction.
- a conventionally known method can be used.
- nickel powder or iron powder may be added as a seed crystal.
- a feature of the present invention resides in a manufacturing method for removing impurities, particularly carbon and sulfur, contained in the powder from the nickel powder obtained above.
- the method for removing carbon and sulfur components of impurities from the nickel powder according to the present invention involves subjecting the sample powder to a washing treatment using water for the sample powder, Nickel obtained by going through a "cleaning process” that removes water-soluble impurities in step and a “roasting process” that separates residual carbon and sulfur that could not be removed in the “cleaning process” by baking at high temperature.
- the impurity concentration in the powder is reduced to produce high purity nickel powder. Therefore, the “washing process” and “roasting process” that characterize the present invention will be described in detail below.
- the nickel powder of the sample powder is washed by a predetermined method to obtain a nickel powder having a reduced concentration of water-soluble impurities.
- a specific cleaning method various methods can be used such as pouring water over nickel powder or raising the water temperature to about 90 ° C. It is also effective to perform cleaning in an atmosphere to which ultrasonic waves are applied.
- the amount of washing water is preferably 1 to 5 times by weight ratio of the amount of nickel to be washed, and preferably 3 times or less. If the amount of washing water is less than 1 time, the amount of washing water may be insufficient, and the removal of carbon and sulfur may be incomplete. Moreover, even if it uses exceeding 5 times, a washing
- the nickel powder from which most of the water-soluble sulfur and carbon have been removed in the washing step is roasted at a high temperature to separate the remaining sulfur and carbon, thereby obtaining a high-purity nickel powder.
- the present invention does not use an oxidizing atmosphere or a completely inert atmosphere for the roasting process, but effectively removes sulfur and carbon in a reducing atmosphere containing a very small amount of hydrogen gas. I found what I could do and completed it.
- the atmosphere in the roasting process of the present invention requires that the concentration of hydrogen gas in an inert atmosphere such as nitrogen be 2 to 4% by weight. If it is less than 2% by weight, the reaction is slow and a sufficient reduction effect is obtained. Absent. Further, a concentration exceeding 4% by weight is not preferable because the reducing power is too strong.
- the roasting temperature is preferably 700 ° C. or more and 1250 ° C. or less, and preferably 1000 ° C. or less.
- separation of carbon and sulfur becomes insufficient.
- the higher the roasting temperature the more efficiently the separation, but the separation hardly increases even when roasting at a temperature exceeding 1000 ° C., especially when the temperature exceeds 1250 ° C., the sintering of nickel powder proceeds, It is not preferable because the solubility is lowered for the use of dissolving nickel powder in an acid.
- Example powder Manufacture of nickel powder (sample powder)
- a batch type autoclave with a capacity of 3 L was used as an experimental apparatus.
- the starting liquid was adjusted, and this starting liquid was put in an inner cylinder can of an autoclave.
- the temperature of the slurry in the inner cylinder can was increased to 185 ° C. using a heat medium heater.
- hydrogen gas in the hydrogen cylinder is blown into the slurry at a flow rate of 4.0 liters / min, and the internal pressure is increased to 3.5 MPa while maintaining the hydrogen reduction reaction.
- Gave rise to The reaction was carried out for 60 minutes from the start of blowing hydrogen gas, the supply of hydrogen gas was stopped after the lapse of time, and then cooled to room temperature with stirring.
- the cooled inner cylinder can was taken out from the autoclave, and the slurry contained in the inner cylinder can was subjected to solid-liquid separation using a filter paper and Nutsche to recover nickel powder by a complex reduction method.
- the recovered nickel powder was about 140 g.
- the reduction rate calculated by dividing the amount of nickel contained in the nickel sulfate solution charged with the amount of nickel powder was about 83%.
- the prepared nickel powder was used as a test powder, and 5 samples were sampled by 10 g.
- each of the separated nickel powders is placed on a filter paper, and pure water with a liquid temperature of 50 ° C. is used as a spray water while sucking it using a vacuum pump, and the amount is changed to 100 ml, 75 ml, 50 ml, 30 ml, 10 ml.
- Each was hung from above and washed with water. After washing with water, each nickel powder was taken out into a watch glass, put in a vacuum dryer and dried overnight to produce a nickel powder with reduced impurities.
- nickel powders having a sulfur grade reduced from 0.8% by weight before washing to less than 0.1% by weight were produced.
- what added 100 ml and 75 ml was the same quality as the case of 50 ml.
- the temperature in the tubular furnace was raised and maintained at 700 ° C., 1000 ° C., 1200 ° C. and 1300 ° C., respectively.
- the same nitrogen gas as the nitrogen gas substituted from the cylinder was held for 1 hour while supplying hydrogen gas to the tubular furnace at a flow rate of 40 ml / min and nitrogen gas at a flow rate of 960 ml / min.
- the hydrogen gas concentration of the supplied gas is 3% by weight.
- Nitrogen and hydrogen gas were supplied for a predetermined time, and then the supply gas was supplied at the same flow rate as nitrogen at the time of raising the temperature at a flow rate of 960 ml / min.
- the furnace temperature was below 70 ° C., the tubular furnace was opened, the nickel powder inside was taken out and analyzed using ICP.
- the analysis result shows that the sulfur quality, which was 0.8% by weight in the sample powder before washing, is reduced to 0.04% by weight in the washing process by roasting at 700 ° C. Was reduced to 0.02% by weight, and further reduced to 0.01% by weight by baking at 1000 ° C.
- the carbon amount of 0.20% by weight was 0.07% by weight after the washing step, 0.05% by weight at 700 ° C. and 0% at 1000 ° C. Reduced to 0.02 wt%.
- the quality was the same as that in the case of 1000 ° C, but the nickel powders were lightly sintered and needed to be crushed.
- the case of 1300 degreeC it was not suitable for the use which nickel powder sintered firmly and melt
- Example 2 [Production of test powder] 10 g of nickel powder produced using hydrogen gas in the same manner as in Example 1 was collected to obtain a sample powder of nickel powder.
- the nickel powder had a sulfur quality of 0.75 wt% and a carbon quality of 0.06 wt%.
- this nickel powder was put into a 100 ml capacity beaker, and 50 ml of 90 ° C. pure water was added thereto. Thereafter, using a stirrer and a heater, the liquid temperature was kept at 90 ° C., and the mixture was stirred at a rotation speed of 400 rpm for 1 hour. After stirring, the mixture was filtered using filter paper and dried using the same vacuum dryer as in Example 1. When the sulfur and carbon of this nickel powder were analyzed, the sulfur quality was reduced to 0.05 wt% and the carbon quality was reduced to 0.02 wt%. Table 2 shows changes in sulfur quality and carbon quality in Example 2.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
Description
非特許文献1記載の方法は、硫酸ニッケル水溶液に錯化剤を混合、錯化処理してニッケルアンミン錯体の溶液を形成し、その溶液を加圧容器に入れて密栓後、150~250℃程度に昇温、保持し、その中に水素ガスを吹き込む、いわゆる錯化還元法と呼ばれる方法で、水素によりニッケルアンミン錯体が還元されてニッケル粉を生成するものである。
酸化ニッケルを230℃ 以上、870℃ 以下の温度範囲に加熱、焙焼して酸化ニッケルを形成する焙焼工程。(6)焙焼工程で得られた酸化ニッケルを、水温50℃以上の水を用いて水洗浄し、次いで50℃以上の温度で假焼することによって、洗浄後酸化ニッケルを形成することを特徴とする洗浄・假焼工程、を経て硫黄を分離したフェロニッケル原料を得るものである。
このように、ニッケル粉の性状への影響を回避しながら硫黄や炭素を効果的にニッケルと分離するのに適した方法は見当たらなかった。
以下、本発明の製造方法を、図面を参照しながら説明する。
本発明は錯化還元法を用いて作製されたニッケル粉に含まれる不純物、特に炭素及び硫黄のニッケル粉からの除去を特徴とするもので、先ず供試粉となるニッケル粉は、図1の上工程として記載される「錯化処理」と「水素還元処理」を経て作製されるニッケル粉である。
本発明に係るニッケル粉から不純物の炭素、硫黄成分を除去する方法は、図1に示されるように、供試粉に対して、供試粉に水を用いた洗浄処理を施し、不純物の中で水溶性不純物を取り除く「洗浄工程」と、「洗浄工程」において取り除けなかった残存炭素及び硫黄を、高温で焙焼処理することにより分離する「焙焼工程」を順に経ることによって、得られるニッケル粉中の不純物濃度を低減して純度の高いニッケル粉を生成するものである。
そこで、以下に本発明における特徴を成す「洗浄工程」及び「焙焼工程」について詳細する。
供試粉のニッケル粉を、所定の方法で洗浄し、水溶性の不純物濃度を低減したニッケル粉を得る工程である。
具体的な洗浄方法は、ニッケル粉にかけ水をしたり、その水温を90℃程度まで上げたりするなど様々な方法を用いることができる。また、超音波を加えた雰囲気下で洗浄することでも効果がある。
洗浄工程で水溶性の硫黄や炭素の大部分を除去したニッケル粉を、高温で焙焼することで、残留した硫黄や炭素を分離し、純度の高いニッケル粉を得る工程である。
本発明は、この焙焼工程の際の雰囲気に、酸化雰囲気、完全な不活性雰囲気を用いるのではなく、ごくわずかな量の水素ガスを含む還元雰囲気中において、効果的に硫黄と炭素を除去できることを見出し、完成せしめたものである。
しかし、700℃未満では、炭素や硫黄の分離が不十分となる。一方、焙焼温度は高い方が、分離は効率よく進むが、1000℃を越えた温度で焙焼しても分離はほとんど増加せず、特に1250℃を越えるとニッケル粉の焼結が進み、ニッケル粉を酸に溶解する用途に対して溶解性が低下するなど好ましくない。
実験装置としてバッチ式の容量3Lのオートクレーブを用いた。純水880mlに試薬硫酸ニッケル六水和物672g(ニッケル純分で150g)、硫酸アンモニウム660gを含む溶液を調製し、これに25%アンモニア水382mlを添加し、合計の液量が2000mlになるように調整して始液とし、この始液をオートクレーブの内筒缶内に入れた。
液温が185℃に到達した時点から、水素ボンベの水素ガスをスラリーに、4.0リットル/minの流量で吹込み、内部圧力を3.5MPaになるように昇圧し維持しながら水素還元反応を生じさせた。
水素ガスの吹き込み開始から60分間反応させ、時間経過後に水素ガスの供給を停止し、その後撹拌しながら室温まで冷却した。
回収したニッケル粉は約140gだった。なお、ニッケル粉量を装入した硫酸ニッケル溶液に含有するニッケル物量除して算出した還元率は約83%だった。
次に、作製したニッケル粉を供試粉として用い、10gずつ、5サンプル分取した。
次に、分取したそれぞれのニッケル粉を濾紙上に乗せ、真空ポンプを用いて吸引しながら液温50℃の純水を、かけ水として100ml、75ml、50ml、30ml、10mlと量を変えて、それぞれの上から掛け、水洗浄した。
水洗浄後、それぞれのニッケル粉を時計皿に取り出し、真空乾燥機に入れて一晩かけて乾燥させて不純物の低減したニッケル粉を作製した。
次に、洗浄工程で50mlの量のかけ水を行った洗浄によって硫黄品位が0.04重量%となったサンプルを10gずつ、4サンプルに分取し、それぞれを市販のブリケットマシン(新東工業株式会社製、BGS-IV)を用いて、10×15×20mmサイズの俵状に成型し、次いでこの成型物を内径60mmの管状炉内にセットし、ボンベから供給した高純度窒素ガスを960ml/minの流量で供給し、管状炉内部の空気を完全に窒素に置換した。
それぞれの温度に達した後、ボンベから水素ガスと置換した窒素と同じ窒素ガスを、水素ガスを毎分40ml、窒素ガスを毎分960mlの流量で管状炉に供給しながら、1時間保持した。供給したガスの水素ガス濃度は3重量%である。
炉内温度が70℃を下回ったところで管状炉を開け、中のニッケル粉を取り出し、ICPを用いて分析した。
実施例1における硫黄品位及び炭素品位の変化を表1に示す。
そこで、以下の実施例では、さらなる洗浄工程の効果の把握を行った。
実施例1と同じ方法で水素ガスを用いて生成したニッケル粉を10g分取し、供試粉のニッケル粉とした。このニッケル粉の硫黄品位は0.75重量%、炭素品位は0.06重量%だった。
次に、このニッケル粉を容量100mlビーカーに入れ、ここに90℃の純水を50ml添加した。その後、攪拌機およびヒーターを用いて、液温を90℃に保持したまま、400rpmの回転数で1時間撹拌した。
撹拌終了後、濾紙を用いて濾過し、実施例1と同じ真空乾燥機を用いて乾燥させた。
このニッケル粉の硫黄及び炭素を分析したところ、硫黄品位0.05重量%まで低減し、炭素品位0.02重量%まで低減した。
実施例2における硫黄品位及び炭素品位の変化を表2に示す。
実施例1と同じ水素還元した供試粉となるニッケル粉を用い、実施例1と同じ方法で水洗浄した洗浄工程後のニッケル粉を5g分取した。このニッケル粉の硫黄品位は、0.8重量%から0.03重量%に低減され、炭素品位も、0.10重量%から0.04重量%へと低減された。
この真空ポンプによる吸引後、超音波洗浄する操作を4回繰り返した。
上記の洗浄で得たニッケル粉を、濾紙を用いて濾過し、時計皿に取り出し、真空乾燥機で一晩乾燥させた。
実施例3における硫黄品位及び炭素品位の変化を表3に示す。
Claims (4)
- 炭素及び硫黄の濃度が低いニッケル粉の製造方法であって、
硫酸ニッケル水溶液に錯化剤を添加して形成したニッケル錯体イオンを含有する溶液を作製する錯化処理と、
加圧容器内に装入した前記ニッケル錯体イオンを含有する溶液を、液温150~250℃に保持し、前記ニッケル錯体イオンを含有する溶液に水素ガスを吹き込んで水素還元を行ってニッケル粉を生成する水素還元処理と、
前記ニッケル粉を水洗浄する水洗浄処理と、
水洗浄処理されたニッケル粉を窒素と水素の混合気体雰囲気下で焙焼する焙焼処理を順に経ることを特徴とする炭素及び硫黄の濃度が低いニッケル粉の製造方法。 - 前記焙焼処理の混合気体における水素濃度が、2~4重量%であることを特徴とする請求項1記載の炭素及び硫黄の濃度が低いニッケル粉の製造方法。
- 前記焙焼処理における温度が、700℃以上、1250℃以下であることを特徴とする請求項1又は2に記載の炭素及び硫黄の濃度が低いニッケル粉の製造方法。
- 前記水洗浄処理における水量が、ニッケル粉の重量に対して1倍量以上、5倍量以下であることを特徴とする請求項1から3のいずれか1項に記載の炭素及び硫黄の濃度が低いニッケル粉の製造方法。
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CA2945918A CA2945918C (en) | 2014-04-15 | 2015-04-13 | Method for producing nickel powder having low carbon concentration and low sulfur concentration |
US15/303,557 US10500644B2 (en) | 2014-04-15 | 2015-04-13 | Method for producing nickel powder having low carbon concentration and low sulfur concentration |
AU2015247017A AU2015247017B2 (en) | 2014-04-15 | 2015-04-13 | Method for Producing Nickel Powder for Reducing Carbon Concentration and Low Sulfur Concentration Contained in Nickel Powder |
EP15779611.1A EP3132874B1 (en) | 2014-04-15 | 2015-04-13 | Method for producing nickel powder having low carbon concentration and low sulfur concentration |
CN201580016554.3A CN106163707B (zh) | 2014-04-15 | 2015-04-13 | 碳及硫的浓度低的镍粉的制造方法 |
PH12016502049A PH12016502049A1 (en) | 2014-04-15 | 2016-10-14 | Method for producing nickel powder having low carbon concentration and low sulfur concentration |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2014083886 | 2014-04-15 | ||
JP2014-083886 | 2014-04-15 | ||
JP2014-167904 | 2014-08-20 | ||
JP2014167904A JP6406613B2 (ja) | 2014-04-15 | 2014-08-20 | 含有する炭素及び硫黄の濃度を低減するニッケル粉の製造方法 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2015159846A1 true WO2015159846A1 (ja) | 2015-10-22 |
Family
ID=54324052
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2015/061358 WO2015159846A1 (ja) | 2014-04-15 | 2015-04-13 | 炭素及び硫黄の濃度が低いニッケル粉の製造方法 |
Country Status (8)
Country | Link |
---|---|
US (1) | US10500644B2 (ja) |
EP (1) | EP3132874B1 (ja) |
JP (1) | JP6406613B2 (ja) |
CN (1) | CN106163707B (ja) |
AU (1) | AU2015247017B2 (ja) |
CA (1) | CA2945918C (ja) |
PH (1) | PH12016502049A1 (ja) |
WO (1) | WO2015159846A1 (ja) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108699627A (zh) * | 2016-02-22 | 2018-10-23 | 住友金属矿山株式会社 | 镍粉的制造方法 |
CN109153081A (zh) * | 2016-05-30 | 2019-01-04 | 住友金属矿山株式会社 | 镍粉的制造方法 |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP6819087B2 (ja) * | 2016-06-21 | 2021-01-27 | 住友金属鉱山株式会社 | ニッケル粉の製造方法、ニッケル粉の製造装置 |
CN107746951A (zh) * | 2017-09-26 | 2018-03-02 | 北京矿冶研究总院 | 一种硫酸盐溶液中镍的分离方法 |
CN111247101B (zh) * | 2017-10-26 | 2023-03-07 | 住友金属矿山株式会社 | 镍复合氧化物和锂镍复合氧化物的制造方法 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS4974160A (ja) * | 1972-10-20 | 1974-07-17 | ||
JPH10509213A (ja) * | 1994-11-14 | 1998-09-08 | ザ ウェスターム コーポレイション | ミクロンサイズのニッケル金属粉末およびその製造方法 |
JP2003514111A (ja) * | 1999-10-29 | 2003-04-15 | ダブリュエムシー・リソーシィズ・リミテッド | ニッケル粉末の脱硫 |
WO2008001741A1 (fr) * | 2006-06-27 | 2008-01-03 | Ishihara Sangyo Kaisha, Ltd. | Fines particules de nickel, procédé de fabrication de celles-ci, et composition fluide les utilisant |
Family Cites Families (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2734821A (en) * | 1956-02-14 | Table ix | ||
CA988306A (en) | 1973-04-09 | 1976-05-04 | International Nickel Company Of Canada | Reduction of nickel oxide |
CN86100739B (zh) * | 1986-01-07 | 1988-06-08 | 中国科学院化工冶金研究所 | 制备超细镍粉的方法 |
CN1060982C (zh) * | 1997-11-17 | 2001-01-24 | 北京有色金属研究总院 | 超细金属粉的制备方法 |
WO2003106022A1 (en) * | 2002-06-12 | 2003-12-24 | The Westaim Corporation | Hydrometallurgical process for production of supported catalysts |
US7658995B2 (en) * | 2004-06-16 | 2010-02-09 | Toho Titanium Co., Ltd. | Nickel powder comprising sulfur and carbon, and production method therefor |
EP1925307A1 (en) | 2006-11-03 | 2008-05-28 | Emotional Brain B.V. | Use of 3-alpha-androstanediol in the treatment of sexual dysfunction |
JP5445777B2 (ja) | 2010-07-28 | 2014-03-19 | 住友金属鉱山株式会社 | 低品位ニッケル酸化鉱石からのフェロニッケル製錬原料の製造方法 |
CN102070203A (zh) * | 2010-11-23 | 2011-05-25 | 金川集团有限公司 | 一种提高羰基镍粉纯度的方法 |
-
2014
- 2014-08-20 JP JP2014167904A patent/JP6406613B2/ja active Active
-
2015
- 2015-04-13 CA CA2945918A patent/CA2945918C/en not_active Expired - Fee Related
- 2015-04-13 AU AU2015247017A patent/AU2015247017B2/en not_active Ceased
- 2015-04-13 US US15/303,557 patent/US10500644B2/en not_active Expired - Fee Related
- 2015-04-13 CN CN201580016554.3A patent/CN106163707B/zh not_active Expired - Fee Related
- 2015-04-13 WO PCT/JP2015/061358 patent/WO2015159846A1/ja active Application Filing
- 2015-04-13 EP EP15779611.1A patent/EP3132874B1/en active Active
-
2016
- 2016-10-14 PH PH12016502049A patent/PH12016502049A1/en unknown
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS4974160A (ja) * | 1972-10-20 | 1974-07-17 | ||
JPH10509213A (ja) * | 1994-11-14 | 1998-09-08 | ザ ウェスターム コーポレイション | ミクロンサイズのニッケル金属粉末およびその製造方法 |
JP2003514111A (ja) * | 1999-10-29 | 2003-04-15 | ダブリュエムシー・リソーシィズ・リミテッド | ニッケル粉末の脱硫 |
WO2008001741A1 (fr) * | 2006-06-27 | 2008-01-03 | Ishihara Sangyo Kaisha, Ltd. | Fines particules de nickel, procédé de fabrication de celles-ci, et composition fluide les utilisant |
Non-Patent Citations (1)
Title |
---|
See also references of EP3132874A4 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108699627A (zh) * | 2016-02-22 | 2018-10-23 | 住友金属矿山株式会社 | 镍粉的制造方法 |
CN109153081A (zh) * | 2016-05-30 | 2019-01-04 | 住友金属矿山株式会社 | 镍粉的制造方法 |
EP3466571A4 (en) * | 2016-05-30 | 2020-01-22 | Sumitomo Metal Mining Co., Ltd. | PROCESS FOR PRODUCING NICKEL POWDER |
Also Published As
Publication number | Publication date |
---|---|
EP3132874B1 (en) | 2019-10-23 |
PH12016502049B1 (en) | 2017-01-09 |
CA2945918C (en) | 2020-07-21 |
CA2945918A1 (en) | 2015-10-22 |
JP2015212411A (ja) | 2015-11-26 |
EP3132874A4 (en) | 2018-01-10 |
US20170043403A1 (en) | 2017-02-16 |
PH12016502049A1 (en) | 2017-01-09 |
AU2015247017A1 (en) | 2016-11-03 |
US10500644B2 (en) | 2019-12-10 |
CN106163707A (zh) | 2016-11-23 |
EP3132874A1 (en) | 2017-02-22 |
JP6406613B2 (ja) | 2018-10-17 |
AU2015247017B2 (en) | 2019-09-12 |
CN106163707B (zh) | 2018-09-07 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP5828923B2 (ja) | ニッケル粉の製造方法 | |
JP6406613B2 (ja) | 含有する炭素及び硫黄の濃度を低減するニッケル粉の製造方法 | |
EP4194572A1 (en) | Method for recycling iron and aluminum in nickel-cobalt-manganese solution | |
JP2015212411A5 (ja) | ||
JPWO2013077296A1 (ja) | 高純度硫酸ニッケルの製造方法 | |
WO2020196046A1 (ja) | ニッケルおよびコバルトを含有する水酸化物からのニッケルおよびコバルト含有溶液の製造方法 | |
CN106629706A (zh) | 一种金刚石刀头回收处理方法 | |
KR20130073507A (ko) | 폐초경 스크랩 재활용을 통한 텅스텐 화합물 및 코발트 화합물의 제조 방법 | |
JP6020971B2 (ja) | コバルト粉の製造方法 | |
CN109112560A (zh) | 一种利用碲化铜制备高纯碲的方法 | |
CN106904664A (zh) | 羟基四氧化三钴及其制备方法 | |
JP5904100B2 (ja) | 中和スラリーの沈降分離方法、並びにニッケル酸化鉱石の湿式製錬方法 | |
CN108349011A (zh) | 钴粉的晶种的制造方法 | |
JP4717917B2 (ja) | スコロダイトの製造方法及び洗浄方法 | |
CN111268655B (zh) | 一种粗碲粉自净化生产二氧化碲的方法 | |
JP2017155253A (ja) | ニッケル粉の製造方法 | |
JP5991309B2 (ja) | 高純度白金粉の製造方法 | |
JP3613443B2 (ja) | タンタルおよび/またはニオブ含有合金の溶解抽出方法 | |
JP6624464B2 (ja) | ニッケル粉の製造方法 | |
JP5762799B2 (ja) | 非鉄製錬中間産物からAsとCuとを分離して回収する方法 | |
JP2023551607A (ja) | リチウムイオン電池からの金属回収 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 15779611 Country of ref document: EP Kind code of ref document: A1 |
|
DPE1 | Request for preliminary examination filed after expiration of 19th month from priority date (pct application filed from 20040101) | ||
WWE | Wipo information: entry into national phase |
Ref document number: 15303557 Country of ref document: US |
|
ENP | Entry into the national phase |
Ref document number: 2945918 Country of ref document: CA |
|
WWE | Wipo information: entry into national phase |
Ref document number: 12016502049 Country of ref document: PH |
|
NENP | Non-entry into the national phase |
Ref country code: DE |
|
ENP | Entry into the national phase |
Ref document number: 2015247017 Country of ref document: AU Date of ref document: 20150413 Kind code of ref document: A |
|
REEP | Request for entry into the european phase |
Ref document number: 2015779611 Country of ref document: EP |
|
WWE | Wipo information: entry into national phase |
Ref document number: 2015779611 Country of ref document: EP |