JPH05255869A - Method for removing nickel in aqueous nickel-containing iron chloride solution - Google Patents
Method for removing nickel in aqueous nickel-containing iron chloride solutionInfo
- Publication number
- JPH05255869A JPH05255869A JP8647092A JP8647092A JPH05255869A JP H05255869 A JPH05255869 A JP H05255869A JP 8647092 A JP8647092 A JP 8647092A JP 8647092 A JP8647092 A JP 8647092A JP H05255869 A JPH05255869 A JP H05255869A
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- Prior art keywords
- iron
- nickel
- aqueous solution
- soln
- chloride
- 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.)
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- Removal Of Specific Substances (AREA)
Abstract
Description
【0001】[0001]
【産業上の利用分野】本発明は、例えば36ニッケル−
64鉄等のアンバー材、42アロイ(Fe:58重量%、N
i:42重量%)、52アロイ(Fe:48〜50重量%、Ni:5
0〜52重量%)等のアロイ材等のニッケルを含む合金を
エッチングして、テレビジョンのシャドウマスクや半導
体用のリードフレーム等を製造する際にエッチッグ液と
して用いられた塩化第二鉄水溶液の廃液の再生に利用さ
れる方法であり、それら廃液中のニッケルを効率的に除
去する方法を提供するものである。BACKGROUND OF THE INVENTION The present invention relates to, for example, 36 nickel-
Amber material such as 64 iron, 42 alloy (Fe: 58% by weight, N
i: 42 wt%), 52 alloy (Fe: 48-50 wt%, Ni: 5
0 to 52% by weight) alloy material such as nickel alloy is etched to produce a ferric chloride aqueous solution used as an etching solution when manufacturing a television shadow mask or a lead frame for a semiconductor. It is a method used for recycling waste liquids and provides a method for efficiently removing nickel in those waste liquids.
【0002】[0002]
【従来の技術】アンバー材、アロイ材等の鉄−ニッケル
合金を精密加工するためのエッチング液として汎用され
ている塩化第二鉄水溶液は、下記反応式(1)及び
(2)で示される様に、エッチングに用いられるに従
い、水溶液中の3価の鉄(塩化第二鉄)が2価の鉄(塩
化第一鉄)に還元され、又ニッケルも蓄積して行き、そ
のエッチング能力が次第に低下して最終的に使用困難な
廃液となってしまうものである。2. Description of the Related Art An aqueous solution of ferric chloride, which is widely used as an etching solution for precision processing of iron-nickel alloys such as amber and alloy materials, has the following reaction formulas (1) and (2). In addition, as it is used for etching, trivalent iron (ferric chloride) in the aqueous solution is reduced to divalent iron (ferrous chloride), and nickel also accumulates, gradually decreasing its etching ability. Finally, it becomes a waste liquid that is difficult to use.
【0003】[0003]
【式1】 Fe + 2FeCl3 → 3FeCl2 ‥‥‥(1)[Formula 1] Fe + 2FeCl 3 → 3FeCl 2 (1)
【0004】[0004]
【式2】 Ni + 2FeCl3 → 2FeCl2 + NiCl2‥‥‥(2)[Formula 2] Ni + 2FeCl 3 → 2FeCl 2 + NiCl 2 (2)
【0005】エッチング廃液は、経済性及び省資源の見
地より、再生しリサイクルすることが望ましいことであ
るが、エッチング廃液には、エッチング液としてのエッ
チング能力を低下させるニッケルが通常数千ppm〜1
万ppm程度存在しており、エッチング廃液を再使用す
るためには、ニッケル含有量を100ppm以下に抑え
る必要がある。従って、従来、エッチング廃液よりニッ
ケルを除去する試みが種々行われている。From the viewpoint of economy and resource saving, it is desirable to recycle and recycle the etching waste liquid. However, in the etching waste liquid, nickel, which lowers the etching ability as the etching liquid, is usually several thousand ppm to 1 ppm.
There is about 10,000 ppm, and it is necessary to suppress the nickel content to 100 ppm or less in order to reuse the etching waste liquid. Therefore, various attempts have hitherto been made to remove nickel from the etching waste liquid.
【0006】これらの方法として、例えば加熱濃縮強酸
性下に塩化ニッケルを晶析除去する方法(特開昭59−
250764号)、ジメチルグリオキシム等のグリオキ
シム類の添加により、ニッケルグリオキシムとして沈澱
除去する方法(特開昭59−190367号)或いは塊
状の金属鉄を添加し除去する方法(特開昭59−121
123号)等が提案されている。As these methods, for example, a method of crystallizing and removing nickel chloride under heating and concentration under strong acidity (JP-A-59-59).
No. 250764), glyoximes such as dimethylglyoxime are added to precipitate and remove as nickel glyoxime (JP-A-59-190367) or lumpy metallic iron is added and removed (JP-A-59-121).
No. 123) has been proposed.
【0007】さらに本発明者らは、より優れた方法とし
て、ニッケルを含有する塩化第一鉄水溶液に100メッ
シュパス以上の鉄粉を添加する方法(特開昭62−19
1428号)、ニッケルを含有する塩化第一鉄水溶液に
比表面積が1m2 /g以上の鉄粉を添加する方法(特開
平3−253584号)を提案した。他方、クロム、ニ
ッケルを含有する塩化鉄水溶液からクロム、ニッケルを
除去する方法も提案している(特公平3−2233
号)。Furthermore, the inventors of the present invention, as a more superior method, add iron powder of 100 mesh or more to an aqueous ferrous chloride solution containing nickel (Japanese Patent Laid-Open No. 62-19).
1428), and a method of adding iron powder having a specific surface area of 1 m 2 / g or more to a nickel-containing ferrous chloride aqueous solution (JP-A-3-253584). On the other hand, a method for removing chromium and nickel from an iron chloride aqueous solution containing chromium and nickel is also proposed (Japanese Patent Publication No. 3-2233).
issue).
【0008】[0008]
【発明が解決しようとする課題】上記塩化鉄水溶液中の
ニッケル除去方法において、ニッケルに対して少量の鉄
粉使用量で、速やかに反応を進行させることが求められ
ており、本発明者らが先に提案した方法は、塩化鉄水溶
液中のニッケルを充分に除去し得る方法として工業的に
優れたものであるが、鉄粉使用量、反応速度の点で未だ
充分なものではなく、反応時間が長くなりがちであっ
た。本発明者らは、上記問題に鑑み、先に提案した塩化
鉄水溶液中のニッケル除去方法をさらに改良するため鋭
意検討を行ったのである。In the above method for removing nickel in an aqueous solution of iron chloride, it is required that the reaction be promptly proceeded with a small amount of iron powder used with respect to nickel. The previously proposed method is industrially excellent as a method capable of sufficiently removing nickel in an iron chloride aqueous solution, but the amount of iron powder used and the reaction rate are not yet sufficient, and the reaction time Tended to be long. In view of the above problems, the present inventors have conducted earnest studies to further improve the previously proposed method for removing nickel in an aqueous solution of iron chloride.
【0009】[0009]
【課題を解決するための手段】本発明者らは、前記課題
を解決するためには、ニッケルを含有し、塩化第二鉄と
塩化第一鉄からなる塩化鉄水溶液に鉄材を加え該水溶液
中の塩化第二鉄を塩化第一鉄に変化させた後、副生する
水酸化鉄或いは含水酸化鉄を分離することなく得られた
水溶液に鉄粉を加えることにより、ニッケル除去が速や
かに進行することを見出し本発明を完成した。Means for Solving the Problems In order to solve the above-mentioned problems, the present inventors added an iron material to an iron chloride aqueous solution containing nickel and consisting of ferric chloride and ferrous chloride, After changing ferric chloride from ferric chloride to ferrous chloride, adding iron powder to the resulting aqueous solution without separating the by-produced iron hydroxide or hydrous iron oxide will rapidly remove nickel. It was found that the present invention has been completed.
【0010】即ち、本発明は、ニッケルを含有する塩化
鉄水溶液に鉄材を加え該水溶液中に存在する塩化第二鉄
を塩化第一鉄に変化させた後、水酸化鉄或いは含水酸化
鉄の存在下に鉄粉を加えニッケルを除去することを特徴
とするニッケル含有塩化鉄水溶液中のニッケル除去方法
に関するものである。以下、本発明を詳細に説明する。That is, according to the present invention, an iron material is added to an iron chloride aqueous solution containing nickel to change ferric chloride present in the aqueous solution to ferrous chloride, and then the presence of iron hydroxide or hydrous iron oxide is present. The present invention relates to a method for removing nickel in a nickel-containing iron chloride aqueous solution, which comprises adding iron powder to the bottom to remove nickel. Hereinafter, the present invention will be described in detail.
【0011】本発明において、ニッケルを含有する塩化
鉄水溶液とは、ニッケル合金を塩化第二鉄水溶液でエッ
チングした廃液等の、塩化第一鉄、塩化第二鉄及びニッ
ケルを含有する水溶液を言う。In the present invention, the iron chloride aqueous solution containing nickel means an aqueous solution containing ferrous chloride, ferric chloride and nickel, such as a waste liquid obtained by etching a nickel alloy with a ferric chloride aqueous solution.
【0012】本発明のニッケル除去方法では、まずニッ
ケルを含有する塩化鉄水溶液に鉄材を加え、(3)式に
示す様に塩化第二鉄を塩化第一鉄に変化させる。In the method for removing nickel of the present invention, first, an iron material is added to an iron chloride aqueous solution containing nickel, and ferric chloride is changed to ferrous chloride as shown in formula (3).
【0013】[0013]
【式3】2FeCl3 + Fe → 3FeCl2 …(3)[Formula 3] 2FeCl 3 + Fe → 3FeCl 2 (3)
【0014】該水溶液中に塩酸が含まれる場合は、
(4)式に示す通りその塩酸により塩化第一鉄が生成す
る。When hydrochloric acid is contained in the aqueous solution,
As shown in formula (4), the hydrochloric acid produces ferrous chloride.
【0015】[0015]
【式4】Fe + 2HCl → FeCl2 + H2 …(4) この場合、水溶液中のニッケルは、一部金属ニッケルの
沈澱になるが、殆どがイオンとして液中に存在する。[Equation 4] Fe + 2HCl → FeCl 2 + H 2 (4) In this case, most of the nickel in the aqueous solution is a precipitate of metallic nickel, but most of it exists as ions in the liquid.
【0016】使用する鉄材の形状としては、いかなる形
状のものでも良く、例えば鉄片、鉄塊、棒状鉄等が挙げ
られる。鉄材の使用量としては、塩化鉄水溶液中の塩化
第二鉄を塩化第一鉄に変化させるのに必要な理論量より
過剰に用い、通常塩化鉄水溶液中の塩化第二鉄に対して
1〜10倍モル使用することが好ましい。反応温度は室
温〜100℃で行うことが好ましく、さらに好ましくは
40〜100℃である。反応時間は、液量、鉄材の種
類、鉄材の量、反応温度等の条件により、種々選択する
ことが出来る。反応の完了は塩化第一鉄濃度を分析する
か、又はORPメータ等で酸化還元電位を測定すること
により確認することが出来る。The iron material to be used may have any shape, and examples thereof include an iron piece, an iron ingot, and a rod-shaped iron. The amount of the iron material used is an excess of the theoretical amount necessary to change ferric chloride in the ferric chloride aqueous solution to ferrous chloride, and is usually 1 to 1 with respect to ferric chloride in the ferric chloride aqueous solution. It is preferable to use a 10-fold molar amount. The reaction temperature is preferably room temperature to 100 ° C, more preferably 40 to 100 ° C. The reaction time can be variously selected depending on conditions such as the liquid amount, the type of iron material, the amount of iron material, the reaction temperature and the like. Completion of the reaction can be confirmed by analyzing the ferrous chloride concentration or measuring the redox potential with an ORP meter or the like.
【0017】鉄粉を加える際に塩化鉄水溶液中に存在さ
せる水酸化鉄或いは含水酸化鉄は、塩化鉄水溶液と鉄材
の反応に伴って微粒子として副生してくる。従来、これ
らの副生物は、濾過等により除去して次工程に使用して
いた。しかしながら、本発明では、それらの水酸化鉄或
いは含水酸化鉄を除去せずあえて存在させ、さらには積
極的に生成させ、副生物ないし生成した水酸化鉄或いは
含水酸化鉄をを分離せず、それらが存在する水溶液に鉄
粉を加えてニッケルを除去することを特徴とするもので
ある。The iron hydroxide or hydrous iron oxide present in the iron chloride aqueous solution when the iron powder is added is by-produced as fine particles as the iron chloride aqueous solution reacts with the iron material. Conventionally, these by-products have been removed by filtration or the like and used in the next step. However, in the present invention, those iron hydroxides or hydrous iron oxides are intentionally present without being removed, and are further actively produced, and by-products or produced iron hydroxides or hydrous iron oxides are not separated, and Fe is added to an aqueous solution in which nickel is present to remove nickel.
【0018】塩化鉄水溶液中の水酸化鉄或いは含水酸化
鉄の含有量としては、0.05重量%〜10重量%であ
ることが好ましく、より好ましくは0.1重量%〜2重
量%である。水酸化鉄或いは含水酸化鉄の含有量が0.
05重量%未満である場合は、本発明の効果が発揮され
ず、他方10重量%を越える場合は、水酸化鉄或いは含
水酸化鉄のスラリーにより水溶液の取扱いが困難とな
る。The content of iron hydroxide or hydrous iron oxide in the iron chloride aqueous solution is preferably 0.05% by weight to 10% by weight, more preferably 0.1% by weight to 2% by weight. .. The content of iron hydroxide or hydrous iron oxide is 0.
If the amount is less than 05% by weight, the effect of the present invention is not exhibited. On the other hand, if the amount is more than 10% by weight, it becomes difficult to handle the aqueous solution due to the slurry of iron hydroxide or hydrous iron oxide.
【0019】塩化鉄水溶液中の水酸化鉄或いは含水酸化
鉄を好ましい含有量にするためには、反応の際に塩化鉄
水溶液と鉄粉の混合液と酸素とを積極的に接触させるこ
とが好ましい。酸素と接触させる方法としては、酸素を
吹き込む方法、或いは酸素雰囲気下、通常大気雰囲気下
に反応液を循環させる方法等を挙げることが出来る。酸
素源としては、酸素或いは酸素混合物を使用することが
出来る。酸素混合物としては、空気、或いは酸素と不活
性ガスの混合物等が挙げられ、安価であることから空気
を使用することが好ましい。又、酸素を吹き込む方法、
液を循環させる方法いずれの方法を使用する場合も、塩
化第一鉄の還元が完了した後も、さらに数時間反応を継
続させることにより、液中の水酸化鉄或いは含水酸化鉄
含有量を好ましい含有量とすることが出来る。In order to obtain a preferable content of iron hydroxide or hydrous iron oxide in the iron chloride aqueous solution, it is preferable that the mixed solution of the iron chloride aqueous solution and the iron powder and oxygen be positively contacted during the reaction. .. Examples of the method of contacting with oxygen include a method of blowing oxygen, a method of circulating a reaction solution in an oxygen atmosphere, or in a normal atmosphere. As the oxygen source, oxygen or an oxygen mixture can be used. Examples of the oxygen mixture include air and a mixture of oxygen and an inert gas. It is preferable to use air because it is inexpensive. Also, a method of blowing oxygen,
In the case of using either method of circulating the liquid, even after the reduction of ferrous chloride is completed, by continuing the reaction for several more hours, the iron hydroxide or hydrous iron oxide content in the liquid is preferable. It can be the content.
【0020】又、反応終了後の水溶液中の水酸化鉄或い
は含水酸化鉄の含有量が0.05重量%に満たない場合
には、別に用意した水酸化鉄或いは含水酸化鉄を加えて
ニッケル除去を行うことも出来る。この場合、水酸化鉄
或いは含水酸化鉄の添加量としては、前記したと同じ様
に塩化鉄水溶液中の含有量が10重量%を越えない範囲
で添加する。When the content of iron hydroxide or hydrous iron oxide in the aqueous solution after the reaction is less than 0.05% by weight, nickel hydroxide is removed by adding separately prepared iron hydroxide or hydrous iron oxide. You can also do In this case, the amount of iron hydroxide or hydrous iron oxide added is, in the same manner as described above, such that the content in the aqueous iron chloride solution does not exceed 10% by weight.
【0021】上記の様にして調製された水酸化鉄或いは
含水酸化鉄の存在する塩化第一鉄水溶液に鉄粉を加える
と、該水溶液中のニッケルが、主として、鉄粉上に付着
し、それらは濾過等により容易に取り除くことが出来
る。この時の鉄粉の作用については、明らかではないが
以下のことが考えられる。 1)極微量の遊離酸との反応によるpHの上昇による水
酸化ニッケルの生成。 2)鉄とのイオン化傾向の差による、金属鉄表面へのニ
ッケル金属の析出。When iron powder is added to the ferrous chloride aqueous solution containing iron hydroxide or hydrous iron oxide prepared as described above, nickel in the aqueous solution mainly adheres to the iron powder, Can be easily removed by filtration or the like. The action of the iron powder at this time is not clear, but the following can be considered. 1) Formation of nickel hydroxide due to increase in pH due to reaction with a very small amount of free acid. 2) Precipitation of nickel metal on the surface of metallic iron due to the difference in ionization tendency with iron.
【0022】塩化第一鉄水溶液に加える鉄粉としては、
細かいものが良く、粗いと除去効率が良くない。粒径と
しては、100メッシュパス以上が好ましく、150〜
350メッシュパスがより好ましい。さらに、比表面積
として、1m2 /g以上を有するものを使用すること
が、除去効率が良いため好ましい。反応温度としては、
常温〜100℃が好ましく、より好ましくは40〜90
℃である。反応時間は、反応条件により種々選択するこ
とが出来るが、反応温度が80℃では1時間以上が好ま
しく、より好ましくは2〜8時間である。鉄粉の添加量
は、反応条件、ニッケル含有量に左右されるが、ニッケ
ルに対して1倍モル以上、好ましくは3〜7倍モルであ
る。As the iron powder added to the ferrous chloride aqueous solution,
Fine ones are good, and coarse ones are not good at removing efficiency. The particle size is preferably 100 mesh pass or more, and 150 to
A 350 mesh pass is more preferred. Further, it is preferable to use a material having a specific surface area of 1 m 2 / g or more because the removal efficiency is good. As the reaction temperature,
Room temperature to 100 ° C is preferable, and more preferably 40 to 90.
℃. The reaction time can be variously selected depending on the reaction conditions, but when the reaction temperature is 80 ° C., it is preferably 1 hour or longer, more preferably 2 to 8 hours. The addition amount of the iron powder depends on the reaction conditions and the nickel content, but is 1 time mol or more, preferably 3 to 7 times mol, relative to nickel.
【0023】以上の方法によりニッケルを除去した塩化
第一鉄水溶液は、(5)式に示す様に塩素化し、塩化第
二鉄水溶液として再使用することができる。The ferrous chloride aqueous solution from which nickel has been removed by the above method can be chlorinated as shown in formula (5) and reused as a ferric chloride aqueous solution.
【0024】[0024]
【式5】2FeCl2 + Cl2 → 2FeCl3 …(5)[Formula 5] 2FeCl 2 + Cl 2 → 2FeCl 3 (5)
【0025】[0025]
【作用】本発明において、塩化第一鉄水溶液中に水酸化
鉄或いは含水酸化鉄が存在するとニッケル除去が促進さ
れる理由は明らかではないが、水溶液中に存在する酸化
鉄或いは含水酸化鉄の微粒子表面は塩基性が高いことに
より、水溶液中のニッケルが該粒子表面上で反応し水酸
化ニッケルとなるため、ニッケル除去が促進されるもの
と推定される。In the present invention, the reason why the removal of nickel is promoted by the presence of iron hydroxide or hydrous iron oxide in the ferrous chloride aqueous solution is not clear, but fine particles of iron oxide or hydrous iron oxide present in the aqueous solution are not clear. It is presumed that since the surface is highly basic, nickel in the aqueous solution reacts on the surface of the particles to form nickel hydroxide, which promotes nickel removal.
【0026】[0026]
【実施例】以下、実施例及び比較例を挙げて本発明を更
に詳しく説明する。なお、各例における「%」は「重量
%」を表す。EXAMPLES The present invention will be described in more detail with reference to Examples and Comparative Examples. In addition, "%" in each example represents "weight%."
【0027】実施例1 側面下部に抜き出し口のある5リットルガラス瓶に、塩
化第二鉄エッチング廃液の希釈水溶液(組成: FeCl3;3
0.52%, FeCl2;7.81%,Ni;7290ppm,HCl;0.04%)4リット
ル(5800g)と鉄片930gを仕込み、反応温度を
温度調節器で70℃に調節し、空気シール下でポンプを
用いて液循環させ4時間反応を行ったところ、反応後の
水溶液中のFeCl3 濃度は0.1%以下になった。更に、4時
間反応を行ったところ、得られた液の組成は、FeCl3;0.
1%以下、FeCl2;41.2% 、酸化鉄及び含水酸化鉄 ;1.0%,
Ni;5830ppmであった。上記反応液700gを濾過せず、
冷却管、温度計、撹拌機を取りつけた1リットルの3ツ
口フラスコに投入し、100メッシュパスの粒径を有し
かつ251メッシュ以上の粒径のものが55%であり、
比表面積が3.01m2 /gである鉄粉15.53g
(対ニッケル4.00倍モル)を仕込み、撹拌しつつ空
気雰囲気下で、80℃、2時間反応させた。得られた反
応液を5B濾紙で濾過した後の濾液中のニッケル含有量
は56ppmで、pHは3.1であった。Example 1 In a 5 liter glass bottle having an outlet at the bottom of the side surface, a dilute aqueous solution of ferric chloride etching waste liquid (composition: FeCl 3 ; 3
0.52%, FeCl 2 ; 7.81%, Ni; 7290ppm, HCl; 0.04%) 4 liters (5800g) and iron pieces 930g were charged, the reaction temperature was adjusted to 70 ° C with a temperature controller, and a pump was used under air sealing. When the liquid was circulated and the reaction was carried out for 4 hours, the FeCl 3 concentration in the aqueous solution after the reaction was 0.1% or less. Furthermore, when the reaction was carried out for 4 hours, the composition of the obtained liquid was FeCl 3 ;
1% or less, FeCl 2 ; 41.2%, iron oxide and hydrous iron oxide; 1.0%,
Ni was 5830 ppm. 700 g of the above reaction solution was not filtered,
It was put into a 1-liter three-necked flask equipped with a cooling tube, a thermometer, and a stirrer, and 55% had a particle size of 100 mesh pass and a particle size of 251 mesh or more,
15.53 g of iron powder having a specific surface area of 3.01 m 2 / g
(4.00 moles relative to nickel) was charged and reacted at 80 ° C. for 2 hours in an air atmosphere while stirring. The nickel content in the filtrate after filtering the obtained reaction liquid through 5B filter paper was 56 ppm, and the pH was 3.1.
【0028】比較例1 実施例1の塩化第二鉄エッチング廃液と鉄片との反応で
得られた反応液1リットルを5B濾紙で濾過した。得ら
れた濾液700gに、実施例1と同様の鉄粉を15.7
4g(対ニッケル4.00倍モル)仕込み、撹拌しつつ
空気雰囲気下で、80℃、2時間反応させた。得られた
反応液を5B濾紙で濾過した後の濾液中のニッケル含有
量は187ppmで、pHは3.2であった。Comparative Example 1 1 liter of the reaction solution obtained by reacting the ferric chloride etching waste liquid of Example 1 with iron pieces was filtered with 5B filter paper. Iron powder similar to that in Example 1 was added to 15.7 g of the obtained filtrate (700 g).
4 g (4.00 moles relative to nickel) was charged and reacted at 80 ° C. for 2 hours in an air atmosphere while stirring. The nickel content in the filtrate after filtering the obtained reaction liquid through 5B filter paper was 187 ppm, and the pH was 3.2.
【0029】実施例2 実施例1において、液循環させ空気を0.5l/min
の割合で溶液中に強制的に吹き込みながら反応を行う以
外は同様の条件で4時間反応を行ったところ、反応後の
水溶液中のFeCl3 濃度は0.1%以下になった。更に、2時
間反応を行ったところ、得られた液の組成は、FeCl3;0.
1%以下、FeCl2;40.55%、酸化鉄及び含水酸化鉄 ;O.5%、
Ni;6023ppmであった。上記反応液700gを濾過せず、
実施例1と同様の鉄粉16.0g(対ニッケル4.00
倍モル)を使用し、実施例1と同様の操作で脱ニッケ
ル、濾過を行ったところ、得られた濾液中のニッケル含
有量は65ppmで、pHは3.2であった。Example 2 In Example 1, the liquid was circulated and air was supplied at 0.5 l / min.
When the reaction was carried out for 4 hours under the same conditions except that the reaction was carried out while forcibly blowing into the solution at a ratio of, the concentration of FeCl 3 in the aqueous solution after the reaction was 0.1% or less. Furthermore, when the reaction was carried out for 2 hours, the composition of the obtained liquid was FeCl 3 ;
1% or less, FeCl 2 ; 40.55%, iron oxide and hydrous iron oxide; O.5%,
Ni was 6023 ppm. 700 g of the above reaction solution was not filtered,
The same iron powder as in Example 1 16.0 g (vs. nickel 4.00)
When the nickel content was 65 ppm and the pH was 3.2, the nickel content in the obtained filtrate was 65 ppm and the pH was 3.2.
【0030】[0030]
【発明の効果】本発明の方法によれば、塩化鉄水溶液中
のニッケルを選択的に短時間で効率よく除去することが
でき、ニッケル合金等のエッチング廃液から塩化第二鉄
水溶液を容易に再生できるので、産業上の寄与の大きな
ものである。According to the method of the present invention, nickel in an aqueous iron chloride solution can be selectively and efficiently removed in a short time, and an aqueous ferric chloride solution can be easily regenerated from an etching waste liquid such as a nickel alloy. Because it can, it is a great contribution to industry.
Claims (1)
加え該水溶液中に存在する塩化第二鉄を塩化第一鉄に変
化させた後、水酸化鉄或いは含水酸化鉄の存在下に鉄粉
を加えニッケルを除去することを特徴とするニッケル含
有塩化鉄水溶液中のニッケル除去方法。1. An iron powder is added to an aqueous iron chloride solution containing nickel to change ferric chloride present in the aqueous solution to ferrous chloride, and then iron powder is produced in the presence of iron hydroxide or hydrous iron oxide. A method for removing nickel from a nickel-containing iron chloride aqueous solution, which comprises adding nickel to remove nickel.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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JP04086470A JP3104720B2 (en) | 1992-03-10 | 1992-03-10 | Nickel removal method from nickel-containing iron chloride aqueous solution |
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---|---|---|---|
JP04086470A JP3104720B2 (en) | 1992-03-10 | 1992-03-10 | Nickel removal method from nickel-containing iron chloride aqueous solution |
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JPH05255869A true JPH05255869A (en) | 1993-10-05 |
JP3104720B2 JP3104720B2 (en) | 2000-10-30 |
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Cited By (1)
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CN112850797A (en) * | 2020-10-26 | 2021-05-28 | 斯瑞尔环境科技股份有限公司 | Production method of ultrapure ferric trichloride |
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1992
- 1992-03-10 JP JP04086470A patent/JP3104720B2/en not_active Expired - Lifetime
Cited By (1)
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CN112850797A (en) * | 2020-10-26 | 2021-05-28 | 斯瑞尔环境科技股份有限公司 | Production method of ultrapure ferric trichloride |
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