JPS6148588A - Method for regenerating waste water after nickel plating as replenisher for electrolytic refining of nickle - Google Patents
Method for regenerating waste water after nickel plating as replenisher for electrolytic refining of nickleInfo
- Publication number
- JPS6148588A JPS6148588A JP16767484A JP16767484A JPS6148588A JP S6148588 A JPS6148588 A JP S6148588A JP 16767484 A JP16767484 A JP 16767484A JP 16767484 A JP16767484 A JP 16767484A JP S6148588 A JPS6148588 A JP S6148588A
- Authority
- JP
- Japan
- Prior art keywords
- soln
- nickel
- waste water
- aqueous solution
- washing
- 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.)
- Granted
Links
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- Electrolytic Production Of Metals (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明はニッケルめっき排水を浄液し、特に合計有機炭
素(以下T00と略称する)を減少させてこれをニッケ
ル電解精製用の補給液として再生する方法に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention purifies nickel plating wastewater, particularly reduces total organic carbon (hereinafter abbreviated as T00), and uses it as a replenishment liquid for nickel electrolytic refining. Regarding how to play.
このめっき排水は、中小企業のめつき工場等Gこおいて
発生するめつき洗浄水等を濃縮したものが対象となる。This plating wastewater is the concentrated plating washing water etc. generated in small and medium-sized plating factories.
該排水のニッケル濃度は比較的濃厚なものとして受は入
れられるが不純物として多量のToo等を含有する。Although the nickel concentration of the wastewater is accepted as relatively high, it contains a large amount of impurities such as Too.
従って、このめっき排水をそのま\ニッケルの電解系に
供給すると、電解液中のTOO濃度に起因するものと思
われる各種のトラブルが発生する。Therefore, if this plating wastewater is supplied as is to the nickel electrolytic system, various problems will occur that are thought to be caused by the TOO concentration in the electrolyte.
例えば電解によってNi種板に電着したニッケルが剥離
したり該ニッケルの硬度が高くなる等である。For example, the nickel electrodeposited on the Ni seed plate may peel off due to electrolysis, or the hardness of the nickel may increase.
上記の現象を避けるためには、ニッケルめっき排水を極
く少量ずつしか電解液に補給することができないので実
用的とは云えなかった。In order to avoid the above phenomenon, nickel plating waste water can only be replenished into the electrolyte in small amounts, which is not practical.
他の方法としては、このニッケルめっき排水にアルカリ
を加えてニッケルを水酸化物として分離し、次いで焙焼
したのち電気炉で溶解してアノードとし、漬液電解する
方法もあるが、この方法は煩雑で且つコスト高になると
いう欠点があった。Another method is to add alkali to this nickel plating wastewater to separate the nickel as hydroxide, then roast it and melt it in an electric furnace to form an anode, followed by immersion electrolysis, but this method is complicated. Moreover, there was a drawback that the cost was high.
本発明の目的は、上記の問題点を解消し、簡便な方法に
よって該めっき排水からニッケル電解精製の電解液に比
較的多量に添加して使用できる硫酸ニッケル水溶液を得
る方法を提供することにある。An object of the present invention is to solve the above-mentioned problems and provide a simple method for obtaining an aqueous nickel sulfate solution from the plating wastewater that can be used by adding it in a relatively large amount to the electrolytic solution for nickel electrorefining. .
本願発明者等は、電気ニッケルをうるための電解液中の
TOO濃度が、得られるニッケル電着物の性状に及ぼす
影響について実験を行なったところ、通常のニッケル電
解液のNi濃度65〜75g7’1の場合TOO濃度は
4 ppm以下とする必要があることを知見した。The inventors of the present application conducted an experiment on the influence of the TOO concentration in the electrolytic solution for obtaining electrolytic nickel on the properties of the obtained nickel electrodeposit, and found that the Ni concentration in a normal nickel electrolytic solution was 65 to 75g7'1 It has been found that the TOO concentration needs to be 4 ppm or less in this case.
TOO濃度がこれ以上の場合、前述した現象が大なり小
なり現われる。そこでニッケルめっき排水を再生して得
たN1濃度65〜75 (y’lの硫酸ニッケル水溶液
を、ニッケル電解精製のため該電解槽! が
ら取り出した電解液に対し容量で約+/+oずっ添加で
きるようにするためには、ニッケルめっき排水を再生し
て得た硫酸ニッケル水溶液中のTOO濃度が4・Opp
m以下となるようにすればよい。If the TOO concentration is higher than this, the above-mentioned phenomenon will occur to a greater or lesser extent. Therefore, an aqueous solution of nickel sulfate with an N1 concentration of 65 to 75 (y'l) obtained by regenerating nickel plating waste water can be added by volume to the electrolyte taken out from the electrolytic tank for nickel electrolytic refining. In order to achieve this, the TOO concentration in the nickel sulfate aqueous solution obtained by regenerating nickel plating wastewater must be 4.Opp.
What is necessary is to make it less than or equal to m.
即ち、本発明はこのような硫酸ニッケル水溶液を、ニッ
ケルめっき排水から得られるようにするため1. P
H8,0〜9.0のアルカリ水溶液を+oC以上に保持
し攪拌されている状態の該水溶液に、ニッケルめっき排
水と炭酸アルカリ水溶液又は水酸化アルカリ水溶液とを
同時に・該水溶液のPR及び温度を維持しながら、該水
溶液の底部に吹き込むようにして添加し、生成した沈殿
を温水によるレバルプ洗浄と、洗浄水を分離する脱水操
作を複数回行ない、少なくとも最終脱水操作で付着水分
35重量%以下としたのち希硫酸に溶解しニッケル濃度
をニッケルの電解精製に適する濃度に調整するようにし
たことにある。That is, the present invention aims to obtain such an aqueous nickel sulfate solution from nickel plating wastewater by: 1. P
Add nickel plating waste water and alkali carbonate aqueous solution or alkali hydroxide aqueous solution simultaneously to the aqueous aqueous solution of H8.0 to 9.0 which is maintained above +oC and stirred. Maintain PR and temperature of the aqueous solution. At the same time, it was added by blowing into the bottom of the aqueous solution, and the resulting precipitate was washed with warm water and dehydrated several times to separate the washing water, so that the adhering moisture was at least 35% by weight in the final dehydration operation. It was then dissolved in dilute sulfuric acid to adjust the nickel concentration to a concentration suitable for electrolytic refining of nickel.
本発明の方法においてPH8〜9.0の範囲で反応させ
る理由は、PHがこれより低いと塩基性硫酸塩との複塩
を一部生成し、これより高いPHではTooの除去が不
充分となるからである。The reason why the reaction is carried out in the pH range of 8 to 9.0 in the method of the present invention is that if the pH is lower than this, some double salt with basic sulfate will be formed, and if the pH is higher than this, the removal of Too will be insufficient. Because it will be.
反応温度を40C以上好ましくは60C以上とするのは
、これ以下では生成物の濾過速度が遅いためである。The reaction temperature is set to 40C or higher, preferably 60C or higher, because below this temperature, the filtration rate of the product is slow.
次にまず反応槽に少量のアルカリ水溶液を用意し、これ
にニッケルめっき排水と炭酸アルカリ塩又は水酸化アル
カリ塩の水溶液を、PH値と温度を保持して同時に吹き
込むようにして添加するのは、従来法のように例えば濃
厚なアルカリ水溶液に所定温度のニッケルめっき排水を
添加すると局部的に濃厚なアルカリとニッケルとの反応
が進行し、正常な炭酸塩または水酸化物が生成しないた
めかToo等の除去率が大幅に低下するためである0
炭酸塩又は水酸化物として沈殿したニッケルの沈殿は強
力な吸引濾過法或は遠心分離法により母液と分離し、得
られたケーキは初工程の温度と同様な温度の温水を大量
に加えてし、<ルブしたのち洗浄水を分離する脱水操作
を2回以上行なう。吸引濾過法を強力に適用する。この
ときの最終脱水操作では付着水分35重量%以下となる
ようにし・この洗浄脱水操作を2回以上行なうのは、1
回では不充分で、2回以上で最終脱水操作で付着水分3
5重量%以下とすることにより、TOCの除去が、後に
・この沈殿を希硫酸に溶解しニッケル濃度をニッケルの
電解精製に適する濃度に調整したときにTooの濃度が
約4・Oppm以下とすることが可能となるからである
。Next, first prepare a small amount of alkaline aqueous solution in the reaction tank, and add nickel plating wastewater and aqueous solution of alkali carbonate or alkali hydroxide to it by simultaneously blowing it while maintaining the pH value and temperature. Too et al. 0 The nickel precipitate as carbonate or hydroxide is separated from the mother liquor by strong suction filtration or centrifugation, and the resulting cake is kept at the temperature of the first step. Add a large amount of hot water at a similar temperature to the water, lube it, and then perform the dehydration operation two or more times to separate the washing water. Apply a strong suction filtration method. In the final dehydration operation at this time, the adhering moisture should be 35% by weight or less. If this washing and dehydration operation is performed more than once,
If 2 times or more is insufficient, the final dehydration operation will remove 30% of the adhering moisture.
By setting the TOC to 5% by weight or less, TOC can be removed later. When this precipitate is dissolved in dilute sulfuric acid and the nickel concentration is adjusted to a concentration suitable for electrolytic refining of nickel, the TOC concentration will be about 4.Oppm or less. This is because it becomes possible.
以下実施例について説明する。 Examples will be described below.
実施例1
容fA 10 iのビーカーに、水に炭酸ナトリウム水
溶液を加えて調整した所定pnで50Cの水溶液者50
0meを入れ、これをスリーワンモーターで攪拌しなが
ら、ニッケル84 g/l 、 T OO6,6g/l
のニッケルめっき排水と150g/lの炭酸ナトリウム
水溶液とを常温で夫々ローラーポンプを用い、該めっき
排水は1分間当り4(00〜500罰、これに対するア
ルカリは夫々1.05〜1.1当量、同時にビーカーの
底部に吹き込むようにして添加し、この間該容器内は湯
煎器で50Cに保持し、pnは手間理化製のPHコント
ローラーにより炭酸ナトリウム水溶液の添加を0N−O
FFさせながら所定PH値に保持しつつ各51のニッケ
ルめっき排水を処理し、反応液の滞留時間は変動させ得
られたスラリーは吸引濾過器(ヌツチェ)で濾過した。Example 1 A 50 C aqueous solution with a predetermined pn prepared by adding an aqueous sodium carbonate solution to water was placed in a beaker with a volume of fA 10 i.
0me, and while stirring this with a three-one motor, 84 g/l of nickel and 6.6 g/l of TOO.
of nickel plating waste water and 150 g/l aqueous sodium carbonate solution at room temperature using a roller pump, the plating waste water was mixed with 4 (00 to 500 equivalents) per minute, and each alkali was 1.05 to 1.1 equivalents per minute. At the same time, add the sodium carbonate aqueous solution by blowing it into the bottom of the beaker.During this time, the inside of the container was maintained at 50C with a water bath, and the pn was adjusted to 0N-O by using a PH controller manufactured by Teirika.
Each of the 51 nickel plating wastewaters was treated while maintaining a predetermined pH value while FF was applied, and the residence time of the reaction solution was varied, and the resulting slurry was filtered with a suction filter (Nutsche).
次に得られたケーキは、100g当り600m(!、
50Cの温水で各30分間レパルブ洗浄を夫々行ない、
その都度吸引濾過器で濾過し、最終回の濾過はケーキの
保有水分が30重量%程度となるまで吸引により脱水し
た。このようにして得られたケーキは1.1当量の希硫
酸で溶解し、更に水を加えてN175gjlの水溶液と
し、そのTOCをJ工S規格に基すいて定量した。その
結果を第1表に示す。Next, the cake obtained was 600 m/100 g (!,
Perform Repulve cleaning with warm water at 50C for 30 minutes each,
Each time, the cake was filtered using a suction filter, and in the final filtration, the cake was dehydrated by suction until the moisture content of the cake became about 30% by weight. The cake thus obtained was dissolved in 1.1 equivalents of dilute sulfuric acid, water was further added to make an aqueous solution containing 175 gjl of N, and the TOC thereof was determined based on the J Engineering S standard. The results are shown in Table 1.
第 1 表
第1表より明らかなように当初6.6gelもあったT
ooを期待値3o ppm以下Oこ、し1ずれも確実G
こクリヤーした。Table 1 As is clear from Table 1, the initial T content was 6.6 gel.
oo is expected value 3o ppm or less O, and 1 deviation is also certainG
I cleared this.
実施例2
85g/lのN1.12g//1のTOOを含むニッケ
ルめっき排水を、アルカリとして200 g/lの水酸
イヒナトリウム水溶液を使用し、反応温度を60Cとし
た以外は実施例1と同様にして脱TOCの処理を行なっ
た。その結果を第2表に示す。但し実験塵9は2回とも
通常の軽い吸引濾過を行なったものである。Example 2 The same procedure as Example 1 was carried out except that nickel plating wastewater containing 85 g/l of N1.12 g//1 TOO was used as an alkali, an aqueous solution of 200 g/l of sodium hydroxide, and the reaction temperature was 60C. TOC removal treatment was performed in the same manner. The results are shown in Table 2. However, the experimental dust 9 was subjected to normal light suction filtration both times.
第 2 表
第2表を見て判るように原料中のToa濃度が実施例1
の約2倍と濃厚になっても、殆んど同様の除去率でTo
oを分離除去し’roa濃度約20〜3o ppmと低
濃度のものが得られた。以上実施例1及び2はレパルプ
洗浄脱水操作を2回行なった場合であり、レパルブ洗浄
脱水操作の回数をさらに多くすると、より’roaの低
いニッケル再生液を得ることが可能である。通常の濾過
法を適用した実験煮9は洗浄脱水方法及び回収が同じで
もT。Table 2 As can be seen from Table 2, the Toa concentration in the raw material was the same as in Example 1.
Even when the concentration is about twice as high as that of To
By separating and removing o, a low-concentration 'roa of about 20 to 3 o ppm was obtained. In Examples 1 and 2, the repulp washing and dehydration operation was performed twice, and by increasing the number of repulp washing and dehydration operations, it is possible to obtain a nickel regenerated liquid with a lower 'roa. Experiment 9, which applied the normal filtration method, was T even though the washing and dehydration method and recovery were the same.
Cの除去が不良であった。Removal of C was poor.
ちなみに第1表試料扁2及び第2表試料扁5の場合洗浄
脱水操作1回のケーキを硫酸で溶解しN175g7’t
の水溶液とした際のTOO濃度は夫々220ppm 1
160 ppmであった。By the way, in the case of Sample Flat 2 in Table 1 and Sample Flat 5 in Table 2, the cake after one washing and dehydration operation was dissolved in sulfuric acid and N175g7't.
The TOO concentration when made into an aqueous solution of each is 220 ppm 1
It was 160 ppm.
このようにニッケルめっき排水中のTOO除去は、一般
的な不純物の除去と比較すると極めて困難であるが、本
発明法を適用すると99.5重量%以上が除去され得ら
れる再生電解液中のToo濃度は、マット電解を行なう
際の電解液の濃度65〜75 g7’l l(iの場合
T O010〜80 ppmまで低下させることができ
る。As described above, removal of TOO from nickel plating wastewater is extremely difficult compared to removal of general impurities, but when the method of the present invention is applied, more than 99.5% by weight of TOO is removed from the resulting recycled electrolyte. The concentration can be lowered to 65 to 75 g7'l l (TO010 to 80 ppm in the case of i) of the electrolytic solution when performing matte electrolysis.
実施例としては特に示さなかったが、本発明法の適用に
よって他の不純物(アルカリ添加により沈殿しないもの
)も同時に除去されるという利点も得られる。尚、該め
っき排水より回収されるニッケルの収率は99.5重量
%以上である。Although not specifically shown as an example, application of the method of the present invention also provides the advantage that other impurities (those that do not precipitate due to the addition of alkali) are also removed at the same time. The yield of nickel recovered from the plating wastewater is 99.5% by weight or more.
本発明法で得られる再生ニッケル水溶液は・そのま\ニ
ッケルマット電解槽より抜き出し電解廃液として浄液し
たのち、該電解槽に給液される上記電解廃液と合流させ
て何ら支障なく使用することができる。The recycled nickel aqueous solution obtained by the method of the present invention can be used as it is without any problems by being extracted from the nickel matte electrolytic cell, purified as an electrolytic waste liquid, and then combined with the electrolytic waste liquid supplied to the electrolytic cell. can.
Claims (1)
上に保持し、攪拌されている状態の該水溶液に、ニッケ
ルめつき排水と炭酸アルカリ水溶液又は水酸化アルカリ
水溶液とを同時に、該水溶液のPH及び温度を維持しつ
つ該水溶液の底部に吹き込むようにして添加し、生成し
た沈殿を温水によるレパルプ洗浄と、洗浄物からの脱水
操作とを複数回行ない最終脱水操作で付着水分35重量
%以下としたのち希硫酸に溶解しニッケル濃度をニッケ
ルの電解精製に適する濃度に調整することを特徴とする
ニッケルめつき排水をニッケルの電解精製用補給液とし
て再生する方法。(1) An alkaline aqueous solution with a pH of 8.0 to 9.0 is maintained at 40°C or higher, and nickel plating wastewater and an alkali carbonate aqueous solution or an alkali hydroxide aqueous solution are simultaneously added to the aqueous solution while it is being stirred. While maintaining the pH and temperature of the aqueous solution, the resulting precipitate is repulped with hot water and dehydrated several times, and the final dehydration process reduces the adhering moisture to 35% by weight. A method for regenerating nickel-plated wastewater as a replenishment solution for electrolytic refining of nickel, which comprises: dissolving it in dilute sulfuric acid to adjust the nickel concentration to a concentration suitable for electrolytic refining of nickel.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP16767484A JPS6148588A (en) | 1984-08-09 | 1984-08-09 | Method for regenerating waste water after nickel plating as replenisher for electrolytic refining of nickle |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP16767484A JPS6148588A (en) | 1984-08-09 | 1984-08-09 | Method for regenerating waste water after nickel plating as replenisher for electrolytic refining of nickle |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS6148588A true JPS6148588A (en) | 1986-03-10 |
JPH0368959B2 JPH0368959B2 (en) | 1991-10-30 |
Family
ID=15854112
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP16767484A Granted JPS6148588A (en) | 1984-08-09 | 1984-08-09 | Method for regenerating waste water after nickel plating as replenisher for electrolytic refining of nickle |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS6148588A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2012255675A (en) * | 2011-06-08 | 2012-12-27 | Sumitomo Metal Mining Co Ltd | Method for measuring total organic carbons |
CN104005049A (en) * | 2014-05-30 | 2014-08-27 | 成都易态科技有限公司 | Insoluble anodic electrodeposition production process for nickel |
-
1984
- 1984-08-09 JP JP16767484A patent/JPS6148588A/en active Granted
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2012255675A (en) * | 2011-06-08 | 2012-12-27 | Sumitomo Metal Mining Co Ltd | Method for measuring total organic carbons |
CN104005049A (en) * | 2014-05-30 | 2014-08-27 | 成都易态科技有限公司 | Insoluble anodic electrodeposition production process for nickel |
Also Published As
Publication number | Publication date |
---|---|
JPH0368959B2 (en) | 1991-10-30 |
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