JPS583937A - Selectively removing method for calcium in solution - Google Patents

Selectively removing method for calcium in solution

Info

Publication number
JPS583937A
JPS583937A JP10130281A JP10130281A JPS583937A JP S583937 A JPS583937 A JP S583937A JP 10130281 A JP10130281 A JP 10130281A JP 10130281 A JP10130281 A JP 10130281A JP S583937 A JPS583937 A JP S583937A
Authority
JP
Japan
Prior art keywords
calcium
soln
metals
nickel
cobalt
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
Application number
JP10130281A
Other languages
Japanese (ja)
Other versions
JPS5944375B2 (en
Inventor
Takashi Ogata
緒方 俊
Iwao Kyono
京野 「巌」
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.)
Eneos Corp
Original Assignee
Nippon Mining Co Ltd
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 Nippon Mining Co Ltd filed Critical Nippon Mining Co Ltd
Priority to JP10130281A priority Critical patent/JPS5944375B2/en
Publication of JPS583937A publication Critical patent/JPS583937A/en
Publication of JPS5944375B2 publication Critical patent/JPS5944375B2/en
Expired legal-status Critical Current

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  • Extraction Or Liquid Replacement (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

PURPOSE:To prevent the occurrence of scale trouble due to Ca in a soln.contg. plural kinds of metals while preventing the loss of the contained metals, by selectively extracting Ca in the soln. with D2EHPA and washing the extracting reagent with nitric acid. CONSTITUTION:To a soln. contg. plural kinds of metals such as Ni and Co is added about 1/10-1/2 time as much D2EHPA as the soln. by volume, and they are agitated at about 300-1,000r.p.m. and about 1.5-3.5pH for about 2-10min to extract Ca in the soln. At this time, to the soln. is added about 10-320g/l ammonium sulfate which prevents a pH reduction and acts as a pH buffer. The extracting reagent contg. a small amount of metals such as Ni and Co extracted together with Ca is scrubbed with a soln. contg. Ca, Ni, etc. acidified by nitric acid to reduce the amount of Ni, Co, etc., and Ca and metals such as Ni and Co are back-extracted with nitric acid having about 50-300g/l concn.

Description

【発明の詳細な説明】 本発明は、溶液中のカルシウムの選択的除去方法に関す
る。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for selectively removing calcium in a solution.

特に、複数の金属を含有する溶液から選択的にカルシウ
ムを除去する方法に関する。
In particular, the present invention relates to a method for selectively removing calcium from a solution containing multiple metals.

例えば、ニッケル、コバルトの抽出分離工程においては
、溶液中のカルシウムが晶出することによ如、抽出槽の
内壁にカルシウムが付着し。
For example, in the extraction and separation process of nickel and cobalt, calcium in the solution crystallizes and adheres to the inner wall of the extraction tank.

核付着によシ内容積が狭くな如、ひいては、連続操業を
不可能としていた。
Due to nuclear adhesion, the internal volume of the cylinder became narrow, making continuous operation impossible.

このため、溶液中のカルシウムをニッケル。For this reason, nickel calcium in solution.

コバルト等の回収金属とは、別に選択的に回収除去する
ことが要望されていた。
There has been a demand for selective recovery and removal separately from recovered metals such as cobalt.

本発明は、かかる要望に応じてなされた発明である。The present invention was made in response to such a demand.

即ち、fB液液中カルシウムを除去する場合において、
  DaHPAでカルシウムを抽出後、硝酸で該抽出剤
を洗浄することを特徴とする溶液中のカルシウムを選択
的に除去する方法に関する。
That is, when removing calcium from fB liquid,
The present invention relates to a method for selectively removing calcium in a solution, which comprises extracting calcium with DaHPA and then washing the extractant with nitric acid.

以下本発明に関し、詳しく説明する。The present invention will be explained in detail below.

本発明は、カルシウムの抽出に関し広く用いられるもの
であるが、以下ニッケル、コバルトを含有する液中のカ
ルシウムの選択的抽出方法を通じて本発明を説明する。
The present invention is widely used in the extraction of calcium, and the present invention will be explained below through a method for selectively extracting calcium from a liquid containing nickel and cobalt.

ニッケルおよびコバルト含有液中に、カルシウムがα0
25〜o、 s t7を前後含有する液から。
In a liquid containing nickel and cobalt, calcium is α0
25~o, from a solution containing around s t7.

ニッケルおよびコバルトを回収するに際し、カルシウム
を前記金属回収前あるいは、後の工程において除去する
ことが、連続操業を可能とする好ましい方法である。
When recovering nickel and cobalt, removing calcium before or after recovering the metals is a preferred method to enable continuous operation.

カルシウムを選択的に抽出する抽出剤とじてはり、Fi
HPAを用いる。
Fi is an extractant that selectively extracts calcium.
Use HPA.

第1図に示すごと<、bgapAはPH1,5〜五5に
することによシ、溶液中のカルシウムを効率よく抽出で
きる。また、0ONiO共抽出を極力少くシ、効率よく
抽出するためには、  1)H2,O〜2.8とすると
とが好ましい。
As shown in FIG. 1, bgapA can efficiently extract calcium from the solution by adjusting the pH to 1.5 to 55. In addition, in order to minimize 0ONiO co-extraction and extract efficiently, it is preferable that 1) H2,O be 2.8 to 2.8.

また、抽出によ如PHが低下することを未然に防止する
ためアンモニアイオンを予め溶液中で含有させておく。
Furthermore, in order to prevent the pH from decreasing due to extraction, ammonia ions are included in the solution in advance.

これは、pHの緩衝剤として好ましい。This is preferred as a pH buffer.

アンモニアイオンは、硫酸アンモンとして10〜320
 f/を含ませる。
Ammonia ion is 10 to 320 as ammonium sulfate.
Include f/.

さらに抽出剤と、処理液の液量比は、  1/1Q〜1
/2が好ましい、より好ましくは177〜1/3である
Furthermore, the liquid volume ratio of extractant and processing liquid is 1/1Q~1
/2 is preferred, and more preferably 177 to 1/3.

攪拌および時間は、5QOrpm〜100 Q rpm
で2〜10分行う。これによシ油層と溶液層とが好まし
く接触する。
Stirring and time are 5Q Orpm to 100 Q rpm
Do this for 2 to 10 minutes. This allows the oil layer and the solution layer to preferably come into contact with each other.

接触後の処理液中のカルシウムはI)H=1.5〜3.
0の場合60〜98q6除去率が得られる。
Calcium in the treatment solution after contact is I)H=1.5-3.
In the case of 0, a 60-98q6 removal rate is obtained.

カルシウムの除去を効率的に行い、同時にニッケル、コ
バルトのロスを最小とする好ましい処理方法としては、
抽出工程でのP H2,0−′5.5とし、カルシウム
を最大限に抽出し、同時に抽出されたニッケル、コバル
トは、スクラビング工程においてPH1,5〜2.0前
後とすることによ如抽出剤中のニッケル、コバルト値を
低下させる方法があシ、この方法を採用することが好ま
しい。
A preferred treatment method that efficiently removes calcium while minimizing loss of nickel and cobalt is:
The pH in the extraction process is adjusted to 2,0-'5.5 to maximize calcium extraction, and the nickel and cobalt extracted at the same time are extracted by adjusting the pH to around 1,5 to 2.0 in the scrubbing process. There is a method of reducing the nickel and cobalt values in the agent, and it is preferable to adopt this method.

スクラビングで使用する液は、硝酸酸性の液であること
が好ましい。カルシウムの溶解度が高いためである。ま
た該液中のカルシウム、ニッケル、コバルト濃度社、抽
出剤中のその濃度よシ高い値にしておくことが好ましい
実施態様でおる。
The liquid used for scrubbing is preferably a nitric acidic liquid. This is due to the high solubility of calcium. In a preferred embodiment, the concentration of calcium, nickel, and cobalt in the liquid is higher than that in the extractant.

スクラビング工程おるいは、抽出工程を経た処理抽出剤
は、逆抽出工程において硝酸洗浄することによ如抽出剤
中のカルシウムを除去する。
The treated extractant that has undergone the scrubbing process or the extraction process is washed with nitric acid in the back extraction process to remove calcium from the extractant.

この工程で使用する硝酸は、50〜s o o y7t
の濃度のものが好ましい。
The nitric acid used in this step is 50 to 7 tons
It is preferable to have a concentration of .

この工程では、抽出剤と洗浄液の比率を3/1〜10/
1とすることが好ましい。
In this step, the ratio of extractant to washing liquid is 3/1 to 10/3.
It is preferable to set it to 1.

また逆抽出においても、硝酸洗浄を2段以上で行うこと
により、抽出剤中へのニッケル、コバルトのロスを防止
し、同時にカルシウムの逆抽出をよシ完全に行い得る。
Also, in back extraction, by performing nitric acid washing in two or more stages, loss of nickel and cobalt into the extractant can be prevented, and at the same time, calcium can be completely back extracted.

即ち、100〜s o o t7tの硝酸を含む液と処
理抽出剤を接触することによシ、抽出剤中のカルシウム
を10 ’9/を以下、ニッケルをi ”p/を以下、
コバルトを10 ”//!、以下とすることが可能であ
る。
That is, by contacting the treated extractant with a solution containing 100 to 7t of nitric acid, calcium in the extractant is reduced to less than 10'9/, nickel is reduced to less than i''p/,
Cobalt can be less than 10''//!.

そして1次の逆抽出においては、処理抽出剤と不純物を
含まない硝酸濃度50〜100 t/lの洗浄液とを6
71〜10/1で接触させることによシ、処理抽出剤中
のカルシウム、ニッケル、コバルトをそれぞれ1 ”/
/を以下となし得る。
In the first back-extraction, the treated extractant and a cleaning solution containing no impurities with a nitric acid concentration of 50 to 100 t/l are mixed into
Calcium, nickel, and cobalt in the treatment extractant are each 1"/1 by contacting at a ratio of 71 to 10/1.
/ can be made as follows.

また第2段の洗浄液を第1段の逆抽出用の液の1部とし
て用いることがより好ましい。
Further, it is more preferable to use the second stage washing liquid as a part of the first stage back extraction liquid.

逆抽出抜液の処理必要液量を減少させ抜液の処理を容易
にするためである。
This is to reduce the amount of liquid required for back extraction liquid extraction and to facilitate the liquid extraction process.

後液中のコバルト、ニッケルについては、公知の除去手
段によυ液中よシカルシウムと分離し回収し、ニッケル
、コバルト製錬の原料として供される。
The cobalt and nickel in the after-liquid are separated from the calcium in the liquid by known removal means and recovered, and used as raw materials for nickel and cobalt smelting.

以上の処理を行うことによシ以下のような効果が得られ
る。
By performing the above processing, the following effects can be obtained.

(1)  液中のカルシウムを選択的に抽出除去し得る
ためカルシウムの晶出によシ起る反応種でのスケールト
ラブルを未然に防止し得た。
(1) Since calcium in the liquid can be selectively extracted and removed, scaling problems caused by reactive species caused by calcium crystallization can be prevented.

(2)  特にニッケル、コバルトの溶媒抽出において
、ニッケル、コバルトのロスがなく、同時にスケールト
ラブルが防止し得る効果を得た。
(2) Particularly in the solvent extraction of nickel and cobalt, there was no loss of nickel and cobalt, and at the same time, scale troubles were prevented.

以下本発明の具体的な実施例について示し。Specific examples of the present invention will be shown below.

さらに本発明を詳細に述べる。Further, the present invention will be described in detail.

実施例 カルシウム145”//l、ニッケル5 o t7t 
Example Calcium 145”//l, Nickel 5 o t7t
.

コバル) 20 r/を含む液とDsFiHPAを含む
抽出剤を、pH2,0において、5:1の比率で接触さ
せた。
A solution containing 20 r/ml of DsFiHPA and an extractant containing DsFiHPA were brought into contact at a ratio of 5:1 at pH 2.0.

液温は60℃、攪拌750 rpmで5分間行つた。The liquid temperature was 60°C and the stirring was performed at 750 rpm for 5 minutes.

この抽出処理によって、処理液中のカルシウムは、56
”//lと低下し、後のコバルト、ニッケルの抽出分離
工程におけるスケールトラブルを回避し得た。
Through this extraction process, calcium in the treatment solution is reduced to 56
”//l, and it was possible to avoid scale troubles in the subsequent extraction and separation process of cobalt and nickel.

さらに、抽出剤中のカルシウムおよび一部抽出されたコ
バルトおよびニッケルを核剤中から除去するため次の処
理を行った。
Furthermore, the following treatment was performed to remove calcium in the extractant and partially extracted cobalt and nickel from the nucleating agent.

スクラビング工程では、前記抽出剤をpH=2.0でカ
ルシウム2.5 f/l、 ニッケル[L96 f/l
 。
In the scrubbing step, the extractant was mixed with calcium 2.5 f/l and nickel [L96 f/l] at pH=2.0.
.

コバルト9.55 f/l 、硝酸70 f/を含む液
と1=5の比率で接触させ、抽出剤中のニッケルをCL
 70 f/lから0.19 t/lと、コバルトをZ
Of/1.から1.9 r/lに低下させた。
Contact with a solution containing 9.55 f/l of cobalt and 70 f/l of nitric acid at a ratio of 1=5 to remove nickel in the extractant from Cl.
70 f/l to 0.19 t/l and Z
Of/1. It was lowered from 1.9 r/l to 1.9 r/l.

該洗浄後液は、前記抽出工程の処理液とした。The post-washing liquid was used as the treatment liquid in the extraction step.

逆抽出工程では、硝酸230 f/を含む液と接触させ
ることによシ、抽出剤中のカルシウムをs o o r
’p7tから10 ’//l K低下させ、 ニアケル
を190 ”//lから1 ’/、/l 、コバルトを
1.99/lから10 ”l/lに低下し得た。
In the back extraction step, calcium in the extractant is removed by contacting with a solution containing 230 f/nitric acid.
It was possible to lower K by 10'//l from 'p7t, reduce Niacel from 190'//l to 1'//l, and reduce cobalt from 1.99/l to 10'/l.

さらに前記抽出剤中のカルシウム、コバルトニッケルを
低下させるために、不純物を含まない硝酸75 f/l
の液で逆抽出を行い、抽出剤中のカルシウム、コバルト
、ニッケルをいずれも1 ’f/l以下になし得た。
Furthermore, to reduce the calcium, cobalt nickel content in the extractant, 75 f/l of pure nitric acid was added.
Back extraction was carried out using this solution, and calcium, cobalt, and nickel in the extractant were all reduced to 1'f/l or less.

以上の処理工程においても、硝酸を使用したため、カル
シウムによるスケールトラブルはなく連続操業が可能で
あった。
Since nitric acid was used in the above treatment steps, there were no scaling problems caused by calcium, and continuous operation was possible.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は、  DIEHPAによる。液中のカルシウム
。 コバルト、ニッケルの抽出曲線を示す。 特許出願人 日本鉱業株式会社 代理人 弁理士(7569)並川啓志
Figure 1 is from DIEHPA. Calcium in liquid. The extraction curves of cobalt and nickel are shown. Patent applicant: Japan Mining Co., Ltd., patent attorney (7569) Keishi Namikawa

Claims (1)

【特許請求の範囲】[Claims] 溶液中のカルシウムを除去する場合においてD*KHP
Aでカルシウムを抽出後、硝酸で該抽出剤を洗浄するこ
とを特徴とする溶液中のカルシウムを選択的に除去する
方法。
D*KHP when removing calcium from a solution
A method for selectively removing calcium in a solution, which comprises extracting calcium with A and then washing the extractant with nitric acid.
JP10130281A 1981-07-01 1981-07-01 Method for selectively removing calcium in solution Expired JPS5944375B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP10130281A JPS5944375B2 (en) 1981-07-01 1981-07-01 Method for selectively removing calcium in solution

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP10130281A JPS5944375B2 (en) 1981-07-01 1981-07-01 Method for selectively removing calcium in solution

Publications (2)

Publication Number Publication Date
JPS583937A true JPS583937A (en) 1983-01-10
JPS5944375B2 JPS5944375B2 (en) 1984-10-29

Family

ID=14297011

Family Applications (1)

Application Number Title Priority Date Filing Date
JP10130281A Expired JPS5944375B2 (en) 1981-07-01 1981-07-01 Method for selectively removing calcium in solution

Country Status (1)

Country Link
JP (1) JPS5944375B2 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60115893U (en) * 1984-01-12 1985-08-05 関塚 司 Hopper device
CN114486377A (en) * 2022-01-27 2022-05-13 上海晶盟硅材料有限公司 Method for extracting dirt on surface of wafer by using VPD machine

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU2002950713A0 (en) 2002-08-09 2002-09-12 Vital Health Sciences Pty Ltd Carrier
WO2006133506A1 (en) 2005-06-17 2006-12-21 Vital Health Sciences Pty Ltd A carrier comprising one or more di and/or mono-(electron transfer agent) phosphate derivatives or complexes thereof
NZ602572A (en) 2010-03-30 2014-11-28 Phosphagenics Ltd Transdermal delivery patch

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60115893U (en) * 1984-01-12 1985-08-05 関塚 司 Hopper device
CN114486377A (en) * 2022-01-27 2022-05-13 上海晶盟硅材料有限公司 Method for extracting dirt on surface of wafer by using VPD machine

Also Published As

Publication number Publication date
JPS5944375B2 (en) 1984-10-29

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