JPS63501072A - Separation method - Google Patents

Separation method

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JPS63501072A
JPS63501072A JP61505625A JP50562586A JPS63501072A JP S63501072 A JPS63501072 A JP S63501072A JP 61505625 A JP61505625 A JP 61505625A JP 50562586 A JP50562586 A JP 50562586A JP S63501072 A JPS63501072 A JP S63501072A
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copper
aqueous solution
selectively recovering
resin
selectively
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グレイグ，ジェームズ　アレクサンダー
ハンコック，ロナルド　ディビッド
リンゼイ，デリック
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ザ　ブリテイツシユ　ピトロ−リアム　コンパニ−　ピ−．エル．シ−．
ユニバーシティ オブ ストラスクライド
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J45/00—Ion-exchange in which a complex or a chelate is formed; Use of material as complex or chelate forming ion-exchangers; Treatment of material for improving the complex or chelate forming ion-exchange properties
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G3/00—Compounds of copper
    • C01G3/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Geology (AREA)
  • Manufacturing & Machinery (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Treatment Of Water By Ion Exchange (AREA)
  • Transition And Organic Metals Composition Catalysts For Addition Polymerization (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

(57)【要約】本公報は電子出願前の出願データであるため要約のデータは記録されません。 (57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

【発明の詳細な説明】 ｕロユ 本発明は、鉱物質分離に関し、更に特別には金属質含有水溶液から銅を分離する ことに関するものである。[Detailed description of the invention] u royu The present invention relates to the separation of minerals, and more particularly to the separation of copper from metal-containing aqueous solutions. It's about things.

例えば、亜鉛は一般にその硫化物の形態で産出し、５０％以上の亜鉛含量を有す る濃縮物は浮遊選鉱によって得られる。硫化亜鉛は焙焼して酸化亜鉛とし、これ を酸抽出して硫酸塩溶液を得ている。亜鉛を電解採取により抽出する前に、銅不 純物を除去するのが望ましい。この銅の除去は、普通溶液に亜鉛粉末を添加して 溶液から銅を置換することにより達成される。しかし、この方法は、更に濾過工 程を必要とする。For example, zinc generally occurs in its sulfide form and has a zinc content of more than 50%. The concentrate is obtained by flotation. Zinc sulfide is roasted to make zinc oxide, which is A sulfate solution is obtained by acid extraction. Before extracting zinc by electrowinning, copper-free It is desirable to remove pure substances. This copper removal is usually done by adding zinc powder to the solution. This is accomplished by displacing copper from the solution. However, this method requires additional filtration. It requires some time.

湿式精錬において、イオン交換樹脂を使用して希薄水溶液を処理することは公知 である。これらイオン交換樹脂は化学的かつ機械的の両方に比較的安定であって 、廃液流れを汚染することは無い。本発明は、金属質含有水溶液から銅を分離す るのに有効な新規キレート交換樹脂の使用に向けられている。It is known that ion exchange resins are used to treat dilute aqueous solutions in hydrometallurgy. It is. These ion exchange resins are relatively stable both chemically and mechanically. , without contaminating the waste stream. The present invention is a method for separating copper from a metal-containing aqueous solution. The aim is to use novel chelate exchange resins that are effective for

それ故、本発明によると、金属質含有水溶液から銅を選択的に回収する方法が提 供され、この方法において、（ａ）　ｐＨ７又はそれ以下の溶液をキレート交換 樹脂と接触して溶液から樹脂上に銅の実質的部分又は総てを選択的に除去し、前 記キレート交換樹脂はアミン置換環状化合物の形態の配位子とメタクリル酸エス テル基質とから成り、（ｂ）選択的に除去された銅は、引続いてキレート交換樹 脂から溶出又は同等の方法により分離される。Therefore, according to the present invention, a method for selectively recovering copper from a metal-containing aqueous solution is proposed. In this method, (a) a solution having a pH of 7 or less is chelate-exchanged; contacting the resin to selectively remove a substantial portion or all of the copper from the solution onto the resin; The chelate exchange resin contains a ligand in the form of an amine-substituted cyclic compound and a methacrylic acid ester. (b) the selectively removed copper is subsequently subjected to a chelation exchange tree. Separated from fat by elution or equivalent method.

アミン置換環状化合物配位子は、２−アミノメチルピリジン（２ＡＭＰｙ）、２ −ビリジルー２−イミダゾール（ＰｙｌＭ）、２−アミノメチルピペリジン（Ａ ＭＰ）、２−アミノエチルピペラジン（ＡＥＰ）、３−アミノプロピル−２−ピ ペリジン（ＡＰＰ）、３−アミノプロピルモルホリン（ＡＰＭ）、フルフリルア ミン（ＦＦ’Ａ）、２−アミノベンゾ−チアゾール（ＡＢＴ）、２−アミノ−チ アゾール（ＡＴ）、２−アミノ−チオフェノール（ＡＴＰ）、２−チオフェンカ ルボン酸ヒドラジブト（ＴＣＡＨ）又は２−アミノエチルピリジン（２ＡＥＰｙ ）であってよい。Amine-substituted cyclic compound ligands include 2-aminomethylpyridine (2AMPy), 2 -pyridy-2-imidazole (PylM), 2-aminomethylpiperidine (A MP), 2-aminoethylpiperazine (AEP), 3-aminopropyl-2-piperazine Peridine (APP), 3-aminopropylmorpholine (APM), furfurylua (FF'A), 2-aminobenzo-thiazole (ABT), 2-amino-thiazole Azole (AT), 2-amino-thiophenol (ATP), 2-thiopheneka Hydrodibonic acid (TCAH) or 2-aminoethylpyridine (2AEPy) ).

好適なメタクリル酸エステル基質はグリシジルメタクリル酸である。A preferred methacrylate substrate is glycidyl methacrylate.

本発明は、実施例によってのみ説明される。The invention is illustrated by examples only.

ポリスチレン（ｐｓ）樹脂は、スチレンとジビニルベンゼンを使用して標準的懸 濁重合法により得られる。樹脂のビーズサイズは使用した特別の方法に左右され 、５０〜１０００μｍの範囲にある。ＰＳ樹脂は比較の目的のため包含される。Polystyrene (PS) resin is a standard suspension using styrene and divinylbenzene. Obtained by turbidity polymerization method. Resin bead size depends on the particular method used. , in the range of 50 to 1000 μm. PS resin is included for comparison purposes.

グリシジルメタクリル酸（ＧＭＡ）基質又は樹脂は、シクロヘキサノールとドデ カノールをプロケンとして使用してグリシジルメタクリル酸とエチレングリコー ルジメタクリル酸の懸濁重合により調製した。グリシジルメタクリル酸とエチレ ングリコールジメタクリル酸（８／２〜６／４．容量／容量）をプロケン（１／ １〜ｌ／２の容量／容量比のモノマ／希釈剤）と共に使用するのが好適である。Glycidyl methacrylic acid (GMA) substrate or resin is a combination of cyclohexanol and dode. Glycidyl methacrylic acid and ethylene glycol using canol as prokene prepared by suspension polymerization of dimethacrylic acid. glycidyl methacrylate and ethyle Glycol dimethacrylic acid (8/2~6/4.vol./vol.) was mixed with Proken (1/2.vol./vol.). It is preferred to use the monomer/diluent with a volume/volume ratio of 1 to 1/2.

プロケンは容量／容量が９／ｌのシクロヘキサノールとドデカノールの混合物で あるのが好適である。Proken is a mixture of cyclohexanol and dodecanol with a volume/volume ratio of 9/l. It is preferable that there be one.

配位子は、エポキシプロピル基を結合した樹脂と直接に過剰の配位子と反応する ことによりＧＭＡ樹脂に結合された。The ligand reacts with excess ligand directly with the resin bonded with epoxypropyl groups. was bonded to the GMA resin.

亜鉛と銅とのイオンを含む酸性溶液から銅イオンの抽出はバッチ試験とカラム試 験によって実施された。Extraction of copper ions from acidic solutions containing zinc and copper ions is performed using batch tests and column tests. It was carried out by experiment.

バッチ試験においては、特に予備処理した樹脂５ｍ１（湿潤沈澱容量−ＷＳＶ） を金属イオン溶液５００ｍ１と接触した。金属イオンの濃度は各１１０００ｐｐ であり、溶液のｐｎは５であった。樹脂は１１２の容器中で撹拌（約３０Ｏｒｐ ｍ）　Ｌ　、装置は２５℃に自動調節した。In batch tests, in particular 5 ml of pretreated resin (wet settling volume - WSV) was contacted with 500 ml of metal ion solution. The concentration of metal ions is 11000pp each. and the pn of the solution was 5. The resin was stirred in a container of 112 (approx. m) L, the apparatus was automatically adjusted to 25°C.

試料（５ｍｌ）が０．１０，３０，６０，１２０．２４０分及び２４時間の間隔 で原子吸光分析により分析するために採取された。樹脂の抽出容量は２４時間試 料と初期供給物との濃度差から決定された。樹脂による抽出イオンのストリッピ ングは溶出剤として１Ｍ硫酸の５００ｍ１を使用してアナログ式方法で実施した 。使用した樹脂の総ては、抽出の使用に先立ち１０％アンモニア水で１時間次い で蒸留水でｐＨ７まで洗浄する予備処理された。Samples (5 ml) were collected at intervals of 0.10, 30, 60, 120, 240 minutes and 24 hours. sampled for analysis by atomic absorption spectrometry. The extraction capacity of the resin is tested for 24 hours. It was determined from the difference in concentration between the sample and the initial feed. Stripping of extracted ions with resin The analysis was carried out using an analog method using 500 ml of 1M sulfuric acid as the eluent. . All resins used were soaked in 10% aqueous ammonia for 1 hour prior to use for extraction. The sample was pretreated by washing with distilled water to pH 7.

第１表は使用した樹脂のデータを示し、第２表はバッチ金属抽出に対するＧＭＡ とＰＳ樹脂の比較結果を示している。Table 1 shows the data for the resins used and Table 2 shows the GMA for batch metal extraction. The results of comparison between PS resin and PS resin are shown.

樹脂データ 第　２　表 ）析溶液に対するバッチ抽出試験 単一カラム試験において、カラムは予備処理樹脂の１０ｍ１（湿潤沈澱容量）で 充填し、樹脂は多孔質フリット又は板によって支持された。　ぜん動ポンプを使 用して１時間当たり１０床容量（ＢＶ）の上向き流れにてカラムを充填し、ｐＨ ５，２５℃にて第２銅（Ｃｕ　）イオン７００ｍｇ／ρを含有する溶液で漏出さ せた。Resin data Table 2 ) Batch extraction test for analytical solution In single column tests, the column was loaded with 10 ml (wet settling volume) of pretreated resin. The resin was supported by a porous frit or plate. Using a peristaltic pump Pack the column with an upward flow of 10 bed volumes (BV) per hour using Leakage in a solution containing 700mg/ρ of cupric (Cu) ions at 5.25℃ I set it.

（漏出は供給濃度の１０％突破事態として為された）。洗浄後カラムを硫酸（１ （ｌｏｇ＃に濃度）で１ｏＢＶ／時間の流速にて溶出した。溶出液を分別して収 集し、原子吸光分析法（ＡＡＳ）にて金属含量を分析し、その結果を第３表に示 した。(The leak occurred as a result of a 10% exceedance of the supply concentration). After washing, the column was soaked in sulfuric acid (1 (concentration in log#) and eluted at a flow rate of 1oBV/hr. Separate and collect the eluate. The metal content was analyzed using atomic absorption spectrometry (AAS), and the results are shown in Table 3. did.

合成溶液から銅の抽出に対する樹脂タイプの効果第４表は、溶液から銅を抽出す る際にカドミウムイオンと亜鉛イオンが存在する効果を示している。単一カラム 試験が使用され、カラムは予備処理樹脂の１０ｍ１（ＹＳＶ）で充填された。３ 回の別々の供給溶液がＧＭＡとＰｓ樹脂カラムを通された。Effect of resin type on extraction of copper from synthetic solution Table 4 shows the effect of resin type on extraction of copper from solution. This shows the effect of the presence of cadmium ions and zinc ions on single column The test was used and the column was packed with 10ml (YSV) of pretreated resin. 3 Two separate feed solutions were passed through the GMA and Ps resin columns.

溶液は、（ａ）第２銅イオン４００ｍｇ／１２　（ｂ）第２銅イオン４００ｍｇ ＃＋８００ｎ＋ｇ＃！カドミウム（２＋）イオン及び（ｃ）第２銅イオン４００ ＋ｎｇ＃！＋カドミウム（２＋）イオン８００＋ｎｇ＃十亜鉛（２＋）イオン１ ５０ｇ／Ｑを含有していた。溶液温度は２５℃、ｐＨは５、流速はｌ０ＢＶ／時 間であった。カドミウムと亜鉛イオンの有意量は、夫々の溶液からＧＭＡ樹脂に よって抽出されなかった。The solution is (a) 400 mg/12 cupric ions (b) 400 mg cupric ions #+800n+g#! Cadmium (2+) ion and (c) cupric ion 400 +ng#! +Cadmium (2+) ion 800+ng #10 Zinc (2+) ion 1 It contained 50g/Q. Solution temperature is 25℃, pH is 5, flow rate is 10BV/hour. It was between. Significant amounts of cadmium and zinc ions were added to the GMA resin from their respective solutions. Therefore, it was not extracted.

合成溶液から銅抽出に対するカドミウムと亜鉛の作用ことによって溶液から銅を 抽出する結果を示し、カラムは直第５表 ＧＭＡ／２ＡＭＰｙ樹脂の直列２つのカラムによる合成溶液からの銅の抽出 結果は、ＧＭＡ／配位子システムがＰＳ／配位子システムと同じ若しくはそれ以 上の効果を有することを示している。ＧＭＡ／配位子システム４はカドミウムイ オン及びカドミウムイオンと亜鉛イオンの存在下において銅抽出が特に効果的で あること国際調査報告 ＡＮＮＥＸ　Ｔｏ　ＴＨＥ　ＩＮＴＥＲＮＡＴＩＯＮＡｒｌ、５ＥＡＲＣＨＲＥ ＰＯＲＴ　ＯＮEffect of cadmium and zinc on copper extraction from synthetic solution The results to be extracted are shown, and the columns are directly in Table 5. Extraction of copper from synthetic solutions by two columns in series of GMA/2AMPy resin The results indicate that the GMA/ligand system is the same as or better than the PS/ligand system. This shows that it has the above effect. GMA/ligand system 4 is cadmium Copper extraction is particularly effective in the presence of zinc ions, cadmium ions, and zinc ions. International research report ANNEX To THE INTERNATION Arl, 5EARCHRE PORT ON

Claims (7)

【特許請求の範囲】[Claims] １．金属質含有水溶液から銅を選択的に回収する方法において、（ａ）ｐＨ７又 はそれ以下の溶液をキレート交換樹脂と接触して溶液から樹脂上に銅の実質的部 分又は総てを選択的に除去し、前記キレート交換樹脂はアミン置換環状化合物の 形態の配位子とメタクリル酸エステル基質とから成り、及び（ｂ）選択的に除去 された銅は、引続いてキレート交換樹脂から分離されることを特徴とする金属質 水溶液から銅を選択的に回収する方法。1. In a method for selectively recovering copper from a metal-containing aqueous solution, (a) pH 7 or The solution is then chelated and exchanged with a resin to transfer a substantial portion of the copper from the solution onto the resin. The chelate exchange resin selectively removes some or all of the amine-substituted cyclic compounds. a methacrylic ester substrate; and (b) selectively removed. The produced copper is subsequently separated from the chelate exchange resin. A method for selectively recovering copper from an aqueous solution. ２．メタクリル酸エステル基質がグリシジルメタクリル酸である請求の範囲第１ 項記載の金属質水溶液から銅を選択的に回収する方法。2. Claim 1, wherein the methacrylic acid ester substrate is glycidyl methacrylic acid. A method for selectively recovering copper from a metallic aqueous solution as described in . ３．アミン置換環状化合物は、２−アミノメチルピリジン（２ＡＭＰｙ），２− ピリジル−２−イミダゾール（ＰｙＩＭ），２−アミノメチルピペリジン（ＡＭ Ｐ），２−アミノエチルピペラジン（ＡＥＰ），３−アミノブロピル−２−ピペ リジン（ＡＰＰ），３−アミノプロピルモルホリン（ＡＰＭ），フルフリルアミ ン（ＦＦＡ），２−アミノベンゾーチアゾール（ＡＢＴ），２−アミノ−チアゾ ール（ＡＴ），２−アミノ−チオフェノール（ＡＴＰ），２−チオフェンカルボ ン酸ヒドラジッド（ＴＣＡＨ）又は２−アミノエチルピリジン（２ＡＥＰｙ）で ある請求の範囲第１項記載の金属質水溶液から銅を選択的に回収する方法。3. The amine-substituted cyclic compound is 2-aminomethylpyridine (2AMPy), 2- Pyridyl-2-imidazole (PyIM), 2-aminomethylpiperidine (AM P), 2-aminoethylpiperazine (AEP), 3-aminopropyl-2-pipe Lysine (APP), 3-aminopropylmorpholine (APM), furfuryl amine (FFA), 2-aminobenzothiazole (ABT), 2-amino-thiazo (AT), 2-amino-thiophenol (ATP), 2-thiophenecarbo acid hydrazide (TCAH) or 2-aminoethylpyridine (2AEPy) A method for selectively recovering copper from a metallic aqueous solution according to claim 1. ４．グリシジルメタクリル酸基質はグリシジルメタクリル酸とエチレングリコー ルジメタクリル酸との懸濁重合により調製される請求の範囲第１項〜第３項のい ずれか１項に記載の金属質水溶液から銅を選択的に回収する方法。4. Glycidyl methacrylate substrate is glycidyl methacrylate and ethylene glycol. The method according to claims 1 to 3 prepared by suspension polymerization with dimethacrylic acid A method for selectively recovering copper from a metallic aqueous solution according to any one of the preceding items. ５．懸濁重合においてシクロヘキサノールとドデカノールとから成るブロゲンが 使用される請求の範囲第４項記載の金属質水溶液から桐を選択的に回収する方法 。5. In suspension polymerization, brogene consisting of cyclohexanol and dodecanol is A method for selectively recovering paulownia from a metallic aqueous solution as set forth in claim 4. . ６．溶液のｐＨは２〜６の範囲にある請求の範囲第１項記載の金属質水溶液から 銅を選択的に回収する方法。6. From the metallic aqueous solution according to claim 1, wherein the pH of the solution is in the range of 2 to 6. A method for selectively recovering copper. ７．銅は溶出によりキレート交換樹脂から引き続き除去される請求の範囲第１項 記載の金属質水溶液から銅を選択的に回収する方法。7. Claim 1: Copper is subsequently removed from the chelate exchange resin by elution. A method for selectively recovering copper from the metal aqueous solution described above.
JP61505625A 1985-10-17 1986-10-17 Separation method Pending JPS63501072A (en)

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GB8525648 1985-10-17
GB858525648A GB8525648D0 (en) 1985-10-17 1985-10-17 Separation process

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JPS63501072A true JPS63501072A (en) 1988-04-21

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BE (1) BE905617A (en)
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JP2004502027A (en) * 1999-12-15 2004-01-22 ブラッコ　イメージング　エッセ　ピ　ア Method for recovering copper from aqueous solutions containing iodinated organic compounds
JP2012036058A (en) * 2010-08-11 2012-02-23 Japan Organo Co Ltd Method for recovering copper sulfate and apparatus for recovering copper sulfate

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GB9305902D0 (en) * 1993-03-22 1993-05-12 Bp Chem Int Ltd Process
US5652348A (en) * 1994-09-23 1997-07-29 Massey University Chromatographic resins and methods for using same
US6176895B1 (en) 1998-11-04 2001-01-23 Desimone Joseph M. Polymers for metal extractions in carbon dioxide
AU2626201A (en) * 2000-01-03 2001-07-16 Juzer Jangbarwala Method and apparatus for metal removal by ion exchange
IL138852A0 (en) * 2000-10-04 2001-10-31 Yeda Res & Dev Ion exchange resins for gold cyanide extraction
CN108250339A (en) * 2018-01-04 2018-07-06 昆明理工大学 A kind of novel chelate resin material and its preparation method and application
WO2023180174A1 (en) * 2022-03-22 2023-09-28 Lanxess Deutschland Gmbh Method for the elution of aluminum ions and/or zinc ions

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US4031038A (en) * 1975-06-16 1977-06-21 The Dow Chemical Company Water insoluble chelate exchange resins having a crosslinked polymer matrix and pendant thereto a plurality of methyleneaminopyridine groups
ZA775398B (en) * 1977-09-07 1979-04-25 Nat Inst Metallurg Selective ion exchange media

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004502027A (en) * 1999-12-15 2004-01-22 ブラッコ　イメージング　エッセ　ピ　ア Method for recovering copper from aqueous solutions containing iodinated organic compounds
JP2012036058A (en) * 2010-08-11 2012-02-23 Japan Organo Co Ltd Method for recovering copper sulfate and apparatus for recovering copper sulfate

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AU6479086A (en) 1987-05-05
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WO1987002273A1 (en) 1987-04-23
BE905617A (en) 1987-04-17

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