JP2013139023A - 有価金属回収用吸着ボールの製造方法、及びこれを用いる流動型連続脱イオン装置 - Google Patents
有価金属回収用吸着ボールの製造方法、及びこれを用いる流動型連続脱イオン装置 Download PDFInfo
- Publication number
- JP2013139023A JP2013139023A JP2012228496A JP2012228496A JP2013139023A JP 2013139023 A JP2013139023 A JP 2013139023A JP 2012228496 A JP2012228496 A JP 2012228496A JP 2012228496 A JP2012228496 A JP 2012228496A JP 2013139023 A JP2013139023 A JP 2013139023A
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- Prior art keywords
- adsorption
- continuous deionization
- fluid
- type continuous
- ball
- 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
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 32
- 239000002184 metal Substances 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 230000000274 adsorptive effect Effects 0.000 title abstract description 8
- 238000011084 recovery Methods 0.000 title abstract description 6
- 150000002739 metals Chemical class 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000001179 sorption measurement Methods 0.000 claims description 65
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 24
- 229910001416 lithium ion Inorganic materials 0.000 claims description 24
- 229910021645 metal ion Inorganic materials 0.000 claims description 16
- 239000000178 monomer Substances 0.000 claims description 16
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 29
- 229910052744 lithium Inorganic materials 0.000 description 29
- 239000003463 adsorbent Substances 0.000 description 22
- 239000013535 sea water Substances 0.000 description 17
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- 239000003431 cross linking reagent Substances 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 6
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- 229910052719 titanium Inorganic materials 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- WVAFEFUPWRPQSY-UHFFFAOYSA-N 1,2,3-tris(ethenyl)benzene Chemical compound C=CC1=CC=CC(C=C)=C1C=C WVAFEFUPWRPQSY-UHFFFAOYSA-N 0.000 description 1
- MYWOJODOMFBVCB-UHFFFAOYSA-N 1,2,6-trimethylphenanthrene Chemical compound CC1=CC=C2C3=CC(C)=CC=C3C=CC2=C1C MYWOJODOMFBVCB-UHFFFAOYSA-N 0.000 description 1
- ZJQIXGGEADDPQB-UHFFFAOYSA-N 1,2-bis(ethenyl)-3,4-dimethylbenzene Chemical group CC1=CC=C(C=C)C(C=C)=C1C ZJQIXGGEADDPQB-UHFFFAOYSA-N 0.000 description 1
- QLLUAUADIMPKIH-UHFFFAOYSA-N 1,2-bis(ethenyl)naphthalene Chemical compound C1=CC=CC2=C(C=C)C(C=C)=CC=C21 QLLUAUADIMPKIH-UHFFFAOYSA-N 0.000 description 1
- HIACAHMKXQESOV-UHFFFAOYSA-N 1,2-bis(prop-1-en-2-yl)benzene Chemical compound CC(=C)C1=CC=CC=C1C(C)=C HIACAHMKXQESOV-UHFFFAOYSA-N 0.000 description 1
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- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- DBSDMAPJGHBWAL-UHFFFAOYSA-N penta-1,4-dien-3-ylbenzene Chemical compound C=CC(C=C)C1=CC=CC=C1 DBSDMAPJGHBWAL-UHFFFAOYSA-N 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
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- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
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- 229910052596 spinel Inorganic materials 0.000 description 1
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
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- C02F1/46109—Electrodes
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- C02F2001/46138—Electrodes comprising a substrate and a coating
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- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
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Abstract
【解決手段】本発明は、有価金属及び有価資源を回収するための吸着ボール、及びその製造方法、吸着ボールを用いて有価金属を回収することができる流動型連続脱イオンモジュール、及びこれを備えた流動型連続脱イオン(Flow Through−Continuous Deionization;FT−CDI)装置の製造方法に関するものである。
【選択図】図1
Description
球状のリチウムイオン吸着剤を製造するために、下記表1のように、NaOHを用いてスチレン(styrene)及びジビニルベンゼン(divinyl benzene)の水分を除去し、リチウムイオンを有する複合金属酸化物としてLi1.33Mn1.67O4(平均粒径60nm)を十分に分散して準備した。蒸留水に前記スチレン単量体の質量に対して0.1%のポリビニルアルコール(Poly(vinyl alcohol)、99%けん化度)を入れて80℃の温度で十分に混合されるように攪拌した。準備した前記単量体混合溶液に単量体の質量に対して0.1%の過酸化ベンゾイル(benzoyl peroxide)及び10%のトルエン(toluene)を混合した。粒子状のLi1.33Mn1.67O4は単量体(monomer)混合溶液に完全に混合されるように強く攪拌し、さらに超音波を用いて30分間分散した。Li1.33Mn1.67O4が添加されたスチレン(styrene)及びジビニルベンゼン(divinyl benzene)が混合した溶液を蒸留水溶液に徐々に滴下しながら強く攪拌し、懸濁重合を行った。
次に、前記で取得した球状の吸着ボールを活性化するために酸処理を施した。酸処理は0.1モルのHCl溶液500mlで100rpmの速度で攪拌する状態で24時間行った。1回活性化した球状の吸着剤は60℃のオーブンで4時間乾燥した後、0.1モルのHCl溶液500mlで1回の反応と同じ速度で攪拌し、24時間2次活性化した。2回活性化した球状の吸着体は前と同様に、60℃のオーブンで4時間乾燥してから、また0.1モルのHCl溶液500mlを用いて3次の活性化を行った。従って、3回のリチウムイオンの脱着過程により球状の吸着ボールを活性化した。
前記で製造した活性化した球状の吸着ボールの吸着性能を確認するために、前記で製造された球状のリチウムイオン吸着剤の吸着効率を測定した。
前記でリチウムイオンが吸着された実施例1で製造した球状の活性化した吸着ボールに対して流動型連続脱イオン装置を用いて脱着を行った結果を図5に示した。球状のリチウムイオン吸着剤の脱着性能を確認するために、図6の流動型連続脱イオンモジュールを備えた流動型連続脱イオン装置として、電極はTi基板にPtをメッキしたものを用いて、流速40ml/min、電圧5.0V、3日間の工程を変数として人工海水(Li 2.0ppm、In 1×10−1ppm、Co 3×10−1ppm、Na 1.1×107ppm、Mg 1.3×106ppm、Ca 4.2×105ppm)2Lで20gの吸着剤を用いて脱着量を測定した。図5のように、球状のリチウムイオン吸着剤の脱着能は、リチウム濃度0.2ppmの人工海水で吸着剤1g当たりリチウム0.14ppmで90%以上のリチウム回収率を確認することができた。
Claims (9)
- 金属複合酸化物粒子を単量体混合物に分散して重合し、焼成したマイクロスフェアを製造する段階と、
前記焼成したマイクロスフェアを無機酸溶液でイオン交換する段階と、
前記イオン交換したマイクロスフェアを乾燥する段階と、
を含む、吸着ボールの製造方法。 - 金属複合酸化物粒子はリチウムイオンを含有したものである、請求項1に記載の吸着ボールの製造方法。
- 焼成は200〜500℃の温度で行われる、請求項1に記載の吸着ボールの製造方法。
- 金属複合酸化物粒子を単量体混合物に分散して重合したマイクロスフェアを乾燥し、無機酸でイオン交換して吸着ボールを製造する段階と、
前記吸着ボールに有価金属イオンを吸着させる段階と、
前記有価金属イオンが吸着された吸着ボールを流動型連続脱イオンモジュールに連続して通過させ、有価金属イオンを回収する段階と、
を含む、流動型連続脱イオン装置を用いる有価金属の回収方法。 - 流動型連続脱イオンモジュールはビード供給ユニット、前記ビード供給ユニットの分離膜、及び電極を積層して備え、前記ビード供給ユニットは金属イオン吸着ビードを流入する流入口及び流出口を有する、請求項4に記載の流動型連続脱イオン装置を用いる有価金属の回収方法。
- 流動型連続脱イオンモジュールに吸着ボールを繰り返して循環して流動させる、請求項4に記載の流動型連続脱イオン装置を用いる有価金属の回収方法。
- 流動型連続脱イオン装置が流動型連続脱イオンモジュールを二つ以上含み、前記二つ以上の流動型連続脱イオンモジュールが連続して連結され、有価金属イオンを回収する、請求項4に記載の流動型連続脱イオン装置を用いる有価金属の回収方法。
- 連続して連結される一つ以上の流動型連続脱イオンモジュールを含み、前記モジュールはビード供給ユニット、前記ビード供給ユニットの分離膜、及び電極を積層して備え、前記ビード供給ユニットは金属イオン吸着ビードを流入する流入口及び流出口を有し、前記モジュールは吸着ボールを連続して循環して流動させる、流動型連続脱イオン装置。
- ビード供給ユニットと分離膜と電極との間には縁部をシールするガスケットが積層され、漏出を防止する、請求項8に記載の流動型連続脱イオン装置。
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