JP7243749B2 - 有価金属の回収方法及び回収装置 - Google Patents
有価金属の回収方法及び回収装置 Download PDFInfo
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- 238000000034 method Methods 0.000 title claims description 30
- 229910052751 metal Inorganic materials 0.000 title claims description 25
- 239000002184 metal Substances 0.000 title claims description 25
- 238000011084 recovery Methods 0.000 title description 11
- 239000000706 filtrate Substances 0.000 claims description 108
- 238000001914 filtration Methods 0.000 claims description 74
- 239000000654 additive Substances 0.000 claims description 58
- 230000000996 additive effect Effects 0.000 claims description 58
- 239000000047 product Substances 0.000 claims description 58
- 239000000463 material Substances 0.000 claims description 46
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 36
- 239000011734 sodium Substances 0.000 claims description 30
- 239000002893 slag Substances 0.000 claims description 28
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 26
- 239000002253 acid Substances 0.000 claims description 25
- 239000011575 calcium Substances 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 150000002739 metals Chemical class 0.000 claims description 21
- 238000005406 washing Methods 0.000 claims description 21
- 238000002386 leaching Methods 0.000 claims description 17
- 239000002699 waste material Substances 0.000 claims description 17
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 16
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 14
- 229910001416 lithium ion Inorganic materials 0.000 claims description 14
- 150000003464 sulfur compounds Chemical class 0.000 claims description 14
- 239000001569 carbon dioxide Substances 0.000 claims description 13
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 12
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 239000000920 calcium hydroxide Substances 0.000 claims description 10
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- 239000007774 positive electrode material Substances 0.000 claims description 10
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 8
- 238000010304 firing Methods 0.000 claims description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 238000007664 blowing Methods 0.000 claims description 7
- 239000007773 negative electrode material Substances 0.000 claims description 6
- 230000033116 oxidation-reduction process Effects 0.000 claims description 6
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 5
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 5
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 claims description 4
- 150000007513 acids Chemical class 0.000 claims description 2
- 150000005323 carbonate salts Chemical class 0.000 claims 1
- 229910052759 nickel Inorganic materials 0.000 description 15
- 229910052782 aluminium Inorganic materials 0.000 description 11
- 229910052748 manganese Inorganic materials 0.000 description 10
- 229910052744 lithium Inorganic materials 0.000 description 9
- 239000000203 mixture Substances 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 6
- 238000000926 separation method Methods 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 4
- 229910052808 lithium carbonate Inorganic materials 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 150000004763 sulfides Chemical class 0.000 description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- MQRJBSHKWOFOGF-UHFFFAOYSA-L disodium;carbonate;hydrate Chemical compound O.[Na+].[Na+].[O-]C([O-])=O MQRJBSHKWOFOGF-UHFFFAOYSA-L 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- RPACBEVZENYWOL-XFULWGLBSA-M sodium;(2r)-2-[6-(4-chlorophenoxy)hexyl]oxirane-2-carboxylate Chemical compound [Na+].C=1C=C(Cl)C=CC=1OCCCCCC[C@]1(C(=O)[O-])CO1 RPACBEVZENYWOL-XFULWGLBSA-M 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
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- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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Description
リチウムイオン二次電池の廃棄物から回収した電池滓14.5gに硫酸(濃度2mol/l)100ml及び過酸化水素水(濃度30質量%)5mlを添加して浸出液を生成した。浸出液を60℃に加熱して4時間攪拌した。その後、この浸出液を室温まで放冷した。
室温まで放冷した浸出液にNaSH水溶液(濃度200g/l)を添加して第1処理物を生成した。NaSH水溶液の添加は、第1処理物のORP(酸化還元電位)が0mV(vs Ag/AgCl)に達するまで行った。次に、第1処理物にNaOH水溶液(濃度25質量%)を添加した。NaOH水溶液の添加については、第1処理物のpHが3.5程度になるように行った。
NaOH水溶液を添加した第1処理物を濾過して第1処理濾液と第1処理残渣とに分離した。
第1処理濾液にNaSH水溶液(濃度200g/l)を添加して第2処理物を生成した。NaSH水溶液の添加については、第2処理物のORP(酸化還元電位)が-420mVになるように行った。
第2処理物を濾過して第2処理濾液と第2処理残渣とに分離した。
第2処理濾液に水酸化カルシウム水溶液を添加して第3処理物を生成した。水酸化カルシウム水溶液の添加は、第3処理物のpHが10.0以上になるように行った。
第3処理物を濾過して第3処理濾液と第3処理残渣とに分離した。
Claims (6)
- リチウムイオン電池の廃棄物から電池滓を取り出す取出工程と、
前記電池滓に酸を添加して浸出液を生成する酸浸出工程と、
前記浸出液に第1添加剤であるNa分を含む第1硫黄化合物を添加して第1処理物を生成し、その後前記第1処理物に水酸化ナトリウムを添加する第1添加工程と、
前記第1処理物を濾過して第1処理濾液とCu分を含む第1処理残渣とに分離する第1濾過工程と、
前記第1処理濾液に第2添加剤であるNa分を含む第2硫黄化合物を添加して第2処理物を生成する第2添加工程と、
前記第2処理物を濾過して第2処理濾液とCo分又は/及びNi分を含む第2処理残渣とに分離する第2濾過工程と、
前記第2処理濾液に第3添加剤である水酸化カルシウムを添加して第3処理物を生成する第3添加工程と、
前記第3処理物を濾過してLi分を含む第3処理濾液と第3処理残渣とに分離する第3濾過工程と、
前記第3処理濾液に第4添加剤である炭酸ナトリウムを添加して第4処理物を生成する第4添加工程と、
前記第4処理物を濾過して第4処理濾液とCa分を含む第4処理残渣とに分離する第4濾過工程と、
前記第4処理濾液を加熱する加熱工程と、
加熱された前記第4処理濾液に炭酸ガスを吹き込むか、あるいは炭酸塩を添加して第5処理物を生成する第5添加工程と、
前記第5処理物を濾過してNa分を含む第5処理濾液とLi分を含む第5処理残渣とに分離する第5濾過工程とを有しており、
前記第2処理物のpHは前記第1処理物のpHよりも大きく、
前記第3処理物のpHは前記第2処理物のpHよりも大きいものとされており、
前記第2添加工程における前記第2添加剤としての前記第2硫黄化合物は、硫化水素ナトリウムであり、
前記第2添加剤の添加は、前記第2処理物のpHが2以上3以下であって、ORP(酸化還元電位)が-420mV以下(vs Ag/AgCl)になるようになされる
ことを特徴とする有価金属の回収方法。 - 前記酸浸出工程において、前記酸である硫酸と過酸化水素とを前記電池滓に添加することを特徴とする請求項1に記載の有価金属の回収方法。
- 前記第3処理残渣をアルカリ性水溶液により洗浄して洗浄物を生成する洗浄工程と、
前記洗浄物を濾過して前記Li分を含む洗浄濾液と洗浄残渣とに分離する洗浄後濾過工程とを有しており、
前記第4添加工程においては、前記第3処理濾液及び前記洗浄濾液から前記第4処理物を生成することを特徴とする請求項1又は2に記載の有価金属の回収方法。 - 前記電池滓は、Ni又は/及びCoを含む正極活物質とグラファイトを含む負極活物質とを有し、
前記電池滓を焼成することにより、前記グラファイトを酸化して炭酸ガスを生成する焼成工程をさらに有しており、
前記酸浸出工程においては、焼成された前記電池滓に前記硫酸を添加することを特徴とする請求項2に記載の有価金属の回収方法。 - 前記加熱工程は、前記第4処理濾液を60℃以上80℃以下に加熱して、前記加熱された第4処理濾液を得るものである、
請求項1~4のいずれか1項に記載の有価金属の回収方法。 - リチウムイオン電池の廃棄物から電池滓を取り出す取出装置と、
前記電池滓に酸を添加して浸出液を生成する酸浸出装置と、
前記浸出液に第1添加剤であるNa分を含む第1硫黄化合物を添加して第1処理物を生成し、その後前記第1処理物に水酸化ナトリウムを添加する第1添加装置と、
前記第1処理物を濾過して第1処理濾液とCu分を含む第1処理残渣とに分離する第1濾過装置と、
前記第1処理濾液に第2添加剤であるNa分を含む第2硫黄化合物を添加して第2処理物を生成する第2添加装置と、
前記第2処理物を濾過して第2処理濾液とCo分又は/及びNi分を含む第2処理残渣とに分離する第2濾過装置と、
前記第2処理濾液に第3添加剤である水酸化カルシウムを添加して第3処理物を生成する第3添加装置と、
前記第3処理物を濾過してLi分を含む第3処理濾液と第3処理残渣とに分離する第3濾過装置と、
前記第3処理濾液に第4添加剤である炭酸ナトリウムを添加して第4処理物を生成する第4添加装置と、
前記第4処理物を濾過して第4処理濾液とCa分を含む第4処理残渣とに分離する第4濾過装置と、
前記第4処理濾液を加熱する加熱装置と、
加熱された前記第4処理濾液に炭酸ガスを吹き込むか、あるいは炭酸塩を添加して第5処理物を生成する第5添加装置と、
前記第5処理物を濾過してNa分を含む第5処理濾液とLi分を含む第5処理残渣とに分離する第5濾過装置とを備えており、
前記第2処理物のpHは前記第1処理物のpHよりも大きく、前記第3処理物のpHは前記第2処理物のpHよりも大きいものとされており、
前記第2添加装置により添加される前記第2添加剤としての前記第2硫黄化合物は、硫化水素ナトリウムであり、
前記第2添加装置は、前記第2添加剤を、前記第2処理物のpHが2以上3以下であって、ORP(酸化還元電位)が-420mV以下(vs Ag/AgCl)になるように添加する構成となっている
ことを特徴とする有価金属の回収装置。
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