JP2018516433A - バイオマスガス化炉残渣を利用するリチウムイオン電池の負極材の調製方法 - Google Patents
バイオマスガス化炉残渣を利用するリチウムイオン電池の負極材の調製方法 Download PDFInfo
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 52
- 239000007773 negative electrode material Substances 0.000 title claims abstract description 46
- 239000002028 Biomass Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000002309 gasification Methods 0.000 claims abstract description 23
- 229920002873 Polyethylenimine Polymers 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000012535 impurity Substances 0.000 claims abstract description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 10
- 239000004094 surface-active agent Substances 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 6
- 238000010298 pulverizing process Methods 0.000 claims abstract description 5
- 239000013067 intermediate product Substances 0.000 claims description 29
- 239000000203 mixture Substances 0.000 claims description 28
- 238000002360 preparation method Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 6
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229940083575 sodium dodecyl sulfate Drugs 0.000 claims description 6
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 6
- 229950004959 sorbitan oleate Drugs 0.000 claims description 6
- PNGBYKXZVCIZRN-UHFFFAOYSA-M sodium;hexadecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCS([O-])(=O)=O PNGBYKXZVCIZRN-UHFFFAOYSA-M 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 claims description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 3
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical group [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- -1 sodium dodecyl fatty acid Chemical class 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 238000002386 leaching Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 229910052757 nitrogen Inorganic materials 0.000 abstract 1
- 239000003575 carbonaceous material Substances 0.000 description 14
- 229910021385 hard carbon Inorganic materials 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 11
- 229910021641 deionized water Inorganic materials 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000003921 oil Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000007670 refining Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000009830 intercalation Methods 0.000 description 3
- 230000002687 intercalation Effects 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000002427 irreversible effect Effects 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000011366 tin-based material Substances 0.000 description 2
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- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
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- 239000004005 microsphere Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
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- 229920005989 resin Polymers 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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Abstract
【解決手段】本発明は、バイオマスガス化炉の残渣を用いてリチウムイオン電池の負極材を調製する方法を開示する。本発明は、1)バイオマスガス化炉の残渣を界面活性剤と混合し、粉砕し、十分に粉砕した後、水洗いして界面活性剤を除去し、浸出させ、残渣を得て待機させる工程と、2)工程1)で得られた残渣に塩酸を投入し、不純物を十分に除去し、残渣を中性になるまで洗浄してから待機させる工程と、3)工程2)で得られた残渣をポリエチレンイミンとエタノールの混合溶液に入れ、振とうさせ、十分に振とうさせた後、ポリエチレンイミンとエタノールを洗浄し、濾過して残渣を得て待機させる工程と、4)工程3)で得られた残渣に質量分率55〜70%の硝酸を入れ、35〜45℃の温度で十分に攪拌し、改質を行い、硝酸を洗浄し、濾過し、乾燥させてリチウムイオン電池の負極材を得る工程を含む。
【選択図】図1
Description
Claims (10)
- バイオマスガス化炉の残渣を利用するリチウムイオン電池の負極材の調製方法であって、
1)バイオマスガス化炉の残渣と界面活性剤を含む水溶液を混合し、粉砕して残渣を分散させ、水洗いして界面活性剤を除去し、浸出させ、得られた残渣を回収して待機させる工程と、
2)前記工程1)で得られた残渣に塩酸を加え、攪拌して不純物を除去し、濾過し、中性になるまで洗浄してから待機させる工程と、
3)前記工程2)で得られた残渣にポリエチレンイミンとエタノールを加え、振とうさせて残渣を分散させ、ポリエチレンイミンとエタノールを洗い流し、濾過して得られた残渣を待機させる工程と、
4)前記工程3)で得られた残渣に質量分率55〜70%の硝酸を加え、35〜45℃の温度で十分に攪拌して酸化改質し、硝酸を洗い流し、濾過および乾燥して、リチウムイオン電池の負極材を得る工程と、
を含む方法。 - 前記工程1)において、界面活性剤がドデシルベンゼンスルホン酸ナトリウム、1-ヘキサデシルスルホン酸ナトリウム、ドデシル硫酸ナトリウム、ラウリルジフェニルエーテルジスルホン酸ナトリウム、ドデシル脂肪酸ナトリウム、F127、P123、オレイン酸ソルビタン、またはそれらの混合物である、請求項1に記載のバイオマスガス化炉の残渣を利用するリチウムイオン電池の負極材の調製方法。
- 前記工程1)において、質量比が残渣:界面活性剤:水= 100:0.5〜5:200〜1000であり、粉砕時間は15〜20分であることを特徴とする、請求項1または2に記載のバイオマスガス化炉の残渣を利用するリチウムイオン電池の負極材の調製方法。
- 前記工程2)において、塩酸の質量分率が20〜25%であり、質量比が中間生成物1:塩酸= 1:8〜20であることを特徴とする、請求項1または2に記載のバイオマスガス化炉の残渣を利用するリチウムイオン電池の負極材の調製方法。
- 前記工程3)において、質量比が残渣:ポリエチレンイミン:エタノール= 10:4〜10:200〜1000であり、振とう時間が0.5〜3時間であることを特徴とする、請求項1または2に記載のバイオマスガス化炉の残渣を利用するリチウムイオン電池の負極材の調製方法。
- 前記工程4)において、質量比が残渣:硝酸= 1:5〜15であり、撹拌時間は0.5〜3時間であることを特徴とする、請求項1または2に記載のバイオマスガス化炉の残渣を利用するリチウムイオン電池の負極材の調製方法。
- 前記工程4)において、前記リチウムイオン電池の負極材の粒径は50〜200mmであり、比表面積は15〜25m2/gであることを特徴とする、請求項1または2に記載のバイオマスガス化炉の残渣を利用するリチウムイオン電池の負極材の調製方法。
- 前記工程1)において、粉砕後の残渣の粒径は5〜20μmであることを特徴とする、請求項1または2に記載のバイオマスガス化炉の残渣を利用するリチウムイオン電池の負極材の調製方法。
- 前記工程1)において、バイオマスガス化炉の残渣の化学組成および質量百分率は、Cが65〜70%、SiO2が13〜18%、CaOが3〜6%、Al2O3が4〜7%、Fe2O3が1〜2%、Na2Oが1〜2%、K2Oが1〜2%、MgOおよびZnOを含む不純物であることを特徴とする、請求項1または2に記載のバイオマスガス化炉の残渣を利用するリチウムイオン電池の負極材の調製方法。
- 前記工程2)において、残渣および塩酸を35〜45℃の温度で0.5〜2時間攪拌することを特徴とする、請求項1または2に記載のバイオマスガス化炉の残渣を利用するリチウムイオン電池の負極材の調製方法。
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PCT/CN2016/079380 WO2016169436A1 (zh) | 2015-04-21 | 2016-04-15 | 利用生物质气化炉滤渣制备锂离子电池负极材料的方法 |
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CN104766952B (zh) | 2017-01-25 |
JP6730312B2 (ja) | 2020-07-29 |
RU2661911C1 (ru) | 2018-07-23 |
WO2016169436A1 (zh) | 2016-10-27 |
AU2016250999B2 (en) | 2019-10-31 |
CN104766952A (zh) | 2015-07-08 |
CA2983604A1 (en) | 2016-10-27 |
AU2016250999A1 (en) | 2017-11-16 |
EP3288103A4 (en) | 2018-11-14 |
US20180040878A1 (en) | 2018-02-08 |
EP3288103A1 (en) | 2018-02-28 |
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