JP6016899B2 - 硫化リチウムの製造方法 - Google Patents
硫化リチウムの製造方法 Download PDFInfo
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- JP6016899B2 JP6016899B2 JP2014513152A JP2014513152A JP6016899B2 JP 6016899 B2 JP6016899 B2 JP 6016899B2 JP 2014513152 A JP2014513152 A JP 2014513152A JP 2014513152 A JP2014513152 A JP 2014513152A JP 6016899 B2 JP6016899 B2 JP 6016899B2
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- lithium
- sulfide
- reaction
- hydrogen sulfide
- lithium sulfide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/22—Alkali metal sulfides or polysulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/32—Non-oxide glass compositions, e.g. binary or ternary halides, sulfides or nitrides of germanium, selenium or tellurium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- 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
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Electrochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
- Secondary Cells (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Glass Melting And Manufacturing (AREA)
- Battery Electrode And Active Subsutance (AREA)
Description
・リチウム金属及び硫黄を混ぜ合わせる(Zusammenreiben);
・液体アンモニア中での硫化アンモニウム又は硫黄とリチウム金属との反応;
・エタノール中でのリチウムエトキシドとH2Sとの反応。
2R−Li + H2S → Li2S + 2RH
2R2N−Li + H2S → Li2S + 2R2NH。
・商業的に入手可能な出発物質の使用;
・Li金属又はLiHのような空気及び水分に感受性の固体を用いる操作の回避;
・適度な温度での反応実施、それにより、加熱又は冷却のための追加のエネルギーが不要である;
・ろ過及び乾燥のような単純な方法による生成物の単離;
・LiSHを破壊するための加熱のような更なる精製工程を回避する、純相の生成物の取得。
温度センサ、ガス導入管(浸漬管)及びガス導出部(ガスメーター及びガススクラバーを経る)を取り付け、不活性化された3l平面すり合わせタイプのジャケット式反応器中に、アルゴン雰囲気下で、n−ブチルリチウム(ヘキサン中2.4M)1000g(1449ml、3.47モル、1.0当量)を装入し、引き続き、更に380mlのヘキサンを添加する。撹拌しながら、該反応溶液を10℃に冷却する。引き続き、10〜15℃で3hかけて、全部で59g(38.7l、1.73モル、0.5当量)の硫化水素を、浸漬管を経て該反応溶液中へ導通する。その際に、無色の固体が沈殿するようになる。該反応懸濁液を、撹拌しやすく維持するために、全部で更に550mlのヘキサンを添加する。ガス導入が終わった後に、反応器内容物を室温(22℃)に加温し、更に2h撹拌する。引き続き、該反応懸濁液を、G3フィルターを通してろ過し、残っている無色の固体を、複数に分けたヘキサンで念入りに洗浄する。得られた固体を、高真空中で室温で恒量まで乾燥させ、引き続き粉末X線回折法(XRD)により分析する。純相の硫化リチウムが得られた。
Claims (5)
- 硫化リチウムの製造方法であって、
リチウムアリール及びリチウムアミドからなる群から選択されるリチウム含有強塩基を硫化水素と、非プロトン性有機溶剤中で−20〜120℃の温度範囲内で不活性条件下で反応させることを特徴とする、硫化リチウムの製造方法。 - リチウムジイソプロピルアミド又はリチウムヘキサメチルジシラジドを使用する、請求項1記載の方法。
- 非プロトン性有機溶剤として、脂肪族炭化水素、芳香族炭化水素又はエーテル系溶剤又はこれらの溶剤の混合物を使用する、請求項1又は2記載の方法。
- 溶剤として、ヘキサン、トルエン、ジエチルエーテル又はTHFを使用する、請求項3記載の方法。
- 該反応を0〜80℃の温度範囲内で行う、請求項1から4までのいずれか1項記載の方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102011076572 | 2011-05-27 | ||
DE102011076572.7 | 2011-05-27 | ||
PCT/EP2012/060014 WO2012163900A2 (de) | 2011-05-27 | 2012-05-29 | Verfahren zur herstellung von lithiumsulfid |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2014518838A JP2014518838A (ja) | 2014-08-07 |
JP6016899B2 true JP6016899B2 (ja) | 2016-10-26 |
Family
ID=46172792
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2014513152A Active JP6016899B2 (ja) | 2011-05-27 | 2012-05-29 | 硫化リチウムの製造方法 |
Country Status (7)
Country | Link |
---|---|
US (1) | US9017582B2 (ja) |
EP (1) | EP2714587B1 (ja) |
JP (1) | JP6016899B2 (ja) |
KR (1) | KR101963297B1 (ja) |
CN (1) | CN103813980B (ja) |
DE (1) | DE102012208982A1 (ja) |
WO (1) | WO2012163900A2 (ja) |
Families Citing this family (17)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP5865268B2 (ja) * | 2011-01-27 | 2016-02-17 | 出光興産株式会社 | アルカリ金属硫化物と導電剤の複合材料 |
CN104609376A (zh) * | 2015-01-30 | 2015-05-13 | 浙江工业大学 | 一种硫化锂粉体的制备方法 |
CN108190845A (zh) * | 2018-01-31 | 2018-06-22 | 湖南省正源储能材料与器件研究所 | 一种制备硫化锂的方法 |
CN110790239B (zh) * | 2019-08-26 | 2022-01-28 | 浙江工业大学 | 一种硫化锂粉体的机械球磨合成方法 |
CN112678781B (zh) * | 2019-10-18 | 2022-04-15 | 天齐锂业(江苏)有限公司 | 硫化锂的制备方法 |
CN111517288A (zh) * | 2020-05-07 | 2020-08-11 | 天目湖先进储能技术研究院有限公司 | 一种合成硫化锂的方法 |
CN112520703B (zh) * | 2020-08-03 | 2022-07-22 | 浙江工业大学 | 一种硫化锂的绿色制备方法 |
CN112408437B (zh) * | 2020-11-19 | 2023-03-28 | 江西天新药业股份有限公司 | 锂盐的回收方法 |
KR20220079456A (ko) | 2020-12-04 | 2022-06-13 | 주식회사 레이크머티리얼즈 | 황화리튬의 제조방법 |
CN112551491B (zh) * | 2020-12-10 | 2022-04-08 | 天津大学 | 一种硫化锂的制备方法、硫化锂及其应用 |
CN112624061B (zh) * | 2020-12-31 | 2022-09-20 | 江西赣锋锂业股份有限公司 | 一种利用工业级丁基锂制备碳/硫化锂正极复合材料的方法 |
CN112624060B (zh) * | 2020-12-31 | 2022-09-20 | 江西赣锋锂业股份有限公司 | 一种利用工业级丁基锂制备高纯硫化锂的方法 |
CN113415812B (zh) * | 2021-06-23 | 2023-03-24 | 高能时代(珠海)新能源科技有限公司 | 一种高纯硫化锂的制备方法及应用 |
US20230150818A1 (en) | 2021-11-16 | 2023-05-18 | Solid Power Operating, Inc. | Lithium sulfide production method |
CN114455550B (zh) * | 2022-01-20 | 2023-07-18 | 湖北索立德新能源科技有限责任公司 | 硫化锂的制备方法 |
WO2023224150A1 (ko) * | 2022-05-20 | 2023-11-23 | 주식회사 솔리드아이오닉스 | 황화리튬 제조 방법 |
KR20240072554A (ko) | 2022-11-17 | 2024-05-24 | 현대자동차주식회사 | 황화수소 가스를 사용하지 않는 황화리튬의 제조방법 |
Family Cites Families (15)
Publication number | Priority date | Publication date | Assignee | Title |
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US3615191A (en) | 1969-08-27 | 1971-10-26 | Lithium Corp | Method of preparing lithium sulfide |
US3642436A (en) | 1969-11-14 | 1972-02-15 | Foote Mineral Co | Method for preparing lithium sulfide compounds |
US4126666A (en) * | 1978-01-25 | 1978-11-21 | Foote Mineral Company | Process for producing high purity lithium sulfide |
JP3816141B2 (ja) | 1996-04-16 | 2006-08-30 | 古河機械金属株式会社 | 硫化リチウムの製造方法 |
US6680145B2 (en) * | 2001-08-07 | 2004-01-20 | 3M Innovative Properties Company | Lithium-ion batteries |
JP2003252610A (ja) | 2001-12-27 | 2003-09-10 | Idemitsu Petrochem Co Ltd | 硫化リチウムの再生方法及びポリアリーレンスルフィドの製造方法 |
WO2004093099A1 (ja) * | 2003-04-15 | 2004-10-28 | Idemitsu Kosan Co., Ltd. | リチウムイオン導電性固体電解質の製造方法及びそれを用いた全固体型二次電池 |
WO2004095474A1 (ja) * | 2003-04-24 | 2004-11-04 | Idemitsu Kosan Co., Ltd. | リチウムイオン伝導性硫化物ガラス及びガラスセラミックスの製造方法並びに該ガラスセラミックスを用いた全固体型電池 |
JP4580149B2 (ja) | 2003-04-24 | 2010-11-10 | 出光興産株式会社 | リチウムイオン伝導性硫化物ガラスの製造方法及びリチウムイオン伝導性硫化物ガラスセラミックスの製造方法 |
KR101109821B1 (ko) | 2003-10-23 | 2012-03-13 | 이데미쓰 고산 가부시키가이샤 | 황화리튬의 정제 방법 |
KR101454501B1 (ko) | 2007-04-16 | 2014-10-23 | 바스프 에스이 | 리튬 풍부 금속 산화물의 제조 방법 |
DE102007048289A1 (de) * | 2007-10-08 | 2009-04-09 | Universität Siegen | Lithium-Argyrodite |
JP5277859B2 (ja) * | 2007-12-03 | 2013-08-28 | セイコーエプソン株式会社 | 硫化物系リチウムイオン伝導性固体電解質ガラスおよび全固体リチウム二次電池 |
JP5460283B2 (ja) * | 2008-12-15 | 2014-04-02 | 出光興産株式会社 | 硫化リチウムの製造方法 |
JP2012176866A (ja) * | 2011-02-25 | 2012-09-13 | Idemitsu Kosan Co Ltd | 硫化物系固体電解質ガラスの製造方法 |
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2012
- 2012-05-29 JP JP2014513152A patent/JP6016899B2/ja active Active
- 2012-05-29 KR KR1020137034805A patent/KR101963297B1/ko active IP Right Grant
- 2012-05-29 CN CN201280025805.0A patent/CN103813980B/zh active Active
- 2012-05-29 EP EP12723872.3A patent/EP2714587B1/de active Active
- 2012-05-29 WO PCT/EP2012/060014 patent/WO2012163900A2/de active Application Filing
- 2012-05-29 DE DE102012208982A patent/DE102012208982A1/de not_active Withdrawn
- 2012-05-29 US US14/119,980 patent/US9017582B2/en active Active
Also Published As
Publication number | Publication date |
---|---|
CN103813980B (zh) | 2016-05-18 |
WO2012163900A3 (de) | 2013-05-30 |
KR20140053034A (ko) | 2014-05-07 |
US20140084224A1 (en) | 2014-03-27 |
JP2014518838A (ja) | 2014-08-07 |
DE102012208982A1 (de) | 2012-11-29 |
EP2714587A2 (de) | 2014-04-09 |
WO2012163900A2 (de) | 2012-12-06 |
CN103813980A (zh) | 2014-05-21 |
KR101963297B1 (ko) | 2019-03-28 |
US9017582B2 (en) | 2015-04-28 |
EP2714587B1 (de) | 2016-04-06 |
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