JPH09268005A - Production of lithium hexafluorophosphase and apparatus therefor - Google Patents
Production of lithium hexafluorophosphase and apparatus thereforInfo
- Publication number
- JPH09268005A JPH09268005A JP10626196A JP10626196A JPH09268005A JP H09268005 A JPH09268005 A JP H09268005A JP 10626196 A JP10626196 A JP 10626196A JP 10626196 A JP10626196 A JP 10626196A JP H09268005 A JPH09268005 A JP H09268005A
- Authority
- JP
- Japan
- Prior art keywords
- lithium hexafluorophosphate
- hydrofluoric acid
- evaporation
- anhydrous hydrofluoric
- pressure
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/005—Lithium hexafluorophosphate
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明はリチウムイオン二次
電池用電解質などに有用な六フッ化リン酸リチウムを、
簡単に大量生産する製造方法並びにこの方法に用いる装
置に関する。TECHNICAL FIELD The present invention relates to a lithium hexafluorophosphate useful as an electrolyte for a lithium ion secondary battery,
The present invention relates to a manufacturing method for mass production easily and an apparatus used for this method.
【０００２】[0002]
【従来の技術】六フッ化リン酸化合物は、周知の通り、
リチウム電池等の高エネルギー電池の電解質をはじめ、
有機合成反応の触媒や半導体のドーピング剤として使用
される有用な化合物である。2. Description of the Related Art Hexafluorophosphoric acid compounds are well known in the art.
Starting with electrolytes for high energy batteries such as lithium batteries,
It is a useful compound used as a catalyst for organic synthesis reactions and as a doping agent for semiconductors.
【０００３】この六フッ化リン酸化合物の代表的なもの
の一つに六フッ化リン酸リチウムがある。Lithium hexafluorophosphate is one of the typical examples of the hexafluorophosphate compound.
【０００４】従来の六フッ化リン酸リチウムの製法につ
いては、多数の製造方法が知られており、その代表的な
方法は無水フッ化水素酸を使用する方法である。Many conventional methods for producing lithium hexafluorophosphate are known, and a typical method is to use anhydrous hydrofluoric acid.
【０００５】この方法では、目的物六フッ化リン酸リチ
ウムは、原則としてフッ化リチウムと五塩化リンを、無
水フッ化水素酸中に投入反応させ、無水フッ化水素酸溶
液として得られ、これから冷却して六フッ化リン酸リチ
ウムを析出させるものである。In this method, the target lithium hexafluorophosphate is obtained as a solution of anhydrous hydrofluoric acid by injecting lithium fluoride and phosphorus pentachloride into anhydrous hydrofluoric acid, as a general rule. It is cooled to deposit lithium hexafluorophosphate.
【０００６】而して従来の六フッ化リン酸リチウムの製
法については、その殆ど全ては、反応方法の改善が主で
あって、工業的規模で大量にしかも簡単に目的物六フッ
化リン酸リチウムを製造する方法については検討されて
いない。特に無水フッ化水素酸溶液中に存在する六フッ
化リン酸リチウムを析出させる方法については、全く検
討されていない。[0006] In most of the conventional methods for producing lithium hexafluorophosphate, the improvement of the reaction method is the main, and a large amount of the objective hexafluorophosphate can be easily prepared on an industrial scale. No method has been investigated for producing lithium. In particular, no study has been made on a method for depositing lithium hexafluorophosphate existing in an anhydrous hydrofluoric acid solution.
【０００７】事実例えば特開平４−１７５２１６号では
１ｌ容器のデータしかなく、また特開平６−０５６４１
３号でも１ｌ容器の実施例しか開示されていない。即ち
工業的規模の実施については全く考慮されていない。In fact, for example, in Japanese Unexamined Patent Publication No. 4-175216, there is only data for a 1 l container, and in Japanese Unexamined Patent Publication No. 06-05641.
No. 3 also discloses only an example of a 1 liter container. That is, no consideration is given to implementation on an industrial scale.
【０００８】[0008]
【発明が解決しようとする課題】本発明が解決しようと
する課題は、工業規模で大量に、六フッ化リン酸リチウ
ムを製造する方法就中その結晶を簡単にしかも容易に析
出させる方法とこの方法に用いる装置とを開発すること
である。The problem to be solved by the present invention is to provide a method for producing lithium hexafluorophosphate in large quantities on an industrial scale, and in particular a method for easily and easily precipitating the crystals thereof. To develop the device used in the method.
【０００９】[0009]
【課題を解決するための手段】この課題は、常法により
製造した、六フッ化リン酸リチウムを含有する無水フッ
化水素酸溶液を、無水フッ化水素酸の蒸発による蒸発潜
熱で該溶液温度を低下させて、六フッ化リン酸リチウム
の結晶を析出させることにより解決される。[Means for Solving the Problem] This problem is obtained by subjecting an anhydrous hydrofluoric acid solution containing lithium hexafluorophosphate produced by a conventional method to the solution temperature by evaporation latent heat by evaporation of anhydrous hydrofluoric acid. Is solved by precipitating crystals of lithium hexafluorophosphate.
【００１０】[0010]
【発明の実施形態】本発明の原理は常法により製造され
た六フッ化リン酸リチウムの無水フッ化水素酸溶液につ
いて、蒸発気化するフッ化水素の蒸発潜熱を利用して、
溶液を冷却させることにある。フッ化水素の蒸発潜熱は
９０ｋｃａｌ／ｋｇと大きく、また真空下で気化しやす
い。この気化による冷却を行うと、外部から冷却するの
と異なり、溶液が均一に冷却されると共に、自身の蒸発
潜熱で冷却するため熱効率が極めて良い特徴を有してい
る。BEST MODE FOR CARRYING OUT THE INVENTION The principle of the present invention relates to a solution of lithium hexafluorophosphate in anhydrous hydrofluoric acid produced by a conventional method, utilizing the latent heat of vaporization of hydrogen fluoride to be vaporized.
To allow the solution to cool. The latent heat of vaporization of hydrogen fluoride is as large as 90 kcal / kg, and it is easily vaporized under vacuum. Unlike the case where it is cooled from the outside, when this cooling by vaporization is carried out, the solution is cooled uniformly, and since it is cooled by its own latent heat of vaporization, it has extremely good thermal efficiency.
【００１１】例えば１００ｋｇの溶液から１時間に５ｋ
ｇのフッ化水素を蒸発させたとすれば、溶液の温度低下
は次のようになる。 ９５×０．５×ｔ＝５×９０ ｔ＝９．５℃ （溶液の比熱 ０．５ｋｃａｌ／ｋｇ，℃） このように少しの蒸発量で大幅に温度低下させることが
出来る。この温度低下は蒸発量の理論に従って温度低下
をさせることが出来る。あまり急激に圧力を変化させる
と溶液の突沸が起こり結晶を細かくしてしまう場合があ
る。この際低速の撹拌をしながら圧力を変化させること
は有効な手段である。For example, 5 k per hour from 100 kg of solution
If g of hydrogen fluoride is evaporated, the temperature drop of the solution is as follows. 95 × 0.5 × t = 5 × 90 t = 9.5 ° C. (specific heat of solution 0.5 kcal / kg, ° C.) As described above, the temperature can be significantly lowered with a small amount of evaporation. This temperature decrease can be made according to the theory of evaporation. If the pressure is changed too rapidly, bumping of the solution may occur and the crystals may become fine. At this time, changing the pressure while stirring at low speed is an effective means.
【００１２】蒸発したフッ化水素を凝縮して反応容器に
戻すと温度低下に寄与する部分は次のようになる。 １００×０．５×ｔ＝５×３０×０．６ （３０：温度差，ＨＦの比熱０．６ｋｃａｌ／ｋｇ，
℃） ｔ＝１．８℃ 蒸発量の寄与の２割程度である。When the evaporated hydrogen fluoride is condensed and returned to the reaction vessel, the portion contributing to the temperature decrease is as follows. 100 × 0.5 × t = 5 × 30 × 0.6 (30: temperature difference, HF specific heat 0.6 kcal / kg,
℃) t = 1.8 ℃ It is about 20% of the contribution of the evaporation amount.
【００１３】このように蒸発したフッ化水素を凝縮回収
すれば溶液量が変化せず不純物の少ない製品を得られる
利点がある。Condensing and recovering the evaporated hydrogen fluoride has the advantage that the amount of the solution does not change and a product with few impurities is obtained.
【００１４】更に本発明を詳しく説明すると以下の通り
である。撹拌機（２）付き耐圧容器（１）に、六フッ化
リン酸リチウムを含有する無水フッ化水素酸溶液を入
れ、好ましくは撹拌機を回転させ、排気を真空用エジェ
クター（４）に接続し、圧力を徐々に低下させ、好まし
くは撹拌下にフッ化水素を蒸発させて、その蒸発潜熱を
利用して溶液温度を低下させていく。圧力は液温度が
０．１〜１０℃／時間低下するように調整していき、液
温度を−３０℃〜−４０℃迄低下させる。液濃縮と温度
低下の両方の影響で六フッ化リン酸リチウムの結晶が析
出してくる。このように真空を利用してフッ化水素の蒸
発による濃縮と蒸発潜熱による溶液の冷却を利用して結
晶を析出させる。The present invention will be described in more detail below. The anhydrous hydrofluoric acid solution containing lithium hexafluorophosphate was placed in a pressure resistant container (1) equipped with a stirrer (2), preferably the stirrer was rotated, and the exhaust was connected to a vacuum ejector (4). The pressure is gradually decreased, and hydrogen fluoride is evaporated, preferably while stirring, and the latent heat of evaporation is used to decrease the solution temperature. The pressure is adjusted so that the liquid temperature is lowered by 0.1 to 10 ° C./hour, and the liquid temperature is lowered to −30 ° C. to −40 ° C. Crystals of lithium hexafluorophosphate precipitate due to the effects of both liquid concentration and temperature decrease. In this way, crystals are deposited by utilizing the concentration of hydrogen fluoride by evaporation using a vacuum and the cooling of the solution by the latent heat of evaporation.
【００１５】また、撹拌機（２）付きの耐圧容器（１）
の排気管と真空用エジェクター（４）との間に、凝縮器
（３）を設置し、蒸発してくるフッ化水素酸を、低温例
えば−４０℃のプラインで冷却し、凝縮させ、凝縮液を
耐圧容器に戻すようにしておく。この耐圧容器（１）に
六フッ化リン酸リチウムを含有する無水フッ化水素酸溶
液を入れ、好ましくは撹拌機（２）を回転させ、排気を
真空用エジェクター（４）に接続し、圧力を徐々に低下
させ、フッ化水素を蒸発させて、その蒸発潜熱を利用し
て液温度を低下させていく。蒸発凝縮した−３０℃のフ
ッ化水素を戻しながら、液温度が０．１〜１０℃／時間
低下するように圧力を調整していき、液温度を−３０〜
−４０℃まで低下させる。この場合は真空を利用してフ
ッ化水素の蒸発による蒸発潜熱を利用し、更に凝縮して
くる低温のフッ化水素を利用して溶液を冷却させること
で結晶を析出させるものである。上記の説明では撹拌機
（２）付耐圧容器（１）を使用した場合であるが、本発
明では必ずしも撹拌しなくとも良く、撹拌機（２）のな
い容器（１）を使用しても良い。A pressure vessel (1) equipped with a stirrer (2)
A condenser (3) is installed between the exhaust pipe and the ejector (4) for vacuum, and the hydrofluoric acid that evaporates is cooled and condensed by a low temperature line of, for example, -40 ° C to condense the condensate. Return to the pressure vessel. Anhydrous hydrofluoric acid solution containing lithium hexafluorophosphate was placed in this pressure vessel (1), preferably the stirrer (2) was rotated, and the exhaust gas was connected to the vacuum ejector (4) to adjust the pressure. The liquid temperature is gradually lowered by evaporating hydrogen fluoride and utilizing the latent heat of vaporization. While returning the evaporated and condensed hydrogen fluoride at −30 ° C., the pressure is adjusted so that the liquid temperature is lowered by 0.1 to 10 ° C./hour, and the liquid temperature is −30 to −30.
Reduce to -40 ° C. In this case, the latent heat of vaporization due to the evaporation of hydrogen fluoride is utilized by utilizing vacuum, and further the low temperature hydrogen fluoride that condenses is used to cool the solution to precipitate crystals. In the above description, the pressure resistant container (1) with a stirrer (2) is used, but in the present invention, it is not always necessary to stir and a container (1) without a stirrer (2) may be used. .
【００１６】本発明に於いて、撹拌を行う場合は、その
構造や種類は特に限定されることはなく、例えば回転羽
根等、適宜な手段で緩やかな撹拌で良い。In the present invention, when stirring is carried out, the structure and kind are not particularly limited, and gentle stirring may be carried out by an appropriate means such as a rotary blade.
【００１７】上記これ等の方法により多量の結晶を析出
させ取り扱うことが出来るようになる。By these methods described above, a large amount of crystals can be deposited and handled.
【００１８】圧力容器は容量に限定されないが、１００
ｌ、１ｍ3、３ｍ3、１０ｍ3、のものを用いることが出
来る。材質はステンレス鋼またはフッ素樹脂のライニン
グを施したもの等が用いられる。凝縮器はポリテトラフ
ルオロエチレンの如きフッ素樹脂製、カーボン製又はス
テンレス製のものを用いることが出来る。エジェクター
はポリ塩化ビニル製やゴムライニング製のものが使用出
来る。The pressure vessel is not limited to a capacity, but may be 100
1, 1 m 3 , 3 m 3 , 10 m 3 can be used. The material used is stainless steel or a fluororesin lining. The condenser may be made of fluororesin such as polytetrafluoroethylene, carbon or stainless steel. Ejectors made of polyvinyl chloride or rubber lining can be used.
【００１９】[0019]
【実施例】以下本発明の実施例を示す。Embodiments of the present invention will be described below.
【００２０】[0020]
【実施例１】撹拌機付きの１００ｌのステンレス製の耐
圧容器（１）に六フッ化リン酸リチウムを含有する２０
℃のフッ化水素溶液を１００ｋｇ入れた。撹拌機（２）
を１０ｒｐｍで回転させながら３℃／分の速度で温度低
下させ、１５時間掛けて−３０℃まで冷却した。蒸発し
たフッ化水素酸は２９０ｋｇであった。固液分離し乾燥
させて製品が１０．５ｋｇ得られた。このものの遊離酸
は１００ｐｐｍで不溶解残分は０．０８％であった。Example 1 A 100 liter pressure-resistant stainless steel vessel (1) equipped with a stirrer containing lithium hexafluorophosphate 20
100 kg of hydrogen fluoride solution at 0 ° C was added. Stirrer (2)
Was rotated at 10 rpm, the temperature was lowered at a rate of 3 ° C./min, and it was cooled to −30 ° C. in 15 hours. The amount of evaporated hydrofluoric acid was 290 kg. After solid-liquid separation and drying, 10.5 kg of a product was obtained. The free acid of this product was 100 ppm and the insoluble residue was 0.08%.
【００２１】[0021]
【実施例２】上記実施例１に於いて、耐圧容器として撹
拌機のつかないものを使用し、且つ撹拌することなく、
５℃／分の速度で温度低下させ、その他は実施例１と同
様に処理した。この結果、製品は１０．３ｋｇ得られ
た。[Embodiment 2] In the above Embodiment 1, a pressure-resistant container without a stirrer is used, and without stirring.
The temperature was lowered at a rate of 5 ° C./minute, and the other treatments were performed in the same manner as in Example 1. As a result, 10.3 kg of the product was obtained.
【００２２】[0022]
【実施例３】下記実施例３の装置を用いて、六フッ化リ
ン酸リチウムを製造した。即ち撹拌機（２）及び凝縮器
（３）付きの１ｍ3のステンレス製の耐圧容器（１）に
六フッ化リン酸リチウムを含有する２５℃のフッ化水素
溶液を１，０００ｋｇ入れた。撹拌機（２）を５ｒｐｍ
で回転させながら３℃／分の速度で温度低下させ、１４
時間掛けて−３０℃まで冷却した。固液分離し、固体を
乾燥させると製品が１０７ｋｇ得られた。このものの遊
離酸は９９ｐｐｍで不溶解残分は０．０７％であった。Example 3 Lithium hexafluorophosphate was produced using the apparatus of Example 3 below. That is, 1,000 kg of a 25 ° C. hydrogen fluoride solution containing lithium hexafluorophosphate was placed in a 1 m 3 stainless steel pressure vessel (1) equipped with a stirrer (2) and a condenser (3). Stirrer (2) 5 rpm
While rotating at a temperature of 3 ℃ / min to reduce the temperature,
It cooled to -30 degreeC over time. Solid-liquid separation was performed, and the solid was dried to obtain 107 kg of a product. The free acid of this product was 99 ppm, and the insoluble residue was 0.07%.
【００２３】[0023]
【実施例４】回転数０〜１０ｒｐｍ可変の撹拌機（２）
付き、直径１ｍ、高さ１．３ｍ、容積１ｍ3のステンレ
ス耐圧容器（１）に、外塔ステンレス製で内部管体は直
径２０ｍｍ、長さ１ｍのカーボンで構成された凝縮器
（３）を設け、耐圧容器（１）とは直径１０ｍｍのＰＦ
Ａパイプで接続する。凝縮器（３）とエジェクター
（４）との間に圧力調整器（５）を取り付ける。耐圧容
器（１）にはマノメーター（６）を取り付ける。エジェ
クターは、エジェクター（４）、水槽（７）及びポンプ
（８）から構成される。[Example 4] A stirrer (2) with a variable rotation speed of 0 to 10 rpm
Attached to a stainless steel pressure vessel (1) with a diameter of 1 m, a height of 1.3 m and a volume of 1 m 3 , a condenser (3) made of outer column stainless steel and having an inner tube body of 20 mm in diameter and 1 m in length made of carbon. Provided with the pressure resistant container (1) and a PF with a diameter of 10 mm
Connect with A pipe. A pressure regulator (5) is attached between the condenser (3) and the ejector (4). A manometer (6) is attached to the pressure vessel (1). The ejector comprises an ejector (4), a water tank (7) and a pump (8).
【図１】図１は本発明装置の一例を示す説明図である。FIG. 1 is an explanatory diagram showing an example of a device of the present invention.
１・・・耐圧反応容器 ２・・・撹拌機 ３・・・凝縮器 ４・・・真空用エジェクター ５・・・圧力調整器 ６・・・マノメーター ７・・・水槽 ８・・・ポンプ 1 ... Pressure resistant reactor 2 ... Stirrer 3 ... Condenser 4 ... Vacuum ejector 5 ... Pressure regulator 6 ... Manometer 7 ... Water tank 8 ... Pump
Claims (5)
ウムを含有する無水フッ化水素酸溶液を、無水フッ化水
素酸の蒸発による蒸発潜熱で該溶液温度を低下させて、
六フッ化リン酸リチウムの結晶を析出させることを特徴
とする六フッ化リン酸リチウムの製造方法。1. An anhydrous hydrofluoric acid solution containing lithium hexafluorophosphate produced by a conventional method is reduced in temperature by the latent heat of vaporization by evaporation of anhydrous hydrofluoric acid,
A method for producing lithium hexafluorophosphate, which comprises depositing crystals of lithium hexafluorophosphate.
拌下に行う請求項１に記載の製造方法。2. The production method according to claim 1, wherein the solution temperature is lowered with stirring.
循環使用する請求項１または２に記載の製造方法。3. Condensing evaporated anhydrous hydrofluoric acid,
The manufacturing method according to claim 1 or 2, which is used in a circulating manner.
要に応じ凝縮器から構成され、該反応容器はステンレス
製又はフッ素樹脂ライニング容器であって、且つ該反応
容器の排気管と真空用エジェクターとを連結し、必要に
応じこれ等の間に凝縮器を設置し、この凝縮器と反応容
器との間に凝縮液を返送するための配管を設けたことを
特徴とする六フッ化リン酸リチウムの製造装置。4. A pressure-resistant reaction container, a vacuum ejector, and, if necessary, a condenser. The reaction container is a stainless steel or fluororesin lining container, and an exhaust pipe of the reaction container and a vacuum ejector are provided. Of the lithium hexafluorophosphate, which is characterized in that a pipe for returning the condensate is provided between the condenser and the reaction vessel. Manufacturing equipment.
に記載の製造装置。5. A pressure-resistant reaction vessel equipped with a stirrer.
3. The manufacturing apparatus according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10626196A JPH09268005A (en) | 1996-04-02 | 1996-04-02 | Production of lithium hexafluorophosphase and apparatus therefor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10626196A JPH09268005A (en) | 1996-04-02 | 1996-04-02 | Production of lithium hexafluorophosphase and apparatus therefor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH09268005A true JPH09268005A (en) | 1997-10-14 |
Family
ID=14429164
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10626196A Pending JPH09268005A (en) | 1996-04-02 | 1996-04-02 | Production of lithium hexafluorophosphase and apparatus therefor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH09268005A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999040027A1 (en) * | 1998-02-03 | 1999-08-12 | Elf Atochem S.A. | METHOD FOR MAKING HEXAFLUOROPHOSPHATE OF A METAL, M(PF6)n, PARTICULARLY OF LiPF6 |
| WO1999062821A1 (en) * | 1998-06-04 | 1999-12-09 | Basf Aktiengesellschaft | METHOD FOR CRYSTALLIZATION OF HIGHLY PURE LiPF6 FROM ORGANIC SOLVENTS |
| WO2009028640A1 (en) | 2007-08-31 | 2009-03-05 | Stella Chemifa Corporation | Method for purifying fluorine compound |
| CN102838103A (en) * | 2012-08-21 | 2012-12-26 | 张家港市亚源高新技术材料有限公司 | Synthesizer for lithium hexafluorophosphate |
| WO2013092986A1 (en) | 2011-12-23 | 2013-06-27 | Lanxess Deutschland Gmbh | Lipf6 solutions |
| WO2013092991A1 (en) | 2011-12-23 | 2013-06-27 | Lanxess Deutschland Gmbh | Lipf6 solutions |
| WO2013092988A1 (en) | 2011-12-23 | 2013-06-27 | Lanxess Deutschland Gmbh | Lipf6 solutions |
| WO2013092990A1 (en) | 2011-12-23 | 2013-06-27 | Lanxess Deutschland Gmbh | Lipf6 solutions |
-
1996
- 1996-04-02 JP JP10626196A patent/JPH09268005A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999040027A1 (en) * | 1998-02-03 | 1999-08-12 | Elf Atochem S.A. | METHOD FOR MAKING HEXAFLUOROPHOSPHATE OF A METAL, M(PF6)n, PARTICULARLY OF LiPF6 |
| WO1999062821A1 (en) * | 1998-06-04 | 1999-12-09 | Basf Aktiengesellschaft | METHOD FOR CRYSTALLIZATION OF HIGHLY PURE LiPF6 FROM ORGANIC SOLVENTS |
| WO2009028640A1 (en) | 2007-08-31 | 2009-03-05 | Stella Chemifa Corporation | Method for purifying fluorine compound |
| US8232436B2 (en) | 2007-08-31 | 2012-07-31 | Stella Chemifa Corporation | Process for purifying a fluorine compound |
| WO2013092986A1 (en) | 2011-12-23 | 2013-06-27 | Lanxess Deutschland Gmbh | Lipf6 solutions |
| WO2013092991A1 (en) | 2011-12-23 | 2013-06-27 | Lanxess Deutschland Gmbh | Lipf6 solutions |
| WO2013092988A1 (en) | 2011-12-23 | 2013-06-27 | Lanxess Deutschland Gmbh | Lipf6 solutions |
| WO2013092990A1 (en) | 2011-12-23 | 2013-06-27 | Lanxess Deutschland Gmbh | Lipf6 solutions |
| JP2015507596A (en) * | 2011-12-23 | 2015-03-12 | ランクセス・ドイチュランド・ゲーエムベーハー | LiPF6 solution |
| CN102838103A (en) * | 2012-08-21 | 2012-12-26 | 张家港市亚源高新技术材料有限公司 | Synthesizer for lithium hexafluorophosphate |
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