JPH0791060B2 - Synthesis method of Li 2) SnO 2) - Google Patents
Synthesis method of Li 2) SnO 2)Info
- Publication number
- JPH0791060B2 JPH0791060B2 JP25652186A JP25652186A JPH0791060B2 JP H0791060 B2 JPH0791060 B2 JP H0791060B2 JP 25652186 A JP25652186 A JP 25652186A JP 25652186 A JP25652186 A JP 25652186A JP H0791060 B2 JPH0791060 B2 JP H0791060B2
- Authority
- JP
- Japan
- Prior art keywords
- aqueous solution
- sno
- lithium hydroxide
- mixing
- tin salt
- 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.)
- Expired - Lifetime
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- Inorganic Compounds Of Heavy Metals (AREA)
Description
【発明の詳細な説明】 （産業上の利用分野） この発明は、Li2SnO3の合成方法に関する。TECHNICAL FIELD The present invention relates to a method for synthesizing Li 2 SnO 3 .
（従来の技術） Li2SnO3はイオン導電材、減速材として利用されている
ことが知られている。(Prior Art) It is known that Li 2 SnO 3 is used as an ion conductive material and a moderator.
このLi2SnO3の合成方法には、水溶液共沈法、あるいは
固相反応法が知られている。As a method for synthesizing this Li 2 SnO 3 , an aqueous solution coprecipitation method or a solid phase reaction method is known.
（従来技術の問題点） このうち、前者の水溶液共沈法は、NaOHでアルカリ性と
し、両者の水酸化物の共沈体を得る方法であるが、NaOH
を使用するため不純物の混入がみられ、純度の高いLi2S
nO3が得られない。そのため減速材、イオン導電材ある
いはブランケット材などとしての利用ができないという
欠点がある。(Problems of the prior art) Among them, the former aqueous solution coprecipitation method is a method of making alkaline with NaOH to obtain a coprecipitate of both hydroxides.
Since impurities are mixed in, the high purity Li 2 S
I can't get nO 3 . Therefore, it has a drawback that it cannot be used as a moderator, an ion conductive material, a blanket material, or the like.
また、後者の固相反応法は、Liの酸化物あるいは炭酸物
などと、Snの酸化物とを所定の混合割合に配合し、これ
を混合したものを熱処理して合成しているが、Liの活性
が強く、高温の熱処理でリチウムの揮発が生じるため組
成が一定せず、また活性の高い遊離リチウムによって白
金などのルツボが腐食されてしまい、高純度のものが合
成できないだけでなく、製造コスト高となる欠点があ
る。In the latter solid-phase reaction method, Li oxide or carbonate is mixed with Sn oxide at a predetermined mixing ratio, and the mixture is heat treated to synthesize Li. Is highly active, and the composition of lithium is volatilized by heat treatment at high temperature, and the highly active free lithium corrodes crucibles such as platinum. There is a drawback that the cost is high.
（発明の目的） したがって、この発明はLi2SnO3が容易に得られるの合
成方法を提供することを目的とする。(Object of the Invention) Accordingly, the object of the present invention is to provide a synthetic method by which Li 2 SnO 3 can be easily obtained.
（発明の概要） この発明にかかるLi2SnO3の合成方法は、 スズ塩の水溶液と水酸化リチウムの水溶液とを混合する
工程と、 前記混合溶液よりLi2Sn（OH）６の沈殿物を得る工程
と、 前記Li2Sn（OH）６を熱処理してLi2SnO3を得る工程と、 からなる。(Summary of the Invention) A method for synthesizing Li 2 SnO 3 according to the present invention comprises a step of mixing an aqueous solution of a tin salt and an aqueous solution of lithium hydroxide, and a step of preparing a Li 2 Sn (OH) 6 precipitate from the mixed solution. And a step of heat-treating the Li 2 Sn (OH) 6 to obtain Li 2 SnO 3 .
また、スズ塩の水溶液と水酸化リチウムの水溶液とを混
合する工程は、スズ塩の水溶液に水酸化リチウムの水溶
液を加えることによって実施することができる。Further, the step of mixing the aqueous solution of tin salt and the aqueous solution of lithium hydroxide can be carried out by adding the aqueous solution of lithium hydroxide to the aqueous solution of tin salt.
さらに、スズ塩の水溶液と水酸化リチウムの水溶液とを
混合する工程は、水酸化リチウムの水溶液にスズ塩の水
溶液を加えることによっても実施することができる。Further, the step of mixing the aqueous solution of tin salt and the aqueous solution of lithium hydroxide can also be carried out by adding the aqueous solution of tin salt to the aqueous solution of lithium hydroxide.
ここで、スズ塩の水溶液と水酸化リチウムの水溶液とを
混合する工程はpHが11.5以上の条件で処理することが好
ましい。これは、pHが11.5未満ではLi2Sn（OH）６が得
られないからである。Here, in the step of mixing the tin salt aqueous solution and the lithium hydroxide aqueous solution, it is preferable to perform the treatment at a pH of 11.5 or higher. This is because if the pH is less than 11.5, Li 2 Sn (OH) 6 cannot be obtained.
（実施例） 以下、この発明を実施例にもとづいて詳細に説明する。(Examples) Hereinafter, the present invention will be described in detail based on Examples.
実施例1. 塩化スズ（SnCl4）の水溶液:0.1mol/を準備し、これ
に水酸化リチウム（LiOH）の水溶液:2mol/をpHが12.0
になるように加えて静置した。この段階で上澄み液を除
去してLi2Sn（OH）６を得た。Example 1. An aqueous solution of tin chloride (SnCl 4 ): 0.1 mol / was prepared, and an aqueous solution of lithium hydroxide (LiOH): 2 mol / was added to the solution at a pH of 12.0.
And left to stand. At this stage, the supernatant was removed to obtain Li 2 Sn (OH) 6 .
次いで、Li2Sn（OH）６を空気中650℃の温度で４時間熱
処理した。Then, Li 2 Sn (OH) 6 was heat-treated in air at a temperature of 650 ° C. for 4 hours.
得られた生成物は分析の結果Li2SnO3であった。The obtained product was Li 2 SnO 3 as a result of analysis.
なお、この実施例のように、塩化スズの水溶液と水酸化
リチウムの水溶液とを混合する工程を、塩化スズの水溶
液に水酸化リチウムの水溶液を加えることによって実施
した場合、上澄み液を除去してLi2Sn（OH）６を得る段
階で、結晶の成長がみられるが、たとえば、メタノール
を加えることが好ましい。As in this example, when the step of mixing the tin chloride aqueous solution and the lithium hydroxide aqueous solution is carried out by adding the lithium hydroxide aqueous solution to the tin chloride aqueous solution, the supernatant liquid is removed. Crystal growth is observed at the stage of obtaining Li 2 Sn (OH) 6 , but it is preferable to add methanol, for example.
実施例2. 水酸化リチウム（LiOH）の水溶液:2mol/を準備し、こ
れに塩化スズ（SnCl4）の水溶液:0.1mol/にpHが12.0
になるように加えてを静置した。Example 2. An aqueous solution of lithium hydroxide (LiOH): 2 mol / was prepared, and an aqueous solution of tin chloride (SnCl 4 ): 0.1 mol / had a pH of 12.0.
In addition, it was left to stand.
この段階で上澄み液を除去してLi2Sn（OH）６を得た。At this stage, the supernatant was removed to obtain Li 2 Sn (OH) 6 .
次いで、Li2Sn（OH）６を空気中650℃の温度で４時間熱
処理した。Then, Li 2 Sn (OH) 6 was heat-treated in air at a temperature of 650 ° C. for 4 hours.
得られた生成物は分析の結果Li2SnO3であった。The obtained product was Li 2 SnO 3 as a result of analysis.
なお、この実施例のように、塩化スズの水溶液と水酸化
リチウムの水溶液とを混合する工程を、塩化スズの水溶
液に水酸化リチウムの水溶液を加えることによって実施
した場合、上澄み液を除去してLi2Sn（OH）６を得る段
階で、結晶の成長がみられるが、たとえば、メタノール
を加えることが好ましい。As in this example, when the step of mixing the tin chloride aqueous solution and the lithium hydroxide aqueous solution is carried out by adding the lithium hydroxide aqueous solution to the tin chloride aqueous solution, the supernatant liquid is removed. Crystal growth is observed at the stage of obtaining Li 2 Sn (OH) 6 , but it is preferable to add methanol, for example.
Li2SnO3そのものを減速材、ブランケット材に使用する
ときは、たとえば、トリチウムが入りやすく、またトリ
チウムが取り出しやすいものがよいので、多孔質の焼結
体が適している。上記した方法で合成した粉体を用いれ
ば多孔質のものが得られやすく、したがって、この発明
方法で得られるLi2SnO3はこのような用途に適したもの
である。また、イオン導電体として使用する際には、他
種イオンのドープが水溶液中で行ない得ることなどか
ら、合成操作の簡略化も図り得るという利点がある。When Li 2 SnO 3 itself is used as a moderator or a blanket material, a porous sintered body is suitable because, for example, it is preferable that tritium can easily enter and tritium can be easily taken out. If the powder synthesized by the above-mentioned method is used, a porous material can be easily obtained. Therefore, Li 2 SnO 3 obtained by the method of the present invention is suitable for such use. Further, when it is used as an ionic conductor, it is possible to dope other species of ions in an aqueous solution, which is advantageous in that the synthetic operation can be simplified.
上記した実施例の他、Li2SnO3のうちSnをAl、Mo、Ｗに
置き換えた化合物の合成についても、この発明方法を適
用することができる。In addition to the examples described above, the method of the present invention can also be applied to the synthesis of compounds in which Sn is replaced by Al, Mo, and W in Li 2 SnO 3 .
（効果） 以上、この発明方法によれば、スズ塩との合成段階で、
NaOHを使用せずに、水酸化リチウムを用いててるため、
不純物の混入がなく、純粋なLi2SnO3が得られるため、
減速材、イオン導電材、ブランケット材などの用途に有
用な方法である。(Effect) As described above, according to the method of the present invention, in the synthesis step with the tin salt,
Because it uses lithium hydroxide without using NaOH,
Since pure Li 2 SnO 3 can be obtained without mixing impurities,
It is a useful method for applications such as moderators, ion conductive materials, and blanket materials.
また、Li2SnO3の焼結体を得るために、Li2Sn（OH）６を
熱処理するが、錯体の形で存在するLi2Sn（OH）６の沈
殿物を熱処理するため、Liの活性そのものが低く、白金
ルツボを腐食する恐れもなく、組成も安定して合成でき
るという効果も有する。Moreover, in order to obtain a sintered body of Li 2 SnO 3 , Li 2 Sn (OH) 6 is heat-treated, but since the precipitate of Li 2 Sn (OH) 6 existing in the form of a complex is heat-treated, The activity itself is low, there is no fear of corroding the platinum crucible, and the composition can be stably synthesized.
Claims (4)
とを混合する工程と、 前記混合溶液よりLi2Sn（OH）６の沈殿物を得る工程
と、 前記Li2Sn（OH）６を熱処理してLi2SnO3を得る工程と、 からなるLi2SnO3の合成方法。1. A step of mixing an aqueous solution of a tin salt and an aqueous solution of lithium hydroxide, a step of obtaining a Li 2 Sn (OH) 6 precipitate from the mixed solution, and a step of obtaining the Li 2 Sn (OH) 6 A step of obtaining Li 2 SnO 3 by heat treatment, and a method of synthesizing Li 2 SnO 3 comprising :
溶液とを混合する工程は、 スズ塩の水溶液に水酸化リチウムの水溶液を加えること
からなる、 特許請求の範囲第（１）項記載のLi2SnO3の合成方法。2. The step of mixing the aqueous solution of tin salt and the aqueous solution of lithium hydroxide comprises adding an aqueous solution of lithium hydroxide to the aqueous solution of tin salt. Li 2 SnO 3 synthesis method.
溶液とを混合する工程は、 水酸化リチウムの水溶液にスズ塩の水溶液を加えること
からなる、 特許請求の範囲第（１）項記載のLi2SnO3の合成方法。3. The method of mixing an aqueous solution of tin salt and an aqueous solution of lithium hydroxide comprises adding an aqueous solution of tin salt to an aqueous solution of lithium hydroxide. Li 2 SnO 3 synthesis method.
溶液とを混合する工程はpHが11.5以上の条件で処理され
る、 特許請求の範囲第（１）項ないし（３）項のいずれか一
項に記載のLi2SnO3の合成方法。4. The step of mixing the aqueous solution of tin salt and the aqueous solution of lithium hydroxide is carried out under the condition of pH of 11.5 or higher. The method for synthesizing Li 2 SnO 3 described in the item 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25652186A JPH0791060B2 (en) | 1986-10-28 | 1986-10-28 | Synthesis method of Li 2) SnO 2) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25652186A JPH0791060B2 (en) | 1986-10-28 | 1986-10-28 | Synthesis method of Li 2) SnO 2) |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63112422A JPS63112422A (en) | 1988-05-17 |
| JPH0791060B2 true JPH0791060B2 (en) | 1995-10-04 |
Family
ID=17293782
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP25652186A Expired - Lifetime JPH0791060B2 (en) | 1986-10-28 | 1986-10-28 | Synthesis method of Li 2) SnO 2) |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0791060B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103153866A (en) * | 2010-08-11 | 2013-06-12 | 伏太斯有限责任公司 | Synthesis of stannane and deuterostannane |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2715651B1 (en) * | 1994-01-28 | 1996-03-01 | Commissariat Energie Atomique | Tritogenic ceramic material containing lithium and its preparation process. |
| CN102420319A (en) * | 2011-11-17 | 2012-04-18 | 西北工业大学 | Preparation method for lithium ion battery cathode material lithium stannate |
| CN110180526B (en) * | 2019-05-10 | 2022-03-25 | 重庆第二师范学院 | Photocatalyst Li2SnO3The preparation method and the application thereof in degrading antibiotics |
-
1986
- 1986-10-28 JP JP25652186A patent/JPH0791060B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103153866A (en) * | 2010-08-11 | 2013-06-12 | 伏太斯有限责任公司 | Synthesis of stannane and deuterostannane |
| TWI547440B (en) * | 2010-08-11 | 2016-09-01 | 液態空氣喬治斯克勞帝方法研究開發股份有限公司 | Synthesis of stannane and deuterostannane |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63112422A (en) | 1988-05-17 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |