JPS5939719A - Manufacture of high purity lithium carbonate - Google Patents
Manufacture of high purity lithium carbonateInfo
- Publication number
- JPS5939719A JPS5939719A JP14766882A JP14766882A JPS5939719A JP S5939719 A JPS5939719 A JP S5939719A JP 14766882 A JP14766882 A JP 14766882A JP 14766882 A JP14766882 A JP 14766882A JP S5939719 A JPS5939719 A JP S5939719A
- Authority
- JP
- Japan
- Prior art keywords
- lithium
- high purity
- lithium carbonate
- perchlorate
- lithium perchlorate
- 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
Abstract
Description
【発明の詳細な説明】
本発明は粗製リチウム化合物よシ高純度の炭酸リチウム
を製造する方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing high purity lithium carbonate from a crude lithium compound.
高純度の炭酸リチウムは近年電子工業材料、光工業材料
としての需要が増大している。これらの材料に使用され
る炭酸リチウムは極めて純度の高いものが要求され、従
来の再結晶あるいは再沈澱法などによる高純度の炭酸リ
チウムの製造法は、極めて手数がかかるだけでなく歩留
りも悪いので、精製にはかなりの経費が必要であった。Demand for high-purity lithium carbonate as a material for electronic and optical industries has increased in recent years. The lithium carbonate used in these materials requires extremely high purity, and conventional methods of producing high-purity lithium carbonate, such as recrystallization or reprecipitation, are not only extremely time-consuming but also have low yields. , Refining required considerable expense.
本発明は粗製リチウム化合物中に含まれる不純物を簡単
かつ効率よく除去し、高純度の炭酸リチウムを製造する
方法を提供するもので、粗製リチウム化合物を過塩素酸
水溶液に溶解し、この溶液を濃縮冷却または単に冷却し
て過塩素酸す１クムの結晶を晶出させて単離した後、水
およびまたは有機溶剤を用いて再結晶させ、次いでこの
結晶を声媒の中でアンモニア性塩基性下で、二酸化炭素
と反応させることから成る。The present invention provides a method for easily and efficiently removing impurities contained in a crude lithium compound and producing high-purity lithium carbonate. Crystals of 1 cum perchlorate are crystallized and isolated by cooling or simply cooling, then recrystallized using water and/or organic solvents, and the crystals are then crystallized in a vocal medium under ammoniacal base. It consists of reacting with carbon dioxide.
本発明の製造法は過塩素酸リチウムの特異の性質を利用
し、リチウムの精製を過塩素酸リチウムの段階で行うこ
とを特徴とし、十分精製したｙＦＩＩｉ塩素酸リチウム
を用いて常法によりアンモニア塩基性の下で、二酸化炭
素と反応させて高純度の炭酸リチウムを得るものである
。The production method of the present invention is characterized by utilizing the unique properties of lithium perchlorate and purifying lithium at the stage of lithium perchlorate. Highly purified lithium carbonate is obtained by reacting with carbon dioxide under the same conditions.
本発明で使用する粗製リチウム化合物としては例えば炭
酸リチクム、水酸化リチウム３、塩化リチウムなどの工
業用リチウム化合物であるが、一般には工業用炭酸リチ
ウムが用いられる。The crude lithium compound used in the present invention includes, for example, industrial lithium compounds such as lithium carbonate, lithium 3 hydroxide, and lithium chloride, but industrial lithium carbonate is generally used.
工業用炭酸リチウムを用いた場合の高純度炭酸リチウム
の製造法について説明すると、市販の工業用炭酸リチウ
ムは通常炭酸リチウムとして９９−以上を含有するが、
不純物として微量のカリウム、ナトリウム、マグネシウ
ム、鉄、カルシウムなどの塩類も含まれている。この粗
製炭酸リチウムから高純度の炭酸リチウムを得るには、
まず仁れを例えば１喚用の６０１％の過塩素酸に溶解さ
せて過塩素酸リチウムにする。過塩素酸リチウムの水に
対する溶解度は大きくもなく、また小さくも欺く中程度
であるので再結晶、精製の目的には好／
都合であり、一般の過塩素酸塩類はアルカリ土金属塩類
をけじめとして水に対する溶解度が大きいので極めて好
都合に精製することができる。過塩素酸リチウムを含有
する水溶液を冷却または濃縮冷却すると過塩素酸リチウ
ムは三水塩の形で比較的大きな取扱い容易な結晶として
析出する。これｔＦ別し、水洗、脱水すればかなり純度
の高い過塩素酸リチウムが得られる。ζうして得られた
過塩素酸リチウムを純水を用いて再結晶を繰返して行な
えば、更に純度の高い過塩素酸リチウムの三水塩が得ら
れる。また過塩素酸リチウムは他の過塩素酸金属塩と異
なり、有機溶剤、特にエーテルに対する溶解度が特異的
に大きいので、精製された三水塩を例えばエチルエーテ
ルに加えれば、過塩素酸リチウムはエーテル層に移り、
他の不純物を水層に残し分離精製することができる。To explain the method for producing high-purity lithium carbonate using industrial lithium carbonate, commercially available industrial lithium carbonate usually contains 99 or more as lithium carbonate,
It also contains trace amounts of salts such as potassium, sodium, magnesium, iron, and calcium as impurities. To obtain high purity lithium carbonate from this crude lithium carbonate,
First, the kernels are dissolved in, for example, 601% perchloric acid to make lithium perchlorate. The solubility of lithium perchlorate in water is neither large nor deceptively small, so it is favorable/convenient for the purpose of recrystallization and purification, and general perchlorates are superior to alkaline earth metal salts. Due to its high solubility in water, it can be purified very conveniently. When an aqueous solution containing lithium perchlorate is cooled or concentrated and cooled, lithium perchlorate precipitates in the form of trihydrate as relatively large crystals that are easy to handle. If this is separated by tF, washed with water, and dehydrated, lithium perchlorate of considerably high purity can be obtained. ζ If the thus obtained lithium perchlorate is repeatedly recrystallized using pure water, a trihydrate of lithium perchlorate with even higher purity can be obtained. Also, unlike other metal perchlorates, lithium perchlorate has a uniquely high solubility in organic solvents, especially ether, so if purified trihydrate is added to ethyl ether, for example, lithium perchlorate will dissolve into ether. Moving on to the layers,
Other impurities can be left in the aqueous layer for separation and purification.
これよシ高純度炭酸リチウムを得るには、かくして精製
された過塩素酸リチウムを純水に溶解し、アンモニアを
加えて塩基性とし、二酸化炭素を吹き込んで炭酸リチウ
ムを沈澱させる。この際加温すると沈澱の生成を容易に
することができる。使昂スるアンモ＝１および二酸化炭
素はできるだけグ
高純度のものが必要であり、アンモニアはガス状のもの
を用いるのが好ま１−＜、二酸化炭素もガス状のものが
望ましい。得られた結晶は水洗、脱水、乾燥して高純度
炭酸リチウムとする。In order to obtain highly purified lithium carbonate, the thus purified lithium perchlorate is dissolved in pure water, ammonia is added to make it basic, and carbon dioxide is blown in to precipitate lithium carbonate. At this time, heating can facilitate the formation of a precipitate. The ammonia and carbon dioxide to be used need to be as highly purified as possible; ammonia is preferably gaseous, and carbon dioxide is also preferably gaseous. The obtained crystals are washed with water, dehydrated, and dried to obtain high purity lithium carbonate.
次に本発明を実施例によシ説明するが、その主旨はこれ
らの例にのみ限定されるものではない。Next, the present invention will be explained with reference to examples, but the gist thereof is not limited only to these examples.
なお実施例中、部は重量部を表わす。In the examples, parts represent parts by weight.
実施例１
工業用炭酸リチウム７５部を水６５０部の中に入れて攪
拌し、これに６０％工業用過塩素酸３２０部を徐々に加
えた。加え終り九ら約１５分間そのｔま攪拌した後、濾
過した。Ｆ液を約４になるまで濃縮し放冷すると過塩素
酸リチウムの三水塩が析出した。これを濾過して水洗し
、遠心分離器で脱水すると２２０部の過塩素酸リチウム
の三水塩が得られ、収率は６Ｂ、８％であった。この結
晶を再び１５０部の純水に入れ攪拌溶解した後、濃縮、
冷却し更に高純度の過塩素酸リチウムを得た。Example 1 75 parts of industrial lithium carbonate were stirred in 650 parts of water, and 320 parts of 60% industrial perchloric acid was gradually added thereto. After the addition was complete, the mixture was stirred for about 15 minutes and then filtered. When the F solution was concentrated to a concentration of about 4 and allowed to cool, trihydrate of lithium perchlorate was precipitated. This was filtered, washed with water, and dehydrated using a centrifuge to obtain 220 parts of lithium perchlorate trihydrate, with a yield of 6B and 8%. The crystals were again put into 150 parts of pure water, stirred and dissolved, and then concentrated.
After cooling, highly purified lithium perchlorate was obtained.
実施例２
工業用炭酸リチウム７５部を水６５０部の中に入れて攪
拌し、これに７０％工業用過塩素酸２６５で濃縮し放冷
すると過塩素酸リチウム三水塩の結晶が析出した。これ
を濾過し、遠心分離器で脱水すると２５０部の過塩素酸
リチウム三水塩が得られ。Example 2 75 parts of industrial lithium carbonate were stirred in 650 parts of water, concentrated with 70% industrial perchloric acid 265, and allowed to cool to precipitate crystals of lithium perchlorate trihydrate. This was filtered and dehydrated using a centrifuge to obtain 250 parts of lithium perchlorate trihydrate.
収率は７ａ１チであった。The yield was 7a1.
これに１０部の純水と３００部のエチルエーテルを加え
、よく振盪してから静置した後、エーテル部を分離し、
減圧でエーテルを除去した。減圧し九デシケータ−の中
で乾燥すると過塩素酸リチウム１４５部が得られた。こ
れを更に純水１５０部の中に投じ、再結晶し高純度の過
塩素酸リチウム三水塩を得た。Add 10 parts of pure water and 300 parts of ethyl ether to this, shake well and leave to stand, then separate the ether part,
Ether was removed under reduced pressure. After drying in a vacuum desiccator, 145 parts of lithium perchlorate was obtained. This was further poured into 150 parts of pure water and recrystallized to obtain highly pure lithium perchlorate trihydrate.
実施例３
実施例１および２の方法で得られた十分に精製された過
塩素酸リチウム三水塩１６０部を純水１６０部と共に容
器に入れ攪拌して溶解し、アンモニアガスを吹込み１次
に二酸化炭素ガスを吹込みながら反応させると炭酸リチ
ウムが沈澱した。計算量のアンモニアガスおよび二酸化
炭素ガスを吹込んだ後、加熱し８０Ｃで一時間更にアン
モニアガスおよび二酸化炭素ガスを吹込んで反応を続け
た。反応液を冷却後、炭酸リチウムを分離し、水洗、乾
燥して高純度炭酸リチウムを得た。収量は６５部、収率
は８８％であった。Example 3 160 parts of sufficiently purified lithium perchlorate trihydrate obtained by the method of Examples 1 and 2 was put into a container with 160 parts of pure water, stirred and dissolved, and ammonia gas was blown into the primary solution. When reacting while blowing carbon dioxide gas into the solution, lithium carbonate precipitated. After blowing in calculated amounts of ammonia gas and carbon dioxide gas, the reaction was continued by heating and blowing in ammonia gas and carbon dioxide gas for one hour at 80C. After cooling the reaction solution, lithium carbonate was separated, washed with water, and dried to obtain high purity lithium carbonate. The yield was 65 parts, or 88%.
含有される不純物の量は次表のごとくであった。The amount of impurities contained was as shown in the following table.
なお表中の数値は騨、ＮＤは検出せずの意味を表わす。In addition, the numerical values in the table represent the value of 0, and ND represents not detected.
また高純度炭酸リチウム（１）および（２）は、それぞ
れ実施例１の方法および実施例２の方法で得られた過塩
素酸リチウムを用いて製造したものである。Further, high purity lithium carbonate (1) and (2) were produced using lithium perchlorate obtained by the method of Example 1 and the method of Example 2, respectively.
Claims (1)
いて再結晶させ、次いでこの結晶を溶媒の中でアンモニ
ア性塩基性下で、二酸化炭素と反応させることを特徴と
する高純度炭酸リチウムの製造法。High purity carbonic acid characterized by crystallizing and isolating it, recrystallizing it using water and/or an organic solvent, and then reacting the crystals with carbon dioxide in a solvent under ammoniacal basicity. Lithium production method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14766882A JPS5939719A (en) | 1982-08-27 | 1982-08-27 | Manufacture of high purity lithium carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14766882A JPS5939719A (en) | 1982-08-27 | 1982-08-27 | Manufacture of high purity lithium carbonate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS5939719A true JPS5939719A (en) | 1984-03-05 |
Family
ID=15435565
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14766882A Pending JPS5939719A (en) | 1982-08-27 | 1982-08-27 | Manufacture of high purity lithium carbonate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5939719A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62252315A (en) * | 1986-04-23 | 1987-11-04 | Nippon Chem Ind Co Ltd:The | High-purity lithium carbonate and production thereof |
| WO1993012034A1 (en) * | 1991-12-12 | 1993-06-24 | Olin Corporation | Process for producing lithium perchlorate |
| KR100725589B1 (en) | 2006-04-19 | 2007-06-08 | 한밭대학교 산학협력단 | Preparation of lithium hydroxide monohydrate from spent lithium carbonate |
| JP2008261339A (en) * | 1996-06-18 | 2008-10-30 | 3M Co | Installation mat and contamination inhibition device |
| CN102139861A (en) * | 2011-05-10 | 2011-08-03 | 湖北百杰瑞新材料有限公司 | Method for producing anhydrous lithium perchlorate |
| JP2012116681A (en) * | 2010-11-30 | 2012-06-21 | Nittetsu Mining Co Ltd | Method for producing lithium carbonate |
| KR101179505B1 (en) | 2010-12-14 | 2012-09-07 | 서강대학교산학협력단 | Preparation of Lithium Hydroxide Monohydrate from Lithium Carbonate |
| US8394333B2 (en) | 2008-12-10 | 2013-03-12 | Nichias Corporation | Holding material for catalytic converter, method for producing the same, and catalytic converter |
| JP2013193940A (en) * | 2012-03-22 | 2013-09-30 | Nittetsu Mining Co Ltd | Method of producing lithium carbonate |
| CN103449481A (en) * | 2012-05-29 | 2013-12-18 | 日铁矿业株式会社 | Preparation method of lithium carbonate |
-
1982
- 1982-08-27 JP JP14766882A patent/JPS5939719A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62252315A (en) * | 1986-04-23 | 1987-11-04 | Nippon Chem Ind Co Ltd:The | High-purity lithium carbonate and production thereof |
| JPH0449489B2 (en) * | 1986-04-23 | 1992-08-11 | Nippon Chemical Ind | |
| WO1993012034A1 (en) * | 1991-12-12 | 1993-06-24 | Olin Corporation | Process for producing lithium perchlorate |
| JP2008261339A (en) * | 1996-06-18 | 2008-10-30 | 3M Co | Installation mat and contamination inhibition device |
| KR100725589B1 (en) | 2006-04-19 | 2007-06-08 | 한밭대학교 산학협력단 | Preparation of lithium hydroxide monohydrate from spent lithium carbonate |
| US8394333B2 (en) | 2008-12-10 | 2013-03-12 | Nichias Corporation | Holding material for catalytic converter, method for producing the same, and catalytic converter |
| JP2012116681A (en) * | 2010-11-30 | 2012-06-21 | Nittetsu Mining Co Ltd | Method for producing lithium carbonate |
| US8920763B2 (en) | 2010-11-30 | 2014-12-30 | Nittetsu Mining Co., Ltd. | Method for producing lithium carbonate |
| KR101179505B1 (en) | 2010-12-14 | 2012-09-07 | 서강대학교산학협력단 | Preparation of Lithium Hydroxide Monohydrate from Lithium Carbonate |
| CN102139861A (en) * | 2011-05-10 | 2011-08-03 | 湖北百杰瑞新材料有限公司 | Method for producing anhydrous lithium perchlorate |
| JP2013193940A (en) * | 2012-03-22 | 2013-09-30 | Nittetsu Mining Co Ltd | Method of producing lithium carbonate |
| US9255011B2 (en) | 2012-03-22 | 2016-02-09 | Nittetsu Mining Co., Ltd. | Method for producing lithium carbonate |
| CN103449481A (en) * | 2012-05-29 | 2013-12-18 | 日铁矿业株式会社 | Preparation method of lithium carbonate |
| CN103449481B (en) * | 2012-05-29 | 2016-08-24 | 日铁矿业株式会社 | The method preparing lithium carbonate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JPS5939719A (en) | Manufacture of high purity lithium carbonate | |
| EP1215209A1 (en) | Method for the production of a crystalline epoxide | |
| US3448119A (en) | Producing tetramethylisoindolenine by heating acetonylacetone in aqueous ammonium salt | |
| US4906778A (en) | Process for the production of aminoguanidine bicarbonate | |
| JP2598703B2 (en) | Method for producing butyl 3 '-(1H-tetrazol-5-yl) oxanilate | |
| US5349074A (en) | Process for pharmaceutical grade high purity hyodeoxycholic acid preparation | |
| US2400934A (en) | Amines and purification thereof | |
| US3023210A (en) | Production of carboxy-substituted heterocyclic compounds | |
| JP2799373B2 (en) | Method for producing sodium azide | |
| US4260837A (en) | Recrystallization of hexsanitrostilbene from nitric acid and water | |
| JPH07278156A (en) | Preparation of dimethylamine - borane | |
| US4211883A (en) | Process for the production of p-(N-methyl)-aminobenzoyl-L-glutamic acid | |
| US4418016A (en) | Method for recovering omega-amino-dodecanoic acid from crystallization mother liquors | |
| JPS588028A (en) | Separation of dipentaerythritol | |
| JPH0468301B2 (en) | ||
| EP0552912A2 (en) | Method for producing 2,6-dihydroxybenzoic acid | |
| JPH10316646A (en) | Production of high-purity crystalline o-methyliso urea acetate and crystalline o-methylisourea acetate obtained by the same | |
| CA2006665C (en) | Process for purification of 1,2-bis (nicotinamido) propane | |
| JP2815438B2 (en) | Purification method of 1,2-bis (nicotinamide) propane | |
| JP2000211905A (en) | Production of aqueous solution of free hydroxylamine | |
| US2993051A (en) | Process for making nicotinamide | |
| JPH05170757A (en) | Production of tocopherol ester | |
| JP2002371061A (en) | Method for treating 1-chlorocarbonylpiperidine derivative hydrochloric acid salt | |
| JPH0264009A (en) | Production of cyanamide | |
| JPH0720926B2 (en) | Method for producing cysteamine hydrochloride |