JP2019510728A - Reuse method of lithium manganate dust - Google Patents
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Abstract
マンガン酸リチウム粉塵、焼結助剤、酸素雰囲気改善剤を脱イオン水に分散させた後、ポリビニルアルコール溶液を加え、次いで噴霧造粒し、焼成して製品を得るマンガン酸リチウム粉塵の再利用方法を提供する。マンガン酸リチウム粉塵に酸素雰囲気改善剤を添加することにより、高温反応時のマンガン酸リチウム材料の酸素空孔の発生が効果的に抑制され、一部の構造的欠陥が修復され、電気化学的性能が改善及び向上される。また、造粒プロセスにより、結晶粒子の成長程度が制御可能となり、結晶凝集体又は二次粒子の形態が球状になる傾向があり、処理された製品のタップ密度が大幅に向上し、加工特性が改善される。 After dispersing lithium manganate dust, sintering aid, and oxygen atmosphere improver in deionized water, add polyvinyl alcohol solution, spray granulate, and calcinate to obtain a product. I will provide a. By adding an oxygen atmosphere improver to lithium manganate dust, the generation of oxygen vacancies in the lithium manganate material at the time of high temperature reaction is effectively suppressed, and some structural defects are repaired, and the electrochemical performance is improved. Is improved and improved. In addition, the granulation process makes it possible to control the degree of growth of crystal particles, the shape of crystal aggregates or secondary particles tends to be spherical, the tap density of the treated product is significantly improved, and the processing characteristics are improved. Be improved.
Description
本発明は、新エネルギー材料製造の技術分野に属し、特にマンガン酸リチウム粉塵の再利用方法に関する。 The present invention belongs to the technical field of new energy material production, and in particular relates to a method for recycling lithium manganate dust.
リチウムイオン電池用正極材料であるマンガン・リチウムの生産過程において、使用の需要を満たすために、高温で焼成反応した後に材料粒子を加工する必要があるので、一般的には気流粉砕又は機械的破砕が用いられている。しかし、このような過程において、多くのマンガン酸リチウム粉塵が発生する。また、この粉塵は、サイズが小さく且つほとんど表面又は構造が損傷した粒子であるので、リチウム電池の充放電時に電解質と反応を起こしやすく、電池特性に悪影響をもたらすので、廃棄される場合が多い。このような粉塵は、特性に対する要求が低い分野に使用されても、製品の粒子径が小さいので、スラリー調製・塗布の作業を行うのが困難であり、実際には市場がない。このような問題により、材料の総合的な利用率が低下するだけでなく、生産コスト、在庫コスト及び処理コストが増加している。 In the production process of manganese and lithium which are positive electrode materials for lithium ion batteries, in order to meet the demand for use, it is necessary to process the material particles after firing reaction at high temperature, so generally it is necessary to use air flow grinding or mechanical crushing. Is used. However, in such a process, a large amount of lithium manganate dust is generated. In addition, since the dust is a particle having a small size and most of the surface or structure is damaged, it tends to react with the electrolyte during charge and discharge of the lithium battery, which adversely affects the battery characteristics and is often discarded. Even if such dust is used in fields where the requirements for properties are low, it is difficult to carry out the task of slurry preparation and application because the particle size of the product is small, and there is practically no market. These problems not only reduce the overall utilization of the material, but also increase production costs, inventory costs and processing costs.
マンガン酸リチウム粉塵の利用率を高めるために、通常、これらの粉塵粒子を再焼結し、焼結助剤を添加することで粒子を結晶凝集体に成長させることにより粒度指標を満足する。しかし、処理する時に依然として多くの問題が存在する。即ち、（１）成長時に粒度が制御されにくく、タップ密度が低すぎ、加工特性が劣り；（２）高温反応により材料の分子構造に「酸素空孔」が発生し、電気化学的特性が劣化し；（３）処理された材料が低価格デジタル製品のみに用いられることができ、付加価値が低い。 In order to increase the utilization rate of lithium manganate dust, usually, these dust particles are re-sintered, and a sintering aid is added to grow the particles into crystal aggregates, thereby satisfying the particle size index. However, there are still many problems in processing. That is, (1) the particle size is difficult to control during growth, the tap density is too low, and the processing characteristics are inferior; (2) "oxygen vacancies" are generated in the molecular structure of the material due to high temperature reaction, and the electrochemical characteristics deteriorate (3) The processed material can be used only for low cost digital products and has low added value.
上記の問題を鑑みて、本発明者は、産業上の利用価値をより有するマンガン酸リチウム粉塵の再利用方法を開発するために、積極的に研究を行っていた。 In view of the above problems, the present inventor has been actively conducting research to develop a method of reusing lithium manganate dust having more industrial utility value.
上記問題を解決するために、本発明は、マンガン酸リチウム粉塵の再利用方法を提供することにより、高温反応によるマンガン酸リチウム材料の酸素空孔の発生を効果的に抑制し、電気化学的特性を向上できるとともに、結晶粒子の成長程度を制御し、処理された製品のタップ密度を増大させ、加工特性を向上できることを目的とする。 In order to solve the above problems, the present invention provides a method for recycling lithium manganate dust to effectively suppress the generation of oxygen vacancies in lithium manganate materials due to high temperature reaction, thereby achieving electrochemical characteristics. It is an object of the present invention to improve the processing characteristics by controlling the growth degree of crystal grains, increasing the tap density of the processed product, and improving the processing characteristics.
本発明が提供するマンガン酸リチウム粉塵の再利用方法は、以下のステップＳ１〜Ｓ４を含み、
ステップＳ１において、脱イオン水に、マンガン酸リチウム粉塵と、焼結助剤と、酸素雰囲気改善剤とを質量比２５０：１：２５で加え、十分に均一に分散させ、ここで、脱イオン水とマンガン酸リチウム粉塵との質量比は１：２であり、焼結助剤はホウ酸であり、酸素雰囲気改善剤は炭酸リチウムと電解二酸化マンガンとを混合してなるものであり、
ステップＳ２において、ステップＳ１で得られた分散液に、固形分含有量が１０％のポリビニルアルコール溶液を加え、均一に撹拌し、ここで、ポリビニルアルコール溶液とマンガン酸リチウム粉塵との質量比は１：１０であり、
ステップＳ３において、ステップＳ２で得られた混合液を噴霧乾燥装置で噴霧乾燥を行うことにより、平均粒子が１００〜２００μｍの粒子を作製し、
ステップＳ４において、ステップＳ３で得られた粒子を焼成装置に入れ、７５０℃〜８５０℃の焼成温度で６時間焼成することにより製品を得る。
The method for recycling lithium manganate dust provided by the present invention includes the following steps S1 to S4,
In step S1, lithium manganese oxide dust, a sintering aid, and an oxygen atmosphere improving agent are added to deionized water at a mass ratio of 250: 1: 25, and dispersed sufficiently uniformly, where deionized water is added. The mass ratio of the powder to lithium manganate dust is 1: 2, the sintering aid is boric acid, and the oxygen atmosphere improving agent is a mixture of lithium carbonate and electrolytic manganese dioxide,
In step S2, a polyvinyl alcohol solution having a solid content of 10% is added to the dispersion obtained in step S1, and the solution is uniformly stirred, where the mass ratio of polyvinyl alcohol solution to lithium manganate dust is 1 : 10,
In step S3, the mixed solution obtained in step S2 is spray-dried with a spray dryer to produce particles having an average particle size of 100 to 200 μm,
In step S4, the particles obtained in step S3 are placed in a calcining apparatus and calcined at a calcination temperature of 750 ° C. to 850 ° C. for 6 hours to obtain a product.
さらに、ステップＳ１において、炭酸リチウムと電解二酸化マンガンとの質量比は１．１：４であり、高温下での化学反応式はＬｉ２ＣＯ３＋４ＭｎＯ２−−−２ＬｉＭｎ２Ｏ４＋ＣＯ２↑＋０．５Ｏ２↑である。
さらに、マンガン酸リチウム粉塵の粒子径は０．１〜１０μｍである。
Furthermore, in step S1, the mass ratio of lithium carbonate to electrolytic manganese dioxide is 1.1: 4, and the chemical reaction formula at high temperature is Li 2 CO 3 +4 MnO 2 −−2 LiMn 2 O 4 + CO 2 ++ 0 .5 O 2 ↑.
Furthermore, the particle size of lithium manganate dust is 0.1 to 10 μm.
上記の実施形態によれば、本発明は、少なくとも以下の利点を有する。本発明は、マンガン酸リチウム粉塵に酸素雰囲気改善剤を添加することにより、高温反応時のマンガン酸リチウム材料の酸素空孔の発生が効果的に抑制され、一部の構造的欠陥が修復され、電気化学的性能が改善及び向上される。また、造粒プロセスにより、結晶粒子の成長程度が制御可能となり、結晶凝集体又は二次粒子の形態が球状になる傾向があり、処理された製品のタップ密度が大幅に向上し、加工特性が改善される。 According to the above embodiments, the present invention has at least the following advantages. According to the present invention, by adding an oxygen atmosphere improving agent to lithium manganate dust, the generation of oxygen vacancies in the lithium manganate material during high temperature reaction is effectively suppressed, and some structural defects are repaired. Electrochemical performance is improved and enhanced. In addition, the granulation process makes it possible to control the degree of growth of crystal particles, the shape of crystal aggregates or secondary particles tends to be spherical, the tap density of the treated product is significantly improved, and the processing characteristics are improved. Be improved.
上記の説明は、本発明の技術解決策の概要であり、本発明の技術手段を理解しやすくするためのものであり、明細書の内容に従って実施されることができる。以下、図面を参照しながら本発明の好ましい実施例を詳しく説明する。 The above description is an outline of the technical solution of the present invention, for the purpose of making the technical means of the present invention easy to understand, and can be implemented in accordance with the contents of the specification. Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the drawings.
以下、図面及び実施例を利用して本発明の具体的な実施形態をさらに詳しく説明する。以下の実施例は、本発明を説明するものであり、本発明の範囲を制限しない。 Hereinafter, specific embodiments of the present invention will be described in more detail using the drawings and examples. The following examples illustrate the invention and do not limit the scope of the invention.
実施例１
マンガン酸リチウム粉塵１００ｇを取り出しホウ酸０．４ｇを加え、さらに、質量比１．１：４である炭酸リチウムと電解二酸化マンガンとを混合してなる酸素雰囲気改善剤１０ｇを加え、脱イオン水５０ｇの存在下で十分に均一に分散させた後、固形分含有量が１０％のＰＶＡ（ポリビニルアルコール）溶液１０ｇを加え、均一に撹拌した。
Example 1
100 g of lithium manganate dust is taken out, 0.4 g of boric acid is added, and 10 g of an oxygen atmosphere improver formed by mixing lithium carbonate having a mass ratio of 1.1: 4 and electrolytic manganese dioxide is further added, and 50 g of deionized water After sufficiently dispersing uniformly in the presence of 10 g of a PVA (polyvinyl alcohol) solution having a solid content of 10% was added and uniformly stirred.
上記混合溶液を噴霧乾燥装置で噴霧乾燥することにより、平均粒子が１００〜２００μｍの粒子を作製した。上記粒子を焼成装置に入れ、焼成温度７５０℃で６時間焼成して製品を得た。 By spray-drying the above mixed solution with a spray dryer, particles having an average particle size of 100 to 200 μm were produced. The particles were placed in a firing apparatus and fired at a firing temperature of 750 ° C. for 6 hours to obtain a product.
炭酸リチウムと電解二酸化マンガンとの高温下での化学反応式は、Ｌｉ２ＣＯ３＋４ＭｎＯ２−−−２ＬｉＭｎ２Ｏ４＋ＣＯ２↑＋０．５Ｏ２↑である。
ここで、ＣＯ２が高温反応の前段に放出され、Ｏ２が高温反応の後段に放出されることにより、焼結過程における酸素雰囲気を改善し、酸素空孔の発生を回避できる。
The chemical reaction formula of lithium carbonate and electrolytic manganese dioxide at high temperature is Li 2 CO 3 +4 MnO 2 -−2 LiMn 2 O 4 + CO 2 ++ 0.5 O 2 ↑.
Here, CO 2 is released to the front stage of the high-temperature reaction and O 2 is released to the rear stage of the high-temperature reaction, so that the oxygen atmosphere in the sintering process can be improved and generation of oxygen vacancies can be avoided.
本実施例におけるマンガン酸リチウム粉塵、処理された製品の関連する特性データを図１、２、３、５に示す。 The relevant characterization data of the lithium manganate dust, treated product in this example are shown in FIGS.
実施例２
酸素雰囲気改善剤を加えない以外、実施例１と同様にして製品を得た。製品の関連する特性データを図１、４、５に示す。
Example 2
A product was obtained in the same manner as Example 1 except that the oxygen atmosphere improving agent was not added. The relevant property data of the product are shown in FIGS.
上記の説明及び図５のサイクル寿命試験データの比較図から明らかになるように、本発明は、マンガン酸リチウム粉塵に酸素雰囲気改善剤を添加することにより、高温反応時のマンガン酸リチウム材料の酸素空孔の発生が効果的に抑制され、一部の構造的欠陥が修復され、電気化学的性能が改善及び向上される。また、造粒プロセスにより、結晶粒子の成長程度が制御可能となり、結晶凝集体又は二次粒子の形態が球状になる傾向があり、処理された製品のタップ密度が大幅に向上し、加工特性が改善される。 As will become apparent from the above description and the comparison of cycle life test data in FIG. 5, the present invention relates to the oxygen of lithium manganate material during high temperature reaction by adding an oxygen atmosphere improver to lithium manganate dust The generation of vacancies is effectively suppressed, some structural defects are repaired, and electrochemical performance is improved and enhanced. In addition, the granulation process makes it possible to control the degree of growth of crystal particles, the shape of crystal aggregates or secondary particles tends to be spherical, the tap density of the treated product is significantly improved, and the processing characteristics are improved. Be improved.
上記の内容は、本発明の好ましい実施形態に過ぎず、本発明を制限するものではない。当業者であれば、本発明の技術原則を逸脱しない限り、いくつかの改良及び変形を加えることができ、これらの改良及び変形も本発明の保護範囲に含まれると理解されるべきである。 The above contents are only preferred embodiments of the present invention and do not limit the present invention. It should be understood by those skilled in the art that some modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations are also included in the protection scope of the present invention.
Claims (3)
ステップＳ１において、脱イオン水にマンガン酸リチウム粉塵と、焼結助剤と、酸素雰囲気改善剤とを質量比２５０：１：２５で加え、十分に均一に分散させ、ここで、脱イオン水とマンガン酸リチウム粉塵との質量比は１：２であり、焼結助剤はホウ酸であり、酸素雰囲気改善剤は炭酸リチウムと電解二酸化マンガンとを混合しなるものであり、
ステップＳ２において、ステップＳ１で得られた分散液に、固形分含有量が１０％のポリビニルアルコール溶液を加え、均一に撹拌し、ここで、ポリビニルアルコール溶液とマンガン酸リチウム粉塵との質量比は１：１０であり、
ステップＳ３において、ステップＳ２で得られた混合液を噴霧乾燥装置で噴霧乾燥を行うことにより、造成平均粒子が１００〜２００μｍの粒子を作製し、
ステップＳ４において、ステップＳ３で得られた粒子を焼成装置に入れ、７５０℃〜８５０℃の焼成温度で６時間焼成することにより製品を得ることを特徴とするマンガン酸リチウム粉塵の再利用方法。 A method for reusing lithium manganate dust including steps S1 to S4, comprising
In step S1, lithium manganese oxide dust, a sintering aid, and an oxygen atmosphere improving agent are added to deionized water at a mass ratio of 250: 1: 25, and dispersed sufficiently uniformly, where deionized water and The mass ratio to lithium manganate dust is 1: 2, the sintering aid is boric acid, and the oxygen atmosphere improving agent is a mixture of lithium carbonate and electrolytic manganese dioxide,
In step S2, a polyvinyl alcohol solution having a solid content of 10% is added to the dispersion obtained in step S1, and the solution is uniformly stirred, where the mass ratio of polyvinyl alcohol solution to lithium manganate dust is 1 : 10,
In step S3, the mixed liquid obtained in step S2 is spray-dried with a spray dryer to produce particles having a formation average particle size of 100 to 200 μm,
In step S4, the particles obtained in step S3 are put in a calcining apparatus and calcined at a calcining temperature of 750 ° C. to 850 ° C. for 6 hours to obtain a product, thereby obtaining a product using lithium manganate dust.
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| PCT/CN2017/115364 WO2018108043A1 (en) | 2016-12-16 | 2017-12-10 | Method for recycling lithium manganate dust |
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