CN209264388U - It is a kind of for separating and collecting the device of the magnetisable material in electrolytic manganese dioxide - Google Patents
It is a kind of for separating and collecting the device of the magnetisable material in electrolytic manganese dioxide Download PDFInfo
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Abstract
本实用新型公开了一种用于分离收集电解二氧化锰中的磁性物质的装置,包括样品瓶、瓶盖、永磁铁、外壳和三维混合器,三维混合器与外壳配合,瓶盖与样品瓶旋紧配合,样品瓶放置在外壳内,外壳的底部平放有四个相吸的永磁铁,外壳与样品瓶外周的缝隙内竖直放置有四组永磁铁。本申请的装置用于分离收集电解二氧化锰中的磁性物质,利用电解二氧化锰产品中的铁磁性杂质和亚铁磁性杂质的特性,采用吸附装置对EMD中的磁性物质进行吸附后,分离/收集和清洗、检测,得出EMD产品中的磁性物质含量结果。本实用新型可以满足二次电源厂家对于EMD产品中的磁性物质的检测要求,可以为改进EMD生产工艺以降低EMD的磁性物质含量提供有效检测手段。
The utility model discloses a device for separating and collecting magnetic substances in electrolytic manganese dioxide, which comprises a sample bottle, a bottle cap, a permanent magnet, a casing and a three-dimensional mixer, the three-dimensional mixer cooperates with the casing, and the bottle cap and the sample bottle Tightly fit, the sample bottle is placed in the shell, four permanent magnets are placed on the bottom of the shell, and four groups of permanent magnets are vertically placed in the gap between the shell and the outer periphery of the sample bottle. The device of the present application is used to separate and collect the magnetic substances in electrolytic manganese dioxide, utilize the characteristics of ferromagnetic impurities and ferrimagnetic impurities in electrolytic manganese dioxide products, and use an adsorption device to adsorb the magnetic substances in EMD, then separate / Collect and clean, test, and obtain the content of magnetic substances in EMD products. The utility model can meet the detection requirements of the secondary power supply manufacturers for the magnetic substance in the EMD product, and can provide an effective detection means for improving the EMD production process to reduce the magnetic substance content of the EMD.
Description
技术领域technical field
本实用新型涉及电解二氧化锰领域,特别是一种用于分离收集电解二氧化锰中的磁性物质的装置。The utility model relates to the field of electrolytic manganese dioxide, in particular to a device for separating and collecting magnetic substances in electrolytic manganese dioxide.
背景技术Background technique
电解二氧化锰(EMD)作为电池的关键材料之一,通过锰浸取→精制除杂→电解→后处理等工序生产得到合格的EMD 产品。反应式:MnSO4 + H2O = MnO2 + H2SO4 + H2 。Electrolytic manganese dioxide (EMD) is one of the key materials for batteries, and qualified EMD products are produced through manganese leaching → refining and impurity removal → electrolysis → post-treatment. Reaction formula: MnSO 4 + H 2 O = MnO 2 + H 2 SO 4 + H 2 .
电解过程中得到的EMD半成品为尺寸较大的块状物,需经过研磨→中和→干燥等处理,将块状EMD半成品加工至电池厂商需要的技术要求(一般粒度要求:D50约为10-100µm)。The EMD semi-finished product obtained in the electrolysis process is a large block, which needs to be processed through grinding→neutralization→drying to process the block EMD semi-finished product to the technical requirements required by the battery manufacturer (general particle size requirement: D50 is about 10- 100µm).
由于EMD半成品硬度高,而研磨件一般为特种钢或合金钢(如Co、Mo、Cr、Ni、Cu、Zn等金属),在半成品的研磨过程中由于机械力化学反应或摩擦力作用,产生大量的研磨件粉末进入EMD产品中,同时将金属杂质带入其中,影响EMD产品质量。如何判断带入杂质的量,也是判断EMD品质的方法。Due to the high hardness of EMD semi-finished products, and the grinding parts are generally special steel or alloy steel (such as Co, Mo, Cr, Ni, Cu, Zn and other metals), due to mechanical chemical reaction or friction during the grinding process of semi-finished products, produce A large amount of abrasive powder enters the EMD product, and at the same time brings metal impurities into it, affecting the quality of the EMD product. How to judge the amount of impurities is also a method to judge the quality of EMD.
目前通用的检测方法是将EMD直接通过酸溶解,用等离子光谱分析金属杂质元素的含量,随着二次电池研究的深入,在锂离子电池正极材料(锰酸锂)的EMD原料中,有些金属单质对电池的危害远远大于金属离子的危害,而现有测试方法只能分析金属杂质的总量,经过研究发现EMD金属单质主要从研磨设备中带入,这些杂质多为铁磁性物质或亚铁磁性物质,都具有磁性。我们把EMD中这种带有磁性的杂质称为磁性物质。At present, the general detection method is to dissolve EMD directly through acid, and analyze the content of metal impurity elements by plasma spectroscopy. Elemental substances are far more harmful to batteries than metal ions, and existing testing methods can only analyze the total amount of metal impurities. After research, it is found that EMD metal elements are mainly brought in from grinding equipment, and these impurities are mostly ferromagnetic substances or sub- Ferromagnetic substances are magnetic. We call this magnetic impurity in EMD as magnetic substance.
锂离子电池正极材料包括钴酸锂(LiCoO2)、锰酸锂(LiMn2O4)、三元材料(LiNiMnCoO2)和磷酸铁锂(LiFePO4)等。近年来,由于人们对锂离子电池正极材料结构及性能研究的越来越全面,越来越深入,发现锂离子电池正极材料中含有磁性金属杂质,这些磁性物质的存在,不仅会降低材料的比容量和能量密度,而且有些磁性杂质溶解在电解液中,发生一系列副反应,降低电池的使用寿命、一致性和安全性能。锂离子电池正极材料中磁性物质对自放电也有直接的影响,且磁性物质含量与电池自放电率成正比,即磁性物质含量越高的正极材料,其组成的电池的自放电率越大。Lithium-ion battery cathode materials include lithium cobalt oxide (LiCoO 2 ), lithium manganese oxide (LiMn 2 O 4 ), ternary materials (LiNiMnCoO 2 ) and lithium iron phosphate (LiFePO 4 ), etc. In recent years, due to the more comprehensive and in-depth research on the structure and performance of lithium-ion battery cathode materials, it has been found that lithium-ion battery cathode materials contain magnetic metal impurities. The existence of these magnetic substances will not only reduce the ratio of materials Capacity and energy density, and some magnetic impurities dissolve in the electrolyte, a series of side reactions occur, reducing the service life, consistency and safety performance of the battery. The magnetic substance in the positive electrode material of lithium ion battery also has a direct impact on self-discharge, and the content of magnetic substance is directly proportional to the self-discharge rate of the battery, that is, the higher the positive electrode material content of the magnetic substance, the greater the self-discharge rate of the battery composed of it.
因此,作为锂离子电池主要正极材料之一的锰酸锂,磁性金属杂质主要由EMD中带入,如何准确分离/收集EMD产品中的磁性物质,以便检测EMD产品中磁性物质的含量对稳定锂离子电池正极材料锰酸锂质量和提高锂离子电池性能具有重要的意义。Therefore, as lithium manganese oxide, one of the main positive electrode materials of lithium-ion batteries, the magnetic metal impurities are mainly brought in by EMD. How to accurately separate/collect the magnetic substances in EMD products in order to detect the content of magnetic substances in EMD products is very important for the stability of lithium It is of great significance to improve the quality of lithium manganese oxide, the positive electrode material of lithium-ion batteries, and improve the performance of lithium-ion batteries.
发明内容Contents of the invention
本实用新型的目的在于提供一种装置,用于分离收集电解二氧化锰中的磁性物质,从而用于分析EMD产品的磁性物质含量。The purpose of the utility model is to provide a device for separating and collecting magnetic substances in electrolytic manganese dioxide, so as to analyze the content of magnetic substances in EMD products.
为实现上述目的,本实用新型的用于分离收集电解二氧化锰中的磁性物质的装置,包括样品瓶、瓶盖、永磁铁、外壳和三维混合器,所述三维混合器与外壳配合,所述瓶盖与样品瓶旋紧配合,样品瓶放置在外壳内,外壳的底部平放有四个相吸的永磁铁,外壳与样品瓶外周的缝隙内竖直放置有四组永磁铁。In order to achieve the above object, the device for separating and collecting magnetic substances in electrolytic manganese dioxide of the present utility model includes a sample bottle, a bottle cap, a permanent magnet, a shell and a three-dimensional mixer, and the three-dimensional mixer cooperates with the shell, and the The bottle cap is tightly fitted with the sample bottle, the sample bottle is placed in the shell, four permanent magnets are placed on the bottom of the shell, and four sets of permanent magnets are vertically placed in the gap between the shell and the sample bottle periphery.
进一步地,所述四组竖直放置的永磁铁为每组两两对称放置。Further, the four sets of vertically placed permanent magnets are placed symmetrically by two in each set.
进一步地,所述四组永磁铁每组由四个相吸的永磁铁组成。Further, each of the four groups of permanent magnets is composed of four mutually attracting permanent magnets.
进一步地,所述样品瓶的形状为长方体。Further, the shape of the sample bottle is a cuboid.
进一步地,所述样品瓶的材质为耐酸腐蚀的非磁性金属或非金属材质。Further, the sample bottle is made of acid-resistant non-magnetic metal or non-metal material.
优选地,所述样品瓶的材质为聚四氟乙烯、PVC、PP中的一种。Preferably, the material of the sample bottle is one of polytetrafluoroethylene, PVC and PP.
进一步地,所述永磁铁的形状为柱状。Further, the shape of the permanent magnet is columnar.
优选地,所述外壳的材质为聚四氟乙烯。Preferably, the material of the shell is polytetrafluoroethylene.
本实用新型的实质性特点和进步是:Substantive features and progress of the present utility model are:
本申请的装置用于分离收集电解二氧化锰中的磁性物质,主要利用铁磁性物质和亚铁磁性物质的磁性特性,采用由样品瓶、外壳、永磁铁、三维混合器组成的吸附装置,对EMD中的磁性物质进行吸附后,分离/收集和清洗、检测,得出EMD产品磁性物质含量结果。本实用新型可有效分离EMD产品中的磁性物质,从而用于分析EMD产品的磁性物质含量,满足二次电源厂家对于EMD产品中的磁性物质的检测要求,可以为改进EMD生产工艺以降低产品中磁性物质含量提供有效的检测方法,从而验证工艺改进的实际效果,更好地控制EMD产品磁性物质的引入,对锰酸锂材料质量的提高,同时对锂离子电池的寿命、一致性、安全性和比容量的提高,有重要意义。The device of the present application is used to separate and collect magnetic substances in electrolytic manganese dioxide, mainly utilizes the magnetic properties of ferromagnetic substances and ferrimagnetic substances, and adopts an adsorption device composed of sample bottles, shells, permanent magnets, and three-dimensional mixers. After the magnetic substance in the EMD is adsorbed, it is separated/collected, cleaned, and detected to obtain the content of the magnetic substance in the EMD product. The utility model can effectively separate the magnetic substance in the EMD product, so as to analyze the magnetic substance content of the EMD product, meet the detection requirements of the secondary power supply manufacturers for the magnetic substance in the EMD product, and can improve the EMD production process to reduce the content of the magnetic substance in the product. The content of magnetic substances provides an effective detection method, so as to verify the actual effect of process improvement, better control the introduction of magnetic substances in EMD products, improve the quality of lithium manganate materials, and at the same time affect the life, consistency and safety of lithium-ion batteries It is of great significance to increase the specific capacity.
附图说明Description of drawings
图1是本实用新型的结构主视图。Fig. 1 is the structural front view of the present utility model.
图2是图1的俯视图。FIG. 2 is a top view of FIG. 1 .
图中零部件序号及名称:The serial numbers and names of parts in the figure:
瓶盖1、样品瓶2、外壳3、永磁铁4。Bottle cap 1, sample bottle 2, shell 3, permanent magnet 4.
具体实施方式Detailed ways
以下结合附图描述本实用新型的实施结构:Describe the implementation structure of the present utility model below in conjunction with accompanying drawing:
本实用新型的的用于分离收集电解二氧化锰中的磁性物质的装置,包括样品瓶2、瓶盖1、永磁铁4、外壳3和三维混合器,三维混合器与外壳3配合,外壳3的材质为聚四氟乙烯。瓶盖1与样品瓶2旋紧配合,样品瓶2放置在外壳3内,外壳3的底部平放有四个相吸的永磁铁4,外壳3与样品瓶2外周的缝隙内竖直放置有四组永磁铁4。The device for separating and collecting magnetic substances in electrolytic manganese dioxide of the present utility model includes a sample bottle 2, a bottle cap 1, a permanent magnet 4, a shell 3 and a three-dimensional mixer, and the three-dimensional mixer cooperates with the shell 3, and the shell 3 The material is polytetrafluoroethylene. The bottle cap 1 is tightly fitted with the sample bottle 2, and the sample bottle 2 is placed in the shell 3. There are four permanent magnets 4 that attract each other on the bottom of the shell 3, and there are vertically placed in the gap between the shell 3 and the sample bottle 2. Four groups of permanent magnets 4.
四组竖直放置的永磁铁4为每组两两对称放置,该四组永磁铁4每组由四个相吸的永磁铁4组成,永磁铁4的形状为柱状。Four groups of vertically placed permanent magnets 4 are placed symmetrically in pairs in each group, and each group of the four groups of permanent magnets 4 is composed of four permanent magnets 4 that attract each other. The permanent magnets 4 are in the shape of columns.
样品瓶2的形状为长方体,样品瓶2外周与外壳3形成相应的缝隙,便于放置永磁铁4。The shape of the sample bottle 2 is a cuboid, and the outer periphery of the sample bottle 2 forms a corresponding gap with the shell 3, which is convenient for placing the permanent magnet 4.
样品瓶2的材质为耐酸腐蚀的非磁性金属或非金属材质。样品瓶2的材质可以是聚四氟乙烯、PVC、PP中的一种。The sample bottle 2 is made of acid-resistant non-magnetic metal or non-metallic material. The material of the sample bottle 2 can be one of polytetrafluoroethylene, PVC, and PP.
外壳3的材质为聚四氟乙烯。The shell 3 is made of polytetrafluoroethylene.
以下结合实施例及工作过程描述本实用新型的工作原理:Describe working principle of the present utility model below in conjunction with embodiment and working process:
本实用新型主要利用杂质的磁性原理,采用由500ml长方体大口样品瓶2、500ml聚四氟乙烯外壳3、柱状永磁铁4(4000GS)、三维混合器组成的吸附装置,对EMD中磁性物质进行吸附后,分离/收集和清洗、检测,得出EMD产品磁性物质含量结果。The utility model mainly utilizes the magnetic principle of impurities, and adopts an adsorption device composed of a 500ml cuboid large-mouth sample bottle 2, a 500ml polytetrafluoroethylene shell 3, a columnar permanent magnet 4 (4000GS), and a three-dimensional mixer to adsorb the magnetic substances in the EMD. Finally, separation/collection, cleaning and detection are carried out to obtain the results of the magnetic substance content of EMD products.
本实用新型的工作原理是:将EMD粉末分散在水溶液中,用由样品瓶2、永磁铁4、外壳3组成的装置,通过三维混合器搅拌,吸附悬浮液中的磁性物质,用醋酸和双氧水清洗磁性物质,用酸溶解磁性物质,得到的滤液用等离子体发射光谱仪测试磁性物质各元素的含量。The working principle of the utility model is: disperse the EMD powder in the aqueous solution, use the device composed of the sample bottle 2, the permanent magnet 4, and the shell 3, stir through the three-dimensional mixer, absorb the magnetic substance in the suspension, and use acetic acid and hydrogen peroxide Cleaning the magnetic substance, dissolving the magnetic substance with acid, and testing the content of each element of the magnetic substance with a plasma emission spectrometer in the obtained filtrate.
具体操作方法:用盐酸将样品瓶2及瓶盖1的内表面清洗干净,放入底部预先并排放有四个相吸柱状永磁铁4的外壳3中,然后在样品瓶2四周与外壳3缝隙内两两对称竖直地塞入放置四组永磁铁4,该四组永磁铁4每组由四个相吸的永磁铁4组成。然后将 EMD放入样品瓶2中,加入蒸馏水,旋紧瓶盖1,放入三维混合器中,让EMD和蒸馏水混合30分钟;倒出瓶内的EMD和水的混合液,用蒸馏水冲洗样品瓶2内壁数次,直至瓶内无明显的颗料状EMD,然后加入醋酸和双氧水混合液,旋紧瓶盖1,上下摇动样品瓶2,使瓶内的剩余EMD充分与醋酸双氧水混合液反应;倒出醋酸双氧水混合液,再用蒸馏水冲洗数次后,旋紧瓶盖1,取出样品瓶2瓶四周的永磁铁4,把瓶内的磁性物质完全转移转移至300ml的烧杯中,加酸溶解磁性物质;用ICP测定溶液中的Fe、Co、Cr、Ni、Co、Cu、 Mo、Zn等金属元素,各元素的总和为磁性物质的量。The specific operation method: clean the inner surface of the sample bottle 2 and the bottle cap 1 with hydrochloric acid, put them into the shell 3 with four mutually attracting columnar permanent magnets 4 arranged side by side in advance at the bottom, and then place the gap between the sample bottle 2 and the shell 3 around the sample bottle 2 Two groups of permanent magnets 4 are placed symmetrically and vertically in pairs, and each group of these four groups of permanent magnets 4 is made up of four permanent magnets 4 that attract each other. Then put the EMD into the sample bottle 2, add distilled water, tighten the bottle cap 1, put it into a three-dimensional mixer, let the EMD and distilled water mix for 30 minutes; pour out the mixture of EMD and water in the bottle, and rinse the sample with distilled water Inner wall of bottle 2 several times, until there is no obvious granular EMD in the bottle, then add the mixture of acetic acid and hydrogen peroxide, tighten the bottle cap 1, shake the sample bottle 2 up and down, so that the remaining EMD in the bottle can fully react with the mixture of acetic acid and hydrogen peroxide Pour out the mixed solution of acetic acid and hydrogen peroxide, then rinse with distilled water for several times, tighten the bottle cap 1, take out the permanent magnet 4 around the sample bottle 2, transfer the magnetic substance in the bottle to a 300ml beaker completely, add acid Dissolve magnetic substances; use ICP to measure Fe, Co, Cr, Ni, Co, Cu, Mo, Zn and other metal elements in the solution, and the sum of each element is the amount of magnetic substances.
Claims (8)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111530470A (en) * | 2020-05-06 | 2020-08-14 | 合肥工业大学 | The preparation method of manganese dioxide and its composite material and the degradation method of sulfadiazine |
| CN113466003A (en) * | 2021-06-21 | 2021-10-01 | 无锡恩捷新材料科技有限公司 | Sample preparation method and sample preparation device for testing sample containing metal foreign matters in ultrahigh molecular weight polyethylene |
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2018
- 2018-11-06 CN CN201821814160.XU patent/CN209264388U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111530470A (en) * | 2020-05-06 | 2020-08-14 | 合肥工业大学 | The preparation method of manganese dioxide and its composite material and the degradation method of sulfadiazine |
| CN111530470B (en) * | 2020-05-06 | 2022-03-18 | 合肥工业大学 | The preparation method of manganese dioxide and its composite material and the degradation method of sulfadiazine |
| CN113466003A (en) * | 2021-06-21 | 2021-10-01 | 无锡恩捷新材料科技有限公司 | Sample preparation method and sample preparation device for testing sample containing metal foreign matters in ultrahigh molecular weight polyethylene |
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