WO2014139200A1 - 一种制备镍钴锰氢氧化物的方法 - Google Patents

一种制备镍钴锰氢氧化物的方法 Download PDF

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WO2014139200A1
WO2014139200A1 PCT/CN2013/074976 CN2013074976W WO2014139200A1 WO 2014139200 A1 WO2014139200 A1 WO 2014139200A1 CN 2013074976 W CN2013074976 W CN 2013074976W WO 2014139200 A1 WO2014139200 A1 WO 2014139200A1
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cobalt
nickel
manganese
source
manganese hydroxide
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PCT/CN2013/074976
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French (fr)
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欧彦楠
李长东
余海军
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佛山市邦普循环科技有限公司
湖南邦普循环科技有限公司
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Priority to US14/775,397 priority Critical patent/US9815709B2/en
Priority to KR1020157028231A priority patent/KR101738498B1/ko
Priority to JP2015549948A priority patent/JP5981049B2/ja
Publication of WO2014139200A1 publication Critical patent/WO2014139200A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the present invention relates to a process for preparing nickel cobalt manganese hydroxide.
  • Nickel-cobalt-manganese hydroxide a nickel-cobalt-manganese ternary precursor, can synthesize lithium nickel cobalt manganese oxide by adding a lithium source. Therefore, nickel-cobalt-manganese hydroxide is an essential material for producing nickel-cobalt-manganese hydride.
  • the size, morphology and structure of nickel-cobalt-manganese hydroxide have a direct influence on the size, morphology and structure of the subsequently processed lithium nickel cobalt manganate. Therefore, the performance of the nickel-cobalt-manganese ternary precursor determines the performance of lithium nickel cobalt manganese oxide.
  • a method for preparing nickel-cobalt-manganese hydroxide is generally carried out by direct precipitation method, and a nickel-cobalt-manganese hydroxide, that is, a nickel-cobalt-manganese ternary precursor, is synthesized by adding a strong alkaline precipitant to a nickel, cobalt and manganese solution.
  • This method is relatively common, but due to the violent reaction, the appearance structure of the nickel-cobalt-manganese ternary precursor is uncontrollable, resulting in low consistency of product performance, affecting the performance of subsequent processing of battery materials.
  • the object of the present invention is to provide a method for preparing nickel-cobalt-manganese hydroxide, A precursor of high quality nickel-cobalt-manganese ternary battery material is obtained.
  • a method of preparing nickel cobalt manganese hydroxide comprising the steps of:
  • step (3) filtering the reaction solution obtained in the step (2), taking the filter residue, respectively washing the filter residue with pure water and ethanol, and then drying, pulverizing and sieving the filter residue to obtain nickel cobalt manganese hydroxide;
  • the nickel source is one of nickel acetate, nickel chloride or nickel sulfate;
  • the cobalt source is one of cobalt acetate, cobalt chloride or cobalt sulfate;
  • the manganese source is one of manganese acetate, manganese chloride or manganese sulfate.
  • the invention adopts microcrystalline cellulose as a template, and nickel, cobalt, manganese ions interact with hydroxyl groups on the surface of microcrystalline cellulose, and can uniformly grow nucleation along the distribution of microcrystalline cellulose hydroxyl groups, thus preparing nickel cobalt manganese
  • the hydroxide has a uniform particle size and a uniform morphology.
  • the present invention uses hexamethylenetetramine to promote nucleation of nickel cobalt manganese hydroxide. Hexamethylenetetramine reacts with water to form OH-, which controls the nucleation of nickel, cobalt and manganese ions on the surface of microcrystalline cellulose. Compared with the traditional direct addition of strong alkaline precipitant, the strong alkaline precipitant makes nickel, cobalt and manganese ions grow rapidly in a short time, and it is difficult to control the nucleation of nickel, cobalt and manganese ions on the surface of microcrystalline cellulose. The product size is large and the topography is inconsistent.
  • the invention adopts the microwave heating method to accelerate the nucleation growth of the nickel-cobalt-manganese hydroxide on the surface of the microcrystalline cellulose, improve the reaction speed, and solve the natural growth time of the nickel-cobalt-manganese hydroxide on the surface of the microcrystalline cellulose. Long question.
  • Example 1 is a scanning electron micrograph of nickel cobalt manganese hydroxide prepared in Example 1.
  • a method of preparing nickel cobalt manganese hydroxide comprising the steps of:
  • the obtained nickel-cobalt-manganese hydroxide has a uniform particle size of about 10 ⁇ m, and the morphology is spherical and the structure is uniform.
  • a method of preparing nickel cobalt manganese hydroxide comprising the steps of:
  • the nickel-cobalt-manganese hydroxide prepared in this example has a particle size and morphology similar to that of the first embodiment, and has a uniform particle size of about 10 ⁇ m, and the morphology is spherical and the structure is uniform.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
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Abstract

一种制备镍钴锰氢氧化物的方法，该方法包括以下步骤：（1）将微晶纤维素溶于水中得到悬浮液；往悬浮液中加入镍源、钴源和锰源，获得含镍、钴、锰的溶液；（2）往含镍、钴、锰的溶液中加入六亚甲基四胺，将反应溶液加热至80-90℃反应5-10min，然后用微波水热合成仪以频率2450MHz加热10-60min；（3）将步骤（2）得到的反应溶液过滤，取滤渣，分别用纯水和乙醇洗涤滤渣，然后将滤渣干燥、粉碎、筛分后得到镍钴锰氢氧化物。上述方法制得的镍钴锰氢氧化物粒径均匀、形貌结构一致，克服了现有的制备镍钴锰氢氧化物的方法由于反应剧烈所造成的产品外观结构不可控、性能不一致的问题。

Description

一种制备镍钴锰氢氧化物的方法
技术领域
本发明涉及一种制备镍钴锰氢氧化物的方法。
背景技术
随着数码产品行业的不断发展，人们对电池的需求日益增加。镍钴锰酸锂是一种重要的锂电池正极材料，生产和使用日益广泛，市场需求量较大。镍钴锰氢氧化物，即镍钴锰三元前驱体，能通过加入锂源合成镍钴锰酸锂，因此，镍钴锰氢氧化物是生产镍钴锰酸锂的必需材料。镍钴锰氢氧化物的尺寸、形貌、结构，对后续加工的镍钴锰酸锂的尺寸、形貌、结构有直接影响。因此，镍钴锰三元前驱体的性能好坏决定了镍钴锰酸锂的性能好坏。
目前制备镍钴锰氢氧化物的方法常用直接沉淀法，通过往镍、钴、锰溶液中加入强碱性沉淀剂，合成镍钴锰氢氧化物，即镍钴锰三元前驱体。这种方法比较普遍，但由于反应剧烈，镍钴锰三元前驱体的外观结构不可控，导致产品性能一致性不高，影响后续加工电池材料的性能。
发明内容
为了克服现有的制备镍钴锰氢氧化物的方法由于反应剧烈所造成的产品外观结构不可控、性能不一致的问题，本发明的目的在于提供一种制备镍钴锰氢氧化物的方法，以获得优质的镍钴锰酸锂三元电池材料的前驱体。
本发明的目的通过下述技术方案实现：
一种制备镍钴锰氢氧化物的方法，包括以下步骤：
（1）将微晶纤维素（作为模板赋形剂）溶于水中，搅匀，得到悬浮液；往悬浮液中加入镍源、钴源和锰源，其中镍源、钴源、锰源的质量比为(1-3):1:(1-1.5)，镍源、钴源、锰源的总质量与微晶纤维素质量之比为(1-3):1，搅匀，获得含镍、钴、锰的溶液；
（2）往含镍、钴、锰的溶液中加入六亚甲基四胺（是弱碱性成核剂），使镍源、钴源、锰源的总质量与六亚甲基四胺质量之比为1:(1-5)，搅匀，获得反应溶液；将反应溶液加热至80-90℃反应5-10min，然后用微波水热合成仪以频率2450MHz加热10-60min；
（3）将步骤（2）得到的反应溶液过滤，取滤渣，分别用纯水和乙醇洗涤滤渣，然后将滤渣干燥、粉碎、筛分后得到镍钴锰氢氧化物；
所述的镍源为醋酸镍、氯化镍或硫酸镍中的一种；
所述的钴源为醋酸钴、氯化钴或硫酸钴中的一种；
所述的锰源为醋酸锰、氯化锰或硫酸锰中的一种。
本发明相对于现有技术具有如下的优点及效果：
1、本发明采用微晶纤维素为模板，镍、钴、锰离子与微晶纤维素表面的羟基作用，能顺着微晶纤维素羟基的分布均匀成核生长，因此制得的镍钴锰氢氧化物粒径均匀，形貌结构一致。
2、本发明采用六亚甲基四胺促进镍钴锰氢氧化物成核。六亚甲基四胺与水反应，逐渐生成OH-，控制镍、钴、锰离子能稳定在微晶纤维素表面成核。与传统的直接添加强碱性沉淀剂相比，强碱性沉淀剂使镍、钴、锰离子短时间快速成核生长，难于控制镍、钴、锰离子稳定在微晶纤维素表面成核，导致产品尺寸较大，形貌结构不一致。
3、本发明采用微波加热法，加快镍钴锰氢氧化物在微晶纤维素表面的成核生长，提高反应速度，解决了镍钴锰氢氧化物在微晶纤维素表面自然生长耗时较长的问题。　　
附图说明
图1是实施例1制备的镍钴锰氢氧化物的扫描电镜图。
具体实施方式
下面结合实施例及附图对本发明作进一步详细的描述，但本发明的实施方式不限于此。
实施例1
一种制备镍钴锰氢氧化物的方法，包括以下步骤：
（1）将2g微晶纤维素溶于80mL水中，搅匀，得到悬浮液；往悬浮液中加入1g醋酸镍、1g醋酸钴、1g醋酸锰，搅匀，获得含镍、钴、锰的溶液；
（2）往含镍、钴、锰的溶液中加入3g六亚甲基四胺，搅匀，获得反应溶液；将反应溶液加热至80℃反应5min，然后用微波水热合成仪（北京祥鹄科技发展有限公司，型号：XH-800S-10；下同）以频率2450MHz加热30min；
（3）将步骤（2）得到的反应溶液过滤，取滤渣，分别用纯水和乙醇洗涤滤渣，然后将滤渣60℃下干燥、粉碎、筛分后得到镍钴锰氢氧化物。
由图1可见，所得到的镍钴锰氢氧化物粒径均匀，约为10μm，形貌均呈球形，结构一致。
实施例2
一种制备镍钴锰氢氧化物的方法，包括以下步骤：
（1）将4g微晶纤维素溶于100mL水中，搅匀，得到悬浮液；往悬浮液中加入2g氯化镍、2g氯化钴、2g氯化锰，搅匀，获得含镍、钴、锰的溶液；
（2）往含镍、钴、锰的溶液中加入6g六亚甲基四胺，搅匀，获得反应溶液；将反应溶液加热至90℃反应10min，然后用微波水热合成仪以频率2450MHz加热60min；
（3）将步骤（2）得到的反应溶液过滤，取滤渣，分别用纯水和乙醇洗涤滤渣，然后将滤渣60℃下干燥、粉碎、筛分后得到镍钴锰氢氧化物。
本实施例制得的镍钴锰氢氧化物，其粒径和形貌与实施例1的相似，粒径均匀，约为10μm，形貌均呈球形，结构一致。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (4)

  1. 一种制备镍钴锰氢氧化物的方法，其特征在于包括以下步骤：
    （1）将微晶纤维素溶于水中，搅匀，得到悬浮液；往悬浮液中加入镍源、钴源和锰源，其中镍源、钴源、锰源的质量比为(1-3):1:(1-1.5)，镍源、钴源、锰源的总质量与微晶纤维素质量之比为(1-3):1，搅匀，获得含镍、钴、锰的溶液；
    （2）往含镍、钴、锰的溶液中加入六亚甲基四胺，使镍源、钴源、锰源的总质量与六亚甲基四胺质量之比为1:(1-5)，搅匀，获得反应溶液；将反应溶液加热至80-90℃反应5-10min，然后用微波水热合成仪以频率2450MHz加热10-60min；
    （3）将步骤（2）得到的反应溶液过滤，取滤渣，分别用纯水和乙醇洗涤滤渣，然后将滤渣干燥、粉碎、筛分后得到镍钴锰氢氧化物。
  2. 根据权利要求1所述的制备镍钴锰氢氧化物的方法，其特征在于：所述的镍源为醋酸镍、氯化镍或硫酸镍中的一种。
  3. 根据权利要求1所述的制备镍钴锰氢氧化物的方法，其特征在于：所述的钴源为醋酸钴、氯化钴或硫酸钴中的一种。
  4. 根据权利要求1所述的制备镍钴锰氢氧化物的方法，其特征在于：所述的锰源为醋酸锰、氯化锰或硫酸锰中的一种。
PCT/CN2013/074976 2013-03-11 2013-04-28 一种制备镍钴锰氢氧化物的方法 WO2014139200A1 (zh)

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JP2015549948A JP5981049B2 (ja) 2013-03-11 2013-04-28 ニッケル−コバルト−マンガンの水酸化物の調製方法

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