CN103137962B - 一种制备镍钴锰氢氧化物的方法 - Google Patents
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- SEVNKUSLDMZOTL-UHFFFAOYSA-H cobalt(2+);manganese(2+);nickel(2+);hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mn+2].[Co+2].[Ni+2] SEVNKUSLDMZOTL-UHFFFAOYSA-H 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 26
- 239000010941 cobalt Substances 0.000 claims abstract description 26
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 18
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 15
- 239000011572 manganese Substances 0.000 claims abstract description 15
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims abstract description 14
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims abstract description 14
- 239000008108 microcrystalline cellulose Substances 0.000 claims abstract description 14
- 229940016286 microcrystalline cellulose Drugs 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000725 suspension Substances 0.000 claims abstract description 10
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims abstract description 5
- 238000012216 screening Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 12
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 3
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 3
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 3
- 229940011182 cobalt acetate Drugs 0.000 claims description 3
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 3
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 3
- 229940071125 manganese acetate Drugs 0.000 claims description 3
- 235000002867 manganese chloride Nutrition 0.000 claims description 3
- 239000011565 manganese chloride Substances 0.000 claims description 3
- 229940099607 manganese chloride Drugs 0.000 claims description 3
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 3
- 229940078494 nickel acetate Drugs 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 2
- 229940099596 manganese sulfate Drugs 0.000 claims description 2
- 235000007079 manganese sulphate Nutrition 0.000 claims description 2
- 239000011702 manganese sulphate Substances 0.000 claims description 2
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract description 4
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 abstract 2
- 238000007796 conventional method Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 abstract 1
- 239000004312 hexamethylene tetramine Substances 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- OVAQODDUFGFVPR-UHFFFAOYSA-N lithium cobalt(2+) dioxido(dioxo)manganese Chemical compound [Li+].[Mn](=O)(=O)([O-])[O-].[Co+2] OVAQODDUFGFVPR-UHFFFAOYSA-N 0.000 description 6
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 description 4
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 description 4
- 229910001437 manganese ion Inorganic materials 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- -1 and therefore Chemical compound 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
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Abstract
本发明公开了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。本发明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
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。
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| CN104167542A (zh) * | 2014-08-06 | 2014-11-26 | 西南民族大学 | 一种锂电池正极材料镍钴锰酸锂粉体及其制备方法 |
| CN104437362B (zh) * | 2014-11-03 | 2017-01-18 | 东北林业大学 | 一种磁性碳微球的水热制备方法 |
| CN107834041A (zh) * | 2017-10-11 | 2018-03-23 | 苏州宇量电池有限公司 | 核壳结构高性能富锂锰基正极材料的制备方法 |
| CN108172822B (zh) * | 2017-12-29 | 2020-10-09 | 昶联金属材料应用制品(广州)有限公司 | 镍钴锰酸锂正极材料及其制备方法 |
| CN109037673A (zh) * | 2018-10-18 | 2018-12-18 | 珠海嘉志科技咨询有限公司 | 一种环保、高效制备镍钴锰三元正极材料前驱体的方法 |
| CN110289175B (zh) * | 2019-07-12 | 2021-09-28 | 大连海事大学 | 一种高容量NiMn2O4微米球/泡沫镍电极材料及其制备方法和应用 |
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| CN112777649A (zh) * | 2021-01-15 | 2021-05-11 | 昆明理工大学 | 一种镍钴锰三元前驱体及其制备方法与应用 |
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