CN1187270C - Preparation method of nickel hydroxy-oxide - Google Patents

Preparation method of nickel hydroxy-oxide Download PDF

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Publication number
CN1187270C
CN1187270C CNB031482031A CN03148203A CN1187270C CN 1187270 C CN1187270 C CN 1187270C CN B031482031 A CNB031482031 A CN B031482031A CN 03148203 A CN03148203 A CN 03148203A CN 1187270 C CN1187270 C CN 1187270C
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China
Prior art keywords
nickel oxide
preparation
hydroxide
product
persulphate
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Expired - Lifetime
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CNB031482031A
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Chinese (zh)
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CN1460645A (en
Inventor
张清顺
常海涛
薛祥峰
陈美娟
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Fujian Nanping Nanfu Battery Co Ltd
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Fujian Nanping Nanfu Battery Co Ltd
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Priority to CNB031482031A priority Critical patent/CN1187270C/en
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    • 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
    • H01M4/24—Electrodes for alkaline accumulators
    • H01M4/32—Nickel oxide or hydroxide electrodes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/04—Oxides; Hydroxides
    • 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
    • H01M4/24—Electrodes for alkaline accumulators
    • H01M4/26—Processes of manufacture
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The present invention discloses a preparation method for nickel oxy-hydroxide as the active material of the positive pole of an alkaline battery. The method comprises the following steps that: nickel hydroxide carries out an oxidation reaction by an oxidizing agent in an alkaline system; obtained suspension reaction products are filtered; then, filtration residues are neutralized, washed and dried, and nickel oxy-hydroxide products are obtained. The nickel oxy-hydroxide solid products can be obtained by using the method of the present invention; the method has the advantages of low production cost and high purity of the products, and can realize industrialization mass production.

Description

The preparation method of hydroxy nickel oxide
Technical field
The invention belongs to chemical field, is the preparation method that is hydroxy nickel oxide about a kind of alkaline cell anode active material.
Background technology
At secondary cell is in the rechargeable cell, and capacity and charge-discharge performance in order to improve battery will use electrode active material, and the oxide compound of nickel is a kind of effective positive active material.But the oxide compound of nickel generally all is the nickel oxide or the nickel hydroxide of divalent, and the research surface, 3 valency nickel ions have good heavy load discharge characteristic with respect to divalent nickel.For example patent application day is that November 14 calendar year 2001, number of patent application are that 99811767.6 Chinese patent application document discloses the alkaline cell that a kind of positive pole contains the hydroxy nickel oxide of 80-10% (weight), and this kind battery has good discharge performance.Yet, there is not commercial hydroxy nickel oxide product in the market, so, the preparation method who the invents a kind of cost-effective hydroxy nickel oxide particularly weight that just seems.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of hydroxy nickel oxide.
The preparation method of hydroxy nickel oxide provided by the invention adopts following chemical reaction and separate mode to make: hydroxy nickel oxide carries out oxidizing reaction by oxygenant by nickel hydroxide and synthesizes in alkaline system, product suspension thing to gained filters, and then filter residue is neutralized, cleans, is drying to obtain the hydroxy nickel oxide product.
The preferred range of the alkaline system pH value control in the described oxidation reaction process is 10-14, passes through to increase OH in the reaction system under strong alkaline condition -Ionic concn promotes the carrying out that react, and improves the transformation efficiency of nickel ion.
The preferable consumption of described oxygenant is a nickel hydroxide weight: oxygenant weight is 1: 1-4 times, excessive oxygenant can promote the 3 valency nickel ions that are oxidized to of divalent nickel ion.
The preferable span of control of pH value after described filter residue neutralization, the cleaning is 5-7.
Described oxygenant can be potassium permanganate, hydrogen peroxide, hypochlorite or persulphate.
Above-mentioned hypochlorite can adopt potassium hypochlorite, clorox or Losantin.
Above-mentioned persulphate can be selected Potassium Persulphate, Sodium Persulfate or ammonium persulphate for use.
OH-ion starting point concentration can be 1-4mol/l in the described alkaline system.
Described alkaline system can be potassium hydroxide or sodium hydroxide alkaline system.
The present invention is under strong alkaline condition, by excessive strong oxidizer hydrogen oxide nickel oxide, make it be oxidized to 3 valency nickel synthesis of hydroxy nickel oxide products from divalent nickel, separating then purifies obtains the hydroxy nickel oxide solid phase prod, and this preparation method's starting material are easy to get, and production process is simple, production cost is low, product purity height, the oxidation ratio of hydroxy nickel oxide can be fit to industrialized mass production more than 40%.
Specific embodiment
Preparation method to hydroxy nickel oxide of the present invention is described further below in conjunction with specific embodiment.
Embodiment 1
In the KOH of 2mol/l solution system, add 100 gram Ni (OH) 2Oxidizer potassium permanganate 100 grams under whipped state, the PH=10-14 of the hierarchy of control in the reaction process reacted after 2 hours, and reaction product is filtered with suspended solids product and solution separating, the filter residue that obtains is neutralized with acid, clean with deionized water then, make that the surperficial pH value of filter residue is 5-7, through drying treatment, obtain the NiOOH powdery product, wherein the transformation efficiency of NiOOH is greatly about 40～45%.
Embodiment 2
In the NaOH of 3mol/l solution, add 100 gram Ni (OH) 2Oxidizer hydrogen peroxide 200 grams under whipped state, the PH=10-14 of the hierarchy of control in the reaction process reacted after 2 hours, and reaction product is filtered suspended solids product and solution separating, the filter residue that obtains is neutralized with acid, clean with deionized water then, make that the surperficial pH value of filter residue is 5-7, through drying treatment, obtain the NiOOH powdery product, wherein the transformation efficiency of NiOOH is greatly about 40～50%.
Embodiment 3
In the NaOH of 4mol/l solution, add 100 gram Ni (OH) 2Oxidizer Potassium Persulphate 300 grams under whipped state, the PH=10-14 of the hierarchy of control in the reaction process reacted after 2 hours, and reaction product is filtered with suspended solids product and solution separating, the product filter residue that obtains is neutralized with acid, clean with deionized water then, make that the surperficial pH value of filter residue is 5-7, through drying treatment, obtain the NiOOH powdery product, wherein the transformation efficiency of NiOOH is greatly about 60～80%.
Embodiment 4
In the KOH of 3mol/l solution, add 100 gram Ni (OH) 2Oxidizer Sodium Persulfate 200 grams under whipped state, the PH=10-14 of the hierarchy of control in the reaction process reacted after 2 hours, and reaction product is filtered suspended solids product and solution separating, the filter residue that obtains is neutralized with acid, clean with deionized water then, make that the surperficial pH value of filter residue is 5-7, through drying treatment, obtain the NiOOH powder-product, wherein the transformation efficiency of NiOOH is greatly about 50～60%.
Embodiment 5
In the NaOH of 1mol/l solution, add 100 gram Ni (OH) 2Oxidizer ammonium persulfate 100 grams under whipped state, the PH=10-14 of the hierarchy of control in the reaction process reacted after 2 hours, and reaction product is filtered suspended solids product and solution separating, the filter residue that obtains is neutralized with acid, clean with deionized water then, make that the surperficial pH value of filter residue is 5-7, through drying treatment, obtain the NiOOH powder-product, wherein the transformation efficiency of NiOOH is greatly about 50～55%.
Embodiment 6
In the KOH of 3mol/l solution, add 100 gram Ni (OH) 2Oxidizer clorox 400 grams under whipped state, the PH=10-14 of the hierarchy of control in the reaction process reacted after 2 hours, and reaction product is filtered suspended solids product and solution separating, the filter residue that obtains is neutralized with acid, clean with deionized water then, make that the surperficial pH value of filter residue is 5-7, through drying treatment, obtain the NiOOH powder-product, wherein the transformation efficiency of NiOOH is greatly about 60～70%.
Embodiment 7
In the NaOH of 4mol/l solution, add 100 gram Ni (OH) 2Oxidizer potassium hypochlorite 300 grams under whipped state, the PH=10-14 of the hierarchy of control in the reaction process reacted after 2 hours, and reaction product is filtered suspended solids product and solution separating, the filter residue that obtains is neutralized with acid, clean with deionized water then, make that the surperficial pH value of filter residue is 5-7, through drying treatment, obtain the NiOOH powder-product, wherein the transformation efficiency of NiOOH is greatly about 50～60%.
Embodiment 8
In the KOH of 4mol/l solution, add 100 gram Ni (OH) 2Oxidizer Losantin 400 grams under whipped state, the PH=10-14 of the hierarchy of control in the reaction process reacted after 2 hours, and reaction product is filtered suspended solids product and solution separating, the filter residue that obtains is neutralized with acid, clean with deionized water then, make that the surperficial pH value of filter residue is 5-7, through drying treatment, obtain the NiOOH powder-product, wherein the transformation efficiency of NiOOH is greatly about 50～60%.
Embodiment 9
In the NaOH of 1mol/l solution, add 100 gram Ni (OH) 2Oxidizer clorox 100 grams under whipped state, the PH=10-14 of the hierarchy of control in the reaction process reacted after 2 hours, and reaction product is filtered suspended solids product and solution separating, the filter residue that obtains is neutralized with acid, clean with deionized water then, make that the surperficial pH value of filter residue is 5-7, through drying treatment, obtain the NiOOH powder-product, wherein the transformation efficiency of NiOOH is greatly about 40～50%.

Claims (3)

1, a kind of preparation method of hydroxy nickel oxide, this method comprises following process: hydroxy nickel oxide by nickel hydroxide at OH -The ion starting point concentration is to carry out oxidizing reaction by oxygenant in the potassium hydroxide of 2-4mol/l or the oxygen sodium oxide alkaline system, the oxygenant consumption is 1-4 a times of nickel hydroxide weight, described oxygenant is potassium permanganate or hydrogen peroxide, hypochlorite, persulphate, and the pH value span of control is 10-14 in the reaction process; React after 2 hours, the suspension reaction product of gained is filtered, then filter residue being neutralized, cleans until pH value is 5-7, is drying to obtain the hydroxy nickel oxide product then.
2, the preparation method of hydroxy nickel oxide as claimed in claim 1 is characterized in that: above-mentioned hypochlorite employing potassium hypochlorite or clorox, Losantin.
3, the preparation method of hydroxy nickel oxide as claimed in claim 1 is characterized in that: above-mentioned persulphate is selected Potassium Persulphate or Sodium Persulfate, ammonium persulphate for use.
CNB031482031A 2003-07-01 2003-07-01 Preparation method of nickel hydroxy-oxide Expired - Lifetime CN1187270C (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI658007B (en) * 2018-03-14 2019-05-01 嘉藥學校財團法人嘉南藥理大學 Method of synthesizing granular basic nickel oxide from nickel-contained wastewater by using fluidized-bed crystallization technology

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100438153C (en) * 2006-07-20 2008-11-26 厦门大学 Positive electrode material of alkaline battery and preparation method
US8043748B2 (en) * 2008-02-07 2011-10-25 Powergenix Systems, Inc. Pasted nickel hydroxide electrode for rechargeable nickel-zinc batteries
CN102887549A (en) * 2012-09-26 2013-01-23 南昌大学 Method for preparing anode material LiLaxNil-xO2 of lithium ion secondary battery
KR20150106955A (en) 2013-01-14 2015-09-22 파워지닉스 시스템즈, 인코포레이티드 Pasted nickel hydroxide electrode and additives for rechargeable alkaline batteries
CN110193294B (en) * 2019-05-30 2021-08-13 广东中膜科技有限公司 Metal nickel-polyvinylidene fluoride composite flat membrane and preparation method and device thereof
CN115893529B (en) * 2022-11-24 2024-07-02 福建南平南孚电池有限公司 Preparation method of nickel oxyhydroxide, nickel oxyhydroxide prepared by preparation method and application of nickel oxyhydroxide

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI658007B (en) * 2018-03-14 2019-05-01 嘉藥學校財團法人嘉南藥理大學 Method of synthesizing granular basic nickel oxide from nickel-contained wastewater by using fluidized-bed crystallization technology

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