CN108123125A - A kind of preparation method of the alkaline secondary cell nickel hydroxide composite material of cladding gamma hydroxy cobalt oxide - Google Patents
A kind of preparation method of the alkaline secondary cell nickel hydroxide composite material of cladding gamma hydroxy cobalt oxide Download PDFInfo
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- CN108123125A CN108123125A CN201711378875.5A CN201711378875A CN108123125A CN 108123125 A CN108123125 A CN 108123125A CN 201711378875 A CN201711378875 A CN 201711378875A CN 108123125 A CN108123125 A CN 108123125A
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- cladding
- nickel hydroxide
- composite material
- cobalt oxide
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/24—Alkaline accumulators
- H01M10/30—Nickel accumulators
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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
- H01M4/36—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
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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
- H01M4/36—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
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- 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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Abstract
The invention discloses a kind of alkaline secondary cell preparation methods of the nickel hydroxide composite material of cladding gamma hydroxy cobalt oxide, include the following steps：(1) aqueous slkali is added in into nickel chloride, manganese sulfate, cobaltous sulfate and deionized water mixing salt solution to be reacted, be dried, must adulterate the ball-shape nickel hydroxide precursor of the cladding cobalt hydroxide of manganese；(2) sodium hydroxide solution is added in, oxygen is passed through and carries out oxidation reaction；(3) washing is repeated with water in the product after oxidation reaction, filtered, dry, sieving, obtain the nickel hydroxide composite material of the cladding gamma hydroxy cobalt oxide of doping manganese.The nickel hydroxide composite material of cladding gamma hydroxy cobalt oxide prepared by the present invention improves uniformity, integrality and the electrical conductance of the conductive network of the oxidized rear coated gamma hydroxy cobalt oxide obtained；It is when for alkaline secondary cell so that battery has high specific capacity and longer service life.
Description
Technical field
The present invention relates to alkaline secondary cell manufacturing technology field more particularly to a kind of alkaline secondary cell cladding γ hydroxyls
The preparation method of the nickel hydroxide composite material of base cobalt oxide.
Background technology
Alkaline Ni-H cell is because its energy density is high, have extended cycle life, can fast charging and discharging, memory-less effect, pollution-free
Etc. excellent overall characteristic, preferred electronic automobile-used power accumulator is known as.As the positive electrode active materials wherein used, hydrogen
The properties of product of nickel oxide directly affect the performance of nickel-hydrogen secondary cell.The performance of positive active material is battery whole synthesis
The key that performance improves, especially as electrical vehicular power accumulator, the high rate during charging-discharging of nickel electrode also needs further
It improves.Nickel hydroxide is a kind of material with semiconductor property, and the resistance between particle inside and particle is very big, causes hydrogen
Nickel oxide is less desirable as the performance of active material assembled battery.
Nickel hydroxide positive plate active material it is initially use be conventional ball-shape nickel hydroxide, be applied to nickel-metal hydride battery
Electrode prepare in also need add in CoO or Co (OH)2Additive, by battery charge initial stage oxidation by the additive
Conductive β-CoOOH are oxidized to, play the function of conductive network.By further the study found that another brilliant
γ-the CoOOH of type have electric conductivity more higher than β-CoOOH, and this γ-CoOOH can form the shape higher than 3.0 valencys
State, its reduction potential in alkaline electrolyte is lower compared with β-CoOOH, it is not easy to the features such as being restored to 2.0 valency state,
It thus can preferably avoid in discharge process the dissolving of cobalt in conductive network, the decline problem for causing positive electrode capacity.It manages herein
On the basis of, people have investigated the preparation method of the nickel hydroxide of coated gamma-CoOOH.
But the nickel hydroxide material of current coated gamma hydroxy cobalt oxide, electric conductivity in such as conductive network,
It is also improved in terms of the electrical performance indexes such as service life cycle, heavy-current discharge performance that integrality and material are shown
Space.
The content of the invention
To overcome above-mentioned deficiency, the present invention provides a kind of nickel hydroxide of alkaline secondary cell with cladding gamma hydroxy cobalt oxide
The preparation method of composite material, the Spherical nickel hydroxide material prepared using this method are had good electric conductivity and followed
Ring stability.
To achieve the above object, the present invention uses following technical scheme：
The first aspect of the invention is to provide a kind of nickel hydroxide of alkaline secondary cell cladding gamma hydroxy cobalt oxide
The preparation method of composite material, includes the following steps：
(1) the ball-shape nickel hydroxide precursor of the cladding cobalt hydroxide of doping manganese and titanium is prepared
Nickel chloride, manganese sulfate, Titanium Nitrate, cobaltous sulfate and deionized water are pressed Ni: Mn: Ti：Co molar ratios are 1: 0.1-0.2
∶0.05-01：The ratio of 0.1-02 prepares nickel chloride, manganese sulfate, Titanium Nitrate, cobaltous sulfate mixing salt solution, prepares enough concentration
For the potassium hydroxide solution of 2-3mol/L；After above-mentioned potassium hydroxide solution solution is put into reactor, then by above-mentioned hybrid metal
Salting liquid is gradually added into reactor under stiring, and it is that pH value is 10-12 to control the mixed solution in reactor, and temperature control exists
60-80 DEG C, product obtained by the reaction is subjected to separation of solid and liquid, with pure water washing to pH7-9, is dried at a temperature of 50-60 DEG C,
Obtain the ball-shape nickel hydroxide precursor of the cladding cobalt hydroxide of doping manganese and titanium；
(2) oxidation reaction
The ball-shape nickel hydroxide precursor for the cladding cobalt hydroxide for adulterating manganese and titanium is added in oxidation reactor, adds in institute
State the sodium hydroxide solution of precursor weight 3-6%, the temperature of the sodium hydroxide solution is 90-110 DEG C, concentration 4-6mol/
L is passed through oxygen and carries out oxidation reaction；
(3) wash, is dry, sieving
Washing is repeated with water in product after oxidation reaction, is filtered, until the product pH value by washing is less than 8,
The temperature of slurry is 60-70 DEG C, is subsequently placed in drying in drier, until the mass percent of reaction product water content is small
It in 1%, is sieved using ultrasonic wave vibrating sieving machine to dried product, obtains cladding γ-hydroxyl oxidation of doping manganese and titanium
The nickel hydroxide composite material of cobalt.
Further, in the alkaline secondary cell system of the nickel hydroxide composite material of cladding gamma hydroxy cobalt oxide
In Preparation Method, Ni: Mn: Ti is pressed described in step (1)：Co molar ratios are 1: 0.13: 0.08：0.1.
Further, in the alkaline secondary cell system of the nickel hydroxide composite material of cladding gamma hydroxy cobalt oxide
In Preparation Method, oxidation reaction technique is described in step (2)：Under stirring condition, 120-140 DEG C of temperature, oxygen flow 0.3-
0.5L/kg nickel hydroxide minutes, when reaction time 1-2 is small.
Further, in the alkaline secondary cell system of the nickel hydroxide composite material of cladding gamma hydroxy cobalt oxide
In Preparation Method, drying temperature described in step (3) is 110-130 DEG C, when drying time is 3-4 small.
Further, in the alkaline secondary cell system of the nickel hydroxide composite material of cladding gamma hydroxy cobalt oxide
In Preparation Method, the mesh number of sieve is 100-150 mesh in ultrasonic wave vibrating sieving machine described in step (3), the frequency of ultrasonic wave vibrating sieving machine
For 30-40KHz.
It is to provide a kind of alkaline secondary cell cladding γ hydroxyls of the method preparation as the second aspect of the invention
The nickel hydroxide composite material of base cobalt oxide.
The present invention compared with prior art, is had the following technical effect that using above-mentioned technical proposal：
The nickel hydroxide composite material of cladding γ-hydroxy cobalt oxide prepared by the present invention, employs three kinds of cobalt, manganese and titanium gold
Belong to element and wet method doping vario-property is carried out to nickel hydroxide, while to improve the capacity of composite material and cyclical stability, also exist
Shaken the conductive network for the coated gamma hydroxy cobalt oxide for sieving the oxidized rear acquisition of raising by oxidation reaction and ultrasonic wave
Uniformity, integrality and electrical conductance, therefore the material is when for alkaline secondary cell so that battery have high specific capacity with
And longer service life.
Specific embodiment
The present invention is described in more detail below by specific embodiment, for a better understanding of the present invention,
But following embodiments are not intended to limit the scope of the invention.
The preparation of 1 alkaline secondary cell of the embodiment nickel hydroxide composite material of cladding gamma hydroxy cobalt oxide
(1) the ball-shape nickel hydroxide precursor of the cladding cobalt hydroxide of doping manganese and titanium is prepared
Nickel chloride, manganese sulfate, Titanium Nitrate, cobaltous sulfate and deionized water are pressed Ni: Mn: Ti：Co molar ratios are 1: 0.1:
0.05:0.2 ratio prepares Ni, Co, Ti, Mn mixing salt solution, prepares the potassium hydroxide solution that enough concentration is 2mol/L；
After above-mentioned aqueous slkali is put into reactor, then above-mentioned mixed salt solution is gradually added into reactor under stiring, controlled
Mixed solution in reactor is that pH value is 10, and temperature is controlled at 60 DEG C, and product obtained by the reaction is carried out separation of solid and liquid, with pure
Water purification is washed to pH7-9, is dried at a temperature of 50 DEG C, before the ball-shape nickel hydroxide for the cladding cobalt hydroxide for obtaining doping manganese and titanium
Body.
(2) oxidation reaction
The ball-shape nickel hydroxide precursor for the cladding cobalt hydroxide for adulterating manganese and titanium is added in oxidation reactor, adds in institute
Precursor weight 3% is stated, concentration at a temperature of 90 °C is the sodium hydroxide solution of 4mol/L, is passed through oxygen and is aoxidized, and is aoxidized
Reaction condition：Under stirring condition, 120 DEG C of temperature, oxygen flow 0.3L/kg nickel hydroxide minutes, when the reaction time 1 is small.
(3) wash, is dry, sieving
Washing is repeated with water in product after oxidation reaction, is filtered, until the product pH value by washing is less than 8,
The temperature of slurry is 60 DEG C, is subsequently placed in drying in drier, and drying temperature is 110 DEG C, when drying time is 3 small, directly
Mass percent to reaction product water content is less than 1%, is sieved using ultrasonic wave vibrating sieving machine to dried product, sieves
The mesh number of net is 100 mesh, and the frequency of ultrasonic wave vibrating sieving machine is 30KHz, obtains cladding γ-hydroxy cobalt oxide of doping manganese and titanium
Nickel hydroxide composite material.
The preparation of 2 alkaline secondary cell of the embodiment nickel hydroxide composite material of cladding gamma hydroxy cobalt oxide
(1) the ball-shape nickel hydroxide precursor of the cladding cobalt hydroxide of doping manganese and titanium is prepared
Nickel chloride, manganese sulfate, Titanium Nitrate, cobaltous sulfate and deionized water are pressed Ni: Mn: Ti:Co molar ratios are 1: 0.2:
0.1:0.1 ratio prepares Ni, Co, Mn, titanium mixing salt solution, prepares the potassium hydroxide solution that enough concentration is 3mol/L；
After above-mentioned aqueous slkali is put into reactor, then above-mentioned mixed salt solution is gradually added into reactor under stiring, controlled
Mixed solution in reactor is that pH value is 12, and temperature is controlled at 80 DEG C, and product obtained by the reaction is carried out separation of solid and liquid, with pure
Water purification is washed to pH7-9, is dried at a temperature of 60 DEG C, before the ball-shape nickel hydroxide for the cladding cobalt hydroxide for obtaining doping manganese and titanium
Body.
(2) oxidation reaction
The ball-shape nickel hydroxide precursor for the cladding cobalt hydroxide for adulterating manganese and titanium is added in oxidation reactor, adds in institute
Precursor weight 6% is stated, the sodium hydroxide solution that the concentration that temperature is 110 DEG C is 6mol/L is passed through oxygen and is aoxidized, oxidation
Reaction condition：Under stirring condition, 140 DEG C of temperature, oxygen flow 0.5L/kg nickel hydroxide minutes, when the reaction time 2 is small.
(3) wash, is dry, sieving
Washing is repeated with water in product after oxidation reaction, is filtered, until the product pH value by washing is less than 8,
The temperature of slurry is 70 DEG C, is subsequently placed in drying in drier, and drying temperature is 130 DEG C, when drying time is 4 small, directly
Mass percent to reaction product water content is less than 1%, is sieved using ultrasonic wave vibrating sieving machine to dried product, sieves
The mesh number of net is 150 mesh, and the frequency of ultrasonic wave vibrating sieving machine is 40KHz, obtains the hydrogen-oxygen of cladding γ-hydroxy cobalt oxide of doping manganese
Change nickel composite material.
Comparative example
It prepares：1M cobalt sulfate solutions, 20% sodium hydroxide solution, 20% ammonia spirit.Main material is put into reactor, is added
Enter pure water, sodium hydroxide solution and ammonia spirit, be made into 200 g/l of nickel hydroxide solid concentration, ammonia density for 5 g/l,
The reaction solution that pH is 9.5, temperature is 60 DEG C；Again by prepared 1M cobalt sulfate solutions, 20% sodium hydroxide solution, 20% ammonium hydroxide
Solution simultaneously and continuously add in into reactor, under 200 revs/min of stirring condition, holding 60 DEG C of temperature of reaction system,
PH is 9.5,5 g/l of ammonia density in system, the reaction time continue 3 it is small when.The cobalt liquor amount added in reaction by cladding hydrogen-oxygen
Change 5% (WT) meters that cobalt amount accounts for nickel hydroxide matrix.By after cladding material filtering, washing to pH be 7.0, then dried at 60 DEG C
The dry nickel hydroxide for obtaining surface cladding cobalt hydroxide.Cobalt oxyhydroxide：By the hydrogen of above-mentioned surface cladding cobalt hydroxide
Nickel oxide is put into oxidation reactor, is warming up to 80 DEG C under agitation, while is slowly added into prepared temperature as 80
DEG C, 50% sodium hydroxide solution, sodium hydroxide solution amount in 4% (WT) of weight of nickel hydroxide ratio add in, simultaneously lead to
Entering oxygen, (oxygen flow is：0.6 liter/kg nickel hydroxide minutes), temperature of reaction system maintain 80 DEG C, oxidization time be 10 points
Clock.After oxidation reaction again by the material after oxidation with pure water washing to pH for 8.0, again at 110 DEG C drying to surface
Coat the nickel hydroxide active substance A of gamma hydroxy cobalt oxide.
Above-described embodiment one, two and comparative example products therefrom are separately added into same amount of sodium carboxymethylcellulose
(CMC) and polytetrafluoroethylene (PTFE) (PTFE) paste, is stirred to obtain, wherein, the quality of sodium carboxymethylcellulose is the 1% of mixture,
The quality of polytetrafluoroethylene (PTFE) is the 3% of mixture.Then by paste full-filling on the nickel foam substrate of 1cm × 1cm, and 60
When vacuum drying 3 is small at DEG C.Dried pole piece is tabletted under 5MPa, and anode is made.By anode obtained and mistake
For the Cd electrode assemblings of amount into cadmium nickel simulated battery, electrolyte is 7mol/L KOH+15g/L LiOH solution.It is 25 in test temperature
Electric performance test is carried out at DEG C, compared with the product of comparative example, specific capacity improves the material of the embodiment one and two after tested
25-35%, service life improve 1.5 times or more.
Specific embodiments of the present invention are described in detail above, but it is intended only as example, it is of the invention and unlimited
It is formed on particular embodiments described above.To those skilled in the art, it is any to the equivalent modifications that carry out of the present invention and
It substitutes also all among scope of the invention.Therefore, the impartial conversion made without departing from the spirit and scope of the invention and
Modification, all should be contained within the scope of the invention.
Claims (6)
1. a kind of alkaline secondary cell preparation method of the nickel hydroxide composite material of cladding gamma hydroxy cobalt oxide, feature exist
In including the following steps：
(1) the ball-shape nickel hydroxide precursor of the cladding cobalt hydroxide of doping manganese and titanium is prepared
Nickel chloride, manganese sulfate, Titanium Nitrate, cobaltous sulfate and deionized water are pressed Ni: Mn: Ti：Co molar ratios are 1: 0.1-0.2:
0.05-01：The ratio of 0.1-02 prepares nickel chloride, manganese sulfate, Titanium Nitrate, cobaltous sulfate mixing salt solution, prepares enough concentration
For the potassium hydroxide solution of 2-3mol/L；After above-mentioned potassium hydroxide solution solution is put into reactor, then by above-mentioned hybrid metal
Salting liquid is gradually added into reactor under stiring, and it is that pH value is 10-12 to control the mixed solution in reactor, and temperature control exists
60-80 DEG C, product obtained by the reaction is subjected to separation of solid and liquid, with pure water washing to pH7-9, is dried at a temperature of 50-60 DEG C,
Obtain the ball-shape nickel hydroxide precursor of the cladding cobalt hydroxide of doping manganese and titanium；
(2) oxidation reaction
The ball-shape nickel hydroxide precursor for the cladding cobalt hydroxide for adulterating manganese and titanium is added in oxidation reactor, before addition is described
The sodium hydroxide solution of body weight 3-6%, the temperature of the sodium hydroxide solution is 90-110 DEG C, concentration 4-6mol/L, is led to
Enter oxygen and carry out oxidation reaction；
(3) wash, is dry, sieving
Washing is repeated with water in product after oxidation reaction, is filtered, until the product pH value by washing is less than 8, washing
It is 60-70 DEG C with the temperature of water, is subsequently placed in drying in drier, until the mass percent of reaction product water content is less than
1%, it is sieved using ultrasonic wave vibrating sieving machine to dried product, obtains cladding γ-hydroxy cobalt oxide of doping manganese and titanium
Nickel hydroxide composite material.
2. the alkaline secondary cell according to claim 1 system of the nickel hydroxide composite material of cladding gamma hydroxy cobalt oxide
Preparation Method, which is characterized in that described to press Ni: Mn: Ti in step (1)：Co molar ratios are 1: 0.13: 0.08：0.1.
3. the alkaline secondary cell according to claim 1 system of the nickel hydroxide composite material of cladding gamma hydroxy cobalt oxide
Preparation Method, which is characterized in that in step (2), the oxidation reaction technique is：Under stirring condition, 120-140 DEG C of temperature, oxygen
Flow 0.3-0.5L/kg nickel hydroxide minutes, when reaction time 1-2 is small.
4. the alkaline secondary cell according to claim 1 system of the nickel hydroxide composite material of cladding gamma hydroxy cobalt oxide
Preparation Method, which is characterized in that in step (3), the drying temperature is 110-130 DEG C, when drying time is 3-4 small.
5. the alkaline secondary cell according to claim 1 system of the nickel hydroxide composite material of cladding gamma hydroxy cobalt oxide
Preparation Method, which is characterized in that in step (3), the mesh number of sieve is 100-150 mesh in the ultrasonic wave vibrating sieving machine, and ultrasonic wave shakes
The frequency of screen(ing) machine is 30-40KHz.
It is 6. a kind of such as alkaline secondary cell prepared by any one of the claim 1-5 the method hydrogen of cladding gamma hydroxy cobalt oxide
Nickel oxide composite material.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5210537A (en) * | 1975-07-15 | 1977-01-26 | Matsushita Electric Ind Co Ltd | Method of producing nickel plate for battery |
| CN1343377A (en) * | 1999-03-10 | 2002-04-03 | H.C.施塔克股份有限公司 | Nickel hydroxide coated with cobaltous hydroxide |
| CN101106193A (en) * | 2007-07-09 | 2008-01-16 | 金天能源材料有限公司 | Preparation method of nickel hydroxide with surface coated with gamma-hydroxy cobalt oxide |
-
2017
- 2017-12-19 CN CN201711378875.5A patent/CN108123125A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5210537A (en) * | 1975-07-15 | 1977-01-26 | Matsushita Electric Ind Co Ltd | Method of producing nickel plate for battery |
| CN1343377A (en) * | 1999-03-10 | 2002-04-03 | H.C.施塔克股份有限公司 | Nickel hydroxide coated with cobaltous hydroxide |
| CN101106193A (en) * | 2007-07-09 | 2008-01-16 | 金天能源材料有限公司 | Preparation method of nickel hydroxide with surface coated with gamma-hydroxy cobalt oxide |
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