CN103545526B - A kind of water system mixes the preparation method of lanthanum lithium titanate cathode size - Google Patents
A kind of water system mixes the preparation method of lanthanum lithium titanate cathode size Download PDFInfo
- Publication number
- CN103545526B CN103545526B CN201310441411.XA CN201310441411A CN103545526B CN 103545526 B CN103545526 B CN 103545526B CN 201310441411 A CN201310441411 A CN 201310441411A CN 103545526 B CN103545526 B CN 103545526B
- Authority
- CN
- China
- Prior art keywords
- lithium titanate
- lanthanum
- hours
- preparation
- lanthanum lithium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
-
- 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
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
- H01M4/622—Binders being polymers
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/626—Metals
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention discloses the preparation method that a kind of water system mixes lanthanum lithium titanate cathode size, comprise the following steps: lanthanum lithium titanate is mixed in a, preparation, b, takes raw material by quality 100%: mix lanthanum lithium titanate 47 ~ 60%, binding agent 0.3 ~ 8%, conductive agent 6 ~ 10%, dispersant 3 ~ 7% and deionized water 25 ~ 40%; C, in deionized water, add dispersant, stir after 12 hours and place 2 ~ 3 days, obtain dispersant mother liquor, add conductive agent to dispersant mother liquor and mix lanthanum lithium titanate, stirring 6 hours, then add binding agent, vacuumize stirring 2 hours, obtain water system and mix lanthanum lithium titanate cathode size.The present invention mixes in lanthanum lithium titanate cathode size process in preparation water system, mix lanthanum lithium titanate and adopt deionization water as solvent, adopt aqueous binder simultaneously, whole water system is made to mix lanthanum lithium titanate cathode size nontoxic, pollution-free, be green energy resource truly, fundamentally solve the problems such as safe, the pollution of lithium electricity; Effectively can be improved the performance of negative material by lithium titanate doping lanthanum, improve the specific capacity of lithium titanate material significantly.
Description
Technical field
The present invention relates to field of lithium technology, particularly provide a kind of water system to mix the preparation method of lanthanum lithium titanate cathode size.
Background technology
Traditional negative material is carbon negative pole material, although Carbon anode is own through successfully commercialization, but the safety problem of its cell safety problem existed particularly under large multiplying power, forces people to find the safe and reliable Novel anode material of embedding lithium under the current potential slightly more positive than Carbon anode.But lithium titanate has poor electron conduction, which limits its high rate capability.Therefore need by improving its conductivity to its modification, thus improve the large high rate performance of lithium titanate, its high reversible electrochemical capacity and good cycle performance will be kept simultaneously.The method can improving lithium titanate high rate performance at present mainly contains: the lithium titanate preparing nanometer particle size, lithium titanate bulk doped and introducing conductive phase.
In prior art, also the negative material relating to relevant doped chemical and lithium titanate combined together and be made into is had, this type of negative material is in the preparation process of doping lithium carbonate, adopt the organic substances such as too much organic solvent, this type organic easily volatilizees and in sintering process, produces a large amount of carbon dioxides in preparation process, substantially the oiliness binding agents such as Kynoar are adopted in addition in negative material preparation process, this negative material preparation technology not only because organic solvent cost is high, and preparation and use process in even more serious to the pollution of environment.Day by day serious along with environmental pollution, people are constantly doing technological innovation, constantly seek the high and lithium titanate anode material of environmental protection of a kind of specific capacity.
Summary of the invention
In view of this, the present invention is directed to the disappearance of prior art existence, its main purpose is to provide the preparation method that a kind of environment-friendly type water system mixes lanthanum lithium titanate cathode size.
For achieving the above object, the present invention adopts following technical scheme: a kind of water system mixes the preparation method of lanthanum lithium titanate cathode size, the raw material of described cathode size include mixes lanthanum lithium titanate, binding agent, conductive agent, dispersant and deionized water, and its preparation method comprises the following steps:
Lanthanum lithium titanate is mixed in a, preparation
1) take a certain amount of titanyl sulfate to join in deionized water and dissolve, dissolution time is 2.5 hours, and water temperature controls between 75 ~ 80 DEG C, filters the aqueous solution obtaining clear after dissolving;
2) in above-mentioned configured aqueous solution of titanyle sulfate, lithium hydroxide is added, undertaken mixing adding stabilizer by the mol ratio of Li:Ti=1.2:1 simultaneously, in this mixed solution, add lanthanum salting liquid, and be that under the condition of 110 ~ 150 DEG C and acidity, hybrid reaction forms colloidal sol in more than 24 hours in temperature;
3) by colloidal sol in vacuum drying oven dry 36 ~ 48 hours, baking temperature is 120 DEG C, after obtaining dry powder grinding, standbyly to burn;
4) at the dry powder high temperature furnace 950 ~ 1200 DEG C after grinding, calcining, calcines 6 ~ 10 hours, must mix lanthanum lithium titanate sample.
B, take raw material by quality 100%: mix lanthanum lithium titanate 47 ~ 60%, binding agent 0.3 ~ 8%, conductive agent 6 ~ 10%, dispersant 3 ~ 7% and deionized water 25 ~ 40%;
C, in deionized water, add dispersant, stir after 12 hours and place 2 ~ 3 days, obtain dispersant mother liquor, add conductive agent to dispersant mother liquor and mix lanthanum lithium titanate, stirring 6 hours, then add binding agent, vacuumize stirring 2 hours, obtain water system and mix lanthanum lithium titanate cathode size.
Described binding agent includes hydroxypropyl methylcellulose 30% ~ 60%, sodium carboxymethylcellulose 30 ~ 40% and the aqueous suspension 30 ~ 40% containing 60 % by weight butadiene-styrene rubber (SBR) by quality 100%.
Described stabilizer is the composition of monoethanolamine and propionic acid, and the mass ratio of this monoethanolamine and propionic acid is 1:3.
Described dispersant is sodium carboxymethylcellulose pyce.
Described conductive agent includes conductive black, carbon nano-tube and electrically conductive graphite, and its mass ratio is conductive black: carbon nano-tube: electrically conductive graphite=3:5:7.
Described conductive agent is the mixture of Graphene and carbon nano-tube, and the mass ratio of this Graphene and carbon nano-tube is 1:3 ~ 5.
The present invention compared with prior art has obvious advantage and beneficial effect, specific as follows:
1, the present invention mixes in lanthanum lithium titanate cathode size process in preparation water system, on the one hand, mixes lanthanum lithium titanate and adopts deionization water as solvent, be dissolved in by inorganic titanium compound in deionized water, has not only reduced cost but also nontoxic pollution-free; On the other hand, adopt aqueous binder, making whole water system mix lanthanum lithium titanate cathode size nontoxic, pollution-free, is green energy resource truly, fundamentally solves the problems such as safe, the pollution of lithium electricity.
2, adopt aqueous binders the formula of aqueous binder is optimized, not only increase the performance of adhesive, can also effectively solve pole piece containing lithium titanate material because of easy water suction the phenomenon of shedding, greatly improve quality and the useful life thereof of product.
3, the present invention adulterates lanthanum under hydrothermal conditions, improves the uniformity of doping and the electric conductivity of material; Effectively can be improved the performance of negative material by lithium titanate doping lanthanum, improve the specific capacity of lithium titanate material significantly.
Embodiment
Embodiment 1
Water system mixes a preparation method for lanthanum lithium titanate cathode size, comprises the following steps:
Lanthanum lithium titanate is mixed in a, preparation
1) take a certain amount of titanyl sulfate to join in deionized water and dissolve, dissolution time is 2.5 hours, and water temperature controls between 75 ~ 80 DEG C, filters the aqueous solution obtaining clear after dissolving;
2) in above-mentioned configured aqueous solution of titanyle sulfate, add lithium hydroxide, undertaken mixing adding stabilizer by the mol ratio of Li:Ti=1.2:1 simultaneously, described stabilizer is the composition of monoethanolamine and propionic acid, and the mass ratio of this monoethanolamine and propionic acid is 1:3.In this mixed solution, add lanthanum salting liquid, and be that under the condition of 110 DEG C and acidity, hybrid reaction forms colloidal sol in more than 24 hours in temperature;
3) by colloidal sol in vacuum drying oven dry 36 hours, baking temperature is 120 DEG C, after obtaining dry powder grinding, standbyly to burn;
4) at the dry powder high temperature furnace 1200 DEG C after grinding, calcining, calcines 6 hours, must mix lanthanum lithium titanate sample.
B, take raw material by quality 100%: mix lanthanum lithium titanate 47%, binding agent 3%, conductive agent 9%, dispersant 3% and deionized water 38%;
C, in deionized water, add sodium carboxymethylcellulose pyce, stir after 12 hours and place 2 days, obtain methylcellulose mother liquid of sodium, add conductive agent to methylcellulose mother liquid of sodium and mix lanthanum lithium titanate, described conductive agent includes conductive black, carbon nano-tube and electrically conductive graphite, and its mass ratio is conductive black: carbon nano-tube: electrically conductive graphite=3:5:7.
Stir 6 hours, then add binding agent, this binding agent includes hydroxypropyl methylcellulose 30%%, sodium carboxymethylcellulose 30% and the aqueous suspension 40% containing 60 % by weight butadiene-styrene rubber (SBR) by quality 100%; Vacuumize stirring 2 hours, obtain water system and mix lanthanum lithium titanate cathode size.
Take a certain amount of water system and mix lanthanum lithium titanate cathode size, when being dried to half-dried for 80 DEG C by battery pole plates manufacture craft, be compressed in copper foil current collector and made negative plate, then be placed in vacuum drying chamber and dry at 150 DEG C, with lithium sheet for positive pole, form lithium ion battery with above-mentioned material, place 12h test.The discharge capacity of first charge-discharge is 1350mAh/g, and first charge-discharge efficiency can reach 95%, and after 300 circulations, stable discharging capacity is 1130mAh/g.
Embodiment 2
Water system mixes a preparation method for lanthanum lithium titanate cathode size, comprises the following steps:
Lanthanum lithium titanate is mixed in a, preparation
1) take a certain amount of titanyl sulfate to join in deionized water and dissolve, dissolution time is 2.5 hours, and water temperature controls between 75 ~ 80 DEG C, filters the aqueous solution obtaining clear after dissolving;
2) in above-mentioned configured aqueous solution of titanyle sulfate, add lithium hydroxide, undertaken mixing adding stabilizer by the mol ratio of Li:Ti=1.2:1 simultaneously, described stabilizer is the composition of monoethanolamine and propionic acid, and the mass ratio of this monoethanolamine and propionic acid is 1:3.In this mixed solution, add lanthanum salting liquid, and be that under the condition of 110 ~ 150 DEG C and acidity, hybrid reaction forms colloidal sol in more than 24 hours in temperature;
3) by colloidal sol in vacuum drying oven dry 38 hours, baking temperature is 120 DEG C, after obtaining dry powder grinding, standbyly to burn;
4) at the dry powder high temperature furnace 1000 DEG C after grinding, calcining, calcines 7 hours, must mix lanthanum lithium titanate sample.
B, take raw material by quality 100%: mix lanthanum lithium titanate 50%, binding agent 8%, conductive agent 10%, dispersant 7% and deionized water 25%;
C, in deionized water, add sodium carboxymethylcellulose pyce, stir after 12 hours and place 3 days, obtain methylcellulose mother liquid of sodium, add conductive agent to methylcellulose mother liquid of sodium and mix lanthanum lithium titanate, described conductive agent includes conductive black, carbon nano-tube and electrically conductive graphite, and its mass ratio is conductive black: carbon nano-tube: electrically conductive graphite=3:5:7.
Stir 6 hours, then add binding agent, this binding agent includes hydroxypropyl methylcellulose 30%, sodium carboxymethylcellulose 30% and the aqueous suspension 40% containing 60 % by weight butadiene-styrene rubber (SBR) by quality 100%; Vacuumize stirring 2 hours, obtain water system and mix lanthanum lithium titanate cathode size.
Take a certain amount of water system and mix lanthanum lithium titanate cathode size, when being dried to half-dried for 80 DEG C by battery pole plates manufacture craft, be compressed in copper foil current collector and made negative plate, then be placed in vacuum drying chamber and dry at 150 DEG C, with lithium sheet for positive pole, form lithium ion battery with above-mentioned material, place 12h test.The discharge capacity of first charge-discharge is 1380mAh/g, and first charge-discharge efficiency can reach 96%, and after 300 circulations, stable discharging capacity is 1240mAh/g.
Embodiment 3
Water system mixes a preparation method for lanthanum lithium titanate cathode size, comprises the following steps:
Lanthanum lithium titanate is mixed in a, preparation
1) take a certain amount of titanyl sulfate to join in deionized water and dissolve, dissolution time is 2.5 hours, and water temperature controls between 75 ~ 80 DEG C, filters the aqueous solution obtaining clear after dissolving;
2) in above-mentioned configured aqueous solution of titanyle sulfate, add lithium hydroxide, undertaken mixing adding stabilizer by the mol ratio of Li:Ti=1.2:1 simultaneously, described stabilizer is the composition of monoethanolamine and propionic acid, and the mass ratio of this monoethanolamine and propionic acid is 1:3.In this mixed solution, add lanthanum salting liquid, and be that under the condition of 130 DEG C and acidity, hybrid reaction forms colloidal sol in more than 24 hours in temperature;
3) by colloidal sol in vacuum drying oven dry 40 hours, baking temperature is 120 DEG C, after obtaining dry powder grinding, standbyly to burn;
4) at the dry powder high temperature furnace 980 DEG C after grinding, calcining, calcines 9 hours, must mix lanthanum lithium titanate sample.
B, take raw material by quality 100%: mix lanthanum lithium titanate 60%, binding agent 5%, conductive agent 6%, dispersant 5% and deionized water 34%;
C, in deionized water, add sodium carboxymethylcellulose pyce, stir after 12 hours and place 2 ~ 3 days, obtain methylcellulose mother liquid of sodium, add conductive agent to methylcellulose mother liquid of sodium and mix lanthanum lithium titanate, this conductive agent includes conductive black, carbon nano-tube and electrically conductive graphite, its mass ratio is conductive black: carbon nano-tube: electrically conductive graphite=3:5:7, stir 6 hours, add binding agent again, this binding agent includes hydroxypropyl methylcellulose 40%, sodium carboxymethylcellulose 30% and the aqueous suspension 30% containing 60 % by weight butadiene-styrene rubber (SBR) by quality 100%; Vacuumize stirring 2 hours, obtain water system and mix lanthanum lithium titanate cathode size.
Take a certain amount of water system and mix lanthanum lithium titanate cathode size, when being dried to half-dried for 80 DEG C by battery pole plates manufacture craft, be compressed in copper foil current collector and made negative plate, then be placed in vacuum drying chamber and dry at 150 DEG C, with lithium sheet for positive pole, form lithium ion battery with above-mentioned material, place 12h test.The discharge capacity of first charge-discharge is 1230mAh/g, and first charge-discharge efficiency can reach 95%, and after 300 circulations, stable discharging capacity is 1090mAh/g.
Embodiment 4
Water system mixes a preparation method for lanthanum lithium titanate cathode size, comprises the following steps:
Lanthanum lithium titanate is mixed in a, preparation
1) take a certain amount of titanyl sulfate to join in deionized water and dissolve, dissolution time is 2.5 hours, and water temperature controls between 75 ~ 80 DEG C, filters the aqueous solution obtaining clear after dissolving;
2) in above-mentioned configured aqueous solution of titanyle sulfate, add lithium hydroxide, undertaken mixing adding stabilizer by the mol ratio of Li:Ti=1.2:1 simultaneously, described stabilizer is the composition of monoethanolamine and propionic acid, and the mass ratio of this monoethanolamine and propionic acid is 1:3.In this mixed solution, add lanthanum salting liquid, and be that under the condition of 130 DEG C and acidity, hybrid reaction forms colloidal sol in more than 24 hours in temperature;
3) by colloidal sol in vacuum drying oven dry 44 hours, baking temperature is 120 DEG C, after obtaining dry powder grinding, standbyly to burn;
4) at the dry powder high temperature furnace 1100 DEG C after grinding, calcining, calcines 8 hours, must mix lanthanum lithium titanate sample.
B, take raw material by quality 100%: mix lanthanum lithium titanate 55%, binding agent 0.3%, conductive agent 10%, dispersant 7% and deionized water 27.7%;
C, in deionized water, add sodium carboxymethylcellulose pyce, stir after 12 hours and place 2.5 days, obtain methylcellulose mother liquid of sodium, add conductive agent to methylcellulose mother liquid of sodium and mix lanthanum lithium titanate, this conductive agent is the mixture of Graphene and carbon nano-tube, the mass ratio of this Graphene and carbon nano-tube is 1:3, stir 6 hours, add binding agent again, this binding agent includes hydroxypropyl methylcellulose 30%%, sodium carboxymethylcellulose 40% and the aqueous suspension 30% containing 60 % by weight butadiene-styrene rubber (SBR) by quality 100%; Vacuumize stirring 2 hours, obtain water system and mix lanthanum lithium titanate cathode size.
Take a certain amount of water system and mix lanthanum lithium titanate cathode size, when being dried to half-dried for 80 DEG C by battery pole plates manufacture craft, be compressed in copper foil current collector and made negative plate, then be placed in vacuum drying chamber and dry at 150 DEG C, with lithium sheet for positive pole, form lithium ion battery with above-mentioned material, place 12h test.The discharge capacity of first charge-discharge is 1350mAh/g, and first charge-discharge efficiency can reach 98%, and after 300 circulations, stable discharging capacity is 1230mAh/g.
Embodiment 5
Water system mixes a preparation method for lanthanum lithium titanate cathode size, comprises the following steps:
Lanthanum lithium titanate is mixed in a, preparation
1) take a certain amount of titanyl sulfate to join in deionized water and dissolve, dissolution time is 2.5 hours, and water temperature controls between 75 ~ 80 DEG C, filters the aqueous solution obtaining clear after dissolving;
2) in above-mentioned configured aqueous solution of titanyle sulfate, add lithium hydroxide, undertaken mixing adding stabilizer by the mol ratio of Li:Ti=1.2:1 simultaneously, described stabilizer is the composition of monoethanolamine and propionic acid, and the mass ratio of this monoethanolamine and propionic acid is 1:3.In this mixed solution, add lanthanum salting liquid, and be that under the condition of 110 ~ 150 DEG C and acidity, hybrid reaction forms colloidal sol in more than 24 hours in temperature;
3) by colloidal sol in vacuum drying oven dry 46 hours, baking temperature is 120 DEG C, after obtaining dry powder grinding, standbyly to burn;
4) at the dry powder high temperature furnace 980 DEG C after grinding, calcining, calcines 10 hours, must mix lanthanum lithium titanate sample.
B, take raw material by quality 100%: mix lanthanum lithium titanate 47%, binding agent 6%, conductive agent 10%, dispersant 3% and deionized water 34%;
C, in deionized water, add sodium carboxymethylcellulose pyce, stir after 12 hours and place 3 days, obtain methylcellulose mother liquid of sodium, add conductive agent to methylcellulose mother liquid of sodium and mix lanthanum lithium titanate, this conductive agent is the mixture of Graphene and carbon nano-tube, the mass ratio of this Graphene and carbon nano-tube is 1:4, stir 6 hours, add binding agent again, this binding agent includes hydroxypropyl methylcellulose 35%, sodium carboxymethylcellulose 35% and the aqueous suspension 30% containing 60 % by weight butadiene-styrene rubber (SBR) by quality 100%; Vacuumize stirring 2 hours, obtain water system and mix lanthanum lithium titanate cathode size.
Take a certain amount of water system and mix lanthanum lithium titanate cathode size, when being dried to half-dried for 80 DEG C by battery pole plates manufacture craft, be compressed in copper foil current collector and made negative plate, then be placed in vacuum drying chamber and dry at 150 DEG C, with lithium sheet for positive pole, form lithium ion battery with above-mentioned material, place 12h test.The discharge capacity of first charge-discharge is 1260mAh/g, and first charge-discharge efficiency can reach 97%, and after 300 circulations, stable discharging capacity is 1210mAh/g.
Embodiment 6
Water system mixes a preparation method for lanthanum lithium titanate cathode size, comprises the following steps:
Lanthanum lithium titanate is mixed in a, preparation
1) take a certain amount of titanyl sulfate to join in deionized water and dissolve, dissolution time is 2.5 hours, and water temperature controls between 75 ~ 80 DEG C, filters the aqueous solution obtaining clear after dissolving;
2) in above-mentioned configured aqueous solution of titanyle sulfate, add lithium hydroxide, undertaken mixing adding stabilizer by the mol ratio of Li:Ti=1.2:1 simultaneously, described stabilizer is the composition of monoethanolamine and propionic acid, and the mass ratio of this monoethanolamine and propionic acid is 1:3.In this mixed solution, add lanthanum salting liquid, and be that under the condition of 120 DEG C and acidity, hybrid reaction forms colloidal sol in more than 24 hours in temperature;
3) by colloidal sol in vacuum drying oven dry 48 hours, baking temperature is 120 DEG C, after obtaining dry powder grinding, standbyly to burn;
4) at the dry powder high temperature furnace 1150 DEG C after grinding, calcining, calcines 7 hours, must mix lanthanum lithium titanate sample.
B, take raw material by quality 100%: mix lanthanum lithium titanate 52%, binding agent 2%, conductive agent 8%, dispersant 5% and deionized water 33%;
C, in deionized water, add sodium carboxymethylcellulose pyce, stir after 12 hours and place 2 ~ 3 days, obtain methylcellulose mother liquid of sodium, add conductive agent to methylcellulose mother liquid of sodium and mix lanthanum lithium titanate, this conductive agent is the mixture of Graphene and carbon nano-tube, the mass ratio of this Graphene and carbon nano-tube is 1:5, stir 6 hours, add binding agent again, this binding agent includes hydroxypropyl methylcellulose 30% ~ 60%, sodium carboxymethylcellulose 30 ~ 40% and the aqueous suspension 30 ~ 40% containing 60 % by weight butadiene-styrene rubber (SBR) by quality 100%; Vacuumize stirring 2 hours, obtain water system and mix lanthanum lithium titanate cathode size.
Take a certain amount of water system and mix lanthanum lithium titanate cathode size, when being dried to half-dried for 80 DEG C by battery pole plates manufacture craft, be compressed in copper foil current collector and made negative plate, then be placed in vacuum drying chamber and dry at 150 DEG C, with lithium sheet for positive pole, form lithium ion battery with above-mentioned material, place 12h test.The discharge capacity of first charge-discharge is 1280mAh/g, and first charge-discharge efficiency can reach 96%, and after 300 circulations, stable discharging capacity is 1130mAh/g.
The above, it is only preferred embodiment of the present invention, not technical scope of the present invention is imposed any restrictions, thus every according to technical spirit of the present invention to any trickle amendment made for any of the above embodiments, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (6)
1. water system mixes a preparation method for lanthanum lithium titanate cathode size, it is characterized in that: the raw material of described cathode size include mixes lanthanum lithium titanate, binding agent, conductive agent, dispersant and deionized water, and its preparation method comprises the following steps:
Lanthanum lithium titanate is mixed in a, preparation
1) take a certain amount of titanyl sulfate to join in deionized water and dissolve, dissolution time is 2.5 hours, and water temperature controls between 75 ~ 80 DEG C, filters the aqueous solution obtaining clear after dissolving;
2) in above-mentioned configured aqueous solution of titanyle sulfate, lithium hydroxide is added, undertaken mixing adding stabilizer by the mol ratio of Li:Ti=1.2:1 simultaneously, in this mixed solution, add lanthanum salting liquid, and be that under the condition of 110 ~ 150 DEG C and acidity, hybrid reaction forms colloidal sol in more than 24 hours in temperature;
3) by colloidal sol in vacuum drying oven dry 36 ~ 48 hours, baking temperature is 120 DEG C, after obtaining dry powder grinding, standbyly to burn;
4) at the dry powder high temperature furnace 950 ~ 1200 DEG C after grinding, calcining, calcines 6 ~ 10 hours, must mix lanthanum lithium titanate sample;
B, take raw material by quality 100%: mix lanthanum lithium titanate 47 ~ 60%, binding agent 0.3 ~ 8%, conductive agent 6 ~ 10%, dispersant 3 ~ 7% and deionized water 25 ~ 40%; Described binding agent includes hydroxypropyl methylcellulose 30% ~ 60%, sodium carboxymethylcellulose 30 ~ 40% and the aqueous suspension 30 ~ 40% containing 60 % by weight butadiene-styrene rubber by quality 100%;
C, in deionized water, add dispersant, stir after 12 hours and place 2 ~ 3 days, obtain dispersant mother liquor, add conductive agent to dispersant mother liquor and mix lanthanum lithium titanate, stirring 6 hours, then add binding agent, vacuumize stirring 2 hours, obtain water system and mix lanthanum lithium titanate cathode size.
2. a kind of water system mixes the preparation method of lanthanum lithium titanate cathode size according to claim 1, it is characterized in that: described stabilizer is the composition of monoethanolamine and propionic acid, and the mass ratio of this monoethanolamine and propionic acid is 1:3.
3. a kind of water system mixes the preparation method of lanthanum lithium titanate cathode size according to claim 1, it is characterized in that: described dispersant is sodium carboxymethylcellulose pyce.
4. a kind of water system mixes the preparation method of lanthanum lithium titanate cathode size according to claim 1, it is characterized in that: described conductive agent includes conductive black, carbon nano-tube and electrically conductive graphite, its mass ratio is conductive black: carbon nano-tube: electrically conductive graphite=3:5:7.
5. a kind of water system mixes the preparation method of lanthanum lithium titanate cathode size according to claim 1, it is characterized in that: described conductive agent is the mixture of Graphene and carbon nano-tube, and the mass ratio of this Graphene and carbon nano-tube is 1:3 ~ 5.
6. a kind of water system mixes the preparation method of lanthanum lithium titanate cathode size according to claim 1, it is characterized in that: described lanthanum salting liquid is that lanthanum sulfate solution and lanthanum nitrate hexahydrate mix.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310441411.XA CN103545526B (en) | 2013-09-25 | 2013-09-25 | A kind of water system mixes the preparation method of lanthanum lithium titanate cathode size |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310441411.XA CN103545526B (en) | 2013-09-25 | 2013-09-25 | A kind of water system mixes the preparation method of lanthanum lithium titanate cathode size |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103545526A CN103545526A (en) | 2014-01-29 |
| CN103545526B true CN103545526B (en) | 2016-01-27 |
Family
ID=49968766
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310441411.XA Active CN103545526B (en) | 2013-09-25 | 2013-09-25 | A kind of water system mixes the preparation method of lanthanum lithium titanate cathode size |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103545526B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105702922A (en) * | 2016-01-22 | 2016-06-22 | 浙江极力动力新能源有限公司 | Zinc oxide modified graphene negative electrode paste of lithium ion battery and preparation method of negative electrode paste |
| CN110534707A (en) * | 2019-08-19 | 2019-12-03 | 江苏特丰新材料科技有限公司 | A kind of preparation method of lithium titanate slurry |
| CN114335544A (en) * | 2022-01-05 | 2022-04-12 | 湖南大晶新材料有限公司 | Water-based binder, lithium ion battery cathode material and lithium ion battery |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102856556A (en) * | 2012-08-23 | 2013-01-02 | 青岛瀚博电子科技有限公司 | Preparation method of cathode slurry for aquo-lithium titanate dynamical type battery |
| CN102969491A (en) * | 2012-10-24 | 2013-03-13 | 中国海洋石油总公司 | Preparation method of cathode material lithium titanate used for lithium battery |
| CN103151508A (en) * | 2013-03-12 | 2013-06-12 | 上海大学 | Lanthanum lithium titanate doped composite negative electrode material of lithium ion battery and preparation method thereof |
-
2013
- 2013-09-25 CN CN201310441411.XA patent/CN103545526B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102856556A (en) * | 2012-08-23 | 2013-01-02 | 青岛瀚博电子科技有限公司 | Preparation method of cathode slurry for aquo-lithium titanate dynamical type battery |
| CN102969491A (en) * | 2012-10-24 | 2013-03-13 | 中国海洋石油总公司 | Preparation method of cathode material lithium titanate used for lithium battery |
| CN103151508A (en) * | 2013-03-12 | 2013-06-12 | 上海大学 | Lanthanum lithium titanate doped composite negative electrode material of lithium ion battery and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103545526A (en) | 2014-01-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107275606B (en) | Carbon-coated spinel lithium manganate nanocomposite and preparation method and application thereof | |
| WO2019091067A1 (en) | Nitrogen-sulfur co-doped carbon coated tin/molybdenum disulfide composite material for lithium ion battery and preparation method therefor | |
| CN104466135A (en) | Method for coating conductive polymer on Ni-Co-Mn acid lithium positive electrode material | |
| CN103779559B (en) | Anode material for lithium-ion batteries Li 2mn 1-Xm xsiO 4the preparation method of/C | |
| CN105552324A (en) | Preparation method for lithium iron phosphate coated lithium nickel cobalt manganese composite material | |
| CN103151508B (en) | Mix composite cathode material for lithium ion cell of lanthanum lithium titanate and preparation method thereof | |
| CN103682316A (en) | Method for preparing ternary anode material of long-service-life and high-capacity lithium ion battery | |
| CN104201363A (en) | Carbon-coated Li3VO4 lithium ion battery anode material and preparation method thereof | |
| CN104600296A (en) | Preparation method of Se-C positive electrode composite material of lithium-selenium battery | |
| CN108123136B (en) | Lead-carbon battery composite negative electrode additive, lead-carbon battery negative electrode, preparation and application | |
| CN104795555A (en) | Aqueous-solution sodium-ion battery and cathode material, preparation method and application thereof | |
| CN108172893A (en) | A kind of lithium ion battery | |
| CN105140493A (en) | Nickel cobalt lithium manganate/graphene/carbon nano tube composite cathode materials and preparation method thereof | |
| CN104362319A (en) | Preparation method of porous tin-carbon composite negative material | |
| CN101841022A (en) | Method for preparing cathode material lithium manganate of lithium ion battery | |
| CN107946564B (en) | Rich in Na4Mn2O5/Na0.7MnO2Composite material and preparation method and application thereof | |
| CN102185163B (en) | Method for preparing inorganic aqueous solution lithium ion battery system by using monocrystal LiMnO (lithium manganese oxide) nanowire | |
| CN103545526B (en) | A kind of water system mixes the preparation method of lanthanum lithium titanate cathode size | |
| CN103035908A (en) | Method for preparing negative electrode plate lead plaster for power type lead acid storage battery | |
| CN103474658B (en) | Flexible lithium ion secondary battery negative pole of a kind of lithium niobate composite carbon nanometer tube and preparation method thereof and application | |
| CN104577079A (en) | Method for preparing tin-carbon composite negative electrode material | |
| CN110649263A (en) | Nickel-ion battery lithium vanadium phosphate positive electrode material, sol-gel preparation method and application | |
| CN104495941A (en) | Preparation method of sodium-ion battery positive electrode material | |
| CN110336017A (en) | A kind of modified lithium manganate and its preparation method and application | |
| WO2019104948A1 (en) | Molybdenum doping-modified lithium manganese oxide composite material, preparation method therefor and lithium ion battery |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20170523 Address after: Yongan City, Fujian province 366000 Gong Chuan Zhen Shui Dong Park No. 38 Patentee after: FUJIAN XFH BATTERY MATERIAL CO., LTD. Address before: 523000 Guangdong city of Dongguan Province Huang Sheng Zhenjiang road before the industrial zone C building C Dongguan City Cheung Fenghua Battery Material Co Ltd Patentee before: Dongguan Xiangfenghua Battery Material Co., Ltd. |