CN105958044A - Modified graphene-doped lithium cobalt oxide electrode material and preparation method thereof - Google Patents
Modified graphene-doped lithium cobalt oxide electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a modified graphene-doped lithium cobalt oxide electrode material and a preparation method thereof. The modified graphene-doped lithium cobalt oxide electrode material is prepared from the following components in parts by weight: 30-40 parts of modified graphene, 28-44 parts of lithium cobalt oxide, 12-18 parts of lithium iron phosphate, 8-10 parts of acrylonitrile, 4-6 parts of nitropyridine and 2-6 parts of sulfosalicylic acid. A prepared lithium ion battery has excellent cycle performance, and the capacity for 2000 times of 1C charging and discharging cycle at normal temperature is maintained to be more than 90%; the capacity for 6C discharging is more than 98% of 1C capacity; the battery cannot break out a fire or explode under a 3C/10V overcharging test; the cycle performance under high temperature is excellent, and the capacity for 1000 times of 1C charging and discharging cycle at the temperature of 60 DEG C is maintained to be more than 88%; and the battery has good safety performance, and cannot explode or break out a fire in the tests of needling, extrusion, overcharging, overdischarging and the like.
Description
Technical field
The present invention relates to a kind of cell art, the cobalt acid lithium electric material of a kind of modified graphene doping and preparation thereof
Method.
Background technology
Lithium ion battery is since commercialization, and the positive electrode used by lithium ion battery is mostly cobalt acid lithium, cobalt acid lithium or ternary
Material etc., its component mainly active material adds conductive agent adding additives again, described active material be cobalt acid lithium, cobalt acid lithium or
Ternary etc.；Negative material uses graphite to be active substance mostly, then adds some conductive agents and binding agent；Its advantage is capacity
Higher, have extended cycle life, but promoter manganese be deficient, expensive and has toxicity, therefore seek price excellent honest and clean, performance can
Lean on, eco-friendly positive electrode becomes the important research direction of lithium ion battery.Spinel-type with cobalt acid lithium as representative is just
Pole material and ternary material layered oxide are in the past decade widely studied, but the defect system being individually present due to it
About their development prospect.It addition, the system of positive and negative pole material composition has a common feature to discharge the later stage exactly, especially
Being at the end of electric discharge, voltage declines very fast, and namely inside this voltage range, the capacity of lithium ion battery is almost
Without.
Summary of the invention
It is an object of the invention to provide cobalt acid lithium electric material of a kind of modified graphene doping and preparation method thereof, on solving
State the problem proposed in background technology.
For achieving the above object, the present invention provides following technical scheme:
A kind of cobalt acid lithium electric material of modified graphene doping, according to the primary raw material of weight portion be: modified graphene 30-40
Part, cobalt acid lithium 28-44 part, LiFePO4 12-18 part, acrylonitrile 8-10 part, nitropyridine 4-6 part, sulfosalisylic
Acid 2-6 part；The preparation method of described modified graphene is: by anti-with dimethyl sulfoxide, glucosan after Graphene oxidation processes
Should, then react with acrylic acid methyl ester., tripolycyanamide, polyvinyl alcohol, glyceramine successively every 5min, vacuum filtration is dried
Obtain.
As the further scheme of the present invention: the cobalt acid lithium electric material of described modified graphene doping, main according to weight portion
Raw material is: modified graphene 33-37 part, cobalt acid lithium 34-41 part, LiFePO4 13-17 part, acrylonitrile 8-10 part,
Nitropyridine 4-6 part, sulfosalicylic acid 2-6 part；The preparation method of described modified graphene is: by Graphene oxidation processes
React with dimethyl sulfoxide, glucosan afterwards, then every 5min successively with acrylic acid methyl ester., tripolycyanamide, polyvinyl alcohol,
Glyceramine reacts, and vacuum filtration is drying to obtain.
As the further scheme of the present invention: the cobalt acid lithium electric material of described modified graphene doping, main according to weight portion
Raw material is: modified graphene 35 parts, cobalt acid lithium 38 parts, LiFePO4 15 parts, acrylonitrile 9 parts, nitropyridine 5 parts,
Sulfosalicylic acid 5 parts；The preparation method of described modified graphene is: by after Graphene oxidation processes with dimethyl sulfoxide, Portugal
Formose Reaction, then react with acrylic acid methyl ester., tripolycyanamide, polyvinyl alcohol, glyceramine successively every 5min, vacuum is taken out
Filter is drying to obtain.
As the further scheme of the present invention: the purity of described Graphene is more than 99.9%.
As the further scheme of the present invention: the mesh number of described cobalt acid lithium is 800 mesh.
As the further scheme of the present invention: the mesh number of described LiFePO4 is 1200 mesh.
The preparation method of the cobalt acid lithium electric material of a kind of modified graphene doping, concretely comprises the following steps:
(1) first, modified graphene is stirred with cobalt acid lithium, LiFePO4, adds concentrated sulphuric acid under nitrogen protection,
At 10 DEG C-20 DEG C, stir 30-60min, make semi-finished product；
(2) last, semi-finished product and acrylonitrile, nitropyridine, sulfosalicylic acid are carried out mixing stirring, speed of agitator is
320r/min, mixing time is 30min, then centrifuge washing, and vacuum lyophilization at a temperature of being subsequently placed at 4 DEG C to obtain final product.
As the further scheme of the present invention: step (1) stirs at 15 DEG C 47min.
Compared with prior art, the invention has the beneficial effects as follows:
Prepared lithium ion battery has the cycle performance of excellence, and under room temperature, 2000 capacity of 1C charge and discharge circulation are maintained at 90%
Above；Under 6C multiplying power, electric discharge is more than the 98% of 1C capacity；3C/10V overcharges test, and battery is the most on fire does not explodes；High temperature follows
Ring is excellent, and at 60 DEG C, 1000 capacity of 1C charge and discharge circulation are maintained at more than 88%；There is good security performance, acupuncture,
Extrude, overcharge, cross put etc. test do not explode, the most on fire.
Detailed description of the invention
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, aobvious
So, described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under not making creative work premise, all
Belong to the scope of protection of the invention.
Embodiment 1
A kind of cobalt acid lithium electric material of modified graphene doping, according to the primary raw material of weight portion be: modified graphene 30 parts,
Cobalt acid lithium 28 parts, LiFePO4 12 parts, acrylonitrile 8 parts, nitropyridine 4 parts, sulfosalicylic acid 2 parts；Described modification
The preparation method of Graphene is: will react with dimethyl sulfoxide, glucosan after Graphene oxidation processes, then depends on every 5min
Secondary reacting with acrylic acid methyl ester., tripolycyanamide, polyvinyl alcohol, glyceramine, vacuum filtration is drying to obtain；Described Graphene
Purity is more than 99.9%；The mesh number of described cobalt acid lithium is 800 mesh；The mesh number of described LiFePO4 is 1200 mesh.
The preparation method of the cobalt acid lithium electric material of a kind of modified graphene doping, concretely comprises the following steps:
(1) first, modified graphene is stirred with cobalt acid lithium, LiFePO4, adds concentrated sulphuric acid under nitrogen protection,
At 10 DEG C, stir 30min, make semi-finished product；
(2) last, semi-finished product and acrylonitrile, nitropyridine, sulfosalicylic acid are carried out mixing stirring, speed of agitator is
320r/min, mixing time is 30min, then centrifuge washing, and vacuum lyophilization at a temperature of being subsequently placed at 4 DEG C to obtain final product.
Embodiment 2
A kind of cobalt acid lithium electric material of modified graphene doping, according to the primary raw material of weight portion be: modified graphene 33 parts,
Cobalt acid lithium 34 parts, LiFePO4 13 parts, acrylonitrile 8 parts, nitropyridine 4 parts, sulfosalicylic acid 2 parts；Described modification
The preparation method of Graphene is: will react with dimethyl sulfoxide, glucosan after Graphene oxidation processes, then depends on every 5min
Secondary reacting with acrylic acid methyl ester., tripolycyanamide, polyvinyl alcohol, glyceramine, vacuum filtration is drying to obtain；Described Graphene
Purity is more than 99.9%；The mesh number of described cobalt acid lithium is 800 mesh；The mesh number of described LiFePO4 is 1200 mesh.
The preparation method of the cobalt acid lithium electric material of a kind of modified graphene doping, concretely comprises the following steps:
(1) first, modified graphene is stirred with cobalt acid lithium, LiFePO4, adds concentrated sulphuric acid under nitrogen protection,
At 10 DEG C, stir 30min, make semi-finished product；
(2) last, semi-finished product and acrylonitrile, nitropyridine, sulfosalicylic acid are carried out mixing stirring, speed of agitator is
320r/min, mixing time is 30min, then centrifuge washing, and vacuum lyophilization at a temperature of being subsequently placed at 4 DEG C to obtain final product.
Embodiment 3
A kind of cobalt acid lithium electric material of modified graphene doping, according to the primary raw material of weight portion be: modified graphene 35 parts,
Cobalt acid lithium 38 parts, LiFePO4 15 parts, acrylonitrile 9 parts, nitropyridine 5 parts, sulfosalicylic acid 5 parts；Described modification
The preparation method of Graphene is: will react with dimethyl sulfoxide, glucosan after Graphene oxidation processes, then depends on every 5min
Secondary reacting with acrylic acid methyl ester., tripolycyanamide, polyvinyl alcohol, glyceramine, vacuum filtration is drying to obtain；Described Graphene
Purity is more than 99.9%；The mesh number of described cobalt acid lithium is 800 mesh；The mesh number of described LiFePO4 is 1200 mesh.
The preparation method of the cobalt acid lithium electric material of a kind of modified graphene doping, concretely comprises the following steps:
(1) first, modified graphene is stirred with cobalt acid lithium, LiFePO4, adds concentrated sulphuric acid under nitrogen protection,
At 15 DEG C, stir 45min, make semi-finished product；
(2) last, semi-finished product and acrylonitrile, nitropyridine, sulfosalicylic acid are carried out mixing stirring, speed of agitator is
320r/min, mixing time is 30min, then centrifuge washing, and vacuum lyophilization at a temperature of being subsequently placed at 4 DEG C to obtain final product.
Embodiment 4
A kind of cobalt acid lithium electric material of modified graphene doping, according to the primary raw material of weight portion be: modified graphene 37 parts,
Cobalt acid lithium 41 parts, LiFePO4 17 parts, acrylonitrile 10 parts, nitropyridine 6 parts, sulfosalicylic acid 6 parts；Described change
The preparation method of property Graphene is: will react with dimethyl sulfoxide, glucosan after Graphene oxidation processes, then every 5min
Reacting with acrylic acid methyl ester., tripolycyanamide, polyvinyl alcohol, glyceramine successively, vacuum filtration is drying to obtain；Described Graphene
Purity be more than 99.9%；The mesh number of described cobalt acid lithium is 800 mesh；The mesh number of described LiFePO4 is 1200 mesh.
The preparation method of the cobalt acid lithium electric material of a kind of modified graphene doping, concretely comprises the following steps:
(1) first, modified graphene is stirred with cobalt acid lithium, LiFePO4, adds concentrated sulphuric acid under nitrogen protection,
At 20 DEG C, stir 60min, make semi-finished product；
(2) last, semi-finished product and acrylonitrile, nitropyridine, sulfosalicylic acid are carried out mixing stirring, speed of agitator is
320r/min, mixing time is 30min, then centrifuge washing, and vacuum lyophilization at a temperature of being subsequently placed at 4 DEG C to obtain final product.
Embodiment 5
A kind of cobalt acid lithium electric material of modified graphene doping, according to the primary raw material of weight portion be: modified graphene 40 parts,
Cobalt acid lithium 44 parts, LiFePO4 18 parts, acrylonitrile 10 parts, nitropyridine 6 parts, sulfosalicylic acid 6 parts；Described change
The preparation method of property Graphene is: will react with dimethyl sulfoxide, glucosan after Graphene oxidation processes, then every 5min
Reacting with acrylic acid methyl ester., tripolycyanamide, polyvinyl alcohol, glyceramine successively, vacuum filtration is drying to obtain；Described Graphene
Purity be more than 99.9%；The mesh number of described cobalt acid lithium is 800 mesh；The mesh number of described LiFePO4 is 1200 mesh.
The preparation method of the cobalt acid lithium electric material of a kind of modified graphene doping, concretely comprises the following steps:
(1) first, modified graphene is stirred with cobalt acid lithium, LiFePO4, adds concentrated sulphuric acid under nitrogen protection,
At 20 DEG C, stir 60min, make semi-finished product；
(2) last, semi-finished product and acrylonitrile, nitropyridine, sulfosalicylic acid are carried out mixing stirring, speed of agitator is
320r/min, mixing time is 30min, then centrifuge washing, and vacuum lyophilization at a temperature of being subsequently placed at 4 DEG C to obtain final product.
Comparative example 1
A kind of cobalt acid lithium electric material of Graphene doping, according to the primary raw material of weight portion be: Graphene 35 parts, cobalt acid lithium
38 parts, LiFePO4 15 parts, acrylonitrile 9 parts, nitropyridine 5 parts, sulfosalicylic acid 5 parts；The mesh of described cobalt acid lithium
Number is 800 mesh；The mesh number of described LiFePO4 is 1200 mesh.
The preparation method of the cobalt acid lithium electric material of a kind of Graphene doping, concretely comprises the following steps:
(1) first, Graphene is stirred with cobalt acid lithium, LiFePO4, makes semi-finished product；
(2) last, semi-finished product and acrylonitrile, nitropyridine, sulfosalicylic acid are carried out mixing stirring, speed of agitator is
320r/min, mixing time is 30min, then centrifuge washing, and vacuum lyophilization at a temperature of being subsequently placed at 4 DEG C to obtain final product.
Comparative example 2
A kind of cobalt acid lithium electric material, according to the primary raw material of weight portion be: cobalt acid lithium 38 parts, LiFePO4 15 parts, propylene
Nitrile 9 parts；The mesh number of described cobalt acid lithium is 800 mesh；The mesh number of described LiFePO4 is 1200 mesh.
The preparation method of a kind of cobalt acid lithium electric material, concretely comprises the following steps:
(1) first, cobalt acid lithium and LiFePO4 are stirred, make semi-finished product；
(2) last, semi-finished product and acrylonitrile are carried out mixing stirring, speed of agitator is 320r/min, and mixing time is 30min,
Then centrifuge washing, vacuum lyophilization at a temperature of being subsequently placed at 4 DEG C, to obtain final product.
Comparative example 3
A kind of cobalt acid lithium electric material of modified graphene doping, according to the primary raw material of weight portion be: modified graphene 35 parts,
Cobalt acid lithium 38 parts, LiFePO4 15 parts, acrylonitrile 9 parts, nitropyridine 5 parts, sulfosalicylic acid 5 parts；Described modification
The preparation method of Graphene is: will react with dimethyl sulfoxide, glucosan after Graphene oxidation processes, then depends on every 5min
Secondary reacting with acrylic acid methyl ester., tripolycyanamide, polyvinyl alcohol, glyceramine, vacuum filtration is drying to obtain；Described Graphene
Purity is more than 99.9%；The mesh number of described cobalt acid lithium is 800 mesh；The mesh number of described LiFePO4 is 1200 mesh.
The preparation method of the cobalt acid lithium electric material of a kind of modified graphene doping, concretely comprises the following steps:
(1) first, modified graphene is stirred with cobalt acid lithium, LiFePO4, makes semi-finished product；
(2) last, semi-finished product and acrylonitrile, nitropyridine, sulfosalicylic acid are carried out mixing stirring, speed of agitator is
320r/min, mixing time is 30min, then centrifuge washing, and vacuum lyophilization at a temperature of being subsequently placed at 4 DEG C to obtain final product.
Test experience
Cobalt acid lithium electricity positive electrode embodiment 1-5 and comparative example 1-3 prepared is prepared as 1665132 model lithium ion powers
Battery (the lamination soft-package battery of model H16*W65*L132mm), compacted density is at 3.0g/cm3Above, volume energy is close
Degree is at more than 450Wh/L；Battery core is under 3.0V-4.2V voltage, and 1C electric discharge gram volume plays more than 120mAh/g.
Prepared lithium ion battery has the cycle performance of excellence, and under room temperature, 2000 capacity of 1C charge and discharge circulation are maintained at 90%
Above；Under 6C multiplying power, electric discharge is more than the 98% of 1C capacity；3C/10V overcharges test, and battery is the most on fire does not explodes；High temperature follows
Ring is excellent, and at 60 DEG C, 1000 capacity of 1C charge and discharge circulation are maintained at more than 88%；There is good security performance, acupuncture,
Extrude, overcharge, cross put etc. test do not explode, the most on fire.Concrete test result is shown in Table 1:
Table 1
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, and do not carrying on the back
In the case of the spirit or essential attributes of the present invention, it is possible to realize the present invention in other specific forms.Therefore, no matter from
From the point of view of which point, all should regard embodiment as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all by fall in the implication of equivalency and scope of claim
Change is included in the present invention.
Although moreover, it will be appreciated that this specification is been described by according to embodiment, but the most each embodiment only comprises
One independent technical scheme, this narrating mode of description is only the most for clarity sake, and those skilled in the art should be by
Description is as an entirety, and the technical scheme in each embodiment can also be through appropriately combined, and forming those skilled in the art can
With other embodiments understood.
Claims (8)
1. the cobalt acid lithium electric material of a modified graphene doping, it is characterised in that according to the primary raw material of weight portion be: change
Property Graphene 30-40 part, cobalt acid lithium 28-44 part, LiFePO4 12-18 part, acrylonitrile 8-10 part, nitropyridine 4-6
Part, sulfosalicylic acid 2-6 part；The preparation method of described modified graphene is: by sub-with dimethyl after Graphene oxidation processes
Sulfone, glucosan react, then react with acrylic acid methyl ester., tripolycyanamide, polyvinyl alcohol, glyceramine successively every 5min,
Vacuum filtration is drying to obtain.
The cobalt acid lithium electric material of modified graphene the most according to claim 1 doping, it is characterised in that described modified stone
The cobalt acid lithium electric material of ink alkene doping, according to the primary raw material of weight portion be: modified graphene 33-37 part, cobalt acid lithium 34-41
Part, LiFePO4 13-17 part, acrylonitrile 8-10 part, nitropyridine 4-6 part, sulfosalicylic acid 2-6 part；Described change
The preparation method of property Graphene is: will react with dimethyl sulfoxide, glucosan after Graphene oxidation processes, then every 5min
Reacting with acrylic acid methyl ester., tripolycyanamide, polyvinyl alcohol, glyceramine successively, vacuum filtration is drying to obtain.
Modified graphene the most according to claim 1 and 2 doping cobalt acid lithium electric material, it is characterised in that described in change
Property Graphene doping cobalt acid lithium electric material, according to the primary raw material of weight portion be: modified graphene 35 parts, cobalt acid lithium 38
Part, LiFePO4 15 parts, acrylonitrile 9 parts, nitropyridine 5 parts, sulfosalicylic acid 5 parts；Described modified graphene
Preparation method is: will react with dimethyl sulfoxide, glucosan after Graphene oxidation processes, then every 5min successively with propylene
Acid methyl ester, tripolycyanamide, polyvinyl alcohol, glyceramine reaction, vacuum filtration is drying to obtain.
The cobalt acid lithium electric material of modified graphene the most according to claim 3 doping, it is characterised in that described Graphene
Purity be more than 99.9%.
The cobalt acid lithium electric material of modified graphene the most according to claim 4 doping, it is characterised in that described cobalt acid lithium
Mesh number be 800 mesh.
The cobalt acid lithium electric material of modified graphene the most according to claim 5 doping, it is characterised in that described iron phosphate
The mesh number of lithium is 1200 mesh.
7. a preparation method for the cobalt acid lithium electric material of the modified graphene doping as described in claim 1-6 is arbitrary, it is special
Levy and be, concretely comprise the following steps:
(1) first, modified graphene is stirred with cobalt acid lithium, LiFePO4, adds concentrated sulphuric acid under nitrogen protection,
At 10 DEG C-20 DEG C, stir 30-60min, make semi-finished product；
(2) last, semi-finished product and acrylonitrile, nitropyridine, sulfosalicylic acid are carried out mixing stirring, speed of agitator is
320r/min, mixing time is 30min, then centrifuge washing, and vacuum lyophilization at a temperature of being subsequently placed at 4 DEG C to obtain final product.
The preparation method of the cobalt acid lithium electric material of modified graphene the most according to claim 7 doping, it is characterised in that
Step (1) stirs at 15 DEG C 45min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107579247A (en) * | 2017-09-17 | 2018-01-12 | 长沙仲善新能源科技有限公司 | Compound lithium cobaltate cathode material of a kind of graphene and preparation method thereof |
| CN110756211A (en) * | 2019-09-29 | 2020-02-07 | 北京石墨烯技术研究院有限公司 | Oxygen electrode catalyst and preparation method and application thereof |
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| CN102527333B (en) * | 2011-12-19 | 2013-10-23 | 山东大学 | Modified graphene oxide, preparation method and application thereof |
| CN103241735B (en) * | 2013-05-17 | 2014-11-05 | 南京理工大学 | Hybrid nanomaterial of melamine chemically-modified graphene oxide and preparation method of hybrid nanomaterial |
| CN104064771A (en) * | 2014-06-18 | 2014-09-24 | 青岛乾运高科新材料股份有限公司 | Efficient graphene coated lithium cobalt oxide battery cathode material and preparation method thereof |
| CN105036124A (en) * | 2015-08-22 | 2015-11-11 | 苏州正业昌智能科技有限公司 | Method for preparing graphene from polysaccharide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107579247A (en) * | 2017-09-17 | 2018-01-12 | 长沙仲善新能源科技有限公司 | Compound lithium cobaltate cathode material of a kind of graphene and preparation method thereof |
| CN110756211A (en) * | 2019-09-29 | 2020-02-07 | 北京石墨烯技术研究院有限公司 | Oxygen electrode catalyst and preparation method and application thereof |
| CN110756211B (en) * | 2019-09-29 | 2020-08-25 | 北京石墨烯技术研究院有限公司 | Oxygen electrode catalyst and preparation method and application thereof |
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