CN106129413A - A kind of modified polythiophene solar energy lithium electricity positive electrode and preparation method thereof - Google Patents
A kind of modified polythiophene solar energy lithium electricity positive electrode and preparation method thereof Download PDFInfo
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- CN106129413A CN106129413A CN201610686126.8A CN201610686126A CN106129413A CN 106129413 A CN106129413 A CN 106129413A CN 201610686126 A CN201610686126 A CN 201610686126A CN 106129413 A CN106129413 A CN 106129413A
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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
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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Abstract
The invention discloses a kind of modified polythiophene solar energy lithium electricity positive electrode and preparation method thereof, described modified polythiophene solar energy lithium electricity positive electrode, according to the primary raw material of weight portion be: modified polythiophene 35 45 parts, lithium acetate 12 18 parts, methyl methacrylate 8 10 parts, tributyl phosphate 26 parts, trishydroxymethylaminomethane 26 parts, nanometer phenyl-magnesium-chloride 0.5 1.5 parts；The preparation method of described modified polythiophene is: mixed with p-methyl benzenesulfonic acid, poly-aluminum chloride-magnesium, sodium sulfide by polythiophene, the lower 135 DEG C of reaction 2h of 7MPa, is vacuum dried and get final product.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 more than 90%；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 circulation 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.
Description
Technical field
The present invention relates to a kind of lithium electro-technical field, specifically a kind of modified polythiophene solar energy lithium electricity positive electrode and
Preparation method.
Background technology
Lithium ion battery has that running voltage is high, specific energy high, has extended cycle life, electric discharge lightweight, white less, memoryless effect
Should be with cost performance advantages of higher, it has also become high power electric vehicle, artificial satellite, the master of Aero-Space lamp field rechargeable type power supply
Object to be selected.It addition, the system of positive and negative pole material composition has a common feature to discharge the later stage exactly, especially at electric discharge knot
Shu Shi, voltage declines very fast, namely inside this voltage range, the capacity of lithium ion battery almost without.
Summary of the invention
It is an object of the invention to provide a kind of modified polythiophene solar energy lithium electricity positive electrode and preparation method thereof, to solve
The problem certainly proposed in above-mentioned background technology.
For achieving the above object, the present invention provides following technical scheme:
A kind of modified polythiophene solar energy lithium electricity positive electrode, according to the primary raw material of weight portion be: modified polythiophene 35-
45 parts, lithium acetate 12-18 part, methyl methacrylate 8-10 part, tributyl phosphate 2-6 part, trishydroxymethylaminomethane 2-6
Part, nanometer phenyl-magnesium-chloride 0.5-1.5 part；The preparation method of described modified polythiophene is: by polythiophene and p-methyl benzenesulfonic acid, gather
Close magnesium chloride, sodium sulfide mixing, the lower 135 DEG C of reaction 2h of 7MPa, it is vacuum dried and get final product.
As the further scheme of the present invention: described modified polythiophene solar energy lithium electricity positive electrode, according to weight portion
Primary raw material is: modified polythiophene 39-42 part, lithium acetate 14-17 part, methyl methacrylate 8-10 part, tributyl phosphate 2-6
Part, trishydroxymethylaminomethane 2-6 part, nanometer phenyl-magnesium-chloride 0.8-1.1 part；The preparation method of described modified polythiophene is:
Polythiophene is mixed with p-methyl benzenesulfonic acid, poly-aluminum chloride-magnesium, sodium sulfide, the lower 135 DEG C of reaction 2h of 7MPa, be vacuum dried and get final product.
As the further scheme of the present invention: described modified polythiophene solar energy lithium electricity positive electrode, according to weight portion
Primary raw material is: modified polythiophene 40 parts, lithium acetate 16 parts, methyl methacrylate 9 parts, tributyl phosphate 4 parts, trihydroxy methyl
Aminomethane 5 parts, nanometer phenyl-magnesium-chloride 0.9 part；The preparation method of described modified polythiophene is: by polythiophene and to toluene sulphur
Acid, poly-aluminum chloride-magnesium, sodium sulfide mixing, the lower 135 DEG C of reaction 2h of 7MPa, it is vacuum dried and get final product.
As the further scheme of the present invention: the purity of described polythiophene is more than 99.9%.
As the further scheme of the present invention: the mesh number of described trishydroxymethylaminomethane is 1200 mesh.
As the further scheme of the present invention: the mesh number of described poly-aluminum chloride-magnesium is 1200 mesh.
The preparation method of a kind of modified polythiophene solar energy lithium electricity positive electrode, concretely comprises the following steps:
(1) first, modified polythiophene is mixed with lithium acetate, the most under nitrogen protection, is heated to 120 DEG C-160 DEG C also
Stirring 60min-90min, makes semi-finished product；
(2) last, by semi-finished product and methyl methacrylate, tributyl phosphate, trishydroxymethylaminomethane, nanometer phenyl
Magnesium chloride carries out mixing stirring, and speed of agitator is 400r/min, and mixing time is 45min, carries out melted mixing subsequently, and vacuum is done
Dry and get final product.
As the further scheme of the present invention: step (1) is heated to 144 DEG C and stirs 80min.
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
More than 90%；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, extruding,
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,
Obviously, 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 modified polythiophene solar energy lithium electricity positive electrode, according to the primary raw material of weight portion be: modified polythiophene 35
Part, lithium acetate 12 parts, methyl methacrylate 8 parts, tributyl phosphate 2 parts, trishydroxymethylaminomethane 2 parts, nanometer phenylchloride
Change 0.5 part of magnesium；The preparation method of described modified polythiophene is: mixed with p-methyl benzenesulfonic acid, poly-aluminum chloride-magnesium, sodium sulfide by polythiophene
Close, the lower 135 DEG C of reaction 2h of 7MPa, be vacuum dried and get final product；The purity of described polythiophene is more than 99.9%；Described trihydroxy methyl ammonia
The mesh number of methylmethane is 1200 mesh；The mesh number of described poly-aluminum chloride-magnesium is 1200 mesh.
The preparation method of a kind of modified polythiophene solar energy lithium electricity positive electrode, concretely comprises the following steps:
(1) first, modified polythiophene is mixed with lithium acetate, the most under nitrogen protection, is heated to 120 DEG C and stirs
60min, makes semi-finished product；
(2) last, by semi-finished product and methyl methacrylate, tributyl phosphate, trishydroxymethylaminomethane, nanometer phenyl
Magnesium chloride carries out mixing stirring, and speed of agitator is 400r/min, and mixing time is 45min, carries out melted mixing subsequently, and vacuum is done
Dry and get final product.
Embodiment 2
A kind of modified polythiophene solar energy lithium electricity positive electrode, according to the primary raw material of weight portion be: modified polythiophene 39
Part, lithium acetate 14 parts, methyl methacrylate 8 parts, tributyl phosphate 2 parts, trishydroxymethylaminomethane 2 parts, nanometer phenylchloride
Change 0.8 part of magnesium；The preparation method of described modified polythiophene is: mixed with p-methyl benzenesulfonic acid, poly-aluminum chloride-magnesium, sodium sulfide by polythiophene
Close, the lower 135 DEG C of reaction 2h of 7MPa, be vacuum dried and get final product；The purity of described polythiophene is more than 99.9%；Described trihydroxy methyl ammonia
The mesh number of methylmethane is 1200 mesh；The mesh number of described poly-aluminum chloride-magnesium is 1200 mesh.
The preparation method of a kind of modified polythiophene solar energy lithium electricity positive electrode, concretely comprises the following steps:
(1) first, modified polythiophene is mixed with lithium acetate, the most under nitrogen protection, is heated to 120 DEG C and stirs
60min, makes semi-finished product；
(2) last, by semi-finished product and methyl methacrylate, tributyl phosphate, trishydroxymethylaminomethane, nanometer phenyl
Magnesium chloride carries out mixing stirring, and speed of agitator is 400r/min, and mixing time is 45min, carries out melted mixing subsequently, and vacuum is done
Dry and get final product.
Embodiment 3
A kind of modified polythiophene solar energy lithium electricity positive electrode, according to the primary raw material of weight portion be: modified polythiophene 40
Part, lithium acetate 16 parts, methyl methacrylate 9 parts, tributyl phosphate 4 parts, trishydroxymethylaminomethane 5 parts, nanometer phenylchloride
Change 0.9 part of magnesium；The preparation method of described modified polythiophene is: mixed with p-methyl benzenesulfonic acid, poly-aluminum chloride-magnesium, sodium sulfide by polythiophene
Close, the lower 135 DEG C of reaction 2h of 7MPa, be vacuum dried and get final product；The purity of described polythiophene is more than 99.9%；Described trihydroxy methyl ammonia
The mesh number of methylmethane is 1200 mesh；The mesh number of described poly-aluminum chloride-magnesium is 1200 mesh.
The preparation method of a kind of modified polythiophene solar energy lithium electricity positive electrode, concretely comprises the following steps:
(1) first, modified polythiophene is mixed with lithium acetate, the most under nitrogen protection, is heated to 144 DEG C and stirs
80min, makes semi-finished product；
(2) last, by semi-finished product and methyl methacrylate, tributyl phosphate, trishydroxymethylaminomethane, nanometer phenyl
Magnesium chloride carries out mixing stirring, and speed of agitator is 400r/min, and mixing time is 45min, carries out melted mixing subsequently, and vacuum is done
Dry and get final product.
Embodiment 4
A kind of modified polythiophene solar energy lithium electricity positive electrode, according to the primary raw material of weight portion be: modified polythiophene 42
Part, lithium acetate 17 parts, methyl methacrylate 10 parts, tributyl phosphate 6 parts, trishydroxymethylaminomethane 6 parts, nanometer phenylchloride
Change 1.1 parts of magnesium；The preparation method of described modified polythiophene is: mixed with p-methyl benzenesulfonic acid, poly-aluminum chloride-magnesium, sodium sulfide by polythiophene
Close, the lower 135 DEG C of reaction 2h of 7MPa, be vacuum dried and get final product；The purity of described polythiophene is more than 99.9%；Described trihydroxy methyl ammonia
The mesh number of methylmethane is 1200 mesh；The mesh number of described poly-aluminum chloride-magnesium is 1200 mesh.
The preparation method of a kind of modified polythiophene solar energy lithium electricity positive electrode, concretely comprises the following steps:
(1) first, modified polythiophene is mixed with lithium acetate, the most under nitrogen protection, is heated to 160 DEG C and stirs
90min, makes semi-finished product；
(2) last, by semi-finished product and methyl methacrylate, tributyl phosphate, trishydroxymethylaminomethane, nanometer phenyl
Magnesium chloride carries out mixing stirring, and speed of agitator is 400r/min, and mixing time is 45min, carries out melted mixing subsequently, and vacuum is done
Dry and get final product.
Embodiment 5
A kind of modified polythiophene solar energy lithium electricity positive electrode, according to the primary raw material of weight portion be: modified polythiophene 45
Part, lithium acetate 18 parts, methyl methacrylate 10 parts, tributyl phosphate 6 parts, trishydroxymethylaminomethane 6 parts, nanometer phenylchloride
Change 1.5 parts of magnesium；The preparation method of described modified polythiophene is: mixed with p-methyl benzenesulfonic acid, poly-aluminum chloride-magnesium, sodium sulfide by polythiophene
Close, the lower 135 DEG C of reaction 2h of 7MPa, be vacuum dried and get final product；The purity of described polythiophene is more than 99.9%；Described trihydroxy methyl ammonia
The mesh number of methylmethane is 1200 mesh；The mesh number of described poly-aluminum chloride-magnesium is 1200 mesh.
The preparation method of a kind of modified polythiophene solar energy lithium electricity positive electrode, concretely comprises the following steps:
(1) first, modified polythiophene is mixed with lithium acetate, the most under nitrogen protection, is heated to 160 DEG C and stirs
90min, makes semi-finished product；
(2) last, by semi-finished product and methyl methacrylate, tributyl phosphate, trishydroxymethylaminomethane, nanometer phenyl
Magnesium chloride carries out mixing stirring, and speed of agitator is 400r/min, and mixing time is 45min, carries out melted mixing subsequently, and vacuum is done
Dry and get final product.
Comparative example 1
A kind of polythiophene solar energy lithium electricity positive electrode, according to the primary raw material of weight portion be: polythiophene 40 parts, lithium acetate
16 parts, methyl methacrylate 9 parts, trishydroxymethylaminomethane 5 parts, nanometer phenyl-magnesium-chloride 0.9 part；Described polythiophene pure
Degree is more than 99.9%；The mesh number of described trishydroxymethylaminomethane is 1200 mesh.
The preparation method of a kind of polythiophene solar energy lithium electricity positive electrode, concretely comprises the following steps:
(1) first, polythiophene is mixed with lithium acetate, the most under nitrogen protection, is heated to 144 DEG C and stirs 80min,
Make semi-finished product；
(2) last, semi-finished product are carried out with methyl methacrylate, trishydroxymethylaminomethane, nanometer phenyl-magnesium-chloride
Mixing stirring, speed of agitator is 400r/min, and mixing time is 45min, carries out melted mixing subsequently, is drying to obtain.
Comparative example 2
A kind of polythiophene solar energy lithium electricity positive electrode, according to the primary raw material of weight portion be: polythiophene 40 parts, lithium acetate
16 parts, methyl methacrylate 9 parts；The purity of described polythiophene is more than 99.9%.
The preparation method of a kind of polythiophene solar energy lithium electricity positive electrode, concretely comprises the following steps:
(1) first, polythiophene is mixed with lithium acetate, the most under nitrogen protection, is heated to 144 DEG C and stirs 80min,
Make semi-finished product；
(2) last, semi-finished product and methyl methacrylate are carried out mixing stirring, speed of agitator is 400r/min, stirring
Time is 45min, carries out melted mixing subsequently, is drying to obtain.
Comparative example 3
A kind of modified polythiophene solar energy lithium electricity positive electrode, according to the primary raw material of weight portion be: modified polythiophene 40
Part, lithium acetate 16 parts, methyl methacrylate 9 parts, trishydroxymethylaminomethane 5 parts, nanometer phenyl-magnesium-chloride 0.9 part；Described
The preparation method of modified polythiophene is: mixed with p-methyl benzenesulfonic acid, poly-aluminum chloride-magnesium, sodium sulfide by polythiophene, lower 135 DEG C of 7MPa
Reaction 2h, is vacuum dried and get final product；The purity of described polythiophene is more than 99.9%；The mesh number of described trishydroxymethylaminomethane is
1200 mesh；The mesh number of described poly-aluminum chloride-magnesium is 1200 mesh.
The preparation method of a kind of modified polythiophene solar energy lithium electricity positive electrode, concretely comprises the following steps:
(1) first, modified polythiophene is mixed with lithium acetate, the most under nitrogen protection, is heated to 144 DEG C and stirs
80min, makes semi-finished product；
(2) last, semi-finished product are carried out with methyl methacrylate, trishydroxymethylaminomethane, nanometer phenyl-magnesium-chloride
Mixing stirring, speed of agitator is 400r/min, and mixing time is 45min, carries out melted mixing subsequently, is drying to obtain.
Test experience
Solar energy lithium electricity positive electrode embodiment 1-5 and comparative example 1-3 prepared is prepared as 1665132 model lithium ions
Electrokinetic cell (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
More than 90%；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, extruding,
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, Er Qie
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 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 wraps
Containing an independent technical scheme, this narrating mode of description is only that for clarity sake those skilled in the art should
Description can also be formed those skilled in the art through appropriately combined as an entirety, the technical scheme in each embodiment
May be appreciated other embodiments.
Claims (8)
1. a modified polythiophene solar energy lithium electricity positive electrode, it is characterised in that be according to the primary raw material of weight portion: modified
Polythiophene 35-45 part, lithium acetate 12-18 part, methyl methacrylate 8-10 part, tributyl phosphate 2-6 part, trihydroxy methyl amino
Methane 2-6 part, nanometer phenyl-magnesium-chloride 0.5-1.5 part；The preparation method of described modified polythiophene is: by polythiophene and to toluene
Sulfonic acid, poly-aluminum chloride-magnesium, sodium sulfide mix, the lower 135 DEG C of reaction 2h of 7MPa, are vacuum dried and get final product.
Modified polythiophene solar energy lithium electricity positive electrode the most according to claim 1, it is characterised in that the poly-thiophene of described modification
Fen solar energy lithium electricity positive electrode, according to the primary raw material of weight portion be: modified polythiophene 39-42 part, lithium acetate 14-17 part,
Methyl methacrylate 8-10 part, tributyl phosphate 2-6 part, trishydroxymethylaminomethane 2-6 part, nanometer phenyl-magnesium-chloride 0.8-
1.1 part；The preparation method of described modified polythiophene is: mixed with p-methyl benzenesulfonic acid, poly-aluminum chloride-magnesium, sodium sulfide by polythiophene,
The lower 135 DEG C of reaction 2h of 7MPa, are vacuum dried and get final product.
Modified polythiophene solar energy lithium electricity positive electrode the most according to claim 1 and 2, it is characterised in that described modification
Polythiophene solar energy lithium electricity positive electrode, according to the primary raw material of weight portion be: modified polythiophene 40 parts, lithium acetate 16 parts, first
Base acrylic acid methyl ester. 9 parts, tributyl phosphate 4 parts, trishydroxymethylaminomethane 5 parts, nanometer phenyl-magnesium-chloride 0.9 part；Described change
Property polythiophene preparation method be: polythiophene is mixed with p-methyl benzenesulfonic acid, poly-aluminum chloride-magnesium, sodium sulfide, 7MPa lower 135 DEG C anti-
Answer 2h, be vacuum dried and get final product.
Modified polythiophene solar energy lithium electricity positive electrode the most according to claim 3, it is characterised in that described polythiophene
Purity is more than 99.9%.
Modified polythiophene solar energy lithium electricity positive electrode the most according to claim 4, it is characterised in that described trihydroxy methyl
The mesh number of aminomethane is 1200 mesh.
Modified polythiophene solar energy lithium electricity positive electrode the most according to claim 5, it is characterised in that described polyaluminium
The mesh number of magnesium is 1200 mesh.
7. a preparation method for the modified polythiophene solar energy lithium electricity positive electrode as described in claim 1-6 is arbitrary, it is special
Levy and be, concretely comprise the following steps:
(1) first, modified polythiophene is mixed with lithium acetate, the most under nitrogen protection, is heated to 120 DEG C-160 DEG C and stirs
60min-90min, makes semi-finished product；
(2) last, by semi-finished product and methyl methacrylate, tributyl phosphate, trishydroxymethylaminomethane, nanometer tetraphenylphosphonium chloride
Magnesium carries out mixing stirring, and speed of agitator is 400r/min, and mixing time is 45min, carries out melted mixing subsequently, and vacuum drying is i.e.
?.
The preparation method of modified polythiophene solar energy lithium electricity positive electrode the most according to claim 7, it is characterised in that step
(1) is heated to 144 DEG C suddenly and stirs 80min.
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