CN106252624A - Cathode of lithium battery poriferous titanium dioxide and preparation method thereof - Google Patents
Cathode of lithium battery poriferous titanium dioxide and preparation method thereof Download PDFInfo
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Abstract
The invention provides the preparation method of a kind of cathode of lithium battery poriferous titanium dioxide, first poriferous titanium dioxide first product is prepared, afterwards poriferous titanium dioxide first product is prepared, after low boiling point organic solvent and halogen-containing silane coupler hybrid reaction by a certain percentage, the poriferous titanium dioxide that silane coupler surface is modified, finally the poriferous titanium dioxide that silane coupler surface is modified is suspended in low boiling point organic solvent, add the imidazoles containing substituent group, it is immersed in after drying in hexafluorophosphoric acid saline solution through washing after reaction, last heat treatment under the atmosphere of inert gases of 500～600 DEG C.The inventive method is simple, the cathode of lithium battery poriferous titanium dioxide prepared, and its Surface coating has N/P/F/Si codope carbon-coating, has higher theoretical specific capacity, electric conductivity, and capability retention is high.
Description
Technical field
The present invention relates to a kind of titanium dioxide and preparation method thereof, particularly to a kind of cathode of lithium battery porous silica
Titanium and preparation method thereof.
Background technology
Along with rapid development of economy, facing mankind the severe challenge of energy crisis and environmental pollution, and countries in the world are all
At the green energy resource constantly seeking more clean environment firendly.Wherein, energy density is high, voltage is high, circulation owing to it has for lithium battery
Life-span length, self-discharge rate are low, memory-less effect, discharge voltage are stable, discharge and recharge is quick and the advantage such as environmental protection, are widely used in
The electronics field such as mobile phone, portable computer, photographing unit, video camera, and application is still among constantly extension,
Become the main selection of sustainable electrokinetic cell, be described as the ideal source of 21 century.
As the main body of storage lithium, negative material plays critically important effect in lithium ion battery, and its capacity is impact electricity
One of key factor of tankage, the quality of its performance directly affects battery capacity and the service life cycle of lithium ion battery.
At present, the lithium ion battery of commercialization mainly uses graphite or modified graphite as negative material.But, the embedding lithium of theory of graphite
Heap(ed) capacity is only 372mAh/g, and irreversible loss is big first, multiplying power discharging property is poor, it addition, when Lithium-ion embeding, portion
The solvent divided also can follow embedding, is susceptible to structural damage；As the improvement to above-mentioned material, nanometer transition metal aoxidizes
Thing is due to its higher theoretical specific capacity, and capability retention is high, causes the extensive concern of researchers, but this kind of transition
Metal oxide materials has bigger volumetric expansion and contraction change during Lithium-ion embeding and abjection, thus causes
The efflorescence of electrode material, and then lose electrical contact with collector, the cycle performance of this type of material of strong influence and application.
Secondly, compared with traditional graphite cathode material, these materials have poor electron conductivity.
Accordingly, it would be desirable to seek more efficient way, prepare the stable higher theoretical specific capacity that has, electric conductivity, and
And the lithium ion battery negative material that capability retention is high.
Summary of the invention
For overcoming defect of the prior art, it is desirable to provide a kind of, there is higher theoretical specific capacity, electric conductivity,
And the cathode of lithium battery poriferous titanium dioxide that capability retention is high, its preparation method is provided simultaneously.The present invention is by following
Scheme realizes:
The preparation method of a kind of cathode of lithium battery poriferous titanium dioxide, comprises the following steps,
Titanium source is joined mixing 0.5～1h in alcohol by I, is slowly added to alkali metal acetate afterwards, mixes 2～3h, by molten
Liquid is transferred in the hydrothermal reaction kettle of polyvinyl fluoride liner, reacts 15～24h at 200～250 DEG C；Through deionized water after cooling
With dehydrated alcohol cyclic washing, it is dried 18～24 hours in the vacuum drying oven of 70～80 DEG C；The product that this step prepares is
Poriferous titanium dioxide first product；
Product, low boiling point organic solvent and halogen-containing silane coupler that step I prepares are risen under mixing condition by II
Temperature, to 65～75 DEG C, reacts 4～6h, and product separates and is dried；The product that this step prepares is that silane coupler surface is modified
Poriferous titanium dioxide；
The product that step II prepares is suspended in low boiling point organic solvent by III, adds containing the imidazoles of substituent group, mixing 4～
8 hours, washing with low boiling point organic solvent afterwards, general washing times is 3～5 times, in the vacuum drying oven of 70～80 DEG C
Be dried after 18～24 hours be dipped in mass concentration be 1.0～2.0%, temperature be in the hexafluorophosphoric acid saline solution of 60～80 DEG C 54～
72 hours, heat treatment 3～5h under the atmosphere of inert gases of 500～600 DEG C.
Further, in described step I, titanium source preferably is selected from the one in titanium tetrachloride, butyl titanate；Alcohol has selected from second
One in alcohol, propanol, isopropanol, butanol, ethylene glycol, glycerol；Alkali metal acetate preferably is selected from sodium acetate, potassium acetate
A kind of；Halogen-containing silane coupler is preferably chloromethyl triethoxysilane, 2-chloroethyl triethoxysilane, γ-chlorine third
One in ethyl triethoxy silicane alkane, γ-r-chloropropyl trimethoxyl silane.
Further, described step III, the imidazoles containing substituent group preferably is selected from 2-phenylimidazole, 2-methylimidazole, 2-isopropyl
One in base imidazoles；Hexafluorophosphate preferably is selected from the one in sodium hexafluoro phosphate, Potassium Hexafluorophosphate.
In described step I, the mass ratio of titanium source, alcohol and alkali metal acetate is preferably 1:(20～30): 3.
Low boiling point organic solvent in described step II, step III is preferably the one in dichloromethane, acetone, ether.
Further, one or more during described noble gas is preferably nitrogen, argon, helium.
Further, in described step II, product, low boiling point organic solvent and the silane coupler that step I prepares
Mass ratio is preferably 1:(3～5): (2～3).
Further, in described step III, product, low boiling point organic solvent and the miaow containing substituent group that step II prepares
The mass ratio of azoles is preferably 2:(5～8): (2～3).
A kind of cathode of lithium battery poriferous titanium dioxide, uses cathode of lithium battery poriferous titanium dioxide as above
Preparation method prepares, and poriferous titanium dioxide Surface coating has N/P/F/Si codope carbon-coating.Described N/P/F/Si codope
The thickness of carbon-coating is preferably 10～20 nanometers.
The present invention compared with prior art has the advantage that
(1) preparation method of the cathode of lithium battery poriferous titanium dioxide of the present invention is simple, and raw material is easy to get, processing ease,
Less demanding to equipment, with low cost, it is simple to large-scale production；
(2) preparation method of the cathode of lithium battery poriferous titanium dioxide of the present invention, due to the stability of loose structure, for
The volumetric expansion of titanium dioxide itself provides machinery support force, during Lithium-ion embeding and abjection, can effectively keep
The integrity of the structure of material, therefore the titanium dioxide of loose structure has stable chemical property；
(3) preparation method of the cathode of lithium battery poriferous titanium dioxide of the present invention, at poriferous titanium dioxide Surface coating
There is the carbon-coating that N/F/Si/P adulterates, the specific capacity of material, electric conductivity can be improved, and the knot of the titanium dioxide of loose structure can be stablized
Structure, it is to avoid have a bigger volumetric expansion during Lithium-ion embeding and abjection and electrode material that contraction change causes
Efflorescence.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, but the invention is not limited in the statement of embodiment.
Embodiment 1
The preparation method of a kind of cathode of lithium battery poriferous titanium dioxide, comprises the following steps,
12g titanium tetrachloride is joined mixing 0.5h in the beaker containing 240g ethylene glycol by I, is slowly added to 36g vinegar afterwards
Acid sodium, remixes 2h, transfers the solution in the hydrothermal reaction kettle of polyvinyl fluoride liner, reacts 15h at 200 DEG C；After cooling
Through deionized water and dehydrated alcohol cyclic washing, it is dried 24 hours in the vacuum drying oven of 70 DEG C, prepares poriferous titanium dioxide
Head product；
II poriferous titanium dioxide head product, 30g dichloromethane and the 20g chloromethyl triethoxysilicane that 10g step I is prepared
Alkane joins in reactor, uses ultra-sonic dispersion method to be uniformly dispersed, is warming up to 65 DEG C under mixing condition, reacts 4h, product
Separate and be dried, prepare the poriferous titanium dioxide that silane coupler surface is modified；
The poriferous titanium dioxide that III silane coupler surface 8g step II prepared is modified is suspended in 20g acetone, adds
Enter 16g 2-phenylimidazole, after mixing 4 hours, wash 3 times with ether, soak after being dried 24 hours in the vacuum drying oven of 70 DEG C
In mass concentration be 1.0%, temperature be the hexafluorophosphoric acid sodium solution of 60 DEG C in 72 hours, heat under the nitrogen atmosphere of 500 DEG C
Process 3h.
Make the cathode of lithium battery poriferous titanium dioxide prepared in aforementioned manners, wrap on the surface of poriferous titanium dioxide
Being covered with N/P/F/Si codope carbon-coating, recording N/P/F/Si codope carbon layers having thicknesses is 10nm.Prepared cathode of lithium battery is used
Poriferous titanium dioxide, Super P and the Kynoar PVDF mix homogeneously of 8:1:1 in mass ratio, instill N-first the most inside
Base pyrrolidone solution (NMP), uniform stirring is become the pasty state viscous solution of thickness, is then evenly coated in by viscous solution by coating machine
On Copper Foil, the Copper Foil coated is dried in 100 DEG C of vacuum drying ovens 24h (removing nmp solvent and a small amount of residual moisture), cold
But take out to room temperature, be compacted after with microtome Copper Foil made the disk of a diameter of 14cm, as cathode pole piece, finally exist
It is full of in the glove box of argon and is assembled into 2016 button cells.By the button cell that assembles on LAND battery test system with
0.1C rate charge-discharge 100 encloses, and records specific discharge capacity and is about 930mAh/g.
Embodiment 2
The preparation method of a kind of cathode of lithium battery poriferous titanium dioxide, comprises the following steps,
12g butyl titanate is joined mixing 0.6h in the beaker containing 260g ethanol by I, is slowly added to 36g vinegar afterwards
Acid potassium, remixes 2.5h, transfers the solution in the hydrothermal reaction kettle of polyvinyl fluoride liner, reacts 18h at 220 DEG C；Cooling
By deionized water and dehydrated alcohol cyclic washing, it is dried 20 hours in the vacuum drying oven of 75 DEG C, prepares porous silica
Titanium head product；
II poriferous titanium dioxide head product, 40g acetone and the 25g γ-chloropropyl triethoxy silicon that 10g step I is prepared
Alkane joins in reactor, uses ultra-sonic dispersion method to be uniformly dispersed, is warming up to 70 DEG C under mixing condition, reacts 5h, product
Separate and be dried, prepare the poriferous titanium dioxide that silane coupler surface is modified；
The poriferous titanium dioxide that III silane coupler surface 8g step II prepared is modified is suspended in 24g dichloromethane
In, add 10g 2-methylimidazole, after mixing 6 hours, wash 5 times with dichloromethane, be dried in the vacuum drying oven of 75 DEG C
Be dipped in after 20 hours mass concentration be 1.5%, temperature be in the hexafluorophosphoric acid potassium solution of 65 DEG C 65 hours, then at the argon of 550 DEG C
Atmosphere encloses lower heat treatment 4h.
Make the cathode of lithium battery poriferous titanium dioxide prepared in aforementioned manners, wrap on the surface of poriferous titanium dioxide
Being covered with N/P/F/Si codope carbon-coating, recording N/P/F/Si codope carbon layers having thicknesses is 15nm.Prepared cathode of lithium battery is used
Poriferous titanium dioxide is prepared as cathode pole piece by the method in embodiment 1 and is fabricated to button cell, by button cell at LAND
Enclose with 0.1C rate charge-discharge 100 on battery test system, record specific discharge capacity and be about 928mAh/g.
Embodiment 3
The preparation method of a kind of cathode of lithium battery poriferous titanium dioxide, comprises the following steps,
12g titanium tetrachloride is joined mixing 0.7h in the beaker containing 300g isopropanol by I, is slowly added to 36g vinegar afterwards
Acid sodium, remixes 2.4h, transfers the solution in the hydrothermal reaction kettle of polyvinyl fluoride liner, reacts 20h at 230 DEG C；Cooling
By deionized water and dehydrated alcohol cyclic washing, it is dried 22 hours in the vacuum drying oven of 77 DEG C, prepares porous silica
Titanium head product；
II poriferous titanium dioxide head product, 45g ether and the 28g 2-chloroethyl triethoxysilicane that 10g step I is prepared
Alkane joins in reactor, uses ultra-sonic dispersion method to be uniformly dispersed, is warming up to 68 DEG C under mixing condition, reacts 5h, product
Separate and be dried, prepare the poriferous titanium dioxide that silane coupler surface is modified；
The poriferous titanium dioxide that III silane coupler surface 8g step II prepared is modified is suspended in 26g acetone, adds
Enter 18g 2-isopropyl base imidazoles, after mixing 7 hours, with washing with acetone 4 times, be dried 18 hours in the vacuum drying oven of 80 DEG C
After be dipped in mass concentration be 1.8%, temperature be in the hexafluorophosphoric acid sodium solution of 70 DEG C 60 hours, then at the helium atmosphere of 600 DEG C
Lower heat treatment 3.5h.
Make the cathode of lithium battery poriferous titanium dioxide prepared in aforementioned manners, wrap on the surface of poriferous titanium dioxide
Being covered with N/P/F/Si codope carbon-coating, recording N/P/F/Si codope carbon layers having thicknesses is 18nm.Prepared cathode of lithium battery is used
Poriferous titanium dioxide is prepared as cathode pole piece by the method in embodiment 1 and is fabricated to button cell, by button cell at LAND
Enclose with 0.1C rate charge-discharge 100 on battery test system, record specific discharge capacity and be about 928.5mAh/g.
Embodiment 4
The preparation method of a kind of cathode of lithium battery poriferous titanium dioxide, comprises the following steps,
12g butyl titanate is joined mixing 0.9h in the beaker containing 340g glycerol by I, is slowly added to 36g afterwards
Potassium acetate, remixes 2.7h, transfers the solution in the hydrothermal reaction kettle of polyvinyl fluoride liner, reacts 23h at 240 DEG C；Cold
But through deionized water and dehydrated alcohol cyclic washing after, it is dried 18 hours in the vacuum drying oven of 80 DEG C, prepares porous dioxy
Change titanium head product；
II poriferous titanium dioxide head product, 45g dichloromethane and the 30g γ-chloropropyl trimethoxy that 10g step I is prepared
Base silane joins in reactor, uses ultra-sonic dispersion method to be uniformly dispersed, is warming up to 72 DEG C under mixing condition, reaction
5.5h, product separates and is dried, prepares the poriferous titanium dioxide that silane coupler surface is modified；
The poriferous titanium dioxide that III silane coupler surface 8g step II prepared is modified is suspended in 30g acetone, adds
Enter 29g 2-methylimidazole, after mixing 7.5 hours, wash 5 times with ether, after being dried 20 hours in the vacuum drying oven of 78 DEG C
Be dipped in mass concentration be 2.0%, temperature be in the hexafluorophosphoric acid sodium solution of 60 DEG C 58 hours, under the helium atmosphere of 520 DEG C
Heat treatment 4h.
Make the cathode of lithium battery poriferous titanium dioxide prepared in aforementioned manners, wrap on the surface of poriferous titanium dioxide
Being covered with N/P/F/Si codope carbon-coating, recording N/P/F/Si codope carbon layers having thicknesses is 20nm.Prepared cathode of lithium battery is used
Poriferous titanium dioxide is prepared as cathode pole piece by the method in embodiment 1 and is fabricated to button cell, by button cell at LAND
Enclose with 0.1C rate charge-discharge 100 on battery test system, record specific discharge capacity and be about 929mAh/g.
Embodiment 5
The preparation method of a kind of cathode of lithium battery poriferous titanium dioxide, comprises the following steps,
12g butyl titanate is joined mixing 1.0h in the beaker containing 360g glycerol by I, is slowly added to 36g afterwards
Sodium acetate, remixes 3h, transfers the solution in the hydrothermal reaction kettle of polyvinyl fluoride liner, reacts 24h at 250 DEG C；Cooling
By deionized water and dehydrated alcohol cyclic washing, it is dried 24 hours in the vacuum drying oven of 78 DEG C, prepares porous silica
Titanium head product；
II poriferous titanium dioxide head product, 50g dichloromethane and the 30g chloromethyl triethoxysilicane that 10g step I is prepared
Alkane joins in reactor, uses ultra-sonic dispersion method to be uniformly dispersed, is warming up to 75 DEG C under mixing condition, reacts 6h, product
Separate and be dried, prepare the poriferous titanium dioxide that silane coupler surface is modified；
The poriferous titanium dioxide that III silane coupler surface 8g step II prepared is modified is suspended in 32g ether, adds
Enter 12g 2-phenylimidazole, after mixing 8 hours, wash 5 times with ether, soak after being dried 20 hours in the vacuum drying oven of 78 DEG C
In mass concentration be 2.0%, temperature be the hexafluorophosphoric acid sodium solution of 70 DEG C in 72 hours, heat under the helium atmosphere of 550 DEG C
Process 4h.
Make the cathode of lithium battery poriferous titanium dioxide prepared in aforementioned manners, wrap on the surface of poriferous titanium dioxide
Being covered with N/P/F/Si codope carbon-coating, recording N/P/F/Si codope carbon layers having thicknesses is 17nm.Prepared cathode of lithium battery is used
Poriferous titanium dioxide is prepared as cathode pole piece by the method in embodiment 1 and is fabricated to button cell, by button cell at LAND
Enclosing with 0.1C rate charge-discharge 100 on battery test system, recording specific discharge capacity is 928mAh/g.
The above, only presently preferred embodiments of the present invention, not the present invention is made any pro forma restriction；All
The those of ordinary skill of the industry all can implement the present invention described in by specification swimmingly；But, all skills being familiar with this specialty
Art personnel in the range of without departing from technical solution of the present invention, available disclosed above technology contents and make a little more
The equivalent variations moved, modify and develop, is the Equivalent embodiments of the present invention；Meanwhile, all substantial technological pair according to the present invention
The change of any equivalent variations that above example is made, modify and differentiation etc., all still fall within the guarantor of technical scheme
Within the scope of protecting.
Claims (10)
1. the preparation method of a cathode of lithium battery poriferous titanium dioxide, it is characterised in that: comprise the following steps,
Titanium source is joined mixing 0.5～1h in alcohol by I, is slowly added to alkali metal acetate afterwards, mixes 2～3h, turned by solution
Move on in the hydrothermal reaction kettle of polyvinyl fluoride liner, at 200～250 DEG C, react 15～24h；Through washing vacuum after cooling
It is dried；
Product, low boiling point organic solvent and halogen-containing silane coupler that step I prepares are warming up under mixing condition by II
65～75 DEG C, reaction 4～6h, separated dry；
The product that step II prepares is suspended in low boiling point organic solvent by III, adds the imidazoles containing substituent group, and mixing 4～8 is little
Time, after through low boiling point organic solvent washing vacuum drying after, be dipped in mass concentration be 1.0～2.0%, temperature be 60～
In the hexafluorophosphoric acid saline solution of 80 DEG C 54～72 hours, heat treatment under the atmosphere of inert gases of 500～600 DEG C.
The preparation method of a kind of cathode of lithium battery poriferous titanium dioxide the most as claimed in claim 1, it is characterised in that: described
In step I, titanium source is the one in titanium tetrachloride, butyl titanate；Alcohol be ethanol, propanol, isopropanol, butanol, ethylene glycol, third
One in triol；Alkali metal acetate is the one in sodium acetate, potassium acetate；Halogen-containing silane coupler is chloromethyl three
In Ethoxysilane, 2-chloroethyl triethoxysilane, γ-chloropropyl triethoxysilane, γ-r-chloropropyl trimethoxyl silane
One.
The preparation method of a kind of cathode of lithium battery poriferous titanium dioxide the most as claimed in claim 1, it is characterised in that: described
Step III, the imidazoles containing substituent group is the one in 2-phenylimidazole, 2-methylimidazole, 2 isopropyl imidazole；Hexafluorophosphate
For the one in sodium hexafluoro phosphate, Potassium Hexafluorophosphate.
The preparation method of a kind of cathode of lithium battery poriferous titanium dioxide the most as claimed in claim 1, it is characterised in that: described
In step I, the mass ratio of titanium source, alcohol and alkali metal acetate is 1:(20～30): 3.
The preparation method of a kind of cathode of lithium battery poriferous titanium dioxide the most as claimed in claim 1, it is characterised in that: described
Low boiling point organic solvent in step II, step III is the one in dichloromethane, acetone, ether.
The preparation method of a kind of cathode of lithium battery poriferous titanium dioxide the most as claimed in claim 1, it is characterised in that: described
Noble gas is one or more in nitrogen, argon, helium.
The preparation method of a kind of cathode of lithium battery poriferous titanium dioxide the most as claimed in claim 1, it is characterised in that: in institute
Stating in step II, the mass ratio of product, low boiling point organic solvent and silane coupler that step I prepares is 1:(3～5): (2～
3)。
8. the preparation method of a kind of cathode of lithium battery poriferous titanium dioxide as described in as arbitrary in claim 1～7, its feature exists
In: in described step III, the mass ratio of product, low boiling point organic solvent and the imidazoles containing substituent group that step II prepares is 2:(5
～8): (2～3).
9. a cathode of lithium battery poriferous titanium dioxide, it is characterised in that: use as arbitrary in claim 1～8 as described in lithium
The preparation method of battery cathode poriferous titanium dioxide prepares, and poriferous titanium dioxide Surface coating has N/P/F/Si codope
Carbon-coating.
10. cathode of lithium battery poriferous titanium dioxide as claimed in claim 9, it is characterised in that: described N/P/F/Si is co-doped with
The thickness of miscellaneous carbon-coating is 10～20 nanometers.
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| CN106784714A (en) * | 2016-12-29 | 2017-05-31 | 陕西煤业化工技术研究院有限责任公司 | A kind of silicon-based composite anode material for Li-ion battery and preparation method thereof |
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| CN109244340A (en) * | 2018-09-12 | 2019-01-18 | 肇庆市华师大光电产业研究院 | A kind of lithium-sulfur cell functionality diaphragm coating material and preparation method thereof |
| CN109244340B (en) * | 2018-09-12 | 2021-07-13 | 肇庆市华师大光电产业研究院 | Functional diaphragm coating material of lithium-sulfur battery and preparation method thereof |
| CN116274330A (en) * | 2023-03-22 | 2023-06-23 | 江苏暨之阳环保科技有限公司 | Method for repairing organic pollutant polluted soil |
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