CN109888220A - A method of lithium cell cathode material is prepared to be pyrolyzed large biological molecule - Google Patents
A method of lithium cell cathode material is prepared to be pyrolyzed large biological molecule Download PDFInfo
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Abstract
The invention discloses a kind of to be pyrolyzed the method that large biological molecule prepares lithium cell cathode material, belongs to battery material technical field.The present invention is first using a variety of large biological molecules as raw material, it is compounded with sepiolite etc. and spinning solution is made, ice crystal electrostatic spinning and dry obtained compound bio macromolecular fiber, after compound bio macromolecular fiber and esters of silicon acis dilution and nanometer iron powder are mixed dispersion again, heating stirring reaction, using filter, washing and drying must load large biological molecule fiber；After load large biological molecule fiber is impregnated with poly-vinyl alcohol solution again, it is dry, and control different heating rates and reaction temperature, pyrolysis large biological molecule is made, then large biological molecule will be pyrolyzed, after superconductive carbon black and battery binder ground and mixed, it is coated in copper foil current collector, after drying, punch to get lithium ion battery negative material.The lithium ion battery negative material of technical solution of the present invention preparation has the characteristics that excellent current density and charge-discharge performance.
Description
Technical field
The invention discloses a kind of to be pyrolyzed the method that large biological molecule prepares lithium cell cathode material, belongs to battery material
Technical field.
Background technique
Cathode refers to current potential in power supply (potential) lower one end.In primary battery, the electrode of oxidation, battery are referred to
The left side is write in reaction.It is the pole that electronics flows out in circuit from the point of view of physical angle.And negative electrode material, then refer in battery
The raw material of cathode is constituted, negative electrode material common at present has carbon negative pole material, tin base cathode material, lithium-containing transition metal nitride
Negative electrode material, alloy type negative material and nanoscale negative electrode material.The cathode of lithium ion battery is by negative electrode active material carbon materials
Material or non-carbon material, adhesive and additive are mixed and made into paste adhesive and are uniformly applied to copper foil two sides, through drying, rolling
At.It is made to lithium ion battery success, can key be prepare the negative electrode material of reversibly de-/embedding lithium ion.
In general, select a kind of good negative electrode material that should follow following principle: specific energy is high；The electrode of opposite lithium electrode
Current potential is low；Discharge and recharge reaction invertibity；With the good compatibility of electrolyte and binder；The small (< 10m of specific surface area2/ g), real density
Height (> 2.0g/cm3)；Size and good mechanical stability in process of intercalation;It is resourceful, it is cheap;Stable in the air, nothing
Toxic side effect.Currently, the negative electrode material for being actually used in lithium ion battery is typically all carbon materials, if graphite, soft carbon are (such as coke
Charcoal etc.), hard carbon etc..The negative electrode material explored has nitride, PAS, tin-based oxide, tin alloy, nanometer anode material, with
And other some intermetallic compounds etc..With the development of mechanization process, the demand to the energy is growing day by day.Energy relations
Develop to items, receives much attention.Fossil fuel is the main body of energy supply at present, but fossil energy is non-renewable energy resources,
And serious environmental pollution is also brought in consumption process, while also all multi-environment along with serious greenhouse effects, haze etc.
Problem.The non-renewable energy resources such as fossil energy gradually reduce and its a series of problem of environmental pollutions of bring, be development in face
Most one of the serious problem faced.With the progress of science and technology, develops reproducible green energy resource, be sustainable development
Inevitable choice and the only way, and solve the most effective approach of current energy problem.It is some new that oneself is increasingly paid close attention to people
Type clean energy resource (such as solar energy, wind energy), these energy are essentially all inexhaustible renewable resource, but they are all
Have the shortcomings that intermittent and randomness common, in order to make up this deficiency, it is currently the only for greatly developing energy storage technology
Approach, also becomes the research hotspot of Present Global science and technology and industrial field, and the development of lithium ion battery energy storage technology is led to energy storage
Domain brings hope.Lithium ion battery has the superior function that does not have of other rechargeable batteries, the voltage of lithium ion battery compared with
Height, circulating battery service life is longer, environmental pollution is smaller, is referred to as " most promising electrochmical power source ".Currently,
The key for improving performance of lithium ion battery is to improve its charging and discharging capacity and cycle charge discharge electrical property, is Study on Li-ion batteries
Emphasis and hot issue.In the research of lithium ion battery, the exploitation of the electrode material of novel high-performance is the emphasis of research,
Wherein negative electrode material plays conclusive effect for improving lithium battery performance.
In use, current density and charge-discharge performance can not be further for conventional lithium ion battery negative electrode material
It is promoted, and bad in product thermal stability, causes the decline of product chemical property obvious, higher level can not be maintained at for a long time
Drawback is that it is promoted and is applied to broader field, meets industrial production demand urgently for the promotion for obtaining more high combination property
Problem to be solved.
Summary of the invention
The present invention solves the technical problem of: in use for conventional lithium ion battery negative electrode material, electricity
Current density and charge-discharge performance can not be promoted further, and bad in product thermal stability, lead to product chemical property
The drawbacks of decline is obvious, can not be maintained at higher level for a long time, provides that a kind of to prepare lithium battery negative to be pyrolyzed large biological molecule
The method of pole material.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A method of lithium cell cathode material, specific preparation step are prepared to be pyrolyzed large biological molecule are as follows:
(1) according to parts by weight, 30~40 parts of Enzymatic Hydrolysis of Chitosan liquid, 8~10 parts of microcrystalline celluloses, 80~120 portions of junket are successively taken
Protein dispersion, 40~50 parts of poly-vinyl alcohol solutions, 8~10 parts of dopamine solutions, 2~3 parts of sour modified meerschaums, 0.1~0.2
Part stannic chloride, 0.2~0.3 part of antimony chloride are dispersed with stirring uniformly, obtain spinning solution；
(2) by after gained spinning solution electrostatic spinning, drying obtains compound bio macromolecular fiber；
(3) according to parts by weight, 40~50 parts of compound bio macromolecular fibers are successively taken, 80~100 parts of esters of silicon acis dilutions, 3
~5 parts of nanometer iron powders, after mixing dispersion, heating stirring reaction, using filter, washing and drying must load large biological molecule fibre
Dimension；
(4) dry after impregnating load large biological molecule fiber with poly-vinyl alcohol solution, under inert gas shielding state,
It is to slowly warm up to 500 DEG C, after 2~3h of insulation reaction, continues to be rapidly heated to 1550 DEG C, after 2~3h of insulation reaction, further rise
Temperature is to 2200~2500 DEG C, cooling after keeping the temperature 2~5min, and discharging must be pyrolyzed large biological molecule；
(5) according to parts by weight, 80~100 parts of pyrolysis large biological molecules are successively taken, 10~15 parts of superconductive carbon blacks, 10~15 parts
Battery binder after ground and mixed, is coated in copper foil current collector, after dry, is punched to get lithium ion battery negative material.
Step (1) the Enzymatic Hydrolysis of Chitosan liquid preparation process are as follows: by chitosan and water be in mass ratio 1:8~1:10 stirring
After mixing, the chitosan enzyme of chitosan mass 1~3% is added, after constant temperature stirring digests 10~20min, heat up enzyme deactivation, concentration,
Obtain Enzymatic Hydrolysis of Chitosan liquid.
Step (1) described microcrystalline cellulose is the microcrystalline cellulose that levelling off degree of polymerization is 100~120.
Step (1) the sour modified meerschaum modifying process are as follows: press the hydrochloric acid that sepiolite and mass fraction are 8~10%
Mass ratio is hydro-thermal reaction after 1:5~1:10 is stirred, and using filter, washing and drying obtain sour modified meerschaum.
It is 1:1~1:3 compounding that step (3) the esters of silicon acis dilution is by ethyl orthosilicate and dehydrated alcohol in mass ratio
It forms.
Step (4) inert gas is nitrogen, helium, any one in argon gas.
Step (4) is described to be to slowly warm up to 500 DEG C are as follows: carries out temperature programming to 300 DEG C with 4~5 DEG C/min rate, continues
Temperature programming is carried out to 500 DEG C with 0.4~0.5 DEG C/min rate.
Step (4) is described to be rapidly heated to 1550 DEG C are as follows: with the progress temperature programming of 10~15 DEG C/min rate to 1200 DEG C,
Continue to carry out temperature programming with 6~8 DEG C/min rate to 1550 DEG C.
Step (5) the battery binder is that carboxymethyl cellulose and water are that 1:5~1:8 is compounded in mass ratio.
The beneficial effects of the present invention are:
(1) technical solution of the present invention is first using chitosan, microcrystalline cellulose, casein, polyvinyl alcohol and dopamine etc. as life
Object macromolecular has carboxyl abundant, hydroxyl and amino isoreactivity functional group in such biological macromolecule material, between each other may be used
Form a large amount of Hydrogenbond, and can by the tin ion to dissociate in system and antimony ion chelating absorption, respin into after fiber with silicon
In the reaction process of acid esters, esters of silicon acis absorbs the water that dehydration condensation is formed between above-mentioned active function groups as dehydrating agent
Point, and the process is uniformly slow, the Effective Regulation hydrolytic process of esters of silicon acis, and hydrolysate crystal once being formed can be fine
Dimension adsorption is fixed, and is effectively prevented the reunion of hydrolysate crystal, so that its size is maintained at nanoscale, and can be in fiber table
Face uniform adsorption ultimately forms the large biological molecule fiber of coated with uniform nano silica, followed by polyethylene
Interaction of hydrogen bond between the hydroxyl and nano silica of alcohol coats layer of polyethylene alcohol in nano-silica surface again,
By the subsequent heating rate of strict control, firstly, surface polyvinyl alcohol and internal organic matter are gradually warm in slow temperature-rise period
Solution is shunk, and intermediate silicon dioxide layer is then used as supporting layer, and as temperature further increases, internal stress increases, and along
Fiber cutting direction is distorted, and so that fiber is changed into hollow three-dimensional spiral structure, and under the high temperature conditions, can be in nanometer iron powder
Under catalysis, makes the silica of middle layer and form carbon-silico-carbo between internal charing organic matter and surface layer charing organic matter
Bonding is learned, to effectively play good bridge joint effect, surface layer and internal layer are securely connected, then through further rising graphitization, most
End form is surface layer at the graphitization carbonaceous that using hollow carbonaceous skeleton as internal layer, fold is shunk, and carbon chemistry of silicones key is intermediate bridge layer
Three layers of composite screw structure；
(2) present invention is effectively increased the thermal stability of product in use, is avoided by the formation of above-mentioned labyrinth
Contraction and expansion of the product in battery charge and discharge process in high/low temperature transition process, keep battery performance can
Long-acting stabilization；And the application, also by the doped tin in system and antimony element, it is effectively fixed that the doping of the two can be bridged structure
Inside system, the electric conductivity of bridging structure not only can be improved, reduce electrode polarization, reduce diffusion impedance；It also helps
Promote the thermal stability of product entirety；In addition, the formation of above-mentioned labyrinth, effectively increases the specific surface area of negative electrode material,
Therefore more ionic transport passages can be provided, due to the presence of hollow structure, can further shortens ion diffusion length, and
The presence of spiral and pleated structure is then conducive to the insertion and abjection of lithium ion, has benefited from the promotion of product thermal stability, can
Ensure that product still keeps good chemical property in high current charge-discharge for a long time.
Specific embodiment
It is in mass ratio that 1:8~1:10 is mixed and poured into beaker by chitosan and water, 10 are stirred with glass bar~
After 20min, then the chitosan enzyme of chitosan mass 1~3% is added into beaker, and beaker is moved into digital display and is tested the speed constant temperature magnetic force
Blender is 32~35 DEG C in temperature, under the conditions of revolving speed is 300~500r/min, after 10~20min of constant temperature stirring enzymatic hydrolysis, rises
Temperature keeps the temperature 10~15min of enzyme deactivation, then material in beaker is transferred in Rotary Evaporators to 90~95 DEG C, in pressure be 420~
Under the conditions of temperature is 75~85 DEG C, 10~15min is concentrated under reduced pressure in 450mmHg, and discharging obtains Enzymatic Hydrolysis of Chitosan liquid；By sepiolite and
The hydrochloric acid that mass fraction is 8~10% be in mass ratio 1:5~1:10 mixing pour into water heating kettle, in temperature be 155~160 DEG C,
Under the conditions of revolving speed is 400~600r/min, after hydro-thermal is stirred to react 3~5h, filtering obtains filter cake, and filter is washed with deionized
Cake is in neutrality up to cleaning solution, then the filter cake after washing is transferred in baking oven, is dried extremely under the conditions of being 105~110 DEG C in temperature
Constant weight obtains sour modified meerschaum；In mass ratio it is that 1:8~1:10 mixes dispersion by casein and water, obtains casein dispersion liquid；It presses
Parts by weight meter successively takes 30~40 parts of Enzymatic Hydrolysis of Chitosan liquid, 8~10 parts of microcrystalline celluloses, 80~120 parts of casein dispersions
Liquid, the poly-vinyl alcohol solution that 40~50 parts of mass fractions are 4~6%, the dopamine solution that 8~10 parts of concentration are 3~5g/L, 2~
3 parts of sour modified meerschaums, 0.1~0.2 part of stannic chloride, 0.2~0.3 part of antimony chloride pour into batch mixer, with blender with 400
~800r/min revolving speed is dispersed with stirring 45~60min, obtains spinning solution；Gained spinning solution is transferred in electrostatic spinning machine again, is spinned
It is 2~4mm at length, diameter is 20~30 μm of fiber, then through drying, obtains compound bio macromolecular fiber；In parts by weight
Meter, successively takes 40~50 parts of compound bio macromolecular fibers, 80~100 parts of esters of silicon acis dilutions, 3~5 parts of nanometer iron powders pour into
It is 85~90 DEG C in temperature, under the conditions of revolving speed is 300~500r/min, heating stirring reacts 3~5h in reaction kettle after drying
Afterwards, it filters, obtains filter residue, and gained filter residue is washed 3~5 times with dehydrated alcohol, then the filter residue after washing is transferred in baking oven, in
Temperature is dried under the conditions of being 105~110 DEG C to constant weight, and large biological molecule fiber must be loaded；Gained is loaded into large biological molecule again
It after the poly-vinyl alcohol solution that fiber mass fraction is 4~6% impregnates 20~30min, takes out, and through vacuum freeze drying, obtains two
Double-steeping large biological molecule fiber, is then transferred in retort, and with 600~800mL/ by secondary dipping large biological molecule fiber
Min rate is passed through inert gas into furnace, under inert gas shielding state, carries out temperature programming extremely with 4~5 DEG C/min rate
300 DEG C, continue to carry out temperature programming with 0.4~0.5 DEG C/min rate to 500 DEG C, after 2~3h of insulation reaction, with 10~15 DEG C/
Min rate carries out temperature programming to 1200 DEG C, continues to carry out temperature programming with 6~8 DEG C/min rate to 1550 DEG C, insulation reaction
After 2~3h, continues to be warming up to 2200~2500 DEG C with 10~15 DEG C/min rate, after keeping the temperature 2~5min, cool to room with the furnace
Temperature, discharging, must be pyrolyzed large biological molecule；According to parts by weight, 80~100 parts of pyrolysis large biological molecules are successively taken, 10~15 parts
Superconductive carbon black, 10~15 parts of battery binders, is poured into mortar, 20~30min of ground and mixed, obtains slurry, then gained is starched
Material is coated in copper foil current collector, after dry, is punched to get lithium ion battery negative material.The microcrystalline cellulose is the limit
The microcrystalline cellulose that the degree of polymerization is 100~120.The esters of silicon acis dilution be by ethyl orthosilicate and dehydrated alcohol in mass ratio
It is compounded for 1:1~1:3.The inert gas is nitrogen, helium, any one in argon gas.The battery binder is
Carboxymethyl cellulose and water are that 1:5~1:8 is compounded in mass ratio.
Example 1
It is in mass ratio that 1:10 is mixed and poured into beaker by chitosan and water, after being stirred 20min with glass bar, then to beaker
The middle chitosan enzyme that chitosan mass 3% is added, and beaker is moved into digital display and is tested the speed constant temperature blender with magnetic force, in temperature be 35 DEG C,
Under the conditions of revolving speed is 500r/min, after constant temperature stirring enzymatic hydrolysis 20min, 95 DEG C is warming up to, keeps the temperature enzyme deactivation 15min, then will be in beaker
Material is transferred in Rotary Evaporators, is 450mmHg in pressure, under the conditions of temperature is 85 DEG C, 15min is concentrated under reduced pressure, discharging obtains shell
Glycan enzymolysis liquid；It is in mass ratio that 1:10 mixing is poured into water heating kettle by the hydrochloric acid that sepiolite and mass fraction are 10%, Yu Wendu
It is 160 DEG C, under the conditions of revolving speed is 600r/min, after hydro-thermal is stirred to react 5h, filtering obtains filter cake, and filter is washed with deionized
Cake is in neutrality up to cleaning solution, then the filter cake after washing is transferred in baking oven, is dried under the conditions of being 110 DEG C in temperature to constant weight,
Obtain sour modified meerschaum；In mass ratio it is that 1:10 mixes dispersion by casein and water, obtains casein dispersion liquid；In parts by weight
Meter successively takes 40 parts of Enzymatic Hydrolysis of Chitosan liquid, and 10 parts of microcrystalline celluloses, 120 parts of casein dispersion liquids, 50 parts of mass fractions are 6%
Poly-vinyl alcohol solution, the dopamine solution that 10 parts of concentration are 5g/L, 3 parts of sour modified meerschaums, 0.2 part of stannic chloride, 0.3 part of chlorination
Antimony pours into batch mixer, is dispersed with stirring 60min with blender with 800r/min revolving speed, obtains spinning solution；Gained spinning solution is turned again
Enter in electrostatic spinning machine, being spun into length is 4mm, and diameter is 30 μm of fiber, then through drying, it is fine to obtain compound bio macromolecular
Dimension；According to parts by weight, 50 parts of compound bio macromolecular fibers are successively taken, 100 parts of esters of silicon acis dilutions, 5 parts of nanometer iron powders,
It is 90 DEG C in temperature, under the conditions of revolving speed is 500r/min, after heating stirring reacts 5h, filtering is obtained in reaction kettle after entering drying
Filter residue, and gained filter residue being washed 5 times with dehydrated alcohol, then the filter residue after washing is transferred in baking oven, in temperature be 110 DEG C of items
It dries under part to constant weight, large biological molecule fiber must be loaded；It is again 6% by gained load large biological molecule fiber mass fraction
Poly-vinyl alcohol solution dipping 30min after, take out, and through vacuum freeze drying, obtain double-steeping large biological molecule fiber, then
Double-steeping large biological molecule fiber is transferred in retort, and inert gas is passed through into furnace with 800mL/min rate, in lazy
Property gas protection status under, with 4 DEG C/min rate carry out temperature programming to 300 DEG C, continue with 0.4 DEG C/min rate carry out program
It is warming up to 500 DEG C, after insulation reaction 2h, temperature programming is carried out to 1200 DEG C with 10 DEG C/min rate, is continued with 6 DEG C/min rate
Temperature programming is carried out to 1550 DEG C, after insulation reaction 3h, continues to be warming up to 2500 DEG C with 15 DEG C/min rate, after keeping the temperature 5min,
It cools to room temperature with the furnace, discharges, large biological molecule must be pyrolyzed；According to parts by weight, 100 parts of pyrolysis large biological molecules are successively taken,
15 parts of superconductive carbon blacks, 15 parts of battery binders, are poured into mortar, ground and mixed 30min, obtain slurry, then gained slurry is applied
It is distributed in copper foil current collector, after dry, punches to get lithium ion battery negative material.The microcrystalline cellulose is limit polymerization
The microcrystalline cellulose that degree is 120.It is 1:3 compounding that the esters of silicon acis dilution is by ethyl orthosilicate and dehydrated alcohol in mass ratio
It forms.The inert gas is nitrogen.The battery binder be carboxymethyl cellulose and water be in mass ratio 1:8 compounding and
At.
Example 2
It is in mass ratio that 1:10 is mixed and poured into beaker by chitosan and water, after being stirred 20min with glass bar, then to beaker
The middle chitosan enzyme that chitosan mass 3% is added, and beaker is moved into digital display and is tested the speed constant temperature blender with magnetic force, in temperature be 35 DEG C,
Under the conditions of revolving speed is 500r/min, after constant temperature stirring enzymatic hydrolysis 20min, 95 DEG C is warming up to, keeps the temperature enzyme deactivation 15min, then will be in beaker
Material is transferred in Rotary Evaporators, is 450mmHg in pressure, under the conditions of temperature is 85 DEG C, 15min is concentrated under reduced pressure, discharging obtains shell
Glycan enzymolysis liquid；It is in mass ratio that 1:10 mixing is poured into water heating kettle by the hydrochloric acid that sepiolite and mass fraction are 10%, Yu Wendu
It is 160 DEG C, under the conditions of revolving speed is 600r/min, after hydro-thermal is stirred to react 5h, filtering obtains filter cake, and filter is washed with deionized
Cake is in neutrality up to cleaning solution, then the filter cake after washing is transferred in baking oven, is dried under the conditions of being 110 DEG C in temperature to constant weight,
Obtain sour modified meerschaum；In mass ratio it is that 1:10 mixes dispersion by casein and water, obtains casein dispersion liquid；In parts by weight
Meter successively takes 40 parts of Enzymatic Hydrolysis of Chitosan liquid, and 10 parts of microcrystalline celluloses, 120 parts of casein dispersion liquids, 50 parts of mass fractions are 6%
Poly-vinyl alcohol solution, the dopamine solution that 10 parts of concentration are 5g/L, 3 parts of sour modified meerschaums pour into batch mixer, use blender
It is dispersed with stirring 60min with 800r/min revolving speed, obtains spinning solution；Gained spinning solution is transferred in electrostatic spinning machine again, spinning growth
Degree is 4mm, and diameter is 30 μm of fiber, then through drying, obtains compound bio macromolecular fiber；According to parts by weight, 50 are successively taken
Part compound bio macromolecular fiber, 100 parts of esters of silicon acis dilutions, 5 parts of nanometer iron powders pour into the reaction kettle after drying, Yu Wen
Degree is 90 DEG C, and under the conditions of revolving speed is 500r/min, after heating stirring reacts 5h, filtering obtains filter residue, and by gained filter residue with anhydrous
Ethanol washing 5 times, then the filter residue after washing is transferred in baking oven, it dries under the conditions of being 110 DEG C in temperature to constant weight, life must be loaded
Object macromolecular fiber；The poly-vinyl alcohol solution that gained load large biological molecule fiber mass fraction is 6% is impregnated into 30min again
Afterwards, it takes out, and through vacuum freeze drying, obtains double-steeping large biological molecule fiber, it is then that double-steeping large biological molecule is fine
Dimension is transferred in retort, and inert gas is passed through into furnace with 800mL/min rate, under inert gas shielding state, with 4
DEG C/min rate carries out temperature programming to 300 DEG C, continue to carry out temperature programming with 0.4 DEG C/min rate to 500 DEG C, insulation reaction
After 2h, temperature programming is carried out to 1200 DEG C with 10 DEG C/min rate, continues to carry out temperature programming with 6 DEG C/min rate to 1550
DEG C, after insulation reaction 3h, continues to be warming up to 2500 DEG C with 15 DEG C/min rate, after keeping the temperature 5min, cool to room temperature with the furnace, out
Material, must be pyrolyzed large biological molecule；According to parts by weight, 100 parts of pyrolysis large biological molecules are successively taken, 15 parts of superconductive carbon blacks, 15
Part battery binder, pours into mortar, ground and mixed 30min, obtains slurry, then gained slurry is coated in copper foil current collector,
After drying, punch to get lithium ion battery negative material.The microcrystalline cellulose is the microcrystalline cellulose that levelling off degree of polymerization is 120
Element.It is that 1:3 is compounded that the esters of silicon acis dilution is by ethyl orthosilicate and dehydrated alcohol in mass ratio.The inert gas
For nitrogen.The battery binder is that carboxymethyl cellulose and water are that 1:8 is compounded in mass ratio.
Example 3
It is in mass ratio that 1:10 is mixed and poured into beaker by chitosan and water, after being stirred 20min with glass bar, then to beaker
The middle chitosan enzyme that chitosan mass 3% is added, and beaker is moved into digital display and is tested the speed constant temperature blender with magnetic force, in temperature be 35 DEG C,
Under the conditions of revolving speed is 500r/min, after constant temperature stirring enzymatic hydrolysis 20min, 95 DEG C is warming up to, keeps the temperature enzyme deactivation 15min, then will be in beaker
Material is transferred in Rotary Evaporators, is 450mmHg in pressure, under the conditions of temperature is 85 DEG C, 15min is concentrated under reduced pressure, discharging obtains shell
Glycan enzymolysis liquid；It is in mass ratio that 1:10 mixing is poured into water heating kettle by the hydrochloric acid that sepiolite and mass fraction are 10%, Yu Wendu
It is 160 DEG C, under the conditions of revolving speed is 600r/min, after hydro-thermal is stirred to react 5h, filtering obtains filter cake, and filter is washed with deionized
Cake is in neutrality up to cleaning solution, then the filter cake after washing is transferred in baking oven, is dried under the conditions of being 110 DEG C in temperature to constant weight,
Obtain sour modified meerschaum；In mass ratio it is that 1:10 mixes dispersion by casein and water, obtains casein dispersion liquid；In parts by weight
Meter successively takes 40 parts of Enzymatic Hydrolysis of Chitosan liquid, and 10 parts of microcrystalline celluloses, 120 parts of casein dispersion liquids, 50 parts of mass fractions are 6%
Poly-vinyl alcohol solution, the dopamine solution that 10 parts of concentration are 5g/L, 3 parts of sour modified meerschaums, 0.2 part of stannic chloride, 0.3 part of chlorination
Antimony pours into batch mixer, is dispersed with stirring 60min with blender with 800r/min revolving speed, obtains spinning solution；Gained spinning solution is turned again
Enter in electrostatic spinning machine, being spun into length is 4mm, and diameter is 30 μm of fiber, then through drying, it is fine to obtain compound bio macromolecular
Dimension；According to parts by weight, 50 parts of compound bio macromolecular fibers, 5 parts of nanometer iron powders, the reaction kettle after pouring into drying are successively taken
In, it is 90 DEG C in temperature, under the conditions of revolving speed is 500r/min, after heating stirring reacts 5h, filtering obtains filter residue, and gained is filtered
Slag is washed 5 times with dehydrated alcohol, then the filter residue after washing is transferred in baking oven, is dried under the conditions of being 110 DEG C in temperature to constant weight,
Large biological molecule fiber must be loaded；The poly-vinyl alcohol solution that gained load large biological molecule fiber mass fraction is 6% is soaked again
It after stain 30min, takes out, and through vacuum freeze drying, obtains double-steeping large biological molecule fiber, it is then that double-steeping biology is big
Molecular fiber is transferred in retort, and inert gas is passed through into furnace with 800mL/min rate, in inert gas shielding state
Under, temperature programming is carried out to 300 DEG C with 4 DEG C/min rate, continues to carry out temperature programming with 0.4 DEG C/min rate to 500 DEG C, protects
After temperature reaction 2h, temperature programming is carried out to 1200 DEG C with 10 DEG C/min rate, continues to carry out temperature programming extremely with 6 DEG C/min rate
1550 DEG C, after insulation reaction 3h, continues to be warming up to 2500 DEG C with 15 DEG C/min rate, after keeping the temperature 5min, cools to room temperature with the furnace,
Discharging, must be pyrolyzed large biological molecule；According to parts by weight, 100 parts of pyrolysis large biological molecules are successively taken, 15 parts of superconductive carbon blacks,
15 parts of battery binders, are poured into mortar, ground and mixed 30min, obtain slurry, then gained slurry is coated on copper foil current collector
On, after dry, punch to get lithium ion battery negative material.The microcrystalline cellulose is that the crystallite that levelling off degree of polymerization is 120 is fine
Dimension element.The inert gas is nitrogen.The battery binder be carboxymethyl cellulose and water be in mass ratio 1:8 compounding and
At.
Example 4
It is in mass ratio that 1:10 is mixed and poured into beaker by chitosan and water, after being stirred 20min with glass bar, then to beaker
The middle chitosan enzyme that chitosan mass 3% is added, and beaker is moved into digital display and is tested the speed constant temperature blender with magnetic force, in temperature be 35 DEG C,
Under the conditions of revolving speed is 500r/min, after constant temperature stirring enzymatic hydrolysis 20min, 95 DEG C is warming up to, keeps the temperature enzyme deactivation 15min, then will be in beaker
Material is transferred in Rotary Evaporators, is 450mmHg in pressure, under the conditions of temperature is 85 DEG C, 15min is concentrated under reduced pressure, discharging obtains shell
Glycan enzymolysis liquid；It is in mass ratio that 1:10 mixing is poured into water heating kettle by the hydrochloric acid that sepiolite and mass fraction are 10%, Yu Wendu
It is 160 DEG C, under the conditions of revolving speed is 600r/min, after hydro-thermal is stirred to react 5h, filtering obtains filter cake, and filter is washed with deionized
Cake is in neutrality up to cleaning solution, then the filter cake after washing is transferred in baking oven, is dried under the conditions of being 110 DEG C in temperature to constant weight,
Obtain sour modified meerschaum；In mass ratio it is that 1:10 mixes dispersion by casein and water, obtains casein dispersion liquid；In parts by weight
Meter successively takes 40 parts of Enzymatic Hydrolysis of Chitosan liquid, and 10 parts of microcrystalline celluloses, 120 parts of casein dispersion liquids, 50 parts of mass fractions are 6%
Poly-vinyl alcohol solution, the dopamine solution that 10 parts of concentration are 5g/L, 3 parts of sour modified meerschaums, 0.2 part of stannic chloride, 0.3 part of chlorination
Antimony pours into batch mixer, is dispersed with stirring 60min with blender with 800r/min revolving speed, obtains spinning solution；Gained spinning solution is turned again
Enter in electrostatic spinning machine, being spun into length is 4mm, and diameter is 30 μm of fiber, then through drying, it is fine to obtain compound bio macromolecular
Dimension；According to parts by weight, 50 parts of compound bio macromolecular fibers, 100 parts of aluminium isopropoxides are successively taken, 5 parts of nanometer iron powders pour into dry
It is 90 DEG C in temperature, under the conditions of revolving speed is 500r/min, after heating stirring reacts 5h, filtering must be filtered in reaction kettle after dry
Slag, and gained filter residue being washed 5 times with dehydrated alcohol, then the filter residue after washing is transferred in baking oven, in temperature be 110 DEG C of conditions
Lower drying must load large biological molecule fiber to constant weight；It is again 6% by gained load large biological molecule fiber mass fraction
It after poly-vinyl alcohol solution impregnates 30min, takes out, and through vacuum freeze drying, obtains double-steeping large biological molecule fiber, then will
Double-steeping large biological molecule fiber is transferred in retort, and inert gas is passed through into furnace with 800mL/min rate, in inertia
Under gas protection status, temperature programming is carried out to 300 DEG C with 4 DEG C/min rate, continues to carry out program liter with 0.4 DEG C/min rate
Temperature is to 500 DEG C, after insulation reaction 2h, carries out temperature programming to 1200 DEG C with 10 DEG C/min rate, continue with 6 DEG C/min rate into
Line program is warming up to 1550 DEG C, after insulation reaction 3h, continues to be warming up to 2500 DEG C with 15 DEG C/min rate, after keeping the temperature 5min, with
Furnace is cooled to room temperature, and discharging must be pyrolyzed large biological molecule；According to parts by weight, 100 parts of pyrolysis large biological molecules are successively taken, 15
Part superconductive carbon black, 15 parts of battery binders pour into mortar, ground and mixed 30min, obtain slurry, then gained slurry is coated with
In in copper foil current collector, after dry, punch to get lithium ion battery negative material.The microcrystalline cellulose is levelling off degree of polymerization
For 120 microcrystalline cellulose.The inert gas is nitrogen.The battery binder be carboxymethyl cellulose and water in mass ratio
It is compounded for 1:8.
Example 5
It is in mass ratio that 1:10 is mixed and poured into beaker by chitosan and water, after being stirred 20min with glass bar, then to beaker
The middle chitosan enzyme that chitosan mass 3% is added, and beaker is moved into digital display and is tested the speed constant temperature blender with magnetic force, in temperature be 35 DEG C,
Under the conditions of revolving speed is 500r/min, after constant temperature stirring enzymatic hydrolysis 20min, 95 DEG C is warming up to, keeps the temperature enzyme deactivation 15min, then will be in beaker
Material is transferred in Rotary Evaporators, is 450mmHg in pressure, under the conditions of temperature is 85 DEG C, 15min is concentrated under reduced pressure, discharging obtains shell
Glycan enzymolysis liquid；It is in mass ratio that 1:10 mixing is poured into water heating kettle by the hydrochloric acid that sepiolite and mass fraction are 10%, Yu Wendu
It is 160 DEG C, under the conditions of revolving speed is 600r/min, after hydro-thermal is stirred to react 5h, filtering obtains filter cake, and filter is washed with deionized
Cake is in neutrality up to cleaning solution, then the filter cake after washing is transferred in baking oven, is dried under the conditions of being 110 DEG C in temperature to constant weight,
Obtain sour modified meerschaum；In mass ratio it is that 1:10 mixes dispersion by casein and water, obtains casein dispersion liquid；In parts by weight
Meter successively takes 40 parts of Enzymatic Hydrolysis of Chitosan liquid, and 10 parts of microcrystalline celluloses, 120 parts of casein dispersion liquids, 50 parts of mass fractions are 6%
Poly-vinyl alcohol solution, the dopamine solution that 10 parts of concentration are 5g/L, 3 parts of sour modified meerschaums, 0.2 part of stannic chloride, 0.3 part of chlorination
Antimony pours into batch mixer, is dispersed with stirring 60min with blender with 800r/min revolving speed, obtains spinning solution；Gained spinning solution is turned again
Enter in electrostatic spinning machine, being spun into length is 4mm, and diameter is 30 μm of fiber, then through drying, it is fine to obtain compound bio macromolecular
Dimension；According to parts by weight, 50 parts of compound bio macromolecular fibers are successively taken, 100 parts of esters of silicon acis dilutions, 5 parts of nanometer iron powders,
It is 90 DEG C in temperature, under the conditions of revolving speed is 500r/min, after heating stirring reacts 5h, filtering is obtained in reaction kettle after entering drying
Filter residue, and gained filter residue being washed 5 times with dehydrated alcohol, then the filter residue after washing is transferred in baking oven, in temperature be 110 DEG C of items
It dries under part to constant weight, large biological molecule fiber must be loaded；It is again 6% by gained load large biological molecule fiber mass fraction
Poly-vinyl alcohol solution dipping 30min after, take out, and through vacuum freeze drying, obtain double-steeping large biological molecule fiber, then
Double-steeping large biological molecule fiber is transferred in retort, and inert gas is passed through into furnace with 800mL/min rate, in lazy
Property gas protection status under, with 4 DEG C/min rate carry out temperature programming to 300 DEG C, continue with 0.4 DEG C/min rate carry out program
It is warming up to 500 DEG C, after insulation reaction 2h, temperature programming is carried out to 1200 DEG C with 10 DEG C/min rate, is continued with 6 DEG C/min rate
Temperature programming is carried out to 1550 DEG C, after insulation reaction 3h, continues to be warming up to 2500 DEG C with 15 DEG C/min rate, after keeping the temperature 5min,
It cools to room temperature with the furnace, discharges, large biological molecule must be pyrolyzed；According to parts by weight, 100 parts of pyrolysis large biological molecules are successively taken,
15 parts of superconductive carbon blacks, 15 parts of battery binders, are poured into mortar, ground and mixed 30min, obtain slurry, then gained slurry is applied
It is distributed in copper foil current collector, after dry, punches to get lithium ion battery negative material.The microcrystalline cellulose is limit polymerization
The microcrystalline cellulose that degree is 120.It is 1:3 compounding that the esters of silicon acis dilution is by ethyl orthosilicate and dehydrated alcohol in mass ratio
It forms.The inert gas is nitrogen.The battery binder be carboxymethyl cellulose and water be in mass ratio 1:8 compounding and
At.
Comparative example: in mass ratio it is that 1:10 mixing is poured into beaker by chitosan and water, is stirred 20min with glass bar
Afterwards, it is added the chitosan enzyme of chitosan mass 3% then into beaker, and beaker is moved into digital display and is tested the speed constant temperature blender with magnetic force, in
Temperature is 35 DEG C, under the conditions of revolving speed is 500r/min, after constant temperature stirring enzymatic hydrolysis 20min, is warming up to 95 DEG C, keeps the temperature enzyme deactivation 15min,
Material in beaker is transferred in Rotary Evaporators again, is that 450mmHg is concentrated under reduced pressure under the conditions of temperature is 85 DEG C in pressure
15min, discharging, obtains Enzymatic Hydrolysis of Chitosan liquid；It is in mass ratio that 1:10 mixing is poured by the hydrochloric acid that sepiolite and mass fraction are 10%
It is 160 DEG C in temperature, under the conditions of revolving speed is 600r/min, after hydro-thermal is stirred to react 5h, filtering obtains filter cake, is used in combination in water heating kettle
Filter cake after washing then is transferred in baking oven until cleaning solution is in neutrality by deionized water washing filter cake, in temperature be 110 DEG C of conditions
Lower drying obtains sour modified meerschaum to constant weight；In mass ratio it is that 1:10 mixes dispersion by casein and water, obtains casein dispersion
Liquid；According to parts by weight, 40 parts of Enzymatic Hydrolysis of Chitosan liquid are successively taken, 10 parts of microcrystalline celluloses, 120 parts of casein dispersion liquids, 50 parts
The poly-vinyl alcohol solution that mass fraction is 6%, the dopamine solution that 10 parts of concentration are 5g/L, 3 parts of sour modified meerschaums pour into mixed
In material machine, 60min is dispersed with stirring with 800r/min revolving speed with blender, obtains spinning solution；Gained spinning solution is transferred to Static Spinning again
In silk machine, being spun into length is 4mm, and diameter is 30 μm of fiber, then through drying, obtains compound bio macromolecular fiber；By weight
Number meter, successively takes 50 parts of compound bio macromolecular fibers, and 5 parts of nanometer iron powders pour into the reaction kettle after drying, are in temperature
90 DEG C, under the conditions of revolving speed is 500r/min, after heating stirring reacts 5h, filtering obtains filter residue, and by gained filter residue dehydrated alcohol
Washing 5 times, then the filter residue after washing is transferred in baking oven, it dries under the conditions of being 110 DEG C in temperature to constant weight, must load biological big
Molecular fiber；After the poly-vinyl alcohol solution that gained load large biological molecule fiber mass fraction is 6% is impregnated 30min again, take
Out, and through vacuum freeze drying, double-steeping large biological molecule fiber is obtained, is then transferred to double-steeping large biological molecule fiber
In retort, and inert gas is passed through into furnace with 800mL/min rate, under inert gas shielding state, with 1.5 DEG C/min
The slow temperature programming of rate is to 550 DEG C, after insulation reaction 3h, continues with the high-speed temperature programmed of 10 DEG C/min rate to 1600 DEG C,
After insulation reaction 3h, continues to be warming up to 2500 DEG C with 15 DEG C/min rate, after keeping the temperature 5min, cool to room temperature with the furnace, discharge, obtain
It is pyrolyzed large biological molecule；According to parts by weight, 100 parts of pyrolysis large biological molecules, 15 parts of superconductive carbon blacks, 15 parts of batteries are successively taken
Binder pours into mortar, ground and mixed 30min, obtains slurry, then gained slurry is coated in copper foil current collector, after dry,
Punching is to get lithium ion battery negative material.The microcrystalline cellulose is the microcrystalline cellulose that levelling off degree of polymerization is 120.It is described
Inert gas is nitrogen.The battery binder is that carboxymethyl cellulose and water are that 1:8 is compounded in mass ratio.
Example 1 to the resulting lithium ion battery negative material of example 5 and comparative example product are subjected to performance detection, it is specific to examine
Survey method is as follows:
Using test specimen as battery cathode, pure metal lithium piece is used as to electrode, Celgard2400 polypropylene as diaphragm, 1mol/L's
LiPF6-EC/DEC (1: 1 volume ratio) solution is electrolyte, is assembled into R2032 button cell.The entire assembling of lithium ion battery
Process carries out in the glove box full of high-purity argon gas protection, and the water, oxygen content in experimentation in glove box are respectively less than
0.1ppm.Working electrode is added in battery case (positive terminal), a certain amount of electrolyte is then added dropwise, places into diaphragm, then drip
Add a certain amount of electrolyte, is put into metal lithium sheet, gasket, spring leaf, covers battery case (negative pole end), then by assembled electricity
Pond is encapsulated on battery sealing machine to get experiment button cell.
Experiment carries out charge-discharge test, the voltage range of charge-discharge test with LAND CT2001A battery test system
For 0.005-3V, current density 50mA/g；Its initial capacity is detected, after 500 charge-discharge cycles, detects its capacity
Conservation rate.
The specific testing result of 1 lithium ion battery negative material of table
By 1 testing result of table it is found that the lithium ion battery negative material of technical solution of the present invention preparation has excellent electric current close
It the characteristics of degree and charge-discharge performance, has broad prospects in the development of battery material technology industry.
Claims (9)
1. a kind of to be pyrolyzed the method that large biological molecule prepares lithium cell cathode material, it is characterised in that specific preparation step are as follows:
(1) according to parts by weight, 30~40 parts of Enzymatic Hydrolysis of Chitosan liquid, 8~10 parts of microcrystalline celluloses, 80~120 portions of junket are successively taken
Protein dispersion, 40~50 parts of poly-vinyl alcohol solutions, 8~10 parts of dopamine solutions, 2~3 parts of sour modified meerschaums, 0.1~0.2
Part stannic chloride, 0.2~0.3 part of antimony chloride are dispersed with stirring uniformly, obtain spinning solution；
(2) by after gained spinning solution electrostatic spinning, drying obtains compound bio macromolecular fiber；
(3) according to parts by weight, 40~50 parts of compound bio macromolecular fibers are successively taken, 80~100 parts of esters of silicon acis dilutions, 3
~5 parts of nanometer iron powders, after mixing dispersion, heating stirring reaction, using filter, washing and drying must load large biological molecule fibre
Dimension；
(4) dry after impregnating load large biological molecule fiber with poly-vinyl alcohol solution, under inert gas shielding state,
It is to slowly warm up to 500 DEG C, after 2~3h of insulation reaction, continues to be rapidly heated to 1550 DEG C, after 2~3h of insulation reaction, further rise
Temperature is to 2200~2500 DEG C, cooling after keeping the temperature 2~5min, and discharging must be pyrolyzed large biological molecule；
(5) according to parts by weight, 80~100 parts of pyrolysis large biological molecules are successively taken, 10~15 parts of superconductive carbon blacks, 10~15 parts
Battery binder after ground and mixed, is coated in copper foil current collector, after dry, is punched to get lithium ion battery negative material.
2. according to claim 1 a kind of to be pyrolyzed the method that large biological molecule prepares lithium cell cathode material, feature
It is step (1) the Enzymatic Hydrolysis of Chitosan liquid preparation process are as follows: by chitosan and water be in mass ratio that 1:8~1:10 is stirred
Afterwards, the chitosan enzyme of chitosan mass 1~3% is added, after constant temperature stirring digests 10~20min, heat up enzyme deactivation, and concentration obtains shell
Glycan enzymolysis liquid.
3. according to claim 1 a kind of to be pyrolyzed the method that large biological molecule prepares lithium cell cathode material, feature
It is that step (1) described microcrystalline cellulose is the microcrystalline cellulose that levelling off degree of polymerization is 100~120.
4. according to claim 1 a kind of to be pyrolyzed the method that large biological molecule prepares lithium cell cathode material, feature
It is step (1) the sour modified meerschaum modifying process are as follows: the hydrochloric acid that sepiolite and mass fraction are 8~10% is pressed into quality
After being stirred for 1:5~1:10, hydro-thermal reaction, using filter, washing and drying obtain sour modified meerschaum.
5. according to claim 1 a kind of to be pyrolyzed the method that large biological molecule prepares lithium cell cathode material, feature
Be step (3) the esters of silicon acis dilution to be by ethyl orthosilicate and dehydrated alcohol be in mass ratio 1:1~1:3 compounding and
At.
6. according to claim 1 a kind of to be pyrolyzed the method that large biological molecule prepares lithium cell cathode material, feature
It is step (4) inert gas for any one in nitrogen, helium, argon gas.
7. according to claim 1 a kind of to be pyrolyzed the method that large biological molecule prepares lithium cell cathode material, feature
Be that step (4) is described and be to slowly warm up to 500 DEG C are as follows: temperature programming is carried out to 300 DEG C with 4~5 DEG C/min rate, continue with
0.4~0.5 DEG C/min rate carries out temperature programming to 500 DEG C.
8. according to claim 1 a kind of to be pyrolyzed the method that large biological molecule prepares lithium cell cathode material, feature
It is that step (4) is described to be rapidly heated to 1550 DEG C are as follows: carry out temperature programming to 1200 DEG C with 10~15 DEG C/min rate, continue
Temperature programming is carried out to 1550 DEG C with 6~8 DEG C/min rate.
9. according to claim 1 a kind of to be pyrolyzed the method that large biological molecule prepares lithium cell cathode material, feature
It is that step (5) the battery binder be carboxymethyl cellulose and water is that 1:5~1:8 is compounded in mass ratio.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110518245A (en) * | 2019-07-26 | 2019-11-29 | 广东工业大学 | It is a kind of with water-absorbing resin prepare carbon material and its lithium-sulphur cell positive electrode in application |
| CN111640945A (en) * | 2020-06-18 | 2020-09-08 | 合肥国轩高科动力能源有限公司 | Lithium ion battery anode slurry and preparation method thereof |
| CN111916691A (en) * | 2019-08-14 | 2020-11-10 | 邵峥业 | Preparation method of lithium battery negative electrode material |
-
2019
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110518245A (en) * | 2019-07-26 | 2019-11-29 | 广东工业大学 | It is a kind of with water-absorbing resin prepare carbon material and its lithium-sulphur cell positive electrode in application |
| CN111916691A (en) * | 2019-08-14 | 2020-11-10 | 邵峥业 | Preparation method of lithium battery negative electrode material |
| CN111916692A (en) * | 2019-08-14 | 2020-11-10 | 邵峥业 | Preparation method of lithium battery negative electrode material |
| CN111640945A (en) * | 2020-06-18 | 2020-09-08 | 合肥国轩高科动力能源有限公司 | Lithium ion battery anode slurry and preparation method thereof |
| CN111640945B (en) * | 2020-06-18 | 2023-01-03 | 合肥国轩高科动力能源有限公司 | Lithium ion battery anode slurry and preparation method thereof |
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