CN108832084A - Lithium-sulfur cell material and preparation method thereof based on discarded cigarette butt biomass resource - Google Patents
Lithium-sulfur cell material and preparation method thereof based on discarded cigarette butt biomass resource Download PDFInfo
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Abstract
The invention belongs to materials, energy technology field, the lithium-sulfur cell material and preparation method thereof specially based on discarded cigarette butt biomass resource.The present invention uses the biomass such as discarded cigarette butt for precursor material, prepares biomass porous carbon by composite graphite alkene, carbonization, further carries sulphur and obtain biomass porous carbon material（S@GO/PC）.The advantages that biomass porous material prepared by the above method is due to its unique graded porous structure, high conductivity and high load sulfur content, when it is as lithium-sulfur cell material, shows high battery specific capacity and excellent cyclical stability.The lithium-sulfur cell material of gained biomass derived of the invention not only has good electric conductivity, carry sulfur content height and excellent performance, and preparation low cost of raw materials is easy to get, large scale preparation can be achieved, and is a kind of preparation method of efficient, economic, environmental protection novel lithium-sulfur cell.
Description
Technical field
The invention belongs to materials, energy technology field, and in particular to a kind of lithium sulphur based on discarded cigarette butt biomass resource
Battery material and preparation method thereof.
Background technique
It is highlighted with the increasingly serious environmental problems with energy deficiency, people are to miniaturization of electronic products, multiplicity
Property and changeability demand it is more more and more urgent, developing, there is the advanced energy storage device gesture of high-energy density and high circulation stability to exist
It must go.Wherein, research hotspot of the lithium-sulfur cell due to higher theoretical specific capacity as countries in the world researcher.Lithium-sulfur cell is
For one kind using lithium metal as cathode, elemental sulfur is the secondary cell of anode, realizes electric energy by the fracture of sulphur-sulfide linkage and regeneration
Mutual conversion between chemical energy.The theoretical specific energy of lithium-sulfur cell can reach 2600 Wh kg-1, be current commercialization lithium from
Sub- battery it is practical 10 times or so of attainable energy density.In addition, sulphur as rich reserves on the earth and theoretical energy it is close
One of higher element is spent, especially has highly important effect in the research application of lithium-sulfur cell in energy storage, and
And it is also equipped with cheap, advantages of environment protection.However, theoretical capacity is high, energy density is big, valence although lithium-sulfur cell has
Cheap, the less toxic and environmental-friendly advantage of lattice, but there are also intrinsic defects to restrict its further commercialized application,
It is mainly manifested in the following aspects：（1）" the shuttle effect " of polysulfide；（2）The poorly conductive of elemental sulfur；（3）Sulphur is filling
Volume expansion in discharge process；（4）Low material sulfur content and low pole piece carrying capacity etc.；These defects result in lithium sulphur in turn
The problems such as utilization rate of battery sulphur reduces, and the cyclical stability of lithium-sulfur cell is deteriorated.
In view of the above-mentioned problems, researchers put forth effort on sulphur anode is carried out it is composite modified to improving its poorly conductive, bright
The inherent shortcomings such as volume change is larger in aobvious shuttle effect and charge and discharge process.One of important directions be by elemental sulfur with
Various carbon materials（Such as one-dimensional carbon nanotube CNT, two-dimensional graphene, three-dimensional porous carbon materials）Carry out compound rear conduct
Lithium-sulfur cell material.But the lithium-sulfur cell material prepared with this method is still faced with that preparation process is cumbersome, cost is high
It is expensive, carry that sulfur content is low, the disadvantages of performance is poor, be not able to satisfy actual demand, therefore urgently develop a kind of novel lithium-sulfur cell material
Material.
Summary of the invention
In order to overcome above-mentioned prior art defect, the purpose of the present invention is to provide have it is high carry sulfur content, high capacity and
The lithium-sulfur cell material of excellent cycling stability, and simple process, low in cost, environmental protection and economy the lithium-sulfur cell material are provided
Preparation method.
Lithium-sulfur cell material provided by the invention, be it is a kind of based on the biomass such as discarded cigarette butt be raw material preparation it is porous
Carbon-simple substance sulfur system, is denoted as S GO/PC.It prepares raw material：Waste biomass material（For example, sharp group, Marlboro, in
The discarded cigarette filter such as China）, graphene oxide, ethyl alcohol, sulphur powder etc..
Porous carbon-simple substance the sulfur system provided by the invention prepared based on biomass such as discarded cigarette butts for raw material（S@GO/
PC）As lithium sulfur battery anode material, and it is used for the lithium-sulfur cell of the composite material, preparation process includes：Using useless
Biological material combined oxidation graphene is abandoned as presoma（GO/BC）, after heat-treating carbonization treatment, further carry sulphur system
The porous carbon materials of standby composite graphite alkene out（It is denoted as S@GO/PC）, and it is used as Lithium-sulphur battery anode material.Due to the material
The advantages that graded porous structure, high conductivity, big specific surface area, which can effectively inhibit the dissolution of more lithium sulfides, favorably
In the diffusion of lithium ion and the infiltration of electrolyte, further increases the chemical property of lithium-sulfur cell and solve part waste
Recycling.
The preparation method of above-mentioned lithium-sulfur cell material S@GO/PC, the specific steps are：
（1）The pretreatment of raw material：The discarded cigarette butt that will be collected into（Main component is cellulose diacetate）Distinguished with ethyl alcohol, water
Supersound washing 3 ~ 5 times, and 2 ~ 24 h are dried in 60 ~ 100 DEG C of thermostatic drying chamber, products therefrom is biomass hole carbon material,
It is denoted as BC；
（2）Prepare the biomass carbon material of composite graphite alkene：By the graphene oxide of 2 ~ 10 mg/mL and 10 ~ 50 mg biology
Matter carbon material（BC）, after 2 ~ 8 h are sufficiently stirred, take out it is compound after sample, be placed in -30 ~ -70 DEG C of freeze drier
In, 24 ~ 36 h are freeze-dried, products therefrom is biomass porous carbon（BC）With graphene composite precursor, it is denoted as GO/
BC；
（3）Utilize the porous carbon materials of GO/BC in-situ construction composite graphite alkene：Take step（2）The GO/BC 20 ~ 70 of preparation
Mg is put into porcelain boat, and porcelain boat is put into tube furnace, is passed through argon gas, is heated to 600 ~ 1000 with the speed of 2 ~ 5 DEG C/min
DEG C, it keeps the temperature 3 ~ 9 h at this temperature to get composite material is arrived, is denoted as GO/PC；Further utilize vacuum sealing tube technology or molten
Melt method and 200 ~ 400 mg sulphur powders are injected into above-mentioned composite material, obtains the porous carbon materials of target product composite graphite alkene, be denoted as
S@GO/PC。
S@GO/PC composite material prepared by the present invention can be used as Lithium-sulphur battery anode material, and be applied to lithium-sulfur cell
Electrochemical property test in, the specific steps are：In glove box, by S@GO/PC composite material anode pole piece, the cathode of preparation
Lithium piece, diaphragm, electrolyte, battery case are combined into button cell together, stand 12 h, test its chemical property.
Advantage of the invention is that：（1）Using discarded cigarette butt as research object, not only cost is very low, abundant raw material, production
Object purity is high has certain economic and feature of environmental protection, meets current sustainable development requirement, and preparation process is simple, is easy to work
Industry metaplasia produces；In addition, preparation process of the invention can also be extended to other biological material to prepare lithium-sulphur cell positive electrode material
Material.（2）Prepared biomass porous carbon composite, due to unique graded porous structure, big specific surface area, height
The advantages that electric conductivity, can not only sufficiently inhibit the dissolution of more lithium sulfides, load more elemental sulfurs, and be conducive to lithium ion
Diffusion and electrolyte infiltration.（3）Practice have shown that the S@GO/PC composite material of 75% ~ 78% sulfur content is used for lithium-sulfur cell
When, under 0.1C current density, first discharge specific capacity is 1200 ~ 1600 mAh g-1, the cycle charge discharge under 0.5C current density
After electricity 100 times, specific discharge capacity is 900 ~ 1000 mAh g-1, in the research of high rate performance, 650 can be also shown under 2C
mAh∙g-1Excellent properties, while there is stable coulombic efficiency.
The present invention provides a kind of low cost, high-performance, biomass porous carbon lithium-sulfur cell materials easy to industrialized production
The preparation method and applications of material.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of biomass porous carbon lithium-sulfur cell material prepared by the embodiment of the present invention 1（SEM）.
Wherein：（a）For low power scanning electron microscope (SEM) photograph,（b）For high power scanning electron microscope (SEM) photograph.
Fig. 2 is the X-ray diffraction energy spectrum analysis of biomass porous carbon lithium-sulfur cell material prepared by the embodiment of the present invention 1
Figure（XRD）.
Fig. 3 is that biomass porous carbon lithium-sulfur cell material battery under the conditions of 0.5 C prepared by the embodiment of the present invention 1 fills
Discharge curve.
Fig. 4 is the high rate performance curve of biomass porous carbon lithium-sulfur cell material prepared by the embodiment of the present invention 1.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention is not limited only to
These embodiments.For a further understanding of the present invention, below with reference to example and attached drawing, the present invention is further described.
Embodiment 1, based on the preparation method and application of lithium-sulfur cell material derived from the biomass resources such as discarded cigarette butt, packet
Include following steps：
（1）The pretreatment of raw material：The Marlboro cigarette butt that will be collected into（Main component is cellulose diacetate）With 95%
Ethyl alcohol, water etc. supersound washing 3 ~ 5 times respectively, and 2 ~ 24 h are dried in 60 DEG C of thermostatic drying chamber, products therefrom is biomass
Carbon material（BC）；
（2）Prepare the biomass carbon material of composite graphite alkene（GO/BC）：By the graphene oxide of 3 ~ 10 mg/mL and 10.0 mg
Biomass carbon material（BC）, after 2 ~ 8 h are sufficiently stirred, take out it is compound after sample, be placed in -50 DEG C of freeze drier, it is cold
Dry 24 ~ 36 h is lyophilized, products therefrom is biomass porous carbon（BC）With graphene composite precursor（GO/BC）；
（3）S@GO/PC composite material is constructed using GO/BC precursor in situ：By step（2）The GO/BC prepared is as forerunner
Body is taken 100 mg to be put into and is placed in porcelain boat, porcelain boat is put into tube furnace, argon gas is passed through, is heated to the speed of 5 DEG C/min
900 DEG C, keep the temperature 6 h at this temperature to get GO/PC composite material is arrived.Further utilize vacuum sealing tube technology or fusion method will
200 ~ 400 mg sulphur powders inject above-mentioned composite material, obtain S@GO/PC.
S@GO/PC composite material prepared by the present invention can be used as Lithium-sulphur battery anode material and be applied to lithium-sulfur cell
In electrochemical property test, the specific steps are：In glove box, by S@GO/PC composite material anode pole piece, the cathode lithium of preparation
Piece, diaphragm, electrolyte, battery case are combined into button cell together, stand 12 h, test its chemical property.
Advantage of the invention is that：（1）Using discarded cigarette butt as research object, not only cost is very low, abundant raw material, production
Object purity is high has certain economic and feature of environmental protection, meets current sustainable development requirement, and preparation process is simple, is easy to work
Industry metaplasia produces；In addition, preparation process of the invention can also be extended to other biological material to prepare lithium-sulphur cell positive electrode material
Material.（2）Prepared biomass porous carbon composite, due to unique graded porous structure, big specific surface area, height
The advantages that electric conductivity, can not only sufficiently inhibit the dissolution of more lithium sulfides, load more elemental sulfurs, and be conducive to lithium ion
Diffusion and electrolyte infiltration.（3）By practice have shown that, the S@GO/PC composite material of 75% ~ 78% sulfur content is used for lithium sulphur
When battery, under 0.1C current density, first discharge specific capacity is 1200 ~ 1600 mAh g-1, recycled under 0.5C current density
After charge and discharge 100 times, specific discharge capacity is 900 ~ 1000 mAh g-1, in the research of high rate performance, can also be shown under 2C
650 mAh∙g-1Excellent properties, while there is stable coulombic efficiency.
Embodiment 2, based on the preparation method and application of lithium-sulfur cell material derived from the biomass resources such as discarded cigarette butt, packet
Include following steps：
（1）The pretreatment of raw material：The Liqun Cigarette cigarette butt that will be collected into（Main component is cellulose diacetate）With 95% second
Alcohol, water etc. supersound washing 3 ~ 5 times respectively, and 2 ~ 24 h are dried in 60 DEG C of thermostatic drying chamber, products therefrom is biomass carbon
Material（BC）；
（2）Prepare the biomass carbon material of composite graphite alkene（GO/BC）：By the graphene oxide of 3 ~ 10 mg/mL and 10.0 mg
Biomass carbon material（BC）, after 2 ~ 8 h are sufficiently stirred, take out it is compound after sample, be placed in -50 DEG C of freeze drier, it is cold
Dry 24 ~ 36 h is lyophilized, products therefrom is biomass porous carbon（BC）With graphene composite precursor（GO/BC）；
（3）S@GO/PC composite material is constructed using GO/BC precursor in situ：By step（2）The GO/BC prepared is as forerunner
Body is taken 100 mg to be put into and is placed in porcelain boat, porcelain boat is put into tube furnace, argon gas is passed through, is heated to the speed of 5 DEG C/min
900 DEG C, keep the temperature 6 h at this temperature to get GO/PC composite material is arrived.Further utilize vacuum sealing tube technology or fusion method will
200 ~ 400 mg sulphur powders inject above-mentioned composite material, obtain S@GO/PC.
S@GO/PC composite material prepared by the present invention can be used as Lithium-sulphur battery anode material and be applied to lithium-sulfur cell
In electrochemical property test, the specific steps are：In glove box, by S@GO/PC composite material anode pole piece, the cathode lithium of preparation
Piece, diaphragm, electrolyte, battery case are combined into button cell together, stand 12 h, test its chemical property.
The present embodiment has the beneficial effect that：Compared with prior art,（1）Using discarded cigarette butt as research object, no
Only cost is very low, abundant raw material, product purity are high, has certain economic and feature of environmental protection, meets current sustainable development requirement, and
And preparation process is simple, it is easy to industrialized production；In addition, preparation process of the invention can also be extended to other biological material use
To prepare lithium sulfur battery anode material.（2）Prepared biomass porous carbon composite, due to unique classifying porous
The advantages that structure, big specific surface area, high conductivity, can not only sufficiently inhibit the dissolution of more lithium sulfides, load more single
Matter sulphur（75%~78%）, and be conducive to the diffusion of lithium ion and the infiltration of electrolyte.（3）By practice have shown that, utilize the biology
When matter porous carbon materials are as lithium sulfur battery anode material, lithium-sulfur cell specific capacity with higher and good cyclicity
Energy.
Embodiment 3, based on the preparation method and application of lithium-sulfur cell material derived from the biomass resources such as discarded cigarette butt, packet
Include following steps：
（1）The pretreatment of raw material：The Marlboro cigarette butt that will be collected into（Main component is cellulose diacetate）With 95% ethyl alcohol,
Water etc. supersound washing 3 ~ 5 times respectively, and 12 h are dried in 60 DEG C of thermostatic drying chamber, products therefrom is biomass carbon material
（BC）；
（2）Prepare the biomass carbon material of composite graphite alkene（GO/BC）：The graphene oxide of 10 mg/mL and 1 ~ 20 mg is raw
Substance carbon material（BC）, after 2 ~ 8 h are sufficiently stirred, take out it is compound after sample, be placed in -50 DEG C of freeze drier, freeze
Dry 24 ~ 36 h, products therefrom is biomass porous carbon（BC）With graphene composite precursor（GO/BC）；
（3）S@GO/PC composite material is constructed using GO/BC precursor in situ：By step（2）The GO/BC prepared is as forerunner
Body is taken 100 mg to be put into and is placed in porcelain boat, porcelain boat is put into tube furnace, argon gas is passed through, is heated to the speed of 2 DEG C/min
600 DEG C, keep the temperature 6 h at this temperature to get GO/PC composite material is arrived.Further utilize vacuum sealing tube technology or fusion method will
200 ~ 400 mg sulphur powders inject above-mentioned composite material, obtain S@GO/PC.
S@GO/PC composite material prepared by the present invention can be used as Lithium-sulphur battery anode material and be applied to lithium-sulfur cell
In electrochemical property test, the specific steps are：In glove box, by S@GO/PC composite material anode pole piece, the cathode lithium of preparation
Piece, diaphragm, electrolyte, battery case are combined into button cell together, stand 12 h, test its chemical property.
The present embodiment has the beneficial effect that：Compared with prior art,（1）Using discarded cigarette butt as research object, no
Only cost is very low, abundant raw material, product purity are high, has certain economic and feature of environmental protection, meets current sustainable development requirement, and
And preparation process is simple, it is easy to industrialized production；In addition, preparation process of the invention can also be extended to other biological material use
To prepare lithium sulfur battery anode material.（2）Prepared biomass porous carbon composite, due to unique classifying porous
The advantages that structure, big specific surface area, high conductivity, can not only sufficiently inhibit the dissolution of more lithium sulfides, load more single
Matter sulphur（75%~78%）, and be conducive to the diffusion of lithium ion and the infiltration of electrolyte.（3）By practice have shown that, utilize the biology
When matter porous carbon materials are as lithium sulfur battery anode material, lithium-sulfur cell specific capacity with higher and good cyclicity
Energy.
Claims (3)
1. a kind of preparation method of the lithium-sulfur cell material based on discarded cigarette butt biomass resource, which is characterized in that specific steps
For：
（1）The pretreatment of raw material：The discarded cigarette butt ethyl alcohol being collected into, water are distinguished supersound washing 3 ~ 5 times, and 60 ~ 100
DEG C thermostatic drying chamber in dry 2 ~ 24 h, products therefrom be biomass hole carbon material, be denoted as BC；
（2）Prepare the biomass carbon material of composite graphite alkene：By the graphene oxide of 2 ~ 20 mg/mL and 10 ~ 50 mg biology
Matter carbon material（BC）, after 2 ~ 8 h are sufficiently stirred, take out it is compound after sample, be placed in -30 ~ -70 DEG C of freeze drier,
24 ~ 36 h are freeze-dried, products therefrom is biomass porous carbon（BC）With graphene composite precursor, it is denoted as GO/BC；
（3）Utilize the porous carbon materials of GO/BC in-situ construction composite graphite alkene：Take step（2）The GO/BC 20 ~ 70 of preparation
Mg is put into porcelain boat, and porcelain boat is put into tube furnace, is passed through argon gas, is heated to 600 ~ 1000 with the speed of 2 ~ 5 DEG C/min
DEG C, it keeps the temperature 3 ~ 9 h at this temperature to get composite material is arrived, is denoted as GO/PC；Further utilize vacuum sealing tube technology or molten
Melt method and 200 ~ 400 mg sulphur powders are injected into above-mentioned composite material, obtain the porous carbon materials of target product composite graphite alkene, remembers
For S@GO/PC.
2. the lithium-sulfur cell material based on discarded cigarette butt biomass resource that a kind of preparation method as described in claim 1 is prepared
Material.
3. the lithium-sulfur cell material as claimed in claim 2 based on discarded cigarette butt biomass resource is as lithium-sulphur cell positive electrode material
The application of material.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109244467A (en) * | 2018-11-30 | 2019-01-18 | 陕西科技大学 | A kind of method that herba setariae viridis grass prepares biological carbon negative pole material |
| CN109360975A (en) * | 2018-11-30 | 2019-02-19 | 陕西科技大学 | A kind of compound bio carbon structure load sulphur preparing process |
| CN109638253A (en) * | 2018-12-14 | 2019-04-16 | 河南豫氢动力有限公司 | A kind of preparation method of porous carbon/stannic oxide composite lithium ion battery cathode material |
| CN110492065A (en) * | 2019-07-26 | 2019-11-22 | 江苏理工学院 | It is a kind of based on the S/Co/CNF composite material and preparation method of discarded cigarette butt and application |
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| CN106602013A (en) * | 2016-12-19 | 2017-04-26 | 中国科学院山西煤炭化学研究所 | Preparation method of sulfur-active carbon/graphene composite material |
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| CN105789550A (en) * | 2016-04-26 | 2016-07-20 | 熊菊莲 | Electrode and preparation method of electrode material |
| US20180083289A1 (en) * | 2016-09-20 | 2018-03-22 | Nanotek Instruments, Inc. | Metal-Sulfur Battery Cathode Containing Humic Acid-Derived Conductive Foam Impregnated with Sulfur or Sulfide |
| CN106532026A (en) * | 2016-12-19 | 2017-03-22 | 中国科学院山西煤炭化学研究所 | Sulfur-activated carbon/graphene composite material and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109244467A (en) * | 2018-11-30 | 2019-01-18 | 陕西科技大学 | A kind of method that herba setariae viridis grass prepares biological carbon negative pole material |
| CN109360975A (en) * | 2018-11-30 | 2019-02-19 | 陕西科技大学 | A kind of compound bio carbon structure load sulphur preparing process |
| CN109244467B (en) * | 2018-11-30 | 2021-04-30 | 陕西科技大学 | Method for preparing biochar negative electrode material from setaria viridis |
| CN109638253A (en) * | 2018-12-14 | 2019-04-16 | 河南豫氢动力有限公司 | A kind of preparation method of porous carbon/stannic oxide composite lithium ion battery cathode material |
| CN110492065A (en) * | 2019-07-26 | 2019-11-22 | 江苏理工学院 | It is a kind of based on the S/Co/CNF composite material and preparation method of discarded cigarette butt and application |
| CN110492065B (en) * | 2019-07-26 | 2022-02-08 | 江苏理工学院 | S/Co/CNF composite material based on waste cigarette ends and preparation method and application thereof |
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