CN111063876A - Graphene/tannin extract furfuryl alcohol resin derived carbon negative electrode material, and preparation method and application thereof - Google Patents
Graphene/tannin extract furfuryl alcohol resin derived carbon negative electrode material, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a graphene/kaki extract furfuryl alcohol resin derived carbon negative electrode material which comprises graphene and kaki extract furfuryl alcohol resin derived carbon, wherein the graphene is coated on the surface of the kaki extract furfuryl alcohol resin derived carbon, the graphene/kaki extract furfuryl alcohol resin derived carbon negative electrode material is formed by pyrolyzing and carbonizing kaki extract furfuryl alcohol resin derived carbon, graphene oxide and a surfactant, and the kaki extract furfuryl alcohol resin derived carbon is formed by carbonizing kaki extract furfuryl alcohol resin prepared from kaki extract, furfuryl alcohol and a curing agent. The invention has the advantages of environmental protection and wide and renewable raw material sources.
Description
Technical Field
The invention relates to the field of electrochemistry and energy materials, in particular to a graphene/tannin extract furfuryl alcohol resin derived carbon negative electrode material and a preparation method and application thereof.
Background
With the rapid development of science and technology, lithium ion batteries have long-term stability and high energy density, and have been widely used in energy storage systems and portable digital devices. Because of the large demand, low preparation cost, environmental protection and high performance of the lithium ion battery, the electrode material thereof draws the attention of the researchers. Among all anode materials used in lithium ion batteries, graphitic carbon is the predominant material in commerce due to its high operating voltage and good electrical conductivity; but due to its limited graphite it is far from meeting the requirements of high energy/power density. Thus, hard carbon (740 mAh g) with high specific capacity-1) Its high carbon properties and hard carbon structure are more stable than graphite materials during charge and discharge, and have gained wide attention. However, the current precursors for preparing hard carbon are mainly petrochemical raw materials, such as phenolic resins, high molecular polymers, pitch, and the like. For example, chinese patent publication No. CN110265660A discloses that a carbon negative electrode material prepared from pitch has disadvantages of long preparation time, complicated steps, and small specific capacity (350 mAh/g), and it is difficult to truly replace the conventional graphite negative electrode material. It is particularly noteworthy that the current raw materials for hard carbon are non-renewable, the price is very easy to fluctuate due to international oil price fluctuation, and the products have more or less problems, such as the release of formaldehyde or other toxic carcinogenic substances during the resin preparation process. Therefore, natural resins made from renewable resources as main raw materials have attracted attention again due to the factors of being green, environmentally friendly, harmless to human body, and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a graphene/kauri furfuryl alcohol resin derived carbon negative electrode material with excellent cycle performance and large specific capacity, and correspondingly, the invention also provides a preparation method and application of the graphene/kauri furfuryl alcohol resin derived carbon negative electrode material.
In order to solve the technical problems, the invention adopts the following technical scheme:
the graphene/kaki extract furfuryl alcohol resin derived carbon negative electrode material comprises graphene and kaki extract furfuryl alcohol resin derived carbon, wherein the graphene is coated on the surface of the kaki extract furfuryl alcohol resin derived carbon, the graphene/kaki extract furfuryl alcohol resin derived carbon negative electrode material is prepared by pyrolyzing and carbonizing kaki extract furfuryl alcohol resin derived carbon, graphene oxide and a surfactant, and the kaki extract furfuryl alcohol resin derived carbon is prepared by carbonizing kaki extract furfuryl alcohol resin prepared from kaki extract, furfuryl alcohol and a curing agent.
Preferably, the curing agent is a sulfur-containing curing agent.
As a general inventive concept, the present invention also provides a method for preparing a graphene/kava furfuryl alcohol resin-derived carbon negative electrode material, comprising the steps of:
s1, taking tannin extract furfuryl alcohol resin as a precursor, heating to 400-600 ℃ in a gas protection atmosphere for pre-carbonization, cooling, grinding, and heating to 900-1200 ℃ in a gas protection atmosphere for pyrolysis carbonization to obtain tannin extract furfuryl alcohol resin derived carbon;
s2, dispersing the tannin extract furfuryl alcohol resin derived carbon and graphene oxide obtained in the step S1 in a solvent to obtain a suspension, adding a surfactant into the suspension, uniformly mixing, filtering, drying, heating to 900-1200 ℃ in a gas protection atmosphere, and carrying out pyrolysis carbonization to obtain the graphene/tannin extract furfuryl alcohol resin derived carbon negative electrode material.
As a further improvement to the above technical solution:
in the step S1 and the step S2, the temperature rise rate of the pre-carbonization and the pyrolysis carbonization is 10-20 ℃/min, and the time of the pre-carbonization and the pyrolysis carbonization is 0.5-5 h.
In the step S2, the surfactant is one of cetyl trimethyl ammonium bromide, polyvinylpyrrolidone and quaternary ammonium salt, and the volume mass ratio of the suspension to the surfactant is 80-150 mL: 1-15 g.
In the step S2, the tannin extract furfuryl alcohol resin-derived carbon and graphene oxide are dispersed in the solvent by ultrasonic dispersion; the solvent is an ethanol solution with the mass fraction of 15-30%; the mass ratio of the tannin extract furfuryl alcohol resin derived carbon to the graphene oxide is 4-8: 0.5-2.
Preferably, in the step S2, the mass ratio of the kava furfuryl alcohol resin derived carbon to the graphene oxide is 5: 1.
In the step S2, the power of ultrasonic dispersion is 100-600W, and the time of ultrasonic dispersion is 20-60 min.
In the step S1, the grinding is ball milling, the ball milling rotation speed is 400-1000 r/min, and the time is 10-60 min.
In the step S1, the ball milling further includes sieving, wherein the mesh size is 40-120 meshes.
In the step S1, the method for preparing the kava extract furfuryl alcohol resin includes:
s1-1, dispersing tannin extract and furfuryl alcohol in deionized water, adding a curing agent, uniformly stirring, and performing hydrothermal treatment at 60 ℃ to obtain a pretreatment solution;
s1-2, curing the pretreatment solution obtained in the step S1-1 at the temperature of 100-150 ℃, and cooling to obtain the tannin extract furfuryl alcohol resin.
In the step S1-1, the volume-mass ratio of the tannin extract to the furfuryl alcohol to the curing agent is 1-6 g: 3-18 g: 2-12 mL.
In the step S1-1, the curing agent is a p-toluenesulfonic acid solution with the mass fraction of 50% -70%.
In the step S1-1, the dispersion mode is ultrasonic dispersion, the ultrasonic power is 100-300W, and the ultrasonic time is 20-40 min.
An application of the graphene/kawasabi furfuryl alcohol resin derived carbon negative electrode material or the graphene/kawasabi furfuryl alcohol resin derived carbon negative electrode material prepared by the preparation method in a lithium ion battery or a sodium ion battery.
The main innovation points of the invention are as follows:
1. the applicant finds through long-term experimental research that in the prior art, the derived carbon is usually prepared by taking fossil fuels such as phenolic resin, other high molecular polymers, asphalt and the like as precursors, and then is applied to the field of negative electrode materials, although the synthetic resin has extremely high weather resistance and mechanical strength, the raw materials of the synthetic resin belong to non-renewable substances, the price is extremely easy to change infrequently due to international oil price fluctuation, and the product has the problems of release of formaldehyde or other toxic carcinogens and the like more or less. The applicant finds that the derived carbon material taking the biomass resin as the precursor can make up the deficiency of the traditional resin in the problems of environment and resource shortage, and the capacity and rate capability of the biomass derived carbon negative electrode material prepared by the prior art are general, so the applicant carries out deep research and development on the technical problem.
2. According to the invention, graphene load modification is carried out on the basis of obtaining tannin extract furfuryl alcohol resin derived carbon, S atoms are doped and the graphene anode material is coated, so that the obtained graphene/tannin extract furfuryl alcohol resin derived carbon anode material has higher first discharge specific capacity and excellent rate capability, and has outstanding advantages compared with the prior art.
Compared with the prior art, the invention has the advantages that:
(1) the graphene/kaki extract furfuryl alcohol resin derived carbon cathode material is used as a cathode material for a lithium/sodium ion battery, has a charge-discharge specific capacity (605 mAh/g) larger than that of graphite (372 mAh/g), and the first charge-discharge capacity and rate capability of the compounded kaki extract furfuryl alcohol resin derived carbon and graphene are improved, so that the graphene/kaki extract furfuryl alcohol resin derived carbon has good electrochemical performance, is pyrolytic derived carbon of a plant kaki extract resin polymer, has high capacity, low manufacturing cost and excellent cycle performance, and has great potential in the fields of research and application of electrochemistry and energy materials.
(2) The preparation method of the graphene/kaki extract furfuryl alcohol resin derived carbon cathode material eliminates the influence of the traditional resin taking fossil raw materials as precursors on the problems of environment and resource shortage, the kaki extract furfuryl alcohol mainly comprises bark extract kaki, agriculture and forestry waste biomass extract furfuryl alcohol and a sulfur-containing curing agent for providing sulfur atoms, the kaki extract furfuryl alcohol resin is used as a carbon source and a heteroatom source and is modified, and the sulfur atom doped kaki extract furfuryl alcohol resin derived carbon is prepared by a step-by-step medium/high temperature pyrolysis method, so that the obtained graphene/kaki extract furfuryl alcohol resin derived carbon cathode material has higher first discharge specific capacity and excellent rate performance, the raw material source is wide and rich, the environment is protected, the large-scale use of dangerous chemicals or fossil raw materials is avoided, and the process is simple and the cost is low.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of tannin extract furfuryl alcohol resin-derived carbon in example 1 of the present invention, wherein a is magnification × 5000 and b is magnification × 20000.
Fig. 2 is a Scanning Electron Microscope (SEM) image of the graphene/kawassan furfuryl alcohol resin-derived carbon negative electrode material in example 1 of the present invention, wherein the magnification of the image a is × 5000, and the magnification of the image b is × 20000.
FIG. 3 is an XRD pattern of graphene/kawasabi resin derived carbon anode material in examples 1-2 of the present invention.
FIG. 4 is a BET diagram of the graphene/kawasabi resin derived carbon negative electrode material in examples 1-2 of the present invention.
Fig. 5 is an XPS plot of graphene/kawasabi resin derived carbon negative electrode material in example 1 of the present invention.
Fig. 6 is a graph of the first charge and discharge curves of the graphene/kawasabi resin derived carbon negative electrode material at a current density of 50mA/g in example 1 of the present invention.
FIG. 7 is a graph showing the first charge and discharge curves of tannin extract furfuryl alcohol resin derived carbon at a current density of 50mA/g in example 1 of the present invention.
Fig. 8 is a graph of the first charge and discharge curves of the graphene/kawasabi resin derived carbon negative electrode material at a current density of 50mA/g in example 2 of the present invention.
FIG. 9 is a graph of rate capability of graphene/kawasabi resin derived carbon negative electrode material in examples 1-2 of the present invention.
Detailed Description
The invention is further described below with reference to the drawings and specific preferred embodiments of the description, without thereby limiting the scope of protection of the invention.
The materials and equipment used in the following examples are commercially available.
Example 1:
a method for preparing a graphene/kava furfuryl alcohol resin-derived carbon negative electrode material of the embodiment includes the following steps:
(1) 60g tannin extract and 180g furfuryl alcohol were treated with 100W ultrasound in 100mL deionized water for 30min, then 8mL65 wt% p-toluenesulfonic acid was added as a curing agent, and magnetic stirring was performed at room temperature for 20 min. Treating the precursor for 1h in a water bath at 60 ℃ by using a rotary evaporator, then pouring the treated precursor into a polytetrafluoroethylene mold, placing the polytetrafluoroethylene mold in a drying oven at 60 ℃ for 2d, a drying oven at 100 ℃ for 1d and a drying oven at 150 ℃ for 1d, cooling to room temperature, and demolding to obtain the dark brown tannin extract furfuryl alcohol resin.
In this example, p-toluenesulfonic acid is a sulfur-containing curing agent, and the tannin furfuryl alcohol resin serves as a carbon source and a heteroatom source in the subsequent steps.
(2) The tannin extract furfuryl alcohol resin obtained in the step (1) is carried out for 10 min under the protection of inert gas-1Heating to 500 deg.C, maintaining the temperature for 1h, pre-carbonizing, cooling, ball-milling, sieving (400 mesh), and keeping at 10 deg.C for 10 min under the protection of inert gas-1Heating to 1000 ℃ and preserving heat for 1h for pyrolysis and carbonization to obtain the tannin extract furfuryl alcohol resin derived carbon.
(3) Sonicating the mixture of 2g of tannin extract furfuryl alcohol resin derived carbon (HC) and 0.4g of Graphene Oxide (GO) obtained in step (2) in a 15% ethanol solution to disperse HC powder and GO flakes. After HC and GO were well dispersed, 0.1g of cetyltrimethylammonium bromide (CTAB) was dissolved in the suspension with magnetic stirring at room temperature. Mixing surfactant, GO and HC in solution, filtering, oven drying, and adding into inert atmosphere at 10 deg.C for min-1And heating to 1000 ℃ and preserving heat for 1h to obtain the graphene/tannin extract furfuryl alcohol resin derived carbon negative electrode material.
In the present embodiment, the surface modifier is cetyl trimethyl ammonium bromide, and in other embodiments, the surface modifier is one of polyvinylpyrrolidone and quaternary ammonium salt, and the same or similar technical effects can be obtained, which is used to better load graphene on the carbon derived from the kauri furfuryl alcohol resin.
In the embodiment, the temperature rising rate of the pre-carbonization and the pyrolysis carbonization is 10 ℃/min, the time of the pre-carbonization and the pyrolysis carbonization is 1h, in other embodiments, the temperature rising rate of the pre-carbonization and the pyrolysis carbonization is 10-20 ℃/min, and the time of the pre-carbonization and the pyrolysis carbonization is 0.5-5 h, which can obtain the same or similar technical effects.
The scanning electron microscope image of the tannin extract furfuryl alcohol resin derived carbon prepared in this example is shown in figure 1, and it can be seen that the material is basically composed of blocky particles with irregular shapes and has glossy surface.
A Scanning Electron Microscope (SEM) of the graphene/kawasabi furfuryl alcohol resin derived carbon negative electrode material prepared in this example is shown in fig. 2, and the reduced graphene is coated on the surface of kawasabi furfuryl alcohol resin derived carbon to form a three-dimensional core-shell structure. The microscopic morphology is beneficial to the storage of lithium/sodium ions, and the charge-discharge capacity and the rate capability of the lithium ion battery are improved when the microscopic morphology is subsequently applied to the lithium ion battery.
The XRD pattern, BET pattern and XPS pattern of the graphene/kawasabi resin derived carbon negative electrode material prepared in this example are shown in fig. 3, fig. 4 and fig. 5, respectively, which indicate that the derived carbon negative electrode material is an amorphous structure, the specific surface area of the composite material coated with graphene is increased, and the material contains S atoms, and the presence of sulfur atoms is beneficial to the improvement of rate capability and cycle performance.
An application of the graphene/kava furfuryl alcohol resin derived carbon negative electrode material prepared in the embodiment includes the following steps:
0.32g of graphene/kawasabi furfuryl alcohol resin derived carbon negative electrode material powder prepared in the embodiment is mixed with conductive carbon black and a binder (PVDF), the mass ratio of the graphene/kawasabi furfuryl alcohol resin derived carbon negative electrode material to the conductive carbon black to the binder is 8: 1, and then the obtained mixture is added into an N-methylpyrrolidone solvent and stirred for 6%h, coating a film on the copper foil to prepare a negative electrode plate; then using a metal lithium sheet as a counter electrode and LiPF6The EC/DMC/EMC (i.e. ethylene carbonate/dimethyl carbonate/ethyl methyl carbonate) mixed solution is used as electrolyte, and LiPF is added into the electrolyte6The concentration of the monomer is 1mol/L, the mass ratio of EC to DMC to EMC is 1: 1, and a Celgard2400 polypropylene film is taken as a diaphragm to assemble the button cell. When the charge and discharge current of the graphene/tannin extract furfuryl alcohol resin derived carbon negative electrode material is 50mA/g, the first specific discharge capacity reaches 746 mAh/g, and the first coulombic efficiency is 65.1%. The first charge-discharge curve is shown in fig. 6, it can be seen that the voltage hysteresis effect between the charge curve and the discharge curve is small, the rate capability is shown in fig. 9, and the requirements of the lithium ion battery on high voltage and high energy density can be met.
According to the application method, the kawasabi furfuryl alcohol resin derived carbon prepared in the embodiment is assembled into the button battery, the first charge-discharge curve is shown in fig. 7, the first specific discharge capacity of the kawasabi furfuryl alcohol resin derived carbon under the condition that the charge-discharge current is 50mA/g is only 605.7mAh/g, the first coulombic efficiency is 53.1%, and the specific capacity data is lower than that of the graphene/kawasabi furfuryl alcohol resin derived carbon negative electrode material obtained in the embodiment 1.
Example 2:
a method for preparing a graphene/kava furfuryl alcohol resin-derived carbon negative electrode material of the embodiment includes the following steps:
(1) 60g tannin extract and 180g furfuryl alcohol were treated with 100W ultrasound in 100mL deionized water for 30min, then 8mL65 wt% p-toluenesulfonic acid was added as a curing agent, and magnetic stirring was performed at room temperature for 20 min. Treating the precursor for 1h in a water bath at 60 ℃ by using a rotary evaporator, then pouring the treated precursor into a polytetrafluoroethylene mold, placing the polytetrafluoroethylene mold in a drying oven at 60 ℃ for 2d, a drying oven at 100 ℃ for 1d and a drying oven at 150 ℃ for 1d, cooling to room temperature, and demolding to obtain the dark brown tannin extract furfuryl alcohol resin.
(2) The tannin extract furfuryl alcohol resin obtained in the step (1) is carried out for 10 min under the protection of inert gas-1Heating to 500 deg.C, maintaining the temperature for 1h, pre-carbonizing, cooling, ball-milling, sieving (400 mesh), and keeping at 10 deg.C for 10 min under the protection of inert gas-1Heating to 1000 deg.C and maintaining for 1hAnd (4) carrying out pyrolysis carbonization to obtain the tannin extract furfuryl alcohol resin derived carbon.
(3) Sonicating the mixture of 2g of tannin extract furfuryl alcohol resin derived carbon (HC) and 0.4g of Graphene Oxide (GO) obtained in step (2) in a 15% ethanol solution to disperse HC powder and GO flakes. After HC and GO were well dispersed, 0.1g of polyvinylpyrrolidone (PVP) was dissolved in the suspension with magnetic stirring at room temperature. Mixing surfactant, GO and HC in solution, filtering, oven drying, and adding into inert atmosphere at 10 deg.C for min-1And heating to 1000 ℃ and preserving heat for 1h to obtain the graphene/tannin extract furfuryl alcohol resin derived carbon negative electrode material.
In this example, the precursor is kavalactone furfuryl alcohol resin, and the method for preparing kavalactone furfuryl alcohol resin-derived carbon in this example is the same as in example 1.
The button cell is assembled according to the application scheme in the example 1, and the first specific discharge capacity of the graphene/kauri furfuryl alcohol resin derived carbon negative electrode material prepared in the example reaches 677.7mAh/g under the condition that the charge and discharge current is 50mA/g, and the first coulombic efficiency is 64.9%. The first charge-discharge curve is shown in fig. 8, it can be seen that the voltage hysteresis effect between the charge curve and the discharge curve is small, the rate capability is shown in fig. 9, and the requirements of the lithium ion battery on high voltage and high energy density can be met.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make many possible variations and modifications to the disclosed embodiments, or equivalent modifications, without departing from the spirit and scope of the invention, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.
Claims (10)
1. A graphene/tannin extract furfuryl alcohol resin derived carbon negative electrode material is characterized in that: the graphene/kaki extract furfuryl alcohol resin derived carbon cathode material comprises graphene and kaki extract furfuryl alcohol resin derived carbon, wherein the graphene is coated on the surface of the kaki extract furfuryl alcohol resin derived carbon, the graphene/kaki extract furfuryl alcohol resin derived carbon cathode material is formed by pyrolysis and carbonization of kaki extract furfuryl alcohol resin derived carbon, graphene oxide and a surfactant, and the kaki extract furfuryl alcohol resin derived carbon is formed by carbonization of kaki extract furfuryl alcohol resin prepared from kaki extract, furfuryl alcohol and a curing agent.
2. A preparation method of a graphene/tannin extract furfuryl alcohol resin derived carbon negative electrode material is characterized by comprising the following steps: the method comprises the following steps:
s1, taking tannin extract furfuryl alcohol resin as a precursor, heating to 400-600 ℃ in a gas protection atmosphere for pre-carbonization, cooling, grinding, and heating to 900-1200 ℃ in a gas protection atmosphere for pyrolysis carbonization to obtain tannin extract furfuryl alcohol resin derived carbon;
s2, dispersing the tannin extract furfuryl alcohol resin derived carbon and graphene oxide obtained in the step S1 in a solvent to obtain a suspension, adding a surfactant into the suspension, uniformly mixing, filtering, drying, heating to 900-1200 ℃ in a gas protection atmosphere, and carrying out pyrolysis carbonization to obtain the graphene/tannin extract furfuryl alcohol resin derived carbon negative electrode material.
3. The method of claim 2, wherein: in the step S1 and the step S2, the temperature rise rate of the pre-carbonization and the pyrolysis carbonization is 10-20 ℃/min, and the time of the pre-carbonization and the pyrolysis carbonization is 0.5-5 h.
4. The production method according to claim 2 or 3, characterized in that: in the step S2, the surfactant is one of cetyl trimethyl ammonium bromide, polyvinylpyrrolidone and quaternary ammonium salt, and the volume mass ratio of the suspension to the surfactant is 80-150 mL: 1-15 g.
5. The production method according to claim 2 or 3, characterized in that: in the step S2, the tannin extract furfuryl alcohol resin-derived carbon and graphene oxide are dispersed in the solvent by ultrasonic dispersion; the solvent is an ethanol solution with the mass fraction of 15-30%; the mass ratio of the tannin extract furfuryl alcohol resin derived carbon to the graphene oxide is 4-8: 0.5-2.
6. The method of claim 5, wherein: in the step S2, the power of ultrasonic dispersion is 100-600W, and the time of ultrasonic dispersion is 20-60 min.
7. The production method according to claim 2 or 3, characterized in that: in the step S1, the grinding is ball milling, the ball milling rotation speed is 400-1000 r/min, and the time is 10-60 min.
8. The production method according to claim 2 or 3, characterized in that: in the step S1, the method for preparing the kava extract furfuryl alcohol resin includes:
s1-1, dispersing tannin extract and furfuryl alcohol in deionized water, adding a curing agent, uniformly stirring, and performing hydrothermal treatment at 60 ℃ to obtain a pretreatment solution;
s1-2, curing the pretreatment solution obtained in the step S1-1 at the temperature of 100-150 ℃, and cooling to obtain the tannin extract furfuryl alcohol resin.
9. The method according to claim 8, wherein: in the step S1-1, the volume-mass ratio of the tannin extract to the furfuryl alcohol to the curing agent is 1-6 g: 3-18 g: 2-12 mL.
10. Use of the graphene/kawasabi furfuryl alcohol resin derived carbon negative electrode material according to claim 1 or the graphene/kawasabi furfuryl alcohol resin derived carbon negative electrode material prepared by the preparation method according to any one of claims 2 to 9 in a lithium ion battery or a sodium ion battery.
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