CN110182806B - Preparation of porous biomass charcoal electrode material derived from chicken twigs - Google Patents
Preparation of porous biomass charcoal electrode material derived from chicken twigs Download PDFInfo
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Abstract
The invention discloses a preparation method of a porous biomass carbon electrode material derived from chicken twigs, belongs to the technical field of supercapacitors, and aims to mainly solve the problems that the existing carbon-based electrode material is low in specific capacitance, low in rate performance and the like. The product takes KOH as a sacrificial template and an activating agent, and prepares the biomass carbon with rich pore channel structures and high graphitization degree through high-temperature carbonization and activation treatment processes. The electrode material used as a working electrode shows high specific capacitance, excellent rate characteristic and good cycling stability, the preparation process is green and environment-friendly, the operation is simple, and the method can be used for synthesizing porous carbon electrode materials derived from other biomass materials.
Description
Technical Field
The invention belongs to the technical field of supercapacitors, and particularly relates to a preparation method of a porous biomass carbon electrode material derived from chicken twigs.
Background
The rapid consumption of fossil energy has a great impact on the world's economy and ecological environment. With the improvement of environmental awareness of people, efficient, clean and safe energy systems are developed and are more and more concerned by researchers. Chemical energy storage is a research hotspot of energy systems. In a plurality of chemical energy storage devices, the super capacitor is widely applied due to the characteristics of safety, high efficiency and sustainability.
The working principle of the double electric layer super capacitor is that energy is stored through a double electric layer formed by an electrode-electrolyte interface, and the double electric layer super capacitor is widely applied due to the advantages of high power density, rapid charge and discharge capacity, wide working temperature range and the like; the electrode material can influence the application of the capacitor in some fields, and in a plurality of electrode materials, the activated carbon material has attracted wide attention due to the characteristics of high specific surface area, good electrochemical property, low price and the like.
The method takes biomass materials with wide raw materials as carbon precursors, has the characteristics of low production cost, environmental friendliness and the like, has non-toxic and safe preparation process and strong feasibility, takes the chicken twigs as the carbon precursors with high carbon content, has the advantages of rich natural resources, strong cold resistance, wide territorial scope and the like, and lays a research foundation for marketized application of the chicken twigs.
Disclosure of Invention
The invention belongs to the technical field of super capacitors, and aims to mainly solve the problems that the existing carbon-based electrode material is low in specific capacitance and rate performance, and the like.
The invention relates to a preparation method of a chicken-wood-strip-derived porous biomass charcoal electrode material, which is characterized in that KOH is used as a sacrificial template and an activating agent for preparing the chicken-wood-strip-derived porous biomass charcoal electrode material, and biomass charcoal with rich pore channel structures and high graphitization degree is prepared through high-temperature carbonization and activation treatment;
KOH is used as a sacrificial template and an activating agent of the chicken-strip-derived porous biomass carbon electrode material;
the porous biomass carbon electrode material derived from the chicken twigs is prepared under the condition of nitrogen protection through high-temperature carbonization and activation processes;
the chicken-tree-strip-derived porous biomass carbon electrode material has ultrahigh graphitization degree and higher specific surface area;
the invention has the beneficial effects that:
compared with the existing supercapacitor electrode material, the porous biomass carbon electrode material derived from the chicken twigs synthesized by the method solves the problems of low specific capacitance, poor reversibility, poor conductivity and the like of the existing carbon-based electrode material, and the prepared porous biomass carbon electrode material derived from the chicken twigs has the characteristics of economic and environment-friendly preparation process, good conductivity, high specific capacitance and the like.
Drawings
Fig. 1 is a scanning electron microscope image of the chicken-wood-strip-derived porous biomass charcoal electrode material obtained in the verification test (i).
Fig. 2 is a transmission electron microscope image of the chicken-wood-strip-derived porous biomass carbon electrode material obtained in the verification test (i).
Fig. 3 is an X-ray powder diffraction pattern of the porous biomass charcoal electrode material derived from the chicken-wood strip obtained in the validation test (one).
Fig. 4 is a cyclic voltammetry Curve (CV) of the porous biomass charcoal electrode material derived from the chicken twigs in the verification test (ii) under different sweep rates;
FIG. 5 is a constant current charging and discharging diagram of the porous biomass charcoal electrode material derived from the chicken twigs in the verification test (III) under different current densities;
fig. 6 is an alternating current impedance diagram of the porous biomass charcoal electrode material derived from the chicken-shoot in the verification test (iv);
fig. 7 is a graph showing the cycle stability of the chicken-wood-strip-derived porous biomass charcoal electrode material synthesized in the verification test (iv).
Detailed Description
The first embodiment is as follows: in the embodiment, KOH is used as a sacrificial template and an activating agent, the chicken tree leaves are used as a carbon precursor, and the porous carbon material with high graphitization degree is prepared through high-temperature carbonization and activation processes.
The second embodiment is as follows: a preparation method of a chicken strip derived porous biomass carbon electrode material comprises the following steps:
firstly, preparation of unactivated carbon material:
firstly, washing collected chicken strips and leaves by deionized water and ethanol for 3-5 times respectively to remove impurities on the surfaces, and then drying the chicken strips and leaves at 60 ℃ for 48-50 hours;
② grinding the dried leaves, weighing 6-8 g, placing in a porcelain boat, and N at 500 DEG C2Protecting and carbonizing for 2h, wherein the heating rate is 5 ℃/min, and then grinding and sample loading are carried out on the obtained black powder A;
secondly, preparing a porous biomass charcoal material:
accurately weighing 0.9-1.1 g of black powder A and 5g of KOH solid, dissolving the black powder A and the KOH solid in 20mL of deionized water, magnetically stirring for 30min to form a mixed solution B, and drying the solution B at 60 ℃ for 48-50 h to form paste C;
② grinding the paste C in a mortar for 30min, then placing the ground paste C in a horizontal tube furnace at 600 ℃ under N2Protecting and activating for 2h, wherein the heating rate is 5 ℃/min, and obtaining black powder D;
thirdly, washing the obtained black powder D for 3-5 times by 0.5mol/L hydrochloric acid solution, then washing for multiple times to remove impurities and redundant hydrochloric acid solution, and drying for 22-24 hours at the temperature of 60 ℃ to obtain a target product black powder E;
in the second step, the mass ratio of the black powder A to the KOH solid is 0.9-1.1 g: 5 g;
in the second step, the volume ratio of the black powder A to the deionized water is 0.9-1.1 g: 20 mL;
the third concrete implementation mode: the first to second differences of this embodiment from the first to second embodiments are: washing the collected chicken twigs and leaves for 5 times by using deionized water and ethanol respectively in the first step to remove impurities on the surfaces, and then drying the chicken twigs and leaves for 48 hours at the temperature of 60 ℃. Other steps and parameters are the same as those in one of the first to second embodiments.
The fourth concrete implementation mode: the present embodiment differs from the first to third embodiments in that: grinding the dried leaves in the step one, weighing 8g of the ground leaves, placing the ground leaves in a porcelain boat at 500 ℃ under N2And (4) performing protective carbonization for 2h, wherein the heating rate is 5 ℃/min, and then grinding and sample loading are performed on the obtained black powder A. Other steps and parameters and embodimentsOne of the three is the same.
The fifth concrete implementation mode: the first to fourth differences of this embodiment from the first to fourth embodiments are: and secondly, accurately weighing 1g of the black powder A and 5g of KOH solid, dissolving the black powder A and the KOH solid in 20mL of deionized water, and magnetically stirring for 30min to form a mixed solution B. Other steps and parameters are the same as those in one of the first to fourth embodiments.
The sixth specific implementation mode: the present embodiment is different from the first to fifth embodiments in that: and drying the solution B for 48 hours at the temperature of 60 ℃ to form paste C. Other steps and parameters are the same as those in one of the first to fifth embodiments.
The seventh embodiment: the present embodiment differs from the first to sixth embodiments in that: washing the obtained black powder D for 3 times by using 0.5mol/L hydrochloric acid solution, and then washing for multiple times to remove impurities and redundant hydrochloric acid solution. Other steps and parameters are the same as those in one of the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from the first to seventh embodiments in that: and thirdly, drying for 24 hours at the temperature of 60 ℃ to obtain the target product black powder E. Other steps and parameters are the same as those in one of the first to seventh embodiments.
The following tests were conducted to confirm the effects of the present invention
Experiment I, a preparation method of the chicken strip derived porous biomass carbon electrode material comprises the following steps:
firstly, preparation of unactivated carbon material:
firstly, washing collected chicken strips and leaves for 5 times respectively by deionized water and ethanol to remove impurities on the surface, and then drying the chicken strips and leaves for 48 hours at the temperature of 60 ℃;
② grinding the dried leaves, weighing 8g, placing in a porcelain boat, and placing at 500 ℃ under N2Protecting and carbonizing for 2h, wherein the heating rate is 5 ℃/min, and then grinding and sample loading are carried out on the obtained black powder A;
secondly, preparing a porous biomass charcoal material:
accurately weighing 1g of black powder A and 5g of KOH solid, dissolving the black powder A and 5g of KOH solid in 20mL of deionized water, magnetically stirring for 30min to form a mixed solution B, and drying the solution B at the temperature of 60 ℃ for 48h to form paste C;
② grinding the paste C in a mortar for 30min, then placing the ground paste C in a horizontal tube furnace at 600 ℃ under N2Protecting and activating for 2h, wherein the heating rate is 5 ℃/min, and obtaining black powder D;
thirdly, washing the obtained black powder D for 3 times by 0.5mol/L hydrochloric acid solution, then washing for multiple times to remove impurities and redundant hydrochloric acid solution, and drying for 24 hours at the temperature of 60 ℃ to obtain a target product black powder E;
and (3) determining the structure and characterizing the morphology of the chicken-tree-strip-derived porous biomass charcoal electrode material obtained in the first test:
determining the structure and characterizing the morphology of the porous biomass carbon electrode material derived from the chicken tree twigs obtained in the first test by using an S-4300 type Scanning Electron Microscope (SEM), a JEM-2010 type Transmission Electron Microscope (TEM) and a TTR-III type X-ray powder diffractometer, so as to obtain a scanning electron microscope image of the porous biomass carbon electrode material derived from the chicken tree twigs in figure 1, a transmission electron microscope image of the porous biomass carbon electrode material derived from the chicken tree twigs in figure 2 and an X-ray powder diffraction image of the porous biomass carbon electrode material derived from the chicken tree twigs in figure 3.
As can be seen from figure 1, the prepared chicken tree strip-derived porous biomass carbon electrode material has a rich pore structure, uniform pore distribution, a honeycomb-like shape and a high specific surface area.
Fig. 2 is a transmission electron microscope image of a chicken-wood-strip-derived porous biomass charcoal electrode material, wherein in the images a and b, the prepared biomass charcoal material has a rich microporous structure, the image b is an enlarged image of the image a, the image c is an enlarged image of the image c, the biomass charcoal material has obvious lattice stripes, the image d is an enlarged image of the image c, and the lattice spacing is 0.32nm, so that the successful preparation of the carbon material is further confirmed, and the electrode material has a high graphitization degree.
Fig. 3 is an X-ray powder diffraction pattern of the porous biomass charcoal electrode material derived from chicken twigs, in which two distinct peak positions are seen at 2 θ values of about 23.5 ° and 44 °, corresponding to (002) and (101) crystal planes, respectively. The X-ray powder diffraction pattern results indicate that the carbon material was successfully prepared.
And (II) verifying the electrochemical behavior of the chicken-wood-strip-derived porous biomass charcoal electrode material obtained in the first test of the application.
Preparation of super capacitor
The porous biomass carbon electrode material derived from the chicken twigs obtained in the first test of the application, acetylene black and Polytetrafluoroethylene (PTFE) are mixed to form an electrode active substance, foamed nickel coated with the active substance is used as a working electrode, saturated calomel is used as a reference electrode, a platinum sheet electrode is used as a counter electrode, and a three-electrode system formed by the electrode active substance, the acetylene black and the PTFE is the supercapacitor.
And secondly, taking the porous biomass carbon electrode material derived from the chicken twigs prepared in the step one as a working electrode, and obtaining cyclic voltammetry curves of the porous biomass carbon electrode material derived from the chicken twigs by the prepared super capacitor under the conditions that sweep rates are respectively 10mV/s, 20mV/s, 30mV/s, 50mV/s, 80mV/s and 100 mV/s.
And (4) conclusion: the cyclic voltammetry curve of the chicken-tree-twig-derived porous biomass carbon electrode material obtained at the sweep rate of 10mV/s-100mV/s as shown in FIG. 4 is obtained, and it can be seen from the figure that the area enclosed by the cyclic voltammetry curve is gradually increased along with the gradual increase of the sweep rate, so that the good multiplying power performance is proved, and the pseudocapacitance performance is proved because a pair of weak redox peaks appear on the curve. These results indicate that the porous biomass charcoal electrode material derived from the chicken twigs can improve the electrochemical activity.
And (III) verifying the charge and discharge performance of the chicken tree strip-derived porous biomass charcoal electrode material obtained in the first experiment.
Preparing a super capacitor: the porous biomass carbon electrode material derived from the chicken twigs obtained in the first test of the application is mixed with acetylene black and PTFE to form an electrode active material, foamed nickel coated with the active material is used as a working electrode, saturated calomel is used as a reference electrode, a platinum sheet electrode is used as a counter electrode, and a three-electrode system is formed to form the supercapacitor.
Testing the charge-discharge performance of the porous biomass carbon electrode material derived from the added chicken twigs under the conditions of current densities of 0.5A/g, 1A/g, 2A/g, 3A/g, 5A/g and 8A/g and potential windows of-1-0V by adopting a constant current charge-discharge method to obtain the charge-discharge curve of the porous biomass carbon electrode material derived from the chicken twigs as shown in figure 5, wherein the specific capacitance at 0.5A/g can be seen to be up to 612.8 F.g-1At 8A/g, 319.6F · g still remains-1The capacitance of (c).
And (IV) verifying the conductivity and the cycling stability of the chicken-wood-strip-derived porous biomass carbon electrode material obtained in the first experiment.
Preparing a super capacitor: the porous biomass carbon electrode material derived from the chicken twigs obtained in the first test of the application is mixed with acetylene black and PTFE to form an electrode active substance, foamed nickel coated with the active substance is used as a working electrode, saturated calomel is used as a reference electrode, a platinum sheet electrode is used as a counter electrode, and a formed three-electrode system is the supercapacitor.
Testing the alternating current impedance spectrum of the porous biomass carbon electrode material derived from the chicken twigs through an electrochemical workstation, wherein the frequency range is 0.05-105Hz, the Nyquist curve obtained consists of two parts, namely a semicircular part of a high-frequency region and a linear part of a low-frequency region. The Nyquist curve shows that the chicken-twigs-derived porous biomass charcoal electrode material has smaller charge transfer resistance, because the charge transfer process between the chicken-twigs-derived porous biomass charcoal electrode material and an electrolyte is faster, thereby indicating the porous structure of the biomass charcoal and the electrode material has higher conductivity. In the low-frequency part, the linear slope of the porous biomass charcoal electrode material derived from the hollow chicken twigs is steeper, which indicates that the porous biomass charcoal electrode material derived from the chicken twigs has smaller ion diffusion resistance. Meanwhile, the capacitance retention rate of the electrode material is calculated through ten thousand cycles of charge and discharge tests, 96.02% of the initial capacitance of the electrode material is still maintained after two thousand cycles of cycle, and the synthesized electrode material is proved to have good conductivity and cycle stability according to the results.
In conclusion, the porous biomass charcoal electrode material derived from the chicken twigs has been successfully prepared, and the prepared electrode material has the advantages of high specific capacitance value, good cycle stability, wide material source, sustainability, green and environment-friendly preparation process and the like.
Claims (1)
1. A preparation method of a porous biomass charcoal electrode material based on chicken tree twigs derivation is characterized by comprising the following steps:
firstly, preparation of unactivated carbon material:
firstly, washing collected chicken strips and leaves by deionized water and ethanol for 3-5 times respectively to remove impurities on the surfaces, and then drying the chicken strips and leaves at 60 ℃ for 48-50 hours;
② grinding the dried leaves, weighing 6-8 g, placing in a porcelain boat, and N at 500 DEG C2Protecting and carbonizing for 2h, wherein the heating rate is 5 ℃/min, and then grinding and sample loading are carried out on the obtained black powder A;
secondly, preparing a porous biomass charcoal material:
accurately weighing 0.9-1.1 g of black powder A and 5g of KOH solid, dissolving the black powder A and the KOH solid in 20mL of deionized water, magnetically stirring for 30min to form a mixed solution B, and drying the solution B at 60 ℃ for 48-50 h to form paste C;
② grinding the paste C in a mortar for 30min, then placing the ground paste C in a horizontal tube furnace at 600 ℃ under N2Protecting and activating for 2h, wherein the heating rate is 5 ℃/min, and obtaining black powder D;
thirdly, washing the obtained black powder D for 3-5 times by 0.5mol/L hydrochloric acid solution, then washing for multiple times to remove impurities and redundant hydrochloric acid solution, and drying for 22-24 hours at the temperature of 60 ℃ to obtain a target product black powder E;
in the second step, the mass ratio of the black powder A to the KOH solid is 0.9-1.1 g: 5 g;
and in the second step, the volume ratio of the black powder A to the deionized water is 0.9-1.1 g: 20 mL.
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