CN110627037B - Preparation method of nitrogen-doped biomass porous carbon nano electrode material - Google Patents
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Abstract
The invention discloses a preparation method of a nitrogen-doped biomass porous carbon nano electrode material, which comprises the steps of cleaning peel biomass by using alcohol under the ultrasonic action, and performing freeze drying and ball milling treatment to obtain powder A; adding a nitric acid solution into the powdery A, and stirring to obtain B; transferring the B into a hydrothermal induction kettle, adding carbon cloth as an induction source, transferring the hydrothermal induction kettle into hydrothermal induction heating equipment for reaction, cooling to room temperature after the reaction is finished, taking out the carbon cloth to scrape the product, washing the product with deionized water and ethanol, centrifuging, and drying to obtain C; mixing and grinding the C, the activating agent and the nitrogen source to obtain D; calcining the D in a protective gas atmosphere, cooling to room temperature after the calcining is finished, washing, filtering and drying the obtained product by deionized water and ethanol, and obtaining the nitrogen-doped biomass porous carbon nano electrode material.
Description
Technical Field
The invention belongs to the field of preparation of biomass carbon materials, and particularly relates to a preparation method of a nitrogen-doped biomass porous carbon nano electrode material.
Background
Biomass energy is one of the important energy sources on which humans rely for survival, and occupies an important position in the whole energy system. Because the fossil energy is gradually exhausted due to excessive exploitation of human beings, the research and development of green and environment-friendly new energy and materials thereof are extremely slow. The biomass carbon prepared from the biomass material has the characteristics of light weight, rich pore structure, large specific surface area, good structural stability, excellent conductivity and the like, and is widely applied to the advanced scientific and technological fields of lithium ion batteries, supercapacitors, gas adsorption and separation, water body purification and the like.
There have been many studies on the application of biomass carbon materials to lithium ion battery cathodes. The introduction of heteroatoms such as N, S, P or O in the porous biomass carbon material can significantly improve the electrochemical, mechanical or electrical conductivity properties. Particularly, the N element can partially replace the C element, so that a plurality of dislocation, bending, dislocation and other defect sites with unpaired electrons are generated on the graphite microcrystal plane layer in the carbon layer; meanwhile, the introduction of nitrogen atoms enables the surface of the material to have alkalinity, so that the surface wettability of the material can be enhanced, and the capacity performance of the material can be improved. The nitrogen-doped porous carbon has high specific surface area, abundant pore structures and a large number of surface nitrogen-containing functional groups, so that the material is endowed with unique properties of energy storage, machinery, electronics, optics, semiconductors and the like.
In the prior art, nitrogen-doped biomass carbon as an electrode material of a lithium ion battery gradually becomes a research hotspot. For example, Gao et al ([ J ]]Journal of Power Sources,2019,415:165-171.) the walnut shell was used as the raw material, the dried sample and urea were soaked together in a ratio of 1:1, the soaked mixture was placed in a tube furnace, argon gas was introduced at 800 ℃ to carbonize for 2 hours to obtain a sample. The nitrogen content of the product prepared by the method is uncontrollable, the calcination temperature is high, and the economic benefit of the product is seriously reduced. Guo et al ([ J)].ACS applied materials&ifaces, 2018,10(44):38376 and 38386) uses squid as a biomass raw material,placing the squid pieces into a tube furnace, and heating at 3 deg.C for min under nitrogen atmosphere-1The temperature rising speed is increased to 600 ℃, the mixture is carbonized for 1 hour under the condition of heat preservation, and then the mixture is naturally cooled to the room temperature. The carbon material was then washed with 1M HCl and sufficient deionized water and freeze dried. The dried sample was further activated at 300 ℃ with air flow to obtain a sample. The raw materials in the method are not biomass wastes and have high cost, the multiplying power performance of the synthesized product is poor, the process flow is complex, and the large-scale popularization is complex. Therefore, the development of a simple and feasible process with wide raw material sources, low cost and excellent electrochemical performance to prepare the nitrogen-doped porous carbon nano material has important significance.
Disclosure of Invention
The invention aims to provide a preparation method of a nitrogen-doped biomass porous carbon nano electrode material, so as to overcome the defects in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a nitrogen-doped biomass porous carbon nano electrode material comprises the following steps:
1) cleaning peel biomass with alcohol under the ultrasonic action, and performing freeze drying and ball milling treatment to obtain powder A;
2) adding a nitric acid solution into the powdery A, and stirring to obtain B;
3) transferring the B into a hydrothermal induction kettle, adding carbon cloth as an induction source, moving the hydrothermal induction kettle into hydrothermal induction heating equipment, heating the hydrothermal induction kettle to 150-180 ℃ from room temperature at an induction frequency of 300-600 KHz, preserving heat for 20-60 min, cooling to room temperature, taking out the carbon cloth, scraping a product, washing the product with deionized water and ethanol, centrifuging, and drying to obtain C;
4) mixing and grinding the C, the activating agent and the nitrogen source to obtain D;
5) and D, heating to 350 ℃ at a heating rate of 3 ℃/min in a protective gas atmosphere, preserving heat for 1h, heating to 500-700 ℃ at a heating rate of 5 ℃/min, preserving heat for 1-3 h, cooling to room temperature, washing, filtering and drying the obtained product by deionized water and ethanol, and thus obtaining the nitrogen-doped biomass porous carbon nano electrode material.
Further, the pericarp biomass in the step 1) is shaddock peel, orange peel, banana peel or longan shell.
Further, in the step 1), the ultrasonic frequency is 40KHz, the freeze drying temperature is-20-10 ℃, the time is 12-24 hours, and the ball milling time is 2-4 hours.
Further, 1-4 g of powdery A is added into every 40-70 mL of nitric acid solution in the step 2), and the concentration of the nitric acid solution is 1-3 mol/L.
Further, in the step 2), magnetic stirring is adopted, and the stirring is carried out for 10-40 min at the rotating speed of 300-600 r/min.
Further, the length, width and height of the carbon cloth in the step 3) are respectively 3cm, 2cm and 0.1cm, and the drying in the step 3) is specifically as follows: drying for 6 hours under an infrared lamp at 50-80 ℃.
Further, in the step 4), the activating agent is zinc nitrate, ferric nitrate, magnesium nitrate or nickel nitrate, and the nitrogen source is one of urea, melamine, ammonium nitrate and ammonium citrate.
Further, the mass ratio of C, the activating agent and the nitrogen source in the step 4) is (1-2) to (1-4).
Further, the grinding time in the step 4) is 10-30 min.
Further, the drying in the step 5) specifically comprises the following steps: dried under vacuum at 70 ℃ for 6 h.
Compared with the prior art, the invention has the following beneficial technical effects:
1. the method selects the wastes such as the pericarp and the like as the biomass carbon source, changes wastes into valuables, is green and environment-friendly, and has extremely high resource advantages and cost advantages.
2. The preparation process of the lithium ion battery cathode material provided by the invention is simple, the conditions are mild and controllable, the production cost is low, the repeatability is high, and the industrial production is easy to realize.
3. The lithium ion battery cathode material synthesized by the invention has a three-dimensional nano-porous nitrogen-containing structure, can provide a large number of reaction active sites, and effectively increases the lithium ion adsorption rate, diffusion rate and electron transmission rate. And the good wettability is beneficial to the diffusion of lithium ions in the boundary of the electrode and the electrolyte and the electrode block.
4. The nitrogen-doped biomass porous carbon nanomaterial prepared by the invention can be applied to lithium ion batteries, can obviously improve the rate capability of the batteries, and has high capacity, excellent cycle stability, thermal stability, chemical stability and mechanical flexibility.
Drawings
FIG. 1 is an SEM image of nitrogen-doped biomass porous carbon nanomaterial of example 3;
FIG. 2 is an XRD pattern of the nitrogen-doped biomass porous carbon nanomaterial in example 3;
fig. 3 is a graph of rate capability of the nitrogen-doped biomass porous carbon nanomaterial of example 3.
Detailed Description
Embodiments of the invention are described in further detail below:
a preparation method of a nitrogen-doped biomass porous carbon nano electrode material. The nitrogen-doped porous carbon nano material can form a sample with a honeycomb-shaped porous three-dimensional carbon nano structure after hydrothermal induction and carbonization treatment. The electrode material is simple in preparation process, environment-friendly in raw materials, capable of changing waste into valuable, and excellent in rate performance when applied to lithium ion batteries.
The method specifically comprises the following steps:
1. ultrasonically cleaning peel biomass such as shaddock peel, orange peel, banana peel and longan shell with alcohol at the frequency of 40KHz, freeze-drying at the temperature of-20-10 ℃ for 12-24 h, and ball-milling for 2-4 h to obtain powder A;
2. weighing 1-4 g of powdery A, adding 40-70 ml of nitric acid with the concentration of 1-3 mol/L into the powdery A, and stirring for 10-40 min at the rotating speed of 300-600 r/min by adopting magnetic stirring to obtain B.
3. And transferring the B into a hydrothermal induction kettle, and adding carbon cloth with the length, width and height of 3cm, 2cm and 0.1cm as an induction source. Moving the hydrothermal induction kettle into hydrothermal induction heating equipment, heating the hydrothermal induction kettle to 150-180 ℃ from room temperature at an induction frequency of 300-600 KHz, preserving the heat for 20-60 min, cooling to room temperature, taking out a carbon cloth scraping product, washing the product with deionized water and ethanol, centrifuging, and drying for 6h under an infrared lamp at 50-80 ℃ to obtain C;
4. c, mixing an activating agent (zinc nitrate, ferric nitrate, magnesium nitrate and nickel nitrate) and a nitrogen source (one or more of urea, melamine, ammonium nitrate and ammonium citrate) according to a mass ratio of C: activating agent: and mixing the nitrogen source in a ratio of 1:1:2, 1:1:3, 1:1:4 and 2:2:1, and grinding the mixture for 10-30 min by using an agate mortar to obtain D.
5. And D, moving the D into a tubular furnace into which nitrogen is introduced, heating to 350 ℃ at the heating rate of 3 ℃/min, preserving heat for 1h, heating to 500-700 ℃ at the heating rate of 5 ℃/min, preserving heat for 1-3 h, and cooling to room temperature. And washing and filtering the obtained product by deionized water and ethanol, and drying in a vacuum oven at 70 ℃ for 6 hours to obtain the nitrogen-doped biomass porous carbon nano material.
The present invention is described in further detail below with reference to examples:
example 1
1. Ultrasonically cleaning pericarp biomass shaddock peel with alcohol at the frequency of 40KHz, freeze-drying at-20 ℃ for 12h, and ball-milling for 2h to obtain powder A;
2. weighing 1g of powder A, adding 40ml of nitric acid with the concentration of 1mol/L into the powder A, and stirring for 10min at the rotating speed of 300r/min by adopting magnetic stirring to obtain B.
3. And transferring the B into a hydrothermal induction kettle, and adding carbon cloth with the length, width and height of 3cm, 2cm and 0.1cm as an induction source. Moving the hydrothermal induction kettle into hydrothermal induction heating equipment, heating the hydrothermal induction kettle to 150 ℃ from room temperature at an induction frequency of 300KHz, preserving heat for 20min, cooling to room temperature, taking out a carbon cloth scraping product, washing the obtained product with deionized water and ethanol, centrifuging, and drying for 6h under an infrared lamp at 50 ℃ to obtain C;
4. c, activating agent zinc nitrate and nitrogen source urea according to the mass ratio of C: zinc nitrate: mixing urea according to the proportion, and grinding for 10min by using an agate mortar to obtain D.
5. And D, moving the D into a tubular furnace into which nitrogen is introduced, heating to 350 ℃ at the heating rate of 3 ℃/min, preserving heat for 1h, heating to 500 ℃ at the heating rate of 5 ℃/min, preserving heat for 1h, and cooling to room temperature. And washing and filtering the obtained product by deionized water and ethanol, and drying in a vacuum oven at 70 ℃ for 6 hours to obtain the nitrogen-doped biomass porous carbon nano material.
Example 2
1. Ultrasonically cleaning peel biomass orange peel with alcohol at the frequency of 40KHz, freeze-drying at-10 ℃ for 16h, and ball-milling for 3h to obtain powder A;
2. weighing 2g of powder A, adding 50ml of nitric acid with the concentration of 2mol/L into the powder A, and stirring for 20min at the rotating speed of 400r/min by adopting magnetic stirring to obtain B.
3. And transferring the B into a hydrothermal induction kettle, and adding carbon cloth with the length, width and height of 3cm, 2cm and 0.1cm as an induction source. Moving the hydrothermal induction kettle into hydrothermal induction heating equipment, heating the hydrothermal induction kettle to 160 ℃ from room temperature at an induction frequency of 400KHz, preserving the temperature for 40min, cooling to room temperature, taking out a carbon cloth scraping product, washing and centrifuging the obtained product by deionized water and ethanol, and drying the product for 6h under an infrared lamp at 60 ℃ to obtain C;
4. c, activating agent ferric nitrate and nitrogen source melamine according to the mass ratio of C: iron nitrate: and (3) mixing melamine in a ratio of 1:1:3, and grinding the mixture for 20min by using an agate mortar to obtain D.
5. And D, moving the D into a tubular furnace into which nitrogen is introduced, heating to 350 ℃ at the heating rate of 3 ℃/min, preserving heat for 1h, heating to 600 ℃ at the heating rate of 5 ℃/min, preserving heat for 2h, and cooling to room temperature. And washing and filtering the obtained product by deionized water and ethanol, and drying in a vacuum oven at 70 ℃ for 6 hours to obtain the nitrogen-doped biomass porous carbon nano material.
Example 3
1. Ultrasonically cleaning peel biomass banana peel with alcohol at the frequency of 40KHz, freeze-drying at the temperature of 0 ℃ for 20h, and then ball-milling for 3h to obtain powder A;
2. weighing 3g of powder A, adding 60ml of nitric acid with the concentration of 2mol/L into the powder A, and stirring for 30min at the rotating speed of 500r/min by adopting magnetic stirring to obtain B.
3. And transferring the B into a hydrothermal induction kettle, and adding carbon cloth with the length, width and height of 3cm, 2cm and 0.1cm as an induction source. Moving the hydrothermal induction kettle into hydrothermal induction heating equipment, heating the hydrothermal induction kettle to 170 ℃ from room temperature at the induction frequency of 500KHz, preserving the heat for 50min, cooling to room temperature, taking out a carbon cloth scraping product, washing and centrifuging the obtained product by deionized water and ethanol, and drying the product for 6h under an infrared lamp at the temperature of 70 ℃ to obtain C;
4. c, activating agent magnesium nitrate and nitrogen source ammonium nitrate according to the mass ratio of C: magnesium nitrate: mixing ammonium nitrate at the ratio of 1:1:4, and grinding with agate mortar for 20min to obtain D.
5. And D, moving the D into a tubular furnace into which nitrogen is introduced, heating to 350 ℃ at the heating rate of 3 ℃/min, preserving heat for 1h, heating to 600 ℃ at the heating rate of 5 ℃/min, preserving heat for 2h, and cooling to room temperature. And washing and filtering the obtained product by deionized water and ethanol, and drying in a vacuum oven at 70 ℃ for 6 hours to obtain the nitrogen-doped biomass porous carbon nano material.
Example 4
1. Ultrasonically cleaning pericarp biomass longan shells with alcohol at the frequency of 40KHz, freeze-drying at the temperature of 10 ℃ for 24 hours, and then ball-milling for 4 hours to obtain powder A;
2. weighing 4g of powder A, adding 70ml of nitric acid with the concentration of 3mol/L into the powder A, and stirring for 40min at the rotating speed of 600r/min by adopting magnetic stirring to obtain B.
3. And transferring the B into a hydrothermal induction kettle, and adding carbon cloth with the length, width and height of 3cm, 2cm and 0.1cm as an induction source. Moving the hydrothermal induction kettle into hydrothermal induction heating equipment, heating the hydrothermal induction kettle to 180 ℃ from room temperature at an induction frequency of 600KHz, preserving the temperature for 60min, cooling to room temperature, taking out a carbon cloth scraping product, washing the obtained product with deionized water and ethanol, centrifuging, and drying for 6h under an infrared lamp at 80 ℃ to obtain C;
4. and C, activating agent nickel nitrate and nitrogen source ammonium citrate according to the mass ratio of C: nickel nitrate: mixing ammonium citrate at a ratio of 2:2:1, and grinding with agate mortar for 30min to obtain D.
5. And D, moving the D into a tubular furnace into which nitrogen is introduced, heating to 350 ℃ at the heating rate of 3 ℃/min, preserving heat for 1h, heating to 700 ℃ at the heating rate of 5 ℃/min, preserving heat for 3h, and cooling to room temperature. And washing and filtering the obtained product by deionized water and ethanol, and drying in a vacuum oven at 70 ℃ for 6 hours to obtain the nitrogen-doped biomass porous carbon nano material.
As can be seen from the SEM image of FIG. 1, the nitrogen-doped biomass carbon material prepared in example 3 has a three-dimensional porous honeycomb-shaped morphology structure. As can be seen from the XRD pattern of fig. 2, the sample of example 3 has more distinct graphite peaks at 24 ° and 43 ° 2 θ angles, indicating that the sample has a higher degree of graphitization. As can be seen from the rate performance plot of FIG. 3, the sample prepared in example 3 was applied to a lithium ion battery at 25mAg-1The capacity of the capacitor reaches 625mAhg at the current density-1When the current density increased to 5000mAg-1The Chen has 505mAhg-1The capacity of (2) can be maintained at 620mAhg when the current density is restored to the initial value-1And thus has excellent rate performance.
Claims (8)
1. The preparation method of the nitrogen-doped biomass porous carbon nano electrode material is characterized by comprising the following steps of:
1) cleaning peel biomass with alcohol under the ultrasonic action, and performing freeze drying and ball milling treatment to obtain powder A;
2) adding a nitric acid solution into the powdery A, and stirring to obtain B;
3) transferring the B into a hydrothermal induction kettle, adding carbon cloth as an induction source, moving the hydrothermal induction kettle into hydrothermal induction heating equipment, heating the hydrothermal induction kettle to 150-180 ℃ from room temperature at an induction frequency of 300-600 kHz, preserving heat for 20-60 min, cooling to room temperature, taking out a carbon cloth scraping product, washing the product with deionized water and ethanol, centrifuging, and drying for 6h under an infrared lamp at 50-80 ℃ to obtain C, wherein the length, the width and the height of the carbon cloth are 3cm, 2cm and 0.1cm respectively;
4) mixing and grinding the C, the activating agent and the nitrogen source to obtain D;
5) and D, heating to 350 ℃ at a heating rate of 3 ℃/min in a protective gas atmosphere, preserving heat for 1h, heating to 500-700 ℃ at a heating rate of 5 ℃/min, preserving heat for 1-3 h, cooling to room temperature, washing, filtering and drying the obtained product by deionized water and ethanol, and thus obtaining the nitrogen-doped biomass porous carbon nano electrode material.
2. The preparation method of the nitrogen-doped biomass porous carbon nano-electrode material according to claim 1, wherein the pericarp biomass in the step 1) is pomelo peel, orange peel, banana peel or longan shell.
3. The preparation method of the nitrogen-doped biomass porous carbon nano electrode material according to claim 1, wherein in the step 1), the ultrasonic frequency is 40kHz, the freeze-drying temperature is-20-10 ℃, the time is 12-24 hours, and the ball milling time is 2-4 hours.
4. The preparation method of the nitrogen-doped biomass porous carbon nano-electrode material according to claim 1, wherein 1-4 g of powdery A is added to every 40-70 mL of nitric acid solution in the step 2), and the concentration of the nitric acid solution is 1-3 mol/L.
5. The preparation method of the nitrogen-doped biomass porous carbon nano-electrode material according to claim 1, wherein in the step 2), magnetic stirring is adopted, and the stirring is carried out at a rotating speed of 300-600 r/min for 10-40 min.
6. The preparation method of the nitrogen-doped biomass porous carbon nano-electrode material as claimed in claim 1, wherein the mass ratio of C, the activating agent and the nitrogen source in the step 4) is (1-2): (1-4).
7. The preparation method of the nitrogen-doped biomass porous carbon nano-electrode material according to claim 1, wherein the grinding time in the step 4) is 10-30 min.
8. The preparation method of the nitrogen-doped biomass porous carbon nano-electrode material according to claim 1, wherein the drying in the step 5) is specifically as follows: dried under vacuum at 70 ℃ for 6 h.
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