CN111129523B - Preparation method of ultrathin flexible carbon nanosheet oxygen reduction catalyst based on anaerobic fermentation biogas residues - Google Patents
Preparation method of ultrathin flexible carbon nanosheet oxygen reduction catalyst based on anaerobic fermentation biogas residues Download PDFInfo
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- CN111129523B CN111129523B CN201911303003.1A CN201911303003A CN111129523B CN 111129523 B CN111129523 B CN 111129523B CN 201911303003 A CN201911303003 A CN 201911303003A CN 111129523 B CN111129523 B CN 111129523B
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- H01M4/90—Selection of catalytic material
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- H01M4/905—Metals or alloys specially used in fuel cell operating at high temperature, e.g. SOFC
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Abstract
The invention discloses a preparation method of an ultrathin flexible carbon nanosheet oxygen reduction catalyst based on anaerobic fermentation biogas residues. The preparation method of the oxygen reduction catalyst comprises the following steps: (1) carrying out an activation reaction on anaerobic fermentation biogas residues serving as a raw material under the protection of inert gas, cooling, and then sequentially carrying out acid washing, water washing and drying to obtain biogas residue biochar; (2) uniformly mixing the biogas residue biochar obtained in the step (1), an iron precursor and a nitrogen precursor, carrying out carbonization reaction in a reaction container under the protection of inert gas, cooling to room temperature after the carbonization reaction, firstly washing a product after the carbonization reaction by using hydrochloric acid, then washing by using deionized water until the pH value of a washing solution is 6-7, and then drying to obtain the oxygen reduction catalyst. The oxygen reduction catalyst prepared by the method has the advantages of large specific surface area, stable performance, better electrochemical activity than that of the traditional Pt/C catalyst and wide applicability.
Description
Technical Field
The invention relates to the technical field of preparation of a biochar material and microbial fuel cells, in particular to a preparation method of an ultrathin flexible carbon nanosheet oxygen reduction catalyst based on anaerobic fermentation biogas residues.
Background
At present, with global warming and increasingly severe environmental pollution, a new green and pollution-free energy technology capable of sustainable development is urgently needed. The microbial fuel cell technology is a green and clean energy technology which takes microbes as a catalyst and directly converts chemical energy in organic matters into electric energy, and is favored by researchers. However, the development of air cathode microbial fuel cells with the most potential applications is limited by the slow kinetics of cathode oxygen reduction, which causes the loss of cathode potential of 0.3-0.4V, and therefore, the introduction of high-activity catalysts is required. Currently, the commonly used cathode oxygen reduction catalysts are Pt and Pt-based noble metal catalysts.
Currently, the development of Pt-based catalysts is limited by their expensive price, and lower reserves. Therefore, the development of cheap, efficient and stable non-noble metal cathode catalysts is of great significance to the development of microbial fuel cells. In recent years, a transition metal-nitrogen-carbon co-doped carbon material serving as a novel non-noble metal oxygen reduction electrocatalyst has the characteristics of low price, easiness in obtaining, high catalytic activity, good stability and the like, shows good applicability in the field of fuel cells, particularly has strong anti-biofilm poisoning performance, and further has a wide application prospect in the field of microbial fuel cells.
Anaerobic fermentation is a process of decomposing most biodegradable organic substances in biomass into energy products, namely biogas, through the biotransformation function of anaerobic microorganisms under certain conditions. The production of byproduct biogas slurry and biogas residue is also accompanied in the production process of the energy product. If the biogas residues are not reasonably treated, environmental burden is caused.
The biogas residue mainly contains organic matters and humic acid, contains rich protein which can reach 10-20 percent calculated by the crude protein content of air-dried substances, and is also rich in N, S, P and other elements, and the existence of the elements just provides necessary conditions for the preparation of the high-activity oxygen reduction biochar catalyst.
Disclosure of Invention
The invention provides a preparation method of an ultrathin flexible carbon nanosheet oxygen reduction catalyst based on anaerobic fermentation biogas residues.
The invention aims to provide a preparation method of an ultrathin flexible carbon nanosheet oxygen reduction catalyst based on anaerobic fermentation biogas residues, which comprises the following steps:
(1) activating anaerobic fermentation biogas residues serving as a raw material at the temperature of 450-800 ℃ for 1-3h under the protection of inert gas, wherein the heating rate is 1-10 ℃/min, cooling after an activation reaction, and then sequentially carrying out acid washing, water washing and drying to obtain biogas residue biochar;
(2) uniformly mixing the biogas residue biochar obtained in the step (1), an iron precursor and a nitrogen precursor, carrying out carbonization reaction for 1-5 h at the temperature of 700-plus-material temperature of 1000 ℃ under the protection of inert gas, wherein the heating rate is 2-10 ℃/min, then cooling to room temperature, soaking and washing a product with dilute hydrochloric acid, washing with deionized water until the pH value is 6-7, and drying the obtained product at the temperature of 60-80 ℃ to obtain the Fe and N co-doped ultrathin flexible carbon nanosheet oxygen reduction catalyst.
Preferably, the specific steps of step (1) are: dispersing anaerobic fermentation biogas residues and an activating agent in deionized water, uniformly stirring the activating agent and the anaerobic fermentation biogas residues at the room temperature, putting a fully mixed suspension into a vacuum drying oven for drying, putting the dried powder into a vacuum tube furnace, carrying out heat treatment at the temperature of 800 ℃ for 1-3h in an inert gas atmosphere at 450 ℃ to obtain a pyrolysis product, heating at the rate of 1-10 ℃/min, dispersing the pyrolysis product into a dilute hydrochloric acid solution, soaking and pickling at the room temperature, washing the pickled pyrolysis product with deionized water until the pH value of a washing solution is 6-7, and drying to obtain biogas residue biochar.
Preferably, the activating agent is selected from more than one of potassium carbonate, sodium hydroxide, potassium hydroxide and phosphoric acid; the precursor of the iron is inorganic salt of the iron, and the inorganic salt of the iron is ferric chloride or ferric nitrate.
Preferably, the anaerobic fermentation biogas residue is selected from one or more of fiber plant fermentation biogas residue, livestock and poultry manure biogas residue and fruit and vegetable waste fermentation biogas residue. The anaerobic fermentation biogas residue is one or more of biomass raw materials such as paper mulberry, cow dung, pig dung, chicken dung and the like, and is solid waste generated after biogas fermentation.
Preferably, the mass ratio of the biogas residue biochar to the iron precursor in the step (2) is 100: 1-200: 1, and the mass ratio of the biogas residue biochar to the nitrogen precursor is 1: 10-1: 30.
The invention also protects the ultrathin flexible carbon nanosheet oxygen reduction catalyst prepared by the preparation method of the ultrathin flexible carbon nanosheet oxygen reduction catalyst based on anaerobic fermentation biogas residues and the application of the catalyst in a microbial fuel cell cathode oxygen reduction catalyst.
Compared with the prior art, the invention has the beneficial effects that: the method takes cheap and easily-obtained biomass waste-anaerobic fermentation biogas residues as a raw material, can realize resource utilization of the waste, has the characteristics of simple preparation process, high carbon yield, low cost and the like, and the prepared biochar catalyst has a micro-mesoporous composite structure on the surface, a developed surface pore structure, a plurality of defect active sites, high nitrogen content, a large specific surface area and good stability, and the electrochemical activity of the obtained catalyst is superior to that of the traditional Pt/C catalyst, so that the method has wide applicability and can be popularized and applied to the related fields of fuel cell cathode oxygen reduction.
Description of the drawings:
FIG. 1 is an SEM image of the activated biochar B-AC catalyst prepared in example 1;
FIG. 2 is an SEM photograph of the B-C catalyst prepared in comparative example 1;
FIG. 3 is a graph showing nitrogen adsorption and desorption of the B-AC catalyst prepared in example 1;
FIG. 4 is a graph showing the nitrogen adsorption and desorption of the catalysts B to C prepared in comparative example 1;
FIG. 5 is a graph of the electrochemical catalytic performance of B-AC, B-C and Pt/C catalysts prepared in example 1 and comparative example 1;
FIG. 6 is a plot of cell system power density for B-AC, B-C and Pt/C catalysts prepared in example 1 and comparative example 1 as cathode catalysts for microbial fuel cells;
FIG. 7 is a cell system polarization curve of B-AC, B-C and Pt/C catalysts prepared in example 1 and comparative example 1 as cathode catalysts for microbial fuel cells.
Detailed Description
The following examples are further illustrative of the present invention and are not intended to be limiting thereof. The equipment and reagents used in the present invention are, unless otherwise specified, conventional commercial products in the art.
Example 1
An ultrathin flexible biochar nanosheet catalyst is prepared by the following steps:
(1) anaerobic fermentation biogas residue carbonization: drying the fiber plant anaerobic fermentation biogas residue at 105 ℃ for 72h, grinding the dried fiber plant anaerobic fermentation biogas residue into powder, dispersing 0.25g of the powdered fiber plant anaerobic fermentation biogas residue (gz) and 0.25g of potassium carbonate into 10mL of deionized water, stirring the mixture at room temperature for 8h, putting the fully mixed suspension into a vacuum drying oven, and drying the suspension at 60 ℃; putting the dried powder into a vacuum tube furnace, and reacting in N2And (2) carrying out heat treatment at 700 ℃ for 2h in the atmosphere, wherein the heating rate is 5 ℃/min, dispersing the pyrolysis product in a 1M HCl solution, soaking and pickling for 12h at room temperature, and then washing the pickled sample with deionized water until the pH value is 6-7 to obtain the biogas residue biochar which is recorded as h-gz.
(2) And (3) Fe-N co-doping of the biogas residue biochar: dispersing 0.25g of h-gz and 5g of Dicyandiamide (DICY) in 10mL of deionized water, adding 2mL of 0.0125M ferric chloride solution, continuously stirring for 8h at room temperature, and drying at 60 ℃; the dried powder is placed in a vacuum tube furnace in N2Carrying out heat treatment at 900 ℃ for 2h in the atmosphere to obtain a pyrolysis product, wherein the heating rate is 3 ℃/min, dispersing the pyrolysis product in a 1M HCl solution, carrying out acid washing at room temperature for 12h, then carrying out deionized water washing until the pH value is 6-7, and finally drying the obtained sample at 60 ℃ to obtain the B-AC catalyst.
The B-AC catalyst obtained is tested, the scanning electron microscope image of the B-AC catalyst is shown in figure 1, and according to the nitrogen adsorption and desorption curve (figure 3), the specific surface area of the B-AC catalyst is 1958.9m according to the BET equation2/g。
Comparative example 1
Same as example 1 except for the difference in step (1): and (3) directly performing the step (2) after drying the anaerobic fermentation biogas residues of the fiber plants, and marking the finally obtained sample as a B-C catalyst.
The B-C catalyst obtained was tested, and its scanning electron microscope is shown in FIG. 2, and its specific surface area was calculated to be 934.96m according to the BET equation from the nitrogen adsorption/desorption curve (FIG. 4)2/g。
Experimental example 1
1. Electrochemical performance test of ultrathin flexible charcoal nanosheet catalyst
The B-AC catalyst prepared in example 1 and the B-C catalyst prepared in comparative example 1 were mixed in N2Or O2The catalyst electrocatalytic performance test was performed in a saturated phosphate buffer system (50mM PBS, pH 7). For comparison, we also tested the CV electrochemical activity of a commercial Pt/C catalyst. CV curves of the B-AC catalyst, the B-C catalyst and the Pt/C catalyst are shown in figure 5, and results show that the B-AC catalyst activated by strong alkali has good catalytic oxygen reduction activity, and is even superior to the traditional Pt/C catalyst.
2. Characteristics of ultrathin flexible biochar nanosheet catalyst in microbial fuel cell
The B-AC catalyst prepared in example 1, the B-C catalyst prepared in comparative example 1 and the Pt/C catalyst were used as cathode catalysts, microbial fuel cells were assembled, and the influence of each catalyst on the output parameters of the cells was examined, as shown in FIGS. 6 and 7, the maximum output voltage of the microbial fuel cell using B-AC as the cathode reached 0.68V, and the maximum power density reached 1320mw/cm2Higher than the maximum power density of the Pt/C catalyst, and more obviously higher than that of the non-activated B-C catalyst, which shows that the activation process plays a great role in improving the performance of the catalyst.
Example 2
An ultrathin flexible charcoal nanosheet catalyst is prepared by the following steps:
(1) anaerobic fermentation biogas residue carbonization: collecting livestock and fowl feces and straw, performing anaerobic fermentation on the biogas residue, drying at 105 deg.C for 72 hr, grinding into powder, and collecting powderDispersing 0.25g of anaerobic fermentation biogas residue (gz) of the shaped livestock and poultry manure and 0.25g of potassium carbonate in 10mL of deionized water, stirring for 8 hours at room temperature, putting the fully mixed suspension into a vacuum drying oven, and drying at 60 ℃; putting the dried powder into a vacuum tube furnace, and reacting in N2And (3) carrying out heat treatment at 450 ℃ for 3h in the atmosphere, wherein the heating rate is 2 ℃/min, dispersing the pyrolysis product in a 1M HCl solution, soaking and pickling for 12h at room temperature, and then washing the pickled sample with deionized water until the pH value is 6-7 to obtain the biogas residue biochar which is recorded as h-gz.
(2) And (3) Fe-N co-doping of the biogas residue biochar: dispersing 0.25g of h-gz and 5g of Dicyandiamide (DICY) in 10mL of deionized water, adding 2mL of 0.0125M ferric chloride solution, continuously stirring for 8h at room temperature, and drying at 60 ℃; the dried powder is placed in a vacuum tube furnace in N2And (2) carrying out heat treatment at 800 ℃ for 3h in the atmosphere to obtain a pyrolysis product, wherein the heating rate is 2 ℃/min, then dispersing the pyrolysis product in a 1M HCl solution, carrying out acid washing at room temperature for 12h, then washing with deionized water until the pH value is 6-7, and finally drying the obtained sample at 80 ℃ to finally obtain the B-AC catalyst.
The B-AC catalyst obtained is tested, and the test shows that the specific surface area is 1938.0m2/g。
Example 3
An ultrathin flexible charcoal nanosheet catalyst is prepared by the following steps:
(1) anaerobic fermentation biogas residue carbonization: taking livestock manure and straw to perform anaerobic fermentation on biogas residues together, drying the biogas residues at 105 ℃ for 72 hours, grinding the biogas residues into powder, taking 1.25g of powdery livestock manure anaerobic fermentation biogas residues (gz) and 0.25g of potassium hydroxide to disperse the powdery livestock manure anaerobic fermentation biogas residues in 15mL of deionized water, stirring the mixture at room temperature for 8 hours, putting the fully mixed suspension into a vacuum drying oven, and drying the suspension at 60 ℃; putting the dried powder into a vacuum tube furnace, and reacting in N2And (2) carrying out heat treatment for 1h at 800 ℃ in the atmosphere, wherein the heating rate is 10 ℃/min, dispersing the pyrolysis product in a 1M HCl solution, soaking and pickling for 12h at room temperature, and then washing the pickled sample with deionized water until the pH value is 6-7 to obtain the biogas residue biochar which is recorded as h-gz.
(2) And (3) Fe-N co-doping of the biogas residue biochar: 0.25g of h-gz and 2.5g of dicyandiamide (D)ICY) is dispersed in 15mL deionized water, then 0.0125M ferric chloride solution is added, the mass ratio of the biogas residue biochar to the iron precursor is 100:1, the mixture is continuously stirred for 8h at room temperature, and the mixture is dried at 60 ℃; the dried powder is placed in a vacuum tube furnace in N2And (2) carrying out heat treatment at 700 ℃ for 5h in the atmosphere to obtain a pyrolysis product, wherein the heating rate is 2 ℃/min, then dispersing the pyrolysis product in a 1M HCl solution, carrying out acid washing at room temperature for 12h, then washing with deionized water until the pH value is 6-7, and finally drying the obtained sample at 80 ℃ to finally obtain the B-AC catalyst.
Example 4
An ultrathin flexible charcoal nanosheet catalyst is prepared by the following steps:
(1) anaerobic fermentation biogas residue carbonization: taking livestock manure and straw to perform anaerobic fermentation on biogas residues together, drying the biogas residues at 105 ℃ for 72 hours, grinding the biogas residues into powder, taking 0.25g of powdery livestock manure anaerobic fermentation biogas residues (gz) and 1.25g of sodium hydroxide to disperse the powdery livestock manure anaerobic fermentation biogas residues in 15mL of deionized water, stirring the mixture at room temperature for 8 hours, putting the fully mixed suspension into a vacuum drying oven, and drying the suspension at 60 ℃; putting the dried powder into a vacuum tube furnace, and reacting in N2And (3) carrying out heat treatment at 450 ℃ for 3h in the atmosphere, wherein the heating rate is 1 ℃/min, dispersing the pyrolysis product in a 1M HCl solution, soaking and pickling for 12h at room temperature, and then washing the pickled sample with deionized water until the pH value is 6-7 to obtain the biogas residue biochar which is recorded as h-gz.
(2) And (3) Fe-N co-doping of the biogas residue biochar: dispersing 0.25g of h-gz and 7.5g of Dicyandiamide (DICY) in 15mL of deionized water, adding 0.0125M of ferric chloride solution to ensure that the mass ratio of the biogas residue biochar to the iron precursor is 200:1, continuously stirring for 8h at room temperature, and drying at 60 ℃; the dried powder is placed in a vacuum tube furnace in N2Carrying out heat treatment at 1000 ℃ for 1h in the atmosphere to obtain a pyrolysis product, wherein the heating rate is 10 ℃/min, dispersing the pyrolysis product in a 1M HCl solution, carrying out acid washing at room temperature for 12h, then carrying out deionized water washing until the pH value is 6-7, and finally drying the obtained sample at 80 ℃ to obtain the B-AC catalyst.
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.
Claims (6)
1. A preparation method of an ultrathin flexible carbon nanosheet oxygen reduction catalyst based on anaerobic fermentation biogas residues is characterized by comprising the following steps:
(1) dispersing anaerobic fermentation biogas residues and an activating agent in deionized water, wherein the mass ratio of the activating agent to the anaerobic fermentation biogas residues is 1: 5-5: 1, uniformly stirring at room temperature, drying a fully mixed suspension in a vacuum drying oven, placing the dried powder in a vacuum tube furnace, carrying out heat treatment at the temperature of 450 ℃ and 800 ℃ for 1-3h in an inert gas atmosphere to obtain a pyrolysis product, wherein the heating rate is 1-10 ℃/min, dispersing the pyrolysis product in a dilute hydrochloric acid solution, soaking and pickling at room temperature, washing the pickled pyrolysis product with deionized water until the pH of a washing solution is 6-7, and drying to obtain biogas residue biochar, wherein the activating agent is more than one selected from potassium carbonate, sodium hydroxide, potassium hydroxide and phosphoric acid;
(2) uniformly mixing the biogas residue biochar obtained in the step (1), an iron precursor and a nitrogen precursor, carrying out carbonization reaction in a reaction container at the temperature of 700-plus-material 1000 ℃ for 1-5 h under the protection of inert gas, wherein the heating rate is 2-10 ℃/min, cooling to room temperature after the carbonization reaction, firstly using dilute hydrochloric acid to soak and wash a product after the carbonization reaction, then using deionized water to wash until the pH value of a washing solution is 6-7, and then drying at the temperature of 60-80 ℃ to obtain the ultrathin flexible carbon nanosheet oxygen reduction catalyst.
2. The preparation method of the ultrathin flexible carbon nanosheet oxygen reduction catalyst based on anaerobic fermentation biogas residue as claimed in claim 1, wherein the anaerobic fermentation biogas residue is selected from one or more of fibrous plant fermentation biogas residue, livestock manure biogas residue and fruit and vegetable waste fermentation biogas residue.
3. The preparation method of the ultrathin flexible carbon nanosheet oxygen reduction catalyst based on anaerobic fermentation biogas residue as claimed in claim 1 or 2, wherein the iron precursor is an inorganic salt of iron, the mass ratio of the biogas residue biochar to the iron precursor in step (2) is 100: 1-200: 1, and the mass ratio of the biogas residue biochar to the nitrogen precursor is 1: 10-1: 30.
4. The preparation method of the ultrathin flexible carbon nanosheet oxygen reduction catalyst based on anaerobic fermentation biogas residue as claimed in claim 1 or 2, wherein the inert gas is nitrogen or argon.
5. The anaerobic fermentation biogas residue-based ultrathin flexible carbon nanosheet oxygen reduction catalyst prepared by the preparation method of the anaerobic fermentation biogas residue-based ultrathin flexible carbon nanosheet oxygen reduction catalyst of claim 1.
6. The use of the ultra-thin flexible carbon nanosheet oxygen reduction catalyst based on anaerobically fermented biogas residue of claim 5 in a microbial fuel cell cathode oxygen reduction catalyst.
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| CN114590792B (en) * | 2022-02-23 | 2023-06-16 | 北京大学深圳研究生院 | Carbon microsphere and preparation method thereof |
| CN114908126A (en) * | 2022-06-15 | 2022-08-16 | 中国科学院广州能源研究所 | Process for coproducing high-quality gas carbon clean recycling product by anaerobic fermentation-pyrolysis coupling |
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