CN109704307B - Preparation and application of sulfur-doped porous carbon based on sterculia lychnophora residue - Google Patents
Preparation and application of sulfur-doped porous carbon based on sterculia lychnophora residue Download PDFInfo
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Abstract
The invention provides a preparation method and application of sulfur-doped porous carbon based on sterculia lychnophora residues, which comprises the following steps: the tea-brewed sterculia lychnophora residue is taken as a raw material, and is carbonized with a sulfur dopant at high temperature under inert atmosphere to obtain sulfur-doped carbon, and then the sulfur-doped porous carbon is obtained through physical activation treatment. The method for preparing the sulfur-doped porous carbon by combining high-temperature carbonization and physical activation has the advantages of simple operation, easily controlled process, no need of washing after activation, reduced production cost, high carbon yield and environmental friendliness; the prepared sulfur-doped porous carbon has a nano-flake structure, controllable specific surface area and pore size distribution, high conductivity and adjustable sulfur content, and is particularly suitable for the fields of heavy metal wastewater treatment, printing and dyeing wastewater adsorption, lithium-sulfur batteries, lithium ion batteries, sodium ion batteries, supercapacitors, catalyst loading and the like.
Description
Technical Field
The invention relates to the field of biomass carbon preparation, in particular to preparation and application of sulfur-doped porous carbon based on sterculia lychnophora residues.
Background
After the first and second industrial revolution, the problems of environmental pollution, energy exhaustion and the like are continuously generated along with the exploitation and utilization of non-renewable resources such as coal, oil, natural gas and the like on the earth. To solve these problems, researchers in various countries are all dedicated to research and develop new clean resources to replace the use of coal, oil and natural gas, such as: wind energy, geothermal energy, solar energy, tidal energy, biomass energy, and the like. The biomass refers to organic substances formed by green plant photosynthesis, including plants, animals and microorganisms except fossil fuels, and excretions and metabolites thereof, and has biological characteristics of renewability, low pollution, wide distribution and the like. Researches find that various agricultural wastes, forestry residues and other biomass raw materials are gradually utilized by various countries every year to produce ethanol, fuel gas, methane, plastics, amino acid, glucose, starch and other biomass energy, materials and chemicals, and biomass carbon materials belong to one of numerous biomass materials.
Boat-fruited sterculia seed, also called boat-fruited sterculia seed, seed of sterculia seed, etc., and dry mature seed of sterculia seed, which is a plant of the family Sterculiaceae, is produced in Thailand, Cambodia, Malaysia, etc. And (4) when the fruits ripen and crack in 4-6 months, harvesting seeds and drying in the sun. It is often used for making tea, and has effects of lowering blood pressure, moistening throat and eliminating phlegm. Generally, the residue after the tea making of the boat-fruited sterculia seed is discarded, which not only causes the waste of resources, but also pollutes the environment. The sterculia scaphigera contains a large amount of saccharides and fatty acids, and is loose and porous, so that the sterculia scaphigera residues after tea making are pyrolyzed at high temperature in an inert atmosphere to obtain the biomass carbon material with rich carbon, high stability and large specific surface, the biomass waste can be fully utilized, and the ecological environment of people is protected.
At present, methods for preparing porous carbon by using biomass (waste) as a raw material mainly include a template method and an activation method. The template method comprises a soft template method and a hard template method. The soft template method uses amphiphilic molecules or copolymers as template agents, and the amphiphilic molecules or copolymers and carbon material precursors pass through hydrogenAnd combining the bonds to obtain the composite nano micelle, curing the precursor to form a three-dimensional cross-linked structure, and finally carbonizing to obtain the ordered porous carbon material. The hard template method is characterized in that a carbon precursor is firstly infiltrated into gaps of a template agent, carbonized after being crosslinked, and then cleaned by strong acid or strong base solution, so that the ordered porous carbon is obtained. However, the template method has limited its large-scale application due to its complex operation, strong corrosion performance, and difficult control. The activation method is divided into chemical activation method and physical activation method, and the chemical activation method is carried out by KOH, H, etc3PO4、K2CO3NaOH, and H2SO4The chemical reagents and the carbon material react in a series of chemical reactions to create micropores. The physical activation method is a method of forming various microporous structures by opening pores, expanding pores, and the like by reacting various components (such as carbon dioxide, water vapor, and the like) in the air with carbon atoms in a carbon material under a high temperature condition. The physical activation has the advantages of simple and clean process, no need of washing after activation, and contribution to meeting the requirement of large-scale industrialized production, and is concerned by scientific researchers of various countries in recent years. In addition, the carbon skeleton is doped with the hetero element (such as N, P, S, B, F) so as to obviously improve the surface properties of the carbon material, such as improving the wettability, the conductivity, the electrocatalytic performance and the like, and the carbon skeleton can also be used as an active site of reaction in electrochemistry.
Disclosure of Invention
The invention provides a preparation method and application of sulfur-doped porous carbon based on sterculia seed residue.
The technical scheme for realizing the invention is as follows:
a preparation method of sulfur-doped porous carbon based on sterculia lychnophora residue comprises the following steps:
(1) peeling off the skin and seeds of the tea-brewed boat-fruited sterculia seed, putting the boat-fruited sterculia seed into a freeze dryer for freeze drying, crushing the boat-fruited sterculia seed by a plant crusher after drying, and sieving the boat-fruited sterculia seed by a screen to obtain boat-fruited sterculia seed residue powder;
(2) putting the sterculia seed residue powder obtained in the step (1) and a sulfur doping agent into a nickel crucible, adding equal volume of alcohol and water, fully mixing uniformly, standing for 24h, putting into a vacuum drying oven for drying, then carbonizing the dried product at high temperature in a protective gas atmosphere, taking out the carbonized product, filtering and washing the carbonized product with acid to be neutral, and drying the obtained filter residue in a vacuum drying oven to obtain sulfur-doped carbon;
(3) and (3) filling the sulfur-doped carbon in the step (3) into a sample tube, placing the sample tube in a tube furnace, heating the sample tube to an activation temperature at a certain heating rate under the protection of protective gas, stopping introducing the protective gas, introducing oxidizing gas with a certain flow rate, activating for a certain time at the activation temperature, stopping introducing the oxidizing gas, cooling the sample tube to room temperature under the protective gas atmosphere, taking out the material, and drying the material in an oven to obtain the sulfur-doped porous carbon.
The temperature of freeze drying in the step (1) is-70 to-50 ℃, the vacuum degree is less than 20pa, the time is 20 to 24 hours, the rotating speed of a plant pulverizer is 1400r/min, and the mesh number of a screen is 100 meshes.
The mass ratio of the sterculia seed residue powder to the sulfur dopant in the step (2) is 20: (1-4); the sulfur dopant in the step (2) is selected from one of elemental sulfur, cysteine, cystine, thioglycolic acid, mercaptoethanol and mercaptopropionic acid.
The temperature of vacuum drying in the step (2) is 100-110 ℃, and the drying time is 10-12 h; the temperature of the high-temperature carbonization in the step (2) is 700-900 ℃, the heating rate is 3-7 ℃/min, and the treatment time is 1-4 h.
The protective gas is 99.99% of nitrogen, argon or helium by mass fraction, and the gas flow is 100-300 sccm.
The acid in the step (2) is hydrochloric acid, sulfuric acid or nitric acid with the concentration of 1-3 mol/L.
In the step (3), the temperature is raised to the activation temperature at a heating rate of 8-10 ℃/min, the introduction of the protective gas is stopped, and then the oxidizing gas is introduced, wherein the oxidizing gas is air, carbon dioxide or water vapor, and the gas flow rate is 500-.
The activation temperature in the step (3) is 800-; the drying temperature in the step (3) is 120-150 ℃, and the drying time is 4-6 h.
The sulfur-doped porous carbon based on the sterculia lychnophora residue is applied to heavy metal wastewater treatment, printing and dyeing wastewater adsorption, lithium-sulfur batteries, lithium ion batteries, sodium ion batteries, super capacitors and catalyst loading.
The invention has the beneficial effects that: the method for preparing the sulfur-doped porous carbon by combining high-temperature carbonization and physical activation has the advantages of simple operation, easily controlled process, no need of washing after activation, reduced production cost, high carbon yield and environmental friendliness; the prepared sulfur-doped porous carbon has a nano-flake structure, controllable specific surface area and pore size distribution, high conductivity and adjustable sulfur content, and is particularly suitable for the fields of heavy metal wastewater treatment, printing and dyeing wastewater adsorption, lithium-sulfur batteries, lithium ion batteries, sodium ion batteries, supercapacitors, catalyst loading and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a scanning electron micrograph of sulfur-doped porous carbon obtained in example 1 of the present invention;
FIG. 2 is a transmission electron micrograph of sulfur-doped porous carbon obtained in example 1 of the present invention;
FIG. 3 is an XRD pattern of sulfur-doped porous carbon obtained in example 1 of the present invention;
fig. 4 is a raman spectrum of the sulfur-doped porous carbon obtained in example 1 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
A preparation method of sulfur-doped porous carbon based on sterculia lychnophora residue comprises the following steps:
(1) peeling off the skin and removing seeds of the tea-soaked boat-fruited sterculia seed, putting the boat-fruited sterculia seed into a freeze dryer for freeze drying at the temperature of minus 60 ℃, the vacuum degree of less than 20pa for 21 hours, then crushing the boat-fruited sterculia seed by using an FZ102 type plant crusher at the rotation speed of 1400r/min, and sieving the boat-fruited sterculia seed by using a 100-mesh sieve to obtain boat-fruited sterculia seed residue powder;
(2) and (2) mixing the following components in percentage by mass: 2, putting the sterculia seed residue powder and cysteine into a nickel crucible, adding alcohol and water with the same volume, fully and uniformly mixing, standing for 24 hours, putting into a 105 ℃ vacuum drying oven, drying for 11 hours, and then carrying out high-temperature carbonization on a product obtained by drying in an argon atmosphere with the mass fraction of 99.99%, wherein the gas flow is 150 sccm; the high-temperature carbonization temperature is 800 ℃, the heating rate is 6 ℃/min, the treatment time is 2h, the carbonized product is taken out and filtered and washed by sulfuric acid with the concentration of 3mol/L until the carbonized product is neutral, and the obtained filter residue is dried in a vacuum drying oven at 100 ℃ for 12h to obtain sulfur-doped carbon;
(3) and (2) filling a certain amount of sulfur-doped carbon into a sample tube, placing the sample tube into a tube furnace, heating the sample tube to 900 ℃ at the heating rate of 9 ℃/min under the protection of argon with the mass fraction of 99.99%, stopping introducing the argon, introducing the carbon dioxide with the gas flow of 600sccm, activating the sample tube at 900 ℃ for 2 hours, stopping introducing the carbon dioxide, continuously cooling the sample tube to room temperature under the argon with the mass fraction of 99.99%, taking out the material, and drying the material in a 130 ℃ oven for 5 hours to obtain the sulfur-doped porous carbon.
Fig. 1 and 2 are a scanning electron microscope image and a transmission electron microscope image of the prepared sulfur-doped porous carbon based on the sterculia lychnophora residue, and it can be seen that the obtained sample has a typical nano-sheet structure and has a large number of pores on the surface, which are caused by activation. No distinct diffraction peaks can be seen in the XRD pattern of fig. 3, indicating that the prepared sulfur-doped porous carbon is amorphous. The presence of the D peak in fig. 4 indicates that the resulting sulfur-doped porous carbon surface has some defects that may be caused by the porosity and functional groups on the carbon material surface; the existence of the G peak indicates that the obtained sulfur-doped porous carbon has good conductivity, and the peak value of the G peak is larger than the D peak, which indicates that the sulfur-doped porous carbon has a certain graphitization degree. Table 1 shows the mass fraction of each element in the sulfur-doped porous carbon, indicating that the prepared carbon sample is indeed sulfur-doped carbon, wherein the mass fraction of the S element is 1.82%. In conclusion, the sulfur-doped porous carbon material based on the sterculia lychnophora residue is successfully prepared.
TABLE 1 Mass fractions of the elements in sulfur-doped porous carbon
Example 2
A preparation method of sulfur-doped porous carbon based on sterculia lychnophora residue comprises the following steps:
(1) peeling off the skin and removing seeds of the tea-soaked boat-fruited sterculia seed, putting the boat-fruited sterculia seed into a freeze dryer for freeze drying at the temperature of minus 70 ℃, the vacuum degree of less than 20pa for 20 hours, then crushing the boat-fruited sterculia seed by using an FZ102 type plant crusher at the rotation speed of 1400r/min, and sieving the boat-fruited sterculia seed by using a 100-mesh sieve to obtain boat-fruited sterculia seed residue powder;
(2) and (2) mixing the following components in percentage by mass: 1, putting the sterculia seed residue powder and sulfur into a nickel crucible, adding alcohol and water with the same volume, fully and uniformly mixing, standing for 24 hours, putting into a 100 ℃ vacuum drying oven for drying for 10 hours, and then carrying out high-temperature carbonization on a product obtained by drying in a nitrogen atmosphere with the mass fraction of 99.99%, wherein the gas flow is 100 sccm; the high-temperature carbonization temperature is 700 ℃, the heating rate is 3 ℃/min, the treatment time is 1h, the carbonized product is taken out, filtered and washed by hydrochloric acid with the concentration of 1mol/L until the carbonized product is neutral, and the obtained filter residue is dried in a vacuum drying oven at the temperature of 110 ℃ for 10h to obtain sulfur-doped carbon;
(3) filling a certain amount of sulfur-doped carbon into a sample tube, placing the sample tube into a tube furnace, heating the sample tube to 800 ℃ at the heating rate of 8 ℃/min under the protection of nitrogen with the mass fraction of 99.99%, stopping introducing the nitrogen with the flow of 100sccm, introducing air with the flow of 500sccm, activating the sample tube at the temperature of 800 ℃ for 1h, stopping introducing the air, continuously cooling the sample tube to room temperature under the nitrogen with the mass fraction of 99.99%, taking out the material, and drying the material in a 120 ℃ oven for 6h to obtain the sulfur-doped porous carbon.
Example 3
A preparation method of sulfur-doped porous carbon based on sterculia lychnophora residue comprises the following steps:
(1) peeling off the skin and removing seeds of the tea-soaked boat-fruited sterculia seed, putting the boat-fruited sterculia seed into a freeze dryer for freeze drying at the temperature of minus 50 ℃, the vacuum degree of less than 20pa for 24 hours, then crushing the boat-fruited sterculia seed by using an FZ102 type plant crusher at the rotation speed of 1400r/min, and sieving the boat-fruited sterculia seed by using a 100-mesh sieve to obtain boat-fruited sterculia seed residue powder;
(2) and (2) mixing the following components in percentage by mass: 3, putting the sterculia seed residue powder and cystine into a nickel crucible, adding alcohol and water with the same volume, fully and uniformly mixing, standing for 24h, putting into a vacuum drying oven at 110 ℃ for drying for 12h, and then carrying out high-temperature carbonization on a product obtained by drying in a helium atmosphere with the mass fraction of 99.99%, wherein the gas flow is 300 sccm; the high-temperature carbonization temperature is 900 ℃, the heating rate is 7 ℃/min, the treatment time is 4h, the carbonized product is taken out and filtered and washed by nitric acid with the concentration of 3mol/L until the carbonized product is neutral, and the obtained filter residue is dried in a vacuum drying oven at the temperature of 110 ℃ for 10h to obtain sulfur-doped carbon;
(3) and (2) filling a certain amount of sulfur-doped carbon into a sample tube, placing the sample tube into a tubular furnace, heating the sample tube to 1000 ℃ at the heating rate of 10 ℃/min under the protection of helium with the mass fraction of 99.99%, stopping introducing the helium with the flow rate of 300sccm, introducing water vapor with the flow rate of 700sccm, activating the sample tube at 1000 ℃ for 4 hours, stopping introducing the water vapor, continuously cooling the sample tube to room temperature under the helium with the mass fraction of 99.99%, taking out the material, and drying the material in a drying oven at 150 ℃ for 4 hours to obtain the sulfur-doped porous carbon.
Example 4
A preparation method of sulfur-doped porous carbon based on sterculia lychnophora residue comprises the following steps:
(1) peeling off the skin and removing seeds of the tea-soaked boat-fruited sterculia seed, putting the boat-fruited sterculia seed into a freeze dryer for freeze drying at the temperature of minus 50 ℃, the vacuum degree of less than 20pa for 21 hours, then crushing the boat-fruited sterculia seed by using an FZ102 type plant crusher at the rotation speed of 1400r/min, and sieving the boat-fruited sterculia seed by using a 100-mesh sieve to obtain boat-fruited sterculia seed residue powder;
(2) and (2) mixing the following components in percentage by mass: 4, putting the sterculia seed residue powder and mercaptoethanol into a nickel crucible, adding alcohol and water with the same volume, fully mixing uniformly, standing for 24 hours, putting into a 105 ℃ vacuum drying oven for drying for 10 hours, and then carrying out high-temperature carbonization on a product obtained by drying in a nitrogen atmosphere with the mass fraction of 99.99%, wherein the gas flow is 200 sccm; the high-temperature carbonization temperature is 850 ℃, the heating rate is 5 ℃/min, the treatment time is 2h, the carbonized product is taken out and filtered and washed by sulfuric acid with the concentration of 2mol/L until the carbonized product is neutral, and the obtained filter residue is dried in a vacuum drying oven at 100 ℃ for 12h to obtain sulfur-doped carbon;
(3) and (2) filling a certain amount of sulfur-doped carbon into a sample tube, placing the sample tube into a tube furnace, heating the sample tube to 950 ℃ at the heating rate of 9 ℃/min under the protection of argon with the mass fraction of 99.99%, stopping introducing the argon, introducing carbon dioxide with the gas flow of 550sccm, activating the sample tube at 950 ℃ for 2 hours, stopping introducing the carbon dioxide, continuously cooling the sample tube to room temperature under the argon with the mass fraction of 99.99%, taking out the material, and drying the material in a 130 ℃ oven for 5 hours to obtain the sulfur-doped porous carbon.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. The preparation method of the sulfur-doped porous carbon based on the sterculia lychnophora residue is characterized by comprising the following steps:
(1) peeling off the peel and seeds of the tea-brewed boat-fruited sterculia seed, and freeze-drying the boat-fruited sterculia seed in a freeze dryer at the temperature of minus 70 to minus 50 ℃ and the vacuum degree of less than 20pa for 20 to 24 hours; drying, pulverizing with a plant pulverizer, and sieving with a screen to obtain semen Scaphii Lychnophori residue powder;
(2) putting the sterculia seed residue powder obtained in the step (1) and a sulfur doping agent into a nickel crucible, adding equal volume of alcohol and water, fully mixing uniformly, standing for 24h, putting into a vacuum drying oven for drying, then performing high-temperature carbonization on a product obtained by drying in a protective gas atmosphere, wherein the temperature of the high-temperature carbonization is 700-;
(3) and (3) filling the sulfur-doped carbon in the step (3) into a sample tube, placing the sample tube in a tube furnace, heating the sample tube to an activation temperature at a heating rate of 8-10 ℃/min under the protection of protective gas, stopping introducing the protective gas, introducing oxidizing gas with a certain flow rate, wherein the oxidizing gas is air, carbon dioxide or water vapor, the gas flow rate is 500-700sccm, after activating for a certain time at the activation temperature, stopping introducing the oxidizing gas, cooling to room temperature under the atmosphere of the protective gas, taking out the material, and drying in an oven to obtain the sulfur-doped porous carbon.
2. The preparation of sulfur-doped porous carbon based on sterculia lychnophora residue according to claim 1, wherein: in the step (1), the rotating speed of the plant pulverizer is 1400r/min, and the mesh number of the screen is 100 meshes.
3. The preparation of sulfur-doped porous carbon based on sterculia lychnophora residue according to claim 1, wherein: the mass ratio of the sterculia seed residue powder to the sulfur dopant in the step (2) is 20: (1-4); the sulfur dopant in the step (2) is selected from one of elemental sulfur, cysteine, cystine, thioglycolic acid, mercaptoethanol and mercaptopropionic acid.
4. The preparation of sulfur-doped porous carbon based on sterculia lychnophora residue according to claim 1, wherein: the temperature of vacuum drying in the step (2) is 100-110 ℃, and the drying time is 10-12 h.
5. The preparation of sulfur-doped porous carbon based on sterculia lychnophora residue according to claim 1, wherein: the protective gas is 99.99% of nitrogen, argon or helium by mass fraction, and the gas flow is 100-300 sccm.
6. The preparation of sulfur-doped porous carbon based on sterculia lychnophora residue according to claim 1, wherein: the acid in the step (2) is hydrochloric acid, sulfuric acid or nitric acid with the concentration of 1-3 mol/L.
7. The preparation of sulfur-doped porous carbon based on sterculia lychnophora residue according to claim 1, wherein: the activation temperature in the step (3) is 800-; the drying temperature in the step (3) is 120-150 ℃, and the drying time is 4-6 h.
8. Use of the scaphium scaphigerum dreg based sulfur doped porous carbon of any one of claims 1 to 7 in heavy metal wastewater treatment, printing and dyeing wastewater adsorption, lithium sulfur batteries, lithium ion batteries, sodium ion batteries, supercapacitors, and catalyst loading.
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