CN114570331A - Nitrogen-doped porous nano biochar, and preparation method and application thereof - Google Patents
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Abstract
The invention provides nitrogen-doped porous nano biochar, a preparation method and application thereof, wherein the method comprises the following steps: 1, mixing apple leaf powder and (KOH or NaOH) in inert gas or N2Carrying out heat preservation treatment at 500-700 ℃ under the protection of atmosphere to obtain a reactant; and 2, removing by-products and impurities in the reactants, and drying to obtain the nitrogen-doped porous nano biochar. The invention uses the waste apple leaves as carbon sourceThe method is simple in process and low in cost, the obtained biochar has a large specific surface area, abundant surface functional groups and a nanoscale 3D porous lamellar structure, can be used as a pollution-free carbon functional material to adsorb and activate PDS to remove organic pollutant tetracycline in water in a synergistic manner, and has potential practical application value.
Description
Technical Field
The invention relates to the field of resource utilization of agricultural and forestry wastes and environmental management, in particular to nitrogen-doped porous nano biochar, a preparation method and application thereof.
Background
With the rapid development of the chemical industry, the production, use and discharge of tens of thousands of chemicals increase the environmental burden and health risks, wherein the drugs and personal care products (PPCPs) are chemicals with large usage and strong universality, and are continuously discharged into environmental water body through human activities in recent years, and the traditional sewage treatment plants cannot completely remove the compounds due to the low biochemical degradation rate of the PPCPs. The accumulation of PPCPs in the natural aquatic environment has a number of potential adverse effects on human health and the ecosystem. Therefore, it has become a global challenge to propose effective strategies to eliminate recalcitrant PPCPs in water.
Tetracycline, a typical PPCPs, has now become one of the antibiotics in larger production and clinical use. Due to good structural stability, the nano-composite material is difficult to degrade in water, is frequently detected in water environment in recent years, and poses serious threats to human beings and aquatic organisms. Advanced oxidation technology based on Peroxydisulfate (PDS) has been recognized as an effective strategy for the removal of organic contaminants from water. However, designing efficient, low cost, pollution-free catalytic materials remains a significant challenge.
Meanwhile, about 9 million tons of agricultural and forestry wastes are generated annually in China, and the agricultural and forestry wastes are now one of major environmental problems in the global scope due to low treatment efficiency and continuous increase. Apple leaves are common agricultural and forestry waste left in the field after apples are harvested, producing about 900 million tons of waste apple leaves each year in china. Generally, apple leaves contain more protein, sugars, vitamins and less hemicellulose, cellulose and lignin, and are a potential biomass resource. However, a large amount of waste apple leaves are directly discarded, incinerated or buried without being recycled, which causes great waste of resources and serious environmental pollution. Therefore, how to select a proper resource utilization mode to convert the waste apple leaves into high value-added products is also very important.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides nitrogen-doped porous nano biochar, a preparation method and application thereof, waste apple leaves are used as a carbon source, the process is simple, the cost is low, and the carbon-doped porous nano biochar can be used as a pollution-free carbon functional material, can adsorb and activate PDS to cooperatively remove organic pollutant tetracycline in water, and has potential practical application value.
The invention is realized by the following technical scheme:
a preparation method of nitrogen-doped porous nano biochar comprises the following steps:
1, mixing apple leaf powder and (KOH or NaOH) in inert gas or N2Carrying out heat preservation treatment at 500-700 ℃ under the protection of atmosphere to obtain a reactant;
and 2, removing by-products and impurities in the reactants, and drying to obtain the nitrogen-doped porous nano biochar.
Preferably, the apple leaves in the step 1 are waste apple leaves.
Preferably, in the step 1, the mass ratio of the apple leaf powder to (KOH or NaOH) is 1: 3.
preferably, in step 1, the mixture of apple leaf powder and (KOH or NaOH) is firstly put in inert gas or N2Under the protection of atmosphere, heating to 350-450 ℃, preserving heat for 1.5-2.5 h, and then heating to 500-700 ℃.
Preferably, in the step 1, the mixture of the apple leaf powder and NaOH is heated to 350-450 ℃ at a heating rate of 3-5 ℃/min, and then the temperature is raised to 500-700 ℃ at a heating rate of 3-5 ℃/min.
Preferably, in the step 1, the mixture of the apple leaf powder and (KOH or NaOH) is subjected to heat preservation treatment at 500-700 ℃ for 2-3 h.
Preferably, in the step 2, the reactant obtained in the step 1 is washed with HCl solution for 2-5 times, and then washed with deionized water for 2-5 times.
Further, drying the cleaned product at 60-90 ℃ in step 2 to obtain the nitrogen-doped porous nano biochar.
A nitrogen-doped porous nano biochar obtained by the preparation method of the nitrogen-doped porous nano biochar.
Application of nitrogen-doped porous nano biochar in removing antibiotics in water.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention relates to a preparation method of nitrogen-doped porous nano biochar, which is characterized in that apple leaf powder and (KOH or NaOH) are uniformly mixed and then are calcined in one step, a carbonized sample reacts with the (KOH or NaOH) at high temperature, the (KOH or NaOH) is used as an activator to improve the porosity and the specific surface area of the biochar, and calcined reactants are cleaned and dried to obtain the porous nano biochar. Compared with the existing synthetic method of the biochar, the biochar obtained by the invention takes the agricultural and forestry waste apple leaves as the raw material for the first time, the apple leaves contain more proteins, sugars, vitamins and less hemicellulose, cellulose and lignin, a green natural carbon source is provided for the preparation of the biochar, the source is wide, the cost is low, and a good economic basis is provided for the large-scale preparation of high-quality biochar; most of the prior art is carbonized firstly, and then the carbonized sample is mixed with an activating agent for calcination, so that the operation process is complicated, the preparation period is long, and the preparation cost is high. In the preparation method of the biochar, the two steps of carbonization and activation are linked together, and the one-step calcination operation is simple and has low cost; the prepared porous nano charcoal is doped with nitrogen, an additional nitrogen source is not required to be added in the preparation process, the nitrogen self-doping can be realized by utilizing the waste apple leaves, a simple and low-cost approach is provided for preparing the nitrogen-doped charcoal, the electronic structure on the surface of the charcoal can be changed by the nitrogen doping, abundant active centers are provided, and the application of the charcoal is expanded. The invention changes waste into valuable, realizes the high-efficiency resource utilization of agricultural and forestry waste apple leaves, provides a low-cost route for the restoration of environmental sewage, and has potential practical application value.
The nitrogen-doped porous nano biochar has a large specific surface area, abundant surface functional groups and a nano-scale 3D porous lamellar structure, and is expected to have a huge application prospect in the fields of super capacitors, lithium ion battery electrode materials, catalyst carriers, environmental pollutant adsorption, photoelectrocatalysis and the like.
The nitrogen-doped porous nano biochar is used as a pollution-free carbon functional material, and can adsorb and activate PDS to remove organic pollutant tetracycline in water in a synergistic manner.
Drawings
Fig. 1 is a photograph of waste apple leaves according to various embodiments of the present invention.
FIG. 2 is a Scanning Electron Microscope (SEM) photograph of the nano biochar prepared at 500 ℃ in example 1 of the present invention.
FIG. 3 is an SEM photograph of nano biochar prepared at 600 ℃ in example 2 of the present invention.
FIG. 4 is an SEM photograph of nano biochar prepared at 700 ℃ in example 3 of the present invention.
FIG. 5 is X-ray photoelectron spectroscopy (XPS) C of nano biochar prepared at 500 deg.C, 600 deg.C, 700 deg.C, respectively, according to the present invention1sSpectra.
FIG. 6 shows XPS N of nano biochar prepared at 500 deg.C, 600 deg.C, 700 deg.C, respectively, in accordance with the present invention1sSpectra.
FIG. 7 shows the IR spectrum of the biochar prepared at 500 deg.C, 600 deg.C, and 700 deg.C, respectively.
FIG. 8 shows the N of the nano biochar prepared by the invention at 500 deg.C, 600 deg.C and 700 deg.C respectively2Adsorption and desorption curve chart.
FIG. 9 is a diagram showing the distribution of pore sizes of the nano biochar prepared at 500 deg.C, 600 deg.C, and 700 deg.C, respectively, in accordance with the present invention.
FIG. 10 is a graph showing the performance of the nano biochar prepared by the present invention for removing tetracycline from water at 700 ℃.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
About 9 million tons of agricultural and forestry wastes are generated every year in China, and due to the low treatment efficiency and the continuous increase of the agricultural and forestry wastes, the agricultural and forestry wastes become one of the major environmental problems in the global scope. Among them, apple leaves (including fallen leaves, leaves in dead branches, etc.) are common agricultural and forestry wastes left in fields after apples are harvested, and about 900 ten thousand tons of apple leaves are produced every year in china. Generally, apple leaves contain more protein, sugars, vitamins and less hemicellulose, cellulose and lignin, and are a potential biomass resource. However, a large amount of waste apple leaves are directly discarded, incinerated or buried without being recycled, which causes great waste of resources and serious environmental pollution. Therefore, the method for converting the waste apple leaves into valuable functional carbon materials by selecting a proper resource utilization mode is a promising strategy, can change waste into valuable, treats waste by waste, and plays a very positive role in solving the problems of energy shortage and ecological environment.
The biochar generally refers to solid biofuel which is produced by pyrolyzing biomass raw materials at a certain temperature under the anaerobic or anoxic condition and has high carbon content and large specific surface area, and is also called as biomass carbon. Biochar is a metal-free material, has small environmental pollution, stable structure, large specific surface area and strong adsorption capacity, and is widely applied to the fields of energy materials, ecological restoration, agriculture and environmental protection.
Under the background, the invention converts the waste apple leaves into the high-value nitrogen-doped porous nano biochar, has low preparation cost and simple process, can be used as a pollution-free carbon functional material to adsorb and activate PDS to cooperatively remove organic pollutants in a water body, and has potential practical application value.
The invention relates to a synthetic method of nitrogen-doped porous nano biochar, which comprises the following steps:
and cleaning waste apple leaves collected in a farmland, drying and grinding into powder. Then mixing the leaf powder and NaOH according to a mass ratio of 1: 3, uniformly mixing and spreading in a porcelain boat in N2Heating to 400 ℃ at a speed of 3-5 ℃/min in a muffle furnace under the protection of atmosphere, preserving heat for 2 hours to fully carbonize the carbonized product, then heating to 500-700 ℃ at the same heating speed, preserving heat for 2-3 hours, reacting the carbonized sample with NaOH at high temperature, using the NaOH as an activator to improve the porosity and specific surface area of the biochar at the stage, and collecting sintered black when the temperature of the muffle furnace is reduced to room temperatureAnd (3) washing the color reactant with 1mol/L HCl solution for 2 times, then washing with deionized water for 2 times, collecting a black sample after washing, and drying at 80 ℃ to obtain the nitrogen-doped porous nano biochar.
For convenience of illustration, in the following examples, nitrogen-doped porous nano biochar prepared at 500 ℃, 600 ℃ and 700 ℃ is named BC-500 ℃, BC-600 ℃ and BC-700 ℃ respectively.
Example 1
1) The waste apple leaves shown in figure 1 are collected, washed clean by deionized water, dried in an oven at 80 ℃ for 24 hours, and then ground into powder by a mortar.
2) Then 1g of tree leaf powder and 3g of NaOH are mixed evenly and spread in a porcelain boat, and N is added2Heating to 400 ℃ in a muffle furnace at a heating rate of 5 ℃/min for 2h under the protection of atmosphere.
3) Then the temperature is raised to 500 ℃ at the heating rate of 5 ℃/min, and the temperature is preserved for 3 h. And when the temperature of the muffle furnace is reduced to room temperature, collecting the sintered black reactant, then cleaning the sintered black reactant for 2 times by using 1mol/L HCl, then cleaning the sintered black reactant for 2 times by using deionized water, collecting the cleaned black sample, and drying the black sample at 80 ℃ for later use.
4) FIG. 2 shows that the SEM image of BC-500 deg.C shows a 3D porous sheet structure with a sheet thickness of about 45 nm. FIG. 5 shows the BC-500 ℃ C1sThe XPS spectrum is composed of C ═ C/C-C, C ═ O, C-O and other groups, and the prepared biochar surface has abundant oxygen-containing functional groups. FIG. 6 shows BC-500 ℃ N1sThe XPS spectrum consists of graphtic N, pyrrole N, pyridine N, etc. groups, indicating that the prepared biochar was successfully doped with nitrogen. The oxygen-containing groups are present on the surface of the glass substrate as shown in the infrared spectrum at BC-500 ℃ of FIG. 7. FIG. 8BC-500 ℃ N2The adsorption and desorption curve shows that the specific surface area is 333g/m2. FIG. 9BC-500 ℃ pore size distribution shows that it is predominantly microporous and mesoporous with an average pore size of 6.5 nm.
Example 2
1) The waste apple leaves shown in figure 1 are collected, washed clean by deionized water, dried in an oven at 80 ℃ for 24 hours, and then ground into powder by a mortar.
2)、1g of leaf powder and 3g of NaOH are mixed evenly and spread in a porcelain boat, and then N2Heating to 400 ℃ in a muffle furnace at a heating rate of 5 ℃/min for 2h under the protection of atmosphere.
3) Then the temperature is raised to 600 ℃ at the heating rate of 5 ℃/min, and the temperature is preserved for 3 h. And when the temperature of the muffle furnace is reduced to room temperature, collecting the sintered black reactant, then cleaning the sintered black reactant for 2 times by using 1mol/L HCl, then cleaning the sintered black reactant for 2 times by using deionized water, collecting the cleaned black sample, and drying the black sample at 80 ℃ for later use.
4) FIG. 3 shows that the SEM photograph of BC-600 ℃ shows a 3D porous sheet structure with a sheet thickness of about 30 nm. FIG. 5 shows BC-600 ℃ C1sThe XPS spectrum consists of C/C-C, C-O, C-O and other groups, and the prepared biochar surface has rich oxygen-containing functional groups. FIG. 6 shows BC-600 ℃ N1sThe XPS spectrum consists of graphtic N, pyrrole N, pyridine N, etc. groups, indicating that the prepared biochar was successfully doped with nitrogen. The oxygen-containing groups are present on the surface of the glass substrate as shown in the infrared spectrum at the temperature of BC-600 ℃ in FIG. 7. FIG. 8BC-600 ℃ N2The adsorption and desorption curve shows that the specific surface area is 447g/m2. FIG. 9BC-600 ℃ pore size distribution shows that it is predominantly microporous and mesoporous with an average pore size of 5 nm.
Example 3
1) The waste apple leaves shown in figure 1 are collected, washed clean by deionized water, dried in an oven at 80 ℃ for 24 hours, and then ground into powder by a mortar.
2) Mixing 1g of leaf powder and 3g of NaOH, spreading the mixture in a porcelain boat, and adding N2Heating to 400 ℃ in a muffle furnace at a heating rate of 5 ℃/min for 2h under the atmosphere protection.
3) Then the temperature is raised to 700 ℃ at the heating rate of 5 ℃/min, and the temperature is kept for 3 h. And when the temperature of the muffle furnace is reduced to room temperature, collecting the sintered black reactant, then cleaning the sintered black reactant for 2 times by using 1mol/L HCl, then cleaning the sintered black reactant for 2 times by using deionized water, collecting the cleaned black sample, and drying the black sample at 80 ℃ for later use.
4) FIG. 4 shows an SEM photograph of BC-700 ℃ showing a 3D porous sheet structure with a sheet thickness of about 10 nm. FIG. 5 shows C at BC-700 deg.C1sXPS spectra are produced by pi-pi vibration,C/C-C, C-O, C-O and other groups, which indicates that the prepared biochar has rich oxygen-containing functional groups on the surface. FIG. 6 shows BC-700 ℃ N1sThe XPS spectrum consists of graphtic N, pyrrole N, pyridine N, etc. groups, indicating that the prepared biochar was successfully doped with nitrogen. The oxygen-containing groups on the surface can be seen from the infrared spectrum at BC-700 ℃ in FIG. 7. FIG. 8BC-700 ℃ N2The adsorption and desorption curve shows that the specific surface area is 739g/m2. FIG. 9BC-700 ℃ pore size distribution plot shows micropores, mesopores, and macropores with an average pore size of 8.0 nm.
5) And performing an experiment for removing the tetracycline in the water body by adopting a catalyst at the temperature of BC-700 ℃, wherein the reaction system is a 60mg/L tetracycline solution, the concentration of PDS is 1.0g/L, the concentration of biochar is 0.2g/L, and the pH value of the solution is 5-9. And adding PDS after adsorbing for 1h, taking 3mL of sample every 20min, and testing the absorbance on an ultraviolet-visible spectrophotometer after passing through a 0.22 mu m filter head. The results are shown in FIG. 10, in which C0At the initial tetracycline concentration, CtThe concentration at time t of degradation. About 30 percent of tetracycline can be adsorbed at the temperature of BC-700 ℃ within 1h, 80 percent of tetracycline can be removed within 2h by adding PDS after the adsorption equilibrium is reached, and the result is that the tetracycline can be removed by the cooperation of adsorption and activation of PDS.
The invention changes waste into valuable, realizes the high-efficiency resource utilization of agricultural and forestry waste apple leaves, provides a low-cost pollution-free route for environmental sewage restoration, and has potential practical application value.
Claims (10)
1. A preparation method of nitrogen-doped porous nano biochar is characterized by comprising the following steps:
1, mixing apple leaf powder and (KOH or NaOH) in inert gas or N2Carrying out heat preservation treatment at 500-700 ℃ under the protection of atmosphere to obtain a reactant;
and 2, removing by-products and impurities in the reactants, and drying to obtain the nitrogen-doped porous nano biochar.
2. The method for preparing nitrogen-doped porous nano biochar as claimed in claim 1, wherein the apple leaves in step 1 are waste apple leaves.
3. The method for preparing nitrogen-doped porous nano biochar according to claim 1, wherein in the step 1, the mass ratio of the apple leaf powder to (KOH or NaOH) is 1: 3.
4. the method for preparing nitrogen-doped porous nano biochar as claimed in claim 1, wherein in step 1, the mixture of apple leaf powder and (KOH or NaOH) is firstly put in inert gas or N2Under the protection of atmosphere, heating to 350-450 ℃, preserving heat for 1.5-2.5 h, and then heating to 500-700 ℃.
5. The method for preparing nitrogen-doped porous nano biochar as claimed in claim 1, wherein in the step 1, the mixture of the apple leaf powder and (KOH or NaOH) is heated to 350-450 ℃ at a heating rate of 3-5 ℃/min, and then the temperature is raised to 500-700 ℃ at a heating rate of 3-5 ℃/min.
6. The preparation method of nitrogen-doped porous nano biochar as claimed in claim 1, wherein in the step 1, the mixture of apple leaf powder and (KOH or NaOH) is subjected to heat preservation treatment at 500-700 ℃ for 2-3 h.
7. The method for preparing nitrogen-doped porous nano biochar according to claim 1, wherein in the step 2, the reactant obtained in the step 1 is washed with HCl solution for 2-5 times, and then washed with deionized water for 2-5 times.
8. The preparation method of the nitrogen-doped porous nano biochar as claimed in claim 7, wherein the cleaned product is dried at 60-90 ℃ in the step 2 to obtain the nitrogen-doped porous nano biochar.
9. The nitrogen-doped porous nano biochar obtained by the preparation method of the nitrogen-doped porous nano biochar obtained according to any one of claims 1-8.
10. Use of the nitrogen-doped porous nano biochar of claim 9 for removing antibiotics from water.
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106006636A (en) * | 2016-05-19 | 2016-10-12 | 中国科学院青岛生物能源与过程研究所 | Biomass-based nitrogen-doped porous carbon material, and preparation method and application thereof |
CN106517183A (en) * | 2016-11-15 | 2017-03-22 | 河南理工大学 | A low-cost simple preparing method for nitrogen-doped porous charcoal with a high specific surface area |
CN109231201A (en) * | 2018-11-05 | 2019-01-18 | 安徽工业大学 | A kind of preparation method of supercapacitor sulphur, nitrogen, phosphor codoping porous carbon materials |
CN112516964A (en) * | 2020-11-16 | 2021-03-19 | 湖南大学 | Nitrogen-doped biochar and preparation method and application thereof |
US20210087062A1 (en) * | 2019-09-25 | 2021-03-25 | King Fahd University Of Petroleum And Minerals | Nitrogen enriched carbon derived from albizia procera leaves |
-
2022
- 2022-03-31 CN CN202210335438.XA patent/CN114570331A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106006636A (en) * | 2016-05-19 | 2016-10-12 | 中国科学院青岛生物能源与过程研究所 | Biomass-based nitrogen-doped porous carbon material, and preparation method and application thereof |
CN106517183A (en) * | 2016-11-15 | 2017-03-22 | 河南理工大学 | A low-cost simple preparing method for nitrogen-doped porous charcoal with a high specific surface area |
CN109231201A (en) * | 2018-11-05 | 2019-01-18 | 安徽工业大学 | A kind of preparation method of supercapacitor sulphur, nitrogen, phosphor codoping porous carbon materials |
US20210087062A1 (en) * | 2019-09-25 | 2021-03-25 | King Fahd University Of Petroleum And Minerals | Nitrogen enriched carbon derived from albizia procera leaves |
CN112516964A (en) * | 2020-11-16 | 2021-03-19 | 湖南大学 | Nitrogen-doped biochar and preparation method and application thereof |
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