CN113926482A - Preparation method and application of biochar composite photocatalytic material - Google Patents
Preparation method and application of biochar composite photocatalytic material Download PDFInfo
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- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 description 1
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- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/56—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/02—Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only
- C09K17/04—Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only applied in a physical form other than a solution or a grout, e.g. as granules or gases
Abstract
The invention discloses a preparation method and application of a biochar composite photocatalytic material, which comprises the following steps: the method comprises the following steps of carbonizing corncobs or peanut shells serving as biomass raw materials to obtain a biochar material; preparation of doped BiVO4(ii) a Adding the obtained biochar material into the mixed solution, carrying out ultrasonic treatment, and adding the obtained doped BiVO4Reacting, cooling, centrifuging, washing the lower precipitate, and grinding to obtain the biochar composite photocatalytic material. The invention utilizes the corncob or the peanut shell as the substrate to prepare the biochar material, thereby changing agricultural solid waste into valuable and reducing the preparation cost. The prepared charcoal material is loose and porous, and has large specific surface area; the obtained biocharThe composite photocatalytic material is applied to soil, not only improves the soil texture, but also can absorb and fix polycyclic aromatic hydrocarbons in the soil due to the distribution of phenolic hydroxyl, carboxyl, anhydride and other groups on the surface of the biochar.
Description
Technical Field
The invention relates to the technical field of organic pollutant treatment and removal, in particular to a preparation method and application of a biochar composite photocatalytic material.
Background
Polycyclic Aromatic Hydrocarbons (PAHs) are organic pollutants with environmental persistence, biological accumulation and high toxicity, and are widely present in environmental media such as atmosphere, water, soil and the like. PAHs have toxicity such as teratogenicity, carcinogenicity and mutagenicity, and have potential harm to human health and ecological environment. The PAHs can enter environmental media such as soil, water and the like through the effects of atmospheric sedimentation, precipitation, surface runoff and the like.
Semiconductor photocatalytic oxidation is one of the most attractive advanced oxidation technologies and is an effective way to degrade organic pollutants in the environment. The photocatalytic oxidation technology can thoroughly mineralize refractory organic matters without generating secondary pollution, so the method has wide application prospect in the aspects of degrading organic pollutants in soil and preventing and controlling toxic and harmful pollutants in river surface sources.
The photocatalytic technology is an energy-saving and efficient green environment-friendly new technology for degrading pollutants through a photocatalytic material, has no secondary pollution, zero energy consumption, can spontaneously treat pollutants without monitoring, and has huge development potential and market utilization value in the aspect of water environment pollution treatment. One of the key problems in photocatalytic research is the development of a low-cost semiconductor photocatalytic material capable of working stably and efficiently under sunlight. However, the existing semiconductor photocatalyst has the defects that firstly, the degradation efficiency of the existing semiconductor photocatalyst on polycyclic aromatic hydrocarbon in soil is low, and the existing semiconductor photocatalyst is difficult to popularize and apply; secondly, most of the photocatalytic materials are semiconductor TiO2However, it shows photochemical activity only in the ultraviolet region because of its wide band gap.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a preparation method and application of a biochar composite photocatalytic material.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a preparation method of a biochar composite photocatalytic material comprises the following steps:
1) the method comprises the following steps of (1) taking corncobs or peanut shells as biomass raw materials, cleaning and drying the biomass raw materials, then crushing, grinding and screening the crushed materials, quickly heating the crushed materials to a certain temperature through a tubular furnace under nitrogen flow with a certain flow rate, and then carbonizing the crushed materials for a period of time to obtain a biochar material;
2) BiVO (BiVO) is prepared by using corn straws as a biological template and hexamethylenetetramine as a nitrogen source through a sol-gel method4；
3) Adding the biochar material obtained in the step 1) into a mixed solution of distilled water and absolute ethyl alcohol, carrying out ultrasonic treatment for 0.6-1h, and adding the doped BiVO obtained in the step 2)4Uniformly stirring, transferring the mixed solution into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a homogeneous reactor, setting the temperature of the homogeneous reactor at 180-.
Further, in the preparation method of the biochar composite photocatalytic material, in the step 1), the drying temperature is 90-110 ℃ and the time is 20-28 h.
Further, in the preparation method of the biochar composite photocatalytic material, in the step 1), the crushed material is ground and then screened by a 0.25mm sieve.
Further, in the preparation method of the biochar composite photocatalytic material, in the step 1), the flow rate of nitrogen flow is 20-40 mL/min.
Further, in the preparation method of the biochar composite photocatalytic material, in the step 1), the crushed material is quickly heated to 500 ℃ by a tubular furnace and then carbonized for 0.5-1.5 h.
Further, in the preparation method of the biochar composite photocatalytic material, in the step 2), the corn straws need to be pretreated, and the pretreatment step comprises the steps of peeling, cutting into cylinders, soaking in dilute hydrochloric acid, washing, drying and calcining.
Further, in the preparation method of the biochar composite photocatalytic material, in the step 3), the volume ratio of distilled water to absolute ethyl alcohol is 1: 1-2.
Further, the preparation method of the biochar composite photocatalytic material comprises the step 3) of mixing the biochar material with BiVO4The mass ratio of (A) to (B) is 4-6: 100.
the biochar composite photocatalytic material prepared by the preparation method is applied as a catalyst. The application mode is that the biochar composite photocatalytic material is added into a polluted soil sample, and the soil is turned over under the irradiation of natural light.
The invention has the beneficial effects that:
1. the invention utilizes the corncob or the peanut shell as the substrate to prepare the biochar material, thereby changing agricultural solid waste into valuable and reducing the preparation cost. The prepared charcoal material is loose and porous, and has large specific surface area. The obtained biological carbon composite photocatalytic material is applied to soil, so that the soil texture is improved, and the biological carbon surface is distributed with phenolic hydroxyl, carboxyl, anhydride and other groups, so that the biological carbon composite photocatalytic material can adsorb and fix polycyclic aromatic hydrocarbons in the soil; and coupled doping BiVO4The photocatalytic oxidation can degrade polycyclic aromatic hydrocarbon molecules into small molecular substances without pollution.
2. BiVO prepared by taking corn straws as template4Successfully copies the honeycomb structure of the corn straw, makes the sample particles smaller than the sample prepared without a template, has good particle dispersibility, and effectively improves BiVO4The initial adsorption capacity promotes the photocatalytic activity; BiVO with unchanged doped N4The crystal forms of (A) are monoclinic scheelite types, and the particles gradually become smaller with the increase of the N doping amount, and the particle size is reduced therewith; doped N-substituted BiVO4Part of O exists in the form of-N-V-O to generate impurity energy level, and N doping causes BiVO4The increase of surface oxygen vacancy and the coordination of the two lead to the narrowing of forbidden band width and the red shift of the light absorption band edge, thus reducing BiVO4The crystal grain size increases the specific surface area, so that the photocatalyst has better photocatalytic activity under natural light, and the activity of the photocatalyst is effectively improved.
Of course, it is not necessary for any one product that embodies the invention to achieve all of the above advantages simultaneously.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a thermogram of peanut hulls in example 1 of the present invention;
FIG. 2 is a thermogram of peanut shells in example 1 of the present invention;
FIG. 3 is an infrared spectrum of peanut shells at different temperatures in example 1 of the present invention;
FIG. 4 is a thermogram of corn cob according to example 2 of the present invention;
FIG. 5 is a thermogram of corn cob according to example 2 of the present invention;
FIG. 6 is an infrared spectrum of corn cob at different temperatures in example 2 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A preparation method of a biochar composite photocatalytic material comprises the following steps:
1) the method comprises the following steps of (1) taking corncobs or peanut shells as biomass raw materials, cleaning, drying and crushing the biomass raw materials, wherein the drying temperature is 90-110 ℃, and the drying time is 20-28 hours; grinding the crushed material, sieving the ground material by a 0.25mm sieve, quickly heating the ground material to the temperature of 300-500 ℃ by a tubular furnace under the nitrogen flow of 20-40mL/min, and carbonizing the ground material for 0.5-1.5h to obtain a biochar material;
2) utilizing corn stalk as biological template and hexamethyleneThe method for preparing the doped BiVO by using the tetramine as a nitrogen source and adopting a sol-gel method4(ii) a The corn stalk is pretreated, the pretreatment step is that the corn stalk is peeled, cut into a cylinder, soaked in dilute hydrochloric acid, washed, dried and calcined;
3) adding the biochar material obtained in the step 1) into a mixed solution formed by mixing distilled water and absolute ethyl alcohol according to the volume ratio of 1:1-2, carrying out ultrasonic treatment for 0.6-1h, and adding the doped BiVO obtained in the step 2)4Biochar material and doped BiVO4The mass ratio of (A) to (B) is 4-6: 100, respectively; stirring uniformly, transferring the mixed solution into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a homogeneous reactor, setting the temperature of the homogeneous reactor at 180-.
The following embodiments are relevant to the present invention:
example 1
Peanut shells are used as biomass raw materials:
the main instruments used in the experimental process of this example were as follows:
in this example, the peanut shells were cleaned of surface dust and impurities with ultrapure water. Drying at 100 deg.C for 24 hr, and grinding with grinder; the preparation process of the biochar is carried out under the protection of nitrogen, the flow velocity of the nitrogen is 30mL/min, and the biochar is prepared by rapidly heating through a tubular furnace at the preparation temperature of 300 ℃, 350 ℃ and 400 ℃.
In this example, the peanut shells are thermally reformed as shown in fig. 1 and 2. The yield of peanut shell biochar is shown in table 1:
TABLE 1
| Temperature (. degree.C.) | 300 | 350 | 400 |
| Yield% | 54.1 | 41.2 | 15.3 |
In this example, the elemental compositions of the biochar from peanut hulls at different temperatures are shown in table 2:
TABLE 2
| Temperature (. degree.C.) | C(％) | H(％) | N(％) | O(％) | H/C | O/ |
| 300 | 74.4 | 4.31 | 1.83 | 16.1 | 0.69 | 0.16 |
| 350 | 74.3 | 4.44 | 1.78 | 17.9 | 0.71 | 0.18 |
| 400 | 53.6 | 4.80 | 1.38 | 39.9 | 1.07 | 0.55 |
In this example, the infrared spectrogram of peanut shell at different temperatures is shown in FIG. 3, from which it can be seen that the absorption peak position is 3760cm-1、2930cm-1、2349cm-1、2076cm-1、1589cm-1、960cm-1、645cm-1To (3).
Example 2
Corncob is used as a biomass raw material:
the main equipment used in the experimental procedure of this example is shown in table 1 above.
In this embodiment, corncobs are used as raw materials, and are put into a tube furnace under nitrogen protection after being cleaned, dried, ground, sieved and the like. The heating rate is 10 ℃/min, and the carbonization temperature is 300 ℃, 400 ℃ and 500 ℃ (carbonization for 1 h).
In this example, the corn cob is thermally heated as shown in fig. 4 and 5. The elemental composition of biochar at different temperatures is shown in table 3:
TABLE 3
| Temperature (. degree.C.) | C(％) | H(％) | N(％) | O(％) | H/C | O/ |
| 300 | 40.0 | 6.00 | 1.09 | 52.7 | 1.80 | 0.99 |
| 400 | 17.1 | 3.98 | 0.42 | 78.5 | 2.79 | 3.44 |
| 500 | 16.9 | 3.26 | 0.42 | 79.3 | 2.31 | 3.52 |
In this example, the infrared spectra of the corn cob at different temperatures are shown in FIG. 6.
Example 3
A preparation method of a biochar composite photocatalytic material comprises the following steps:
1) corncobs are used as biomass raw materials, the biomass raw materials are cleaned, dried and then crushed, the drying temperature is 100 ℃, and the drying time is 24 hours; grinding the crushed materials, sieving the ground materials by a 0.25mm sieve, quickly heating the ground materials to 300 ℃ by a tubular furnace under 30mL/min nitrogen flow, and carbonizing the ground materials for 1h to obtain a biochar material;
2) BiVO (BiVO) is prepared by using corn straws as a biological template and hexamethylenetetramine as a nitrogen source through a sol-gel method4(ii) a The corn stalk is pretreated, the pretreatment step is that the corn stalk is peeled, cut into a cylinder, soaked in dilute hydrochloric acid, washed, dried and calcined;
3) adding the biochar material obtained in the step 1) into a mixed solution formed by mixing distilled water and absolute ethyl alcohol according to the volume ratio of 1:1, carrying out ultrasonic treatment for 1h, and adding the doped BiVO obtained in the step 2)4Biochar material and doped BiVO4The mass ratio of (A) to (B) is 5: 100, respectively; stirring uniformly, transferring the mixed solution into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a homogeneous reactor, setting the temperature of the homogeneous reactor to 190 ℃, continuously reacting for 20 hours, cooling, centrifuging, washing a lower precipitate, and grinding to obtain the biochar composite photocatalytic material.
Example 4
A preparation method of a biochar composite photocatalytic material comprises the following steps:
1) peanut shells are used as biomass raw materials, the biomass raw materials are cleaned, dried and then crushed, the drying temperature is 100 ℃, and the drying time is 24 hours; grinding the crushed materials, sieving the ground materials by a 0.25mm sieve, quickly heating the ground materials to 400 ℃ through a tubular furnace under 30mL/min nitrogen flow, and then carbonizing the ground materials for 1h to obtain a biochar material;
2) BiVO (BiVO) is prepared by using corn straws as a biological template and hexamethylenetetramine as a nitrogen source through a sol-gel method4(ii) a The corn stalk is pretreated, the pretreatment step is that the corn stalk is peeled, cut into a cylinder, soaked in dilute hydrochloric acid, washed, dried and calcined;
3) adding the biochar material obtained in the step 1) into a mixed solution formed by mixing distilled water and absolute ethyl alcohol according to the volume ratio of 1:2, carrying out ultrasonic treatment for 1h, and adding the doped BiVO obtained in the step 2)4Biochar material and doped BiVO4The mass ratio of (A) to (B) is 6: 100, respectively; stirring uniformly, transferring the mixed solution into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a homogeneous reactor, setting the temperature of the homogeneous reactor at 200 ℃, continuously reacting for 12 hours, cooling, centrifuging, washing a lower precipitate, and grinding to obtain the biochar composite photocatalytic material.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (10)
1. A preparation method of a biochar composite photocatalytic material is characterized by comprising the following steps:
1) the method comprises the following steps of (1) taking corncobs or peanut shells as biomass raw materials, cleaning and drying the biomass raw materials, then crushing, grinding and screening the crushed materials, quickly heating the crushed materials to a certain temperature through a tubular furnace under nitrogen flow with a certain flow rate, and then carbonizing the crushed materials for a period of time to obtain a biochar material;
2) BiVO (BiVO) is prepared by using corn straws as a biological template and hexamethylenetetramine as a nitrogen source through a sol-gel method4；
3) Adding the biochar material obtained in the step 1) into a mixed solution of distilled water and absolute ethyl alcohol, carrying out ultrasonic treatment for 0.6-1h, and adding the doped BiVO obtained in the step 2)4Uniformly stirring, transferring the mixed solution into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a homogeneous reactor, setting the temperature of the homogeneous reactor at 180-.
2. The method for preparing the biochar composite photocatalytic material as recited in claim 1, wherein the biochar composite photocatalytic material comprises the following steps: in the step 1), the drying temperature is 90-110 ℃ and the drying time is 20-28 h.
3. The method for preparing the biochar composite photocatalytic material as recited in claim 1, wherein the biochar composite photocatalytic material comprises the following steps: in step 1), the ground material is sieved through a 0.25mm sieve.
4. The method for preparing the biochar composite photocatalytic material as recited in claim 1, wherein the biochar composite photocatalytic material comprises the following steps: in step 1), the flow rate of the nitrogen flow is 20-40 mL/min.
5. The method for preparing the biochar composite photocatalytic material as recited in claim 1, wherein the biochar composite photocatalytic material comprises the following steps: in the step 1), the crushed material is carbonized for 0.5 to 1.5 hours after being rapidly heated to 500 ℃ by a tubular furnace.
6. The method for preparing the biochar composite photocatalytic material as recited in claim 1, wherein the biochar composite photocatalytic material comprises the following steps: in the step 2), the corn straws need to be pretreated, and the pretreatment step comprises the steps of peeling, cutting into cylinders, soaking in dilute hydrochloric acid, and then washing, drying and calcining.
7. The method for preparing the biochar composite photocatalytic material as recited in claim 1, wherein the biochar composite photocatalytic material comprises the following steps: in the step 3), the volume ratio of the distilled water to the absolute ethyl alcohol is 1: 1-2.
8. The method for preparing the biochar composite photocatalytic material as recited in claim 1, wherein the biochar composite photocatalytic material comprises the following steps: in the step 3), the biochar material and the doped BiVO4The mass ratio of (A) to (B) is 4-6: 100.
9. use of the biochar composite photocatalytic material prepared by the preparation method according to any one of claims 1 to 8 as a catalyst.
10. The use of claim 9, wherein the biochar composite photocatalytic material is added to a contaminated soil sample, and the soil is turned under natural light irradiation.
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| CN115178281A (en) * | 2022-07-27 | 2022-10-14 | 云南大学 | Bismuth vanadate-silver iodide-biochar composite material as well as preparation method and application thereof |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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