CN112691666A - Amorphous iron oxyhydroxide-biochar composite material and preparation method thereof - Google Patents
Amorphous iron oxyhydroxide-biochar composite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides an amorphous iron oxyhydroxide-biochar composite material and a preparation method thereof, and relates to the technical field of amorphous materials. The preparation method provided by the invention comprises the following steps: carbonizing biomass containing silicon dioxide to obtain a biochar material; and mixing the biochar material with an iron salt aqueous solution, and carrying out hydrothermal reaction under an alkaline condition to obtain the amorphous FeOOH-biochar composite material. According to the invention, the biomass rich in silicon dioxide is used as a raw material to prepare the porous biochar material, the biochar material can be used as a carrier of the composite material on one hand, and meanwhile, the silicon dioxide also provides a necessary silicon source for inhibiting the crystallization of the iron oxyhydroxide, so that the structural disorder of the iron oxyhydroxide is ensured, and the amorphous iron oxyhydroxide-biochar composite material is obtained. The preparation method provided by the invention has simple process, the whole process is carried out in the water phase, and the preparation method is beneficial to large-scale production and application.
Description
Technical Field
The invention relates to the technical field of amorphous materials, in particular to an amorphous iron oxyhydroxide-biochar composite material and a preparation method thereof.
Background
The nano amorphous metal material has been widely applied to a plurality of fields such as environmental management and energy storage, wherein the iron-based amorphous material has received extensive attention from researchers due to the advantages of wide sources, no secondary pollution, high adsorption and catalysis efficiency and the like. But the iron-based material can generate crystallization, aggregation and growth phenomena in the reaction process to form a certain crystal structure, thereby destroying the amorphous structure of the iron-based material and reducing the efficiency of the iron-based material. Therefore, the preparation of high purity amorphous iron-based materials has been the focus of attention of researchers. Meanwhile, the nano material has an agglomeration phenomenon in the preparation process, and the iron-based amorphous material is loaded on a carrier with a high specific surface area to prepare a corresponding composite material, so that the agglomeration of the nano material is effectively reduced, and more active sites are exposed.
At present, the main method for inhibiting the crystallization of the iron-based material is to use organic phase ethanol as a reaction solvent to replace water, and the influence of ethanol as the reaction solvent on the crystallization of the iron-based material is studied in "Synthesis and Properties of a high-capacity iron oxide adsorbent for fluorine removal from driving water" (Applied Surface Science, 2017, 425, 272 and 281), and the article indicates that ethanol as the reaction solvent effectively inhibits the crystallization of the iron-based material, thereby generating the amorphous iron-based material with higher adsorption capacity. However, ethanol is not suitable for long-distance transportation, the high-purity ethanol solvent is high in price, and meanwhile, the flammability of ethanol increases the risk of preparation, and large-scale integrated production is not facilitated.
Disclosure of Invention
The invention aims to provide an amorphous iron oxyhydroxide-biochar composite material and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of an amorphous iron oxyhydroxide-biochar composite material, which comprises the following steps:
carbonizing biomass containing silicon dioxide to obtain a biochar material;
and mixing the biochar material with an iron salt aqueous solution, and carrying out hydrothermal reaction under an alkaline condition to obtain the amorphous FeOOH-biochar composite material.
Preferably, the carbonization temperature is 400-600 ℃, and the carbonization time is 1-2 h.
Preferably, the aqueous iron salt solution is an aqueous ferric nitrate solution; the mass concentration of the ferric salt aqueous solution is 1 g/L-5 g/L.
Preferably, the mass ratio of the biochar material to the iron salt in the iron salt aqueous solution is 1: 2-4.
Preferably, the pH value of the alkaline condition is 11.93-12.03.
Preferably, the temperature of the hydrothermal reaction is 50-70 ℃; the pressure of the hydrothermal reaction is 1-1.5 MPa; the time of the hydrothermal reaction is 12-36 h.
Preferably, after the hydrothermal reaction, the method further comprises: and sequentially cleaning, carrying out solid-liquid separation and drying on a product obtained by the hydrothermal reaction to obtain the amorphous FeOOH-biochar composite material.
Preferably, the content of silica in the silica-containing biomass is 2% to 10%.
Preferably, the biomass containing silicon dioxide comprises one or more of corn stover, wheat straw and cotton straw.
The invention provides the amorphous FeOOH-biochar composite material prepared by the preparation method in the technical scheme.
The invention provides a preparation method of an amorphous iron oxyhydroxide-biochar composite material, which comprises the following steps: carbonizing biomass containing silicon dioxide to obtain a biochar material; and mixing the biochar material with an iron salt aqueous solution, and carrying out hydrothermal reaction under an alkaline condition to obtain the amorphous FeOOH-biochar composite material. According to the invention, the biomass rich in silicon dioxide is used as a raw material to prepare the porous biochar material, the biochar material can be used as a carrier of the composite material on one hand, and meanwhile, the silicon dioxide also provides a necessary silicon source for inhibiting the crystallization of the iron oxyhydroxide, so that the structural disorder of the iron oxyhydroxide is ensured, and the amorphous iron oxyhydroxide-biochar composite material is obtained. The preparation method provided by the invention has the advantages of simple process, easily obtained raw materials and low cost, the whole process is carried out in the water phase, ethanol is not required to be added to inhibit the crystallization of the iron-based material, the preparation cost and the risk are reduced, and the preparation method is beneficial to large-scale production and application.
Drawings
FIG. 1 is XRD patterns of examples 1 to 3 and the verification example;
FIG. 2 is an EDS diagram of the biochar material prepared in example 1;
fig. 3 is an EDS diagram of a biochar material prepared in the validation example.
Detailed Description
The invention provides a preparation method of an amorphous iron oxyhydroxide-biochar composite material, which comprises the following steps:
carbonizing biomass containing silicon dioxide to obtain a biochar material;
and mixing the biochar material with an iron salt aqueous solution, and carrying out hydrothermal reaction under an alkaline condition to obtain the amorphous FeOOH-biochar composite material.
In the present invention, unless otherwise specified, the starting materials for the preparation are all commercially available products well known to those skilled in the art.
According to the invention, the biomass containing silicon dioxide is carbonized to obtain the biochar material. In the present invention, the silica content of the silica-containing biomass is preferably 2%, more preferably 10%. In the present invention, the biomass containing silicon dioxide preferably comprises one or more of corn stover, wheat straw, and cotton straw.
In the invention, before the biomass containing silicon dioxide is carbonized, pretreatment is preferably carried out; the pretreatment preferably comprises: and sequentially crushing, cleaning and drying the biomass containing the silicon dioxide. In the invention, the particle size of the biomass obtained after crushing is preferably 0.1-0.3 mm, and more preferably 0.15-0.20 mm; the washing is preferably water washing, and the impurities are removed by washing. In the invention, the drying temperature is preferably 90-110 ℃, and more preferably 100-105 ℃; the drying time is preferably 12-36 h, and more preferably 24 h.
In the invention, the carbonization temperature is preferably 400-600 ℃, and more preferably 500-550 ℃; the carbonization time is preferably 1-2 h. In the present invention, the carbonization is preferably performed under a nitrogen atmosphere. In the carbonization process, the organic matter is cracked and condensed into a six-membered ring carbon structure.
In the invention, preferably, after the carbonization, the obtained product is washed and dried sequentially. In the invention, the number of times of water washing is preferably 4-8, and the ash content remained in the product is removed through water washing. In the invention, the drying temperature is preferably 90-110 ℃, and more preferably 100-105 ℃; the drying time is preferably 12-30 h, and more preferably 24 h.
In the invention, the average pore diameter of the biochar material is preferably 2-5 nm, and the specific surface area is preferably 100-300 m2(ii) in terms of/g. In the present invention, the content of silica in the biochar material is preferably 10%.
After the biochar material is obtained, the biochar material and a ferric salt aqueous solution are mixed, and hydrothermal reaction is carried out under an alkaline condition to obtain the amorphous FeOOH-biochar composite material. In the present invention, the aqueous iron salt solution is preferably an aqueous ferric nitrate solution; the mass concentration of the ferric salt water solution is preferably 1-5 g/L, and more preferably 2-3 g/L. In the invention, the mass ratio of the biochar material to the iron salt in the iron salt aqueous solution is preferably 1: 2-4, and more preferably 1: 3-4. The effect of the invention for limiting the dosage ratio is to control the crystalline amorphous morphology of the iron-based material.
In the present invention, the biochar material and the aqueous solution of ferric salt are preferably mixed under stirring, more preferably, under magnetic stirring; the rotating speed of the stirring is preferably 500-1000 rpm, more preferably 800-900 rpm, and the stirring time is preferably 12-30 h, more preferably 24 h. According to the invention, the biochar material and the ferric salt aqueous solution are fully mixed, so that iron ions in the ferric salt aqueous solution can be fully adsorbed on the surface of the biochar material.
In the invention, the pH value of the alkaline condition is preferably 11.93-12.03, and more preferably 12-12.03. The invention can provide the energy necessary for the reaction by carrying out the hydrothermal reaction under the alkaline condition. In the present invention, the agent providing the alkaline condition is preferably a sodium hydroxide solution; the concentration of the sodium hydroxide solution is preferably 1 mol/L. In a specific embodiment of the present invention, the biochar material and the aqueous solution of ferric salt are mixed first, and then the sodium hydroxide solution is added dropwise to the obtained mixed solution. In a specific embodiment of the present invention, the dropping rate of the sodium hydroxide solution is preferably 1 mL/min.
In the invention, the hydrothermal reaction is preferably carried out in a hydrothermal reaction kettle, and the temperature of the hydrothermal reaction is preferably 50-70 ℃, more preferably 60-65 ℃; the pressure of the hydrothermal reaction is preferably 1-1.5 MPa, and more preferably 1.2-1.4 MPa; the hydrothermal reaction time is preferably 12 hours, more preferably 24 hours. In the hydrothermal reaction process, the change of the materials is that dissolved iron ions are gradually converted into solid materials under the heating condition.
In the present invention, after the hydrothermal reaction, it is preferable to further include: and sequentially cleaning, carrying out solid-liquid separation and drying on a product obtained by the hydrothermal reaction to obtain the amorphous FeOOH-biochar composite material. In the present invention, the washing is preferably water washing; the solid-liquid separation mode is preferably filtration; in the invention, solid substances obtained by solid-liquid separation are preferably dried; the drying temperature is preferably 50-70 ℃, and the drying time is preferably 24 hours.
The invention provides the amorphous FeOOH-biochar composite material prepared by the preparation method in the technical scheme. In the invention, the average pore diameter of the amorphous FeOOH-biochar composite material is preferably 2-5 nm, and the specific surface area is preferably 100-300 m2/g。
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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.
Example 1
Pulverizing corn stalk with 10% silicon dioxide content to particle size of 0.15mm, washing with water, oven drying at 105 deg.C for 24 hr, heating at 600 deg.C for 2 hr, and carbonizing; washing the obtained carbonized product with water for 8 times, and drying for 24 hours at the temperature of 110 ℃ to obtain a biochar material;
putting the biochar material into an iron nitrate aqueous solution with the mass concentration of 5g/L, wherein the mass ratio of the biochar material to the iron nitrate is 1:4, slowly stirring the mixture for 24 hours at the rotating speed of 500rpm, dropwise adding a sodium hydroxide solution with the concentration of 1mol/L into the obtained mixed solution to ensure that the pH of the solution is 12.03, transferring the solution into a hydrothermal reaction kettle for hydrothermal reaction within 1 minute, wherein the temperature of the hydrothermal reaction is 60 ℃, the pressure is 1MPa, and the time is 24 hours;
and washing a product obtained after the hydrothermal reaction by using deionized water, then carrying out suction filtration, and drying the obtained solid substance at the temperature of 50 ℃ for 24 hours to obtain the amorphous FeOOH-biochar composite material.
Example 2
Pulverizing corn stalk with 10% silicon dioxide content to particle size of 0.15mm, washing with water, oven drying at 105 deg.C for 24 hr, heating at 500 deg.C for 2 hr, and carbonizing; washing the obtained carbonized product with water for 8 times, and drying for 24 hours at the temperature of 110 ℃ to obtain a biochar material;
putting the biochar material into an iron nitrate aqueous solution with the mass concentration of 5g/L, wherein the mass ratio of the biochar material to the iron nitrate is 1:4, slowly stirring the mixture for 24 hours at the rotating speed of 500rpm, dropwise adding a sodium hydroxide solution with the concentration of 1mol/L into the obtained mixed solution to ensure that the pH of the solution is 12.03, transferring the solution into a hydrothermal reaction kettle for hydrothermal reaction within 1 minute, wherein the temperature of the hydrothermal reaction is 60 ℃, the pressure is 1MPa, and the time is 24 hours;
and washing a product obtained after the hydrothermal reaction by using deionized water, then carrying out suction filtration, and drying the obtained solid substance at the temperature of 50 ℃ for 24 hours to obtain the amorphous FeOOH-biochar composite material.
Example 3
Pulverizing corn stalk with 10% silicon dioxide content to particle size of 0.15mm, washing with water, oven drying at 105 deg.C for 24 hr, heating at 400 deg.C for 2 hr, and carbonizing; washing the obtained carbonized product with water for 8 times, and drying for 24 hours at the temperature of 110 ℃ to obtain a biochar material;
putting the biochar material into an iron nitrate aqueous solution with the mass concentration of 5g/L, wherein the mass ratio of the biochar material to the iron nitrate is 1:4, slowly stirring the mixture for 24 hours at the rotating speed of 500rpm, dropwise adding a sodium hydroxide solution with the concentration of 1mol/L into the obtained mixed solution to ensure that the pH of the solution is 12.03, transferring the solution into a hydrothermal reaction kettle for hydrothermal reaction within 1 minute, wherein the temperature of the hydrothermal reaction is 60 ℃, the pressure is 1MPa, and the time is 24 hours;
and washing a product obtained after the hydrothermal reaction by using deionized water, then carrying out suction filtration, and drying the obtained solid substance at the temperature of 50 ℃ for 24 hours to obtain the amorphous FeOOH-biochar composite material.
Verification example
Pulverizing corn stalk with 10% silicon dioxide content to particle size of 0.15mm, washing with water, oven drying at 105 deg.C for 24 hr, heating at 600 deg.C for 2 hr, and carbonizing; washing the obtained carbonized product with water for 8 times, and drying for 24 hours at the temperature of 110 ℃ to obtain a biochar material;
soaking the biochar material in 48% hydrofluoric acid for 24h, wherein the solid-to-liquid ratio of the biochar material to the hydrofluoric acid is 1g:20mL, so as to obtain the biochar treated by the hydrofluoric acid;
putting the biochar material treated by the hydrofluoric acid into an iron nitrate aqueous solution with the mass concentration of 5g/L, wherein the mass ratio of the biochar material to the iron nitrate is 1:4, slowly stirring at the rotating speed of 500rpm for 24 hours, dropwise adding a sodium hydroxide solution with the concentration of 1mol/L into the obtained mixed solution to ensure that the pH of the solution is 12.03, transferring the solution into a hydrothermal reaction kettle for hydrothermal reaction within 1min, wherein the temperature of the hydrothermal reaction is 60 ℃, the pressure is 1MPa, and the time is 24 hours;
and washing a product obtained after the hydrothermal reaction by using deionized water, then carrying out suction filtration, and drying the obtained solid substance for 24 hours (time) at the temperature of 50 ℃ to obtain the crystalline state iron oxyhydroxide-biochar composite material.
Test example
The XRD patterns of examples 1 to 3 and the verification example are shown in fig. 1, and it can be seen from fig. 1 that the amorphous iron oxyhydroxide-biochar composite materials prepared in examples 1 to 3 have no obvious peak formed by metal crystal, and the peak is only a characteristic peak of carbon material; in the verification example, the composite material obtained by using the biochar treated by hydrofluoric acid shows the characteristic peak of alpha-FeOOH.
The EDS of the biochar material prepared in example 1 is shown in fig. 2, and it can be seen from fig. 2 that the hydrofluoric acid prepared contains a large amount of silicon element.
An EDS diagram of the crystalline iron oxyhydroxide-biochar composite material prepared in the validation example is shown in fig. 3, and as can be seen from fig. 3, the content of silicon element in the biochar treated by hydrofluoric acid is remarkably reduced, which indicates that the silicon element has an obvious inhibiting effect on the crystallization of the material.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The preparation method of the amorphous iron oxyhydroxide-biochar composite material is characterized by comprising the following steps of:
carbonizing biomass containing silicon dioxide to obtain a biochar material;
and mixing the biochar material with an iron salt aqueous solution, and carrying out hydrothermal reaction under an alkaline condition to obtain the amorphous FeOOH-biochar composite material.
2. The preparation method according to claim 1, wherein the carbonization temperature is 400-600 ℃, and the carbonization time is 1-2 h.
3. The method according to claim 1, wherein the aqueous iron salt solution is an aqueous ferric nitrate solution; the mass concentration of the ferric salt water solution is 1-5 g/L.
4. The preparation method according to claim 1 or 3, wherein the mass ratio of the biochar material to the iron salt in the iron salt aqueous solution is 1: 2-4.
5. The method according to claim 1, wherein the alkaline condition has a pH of 11.93 to 12.03.
6. The preparation method according to claim 1, wherein the temperature of the hydrothermal reaction is 50-70 ℃; the pressure of the hydrothermal reaction is 1-1.5 MPa; the time of the hydrothermal reaction is 12-36 h.
7. The method according to claim 1, further comprising, after the hydrothermal reaction: and sequentially cleaning, carrying out solid-liquid separation and drying on a product obtained by the hydrothermal reaction to obtain the amorphous FeOOH-biochar composite material.
8. The method according to claim 1, wherein the silica content of the silica-containing biomass is 2 to 10%.
9. The method of claim 1 or 8, wherein the silica-containing biomass comprises one or more of corn stover, wheat straw, and cotton stover.
10. The amorphous FeOOH-biochar composite prepared by the preparation method of any one of claims 1-9.
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Cited By (2)
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| CN113842881A (en) * | 2021-09-28 | 2021-12-28 | 厦门大学嘉庚学院 | Oyster shell powder reinforced charcoal for removing micro-plastics in mariculture water body and preparation method and application thereof |
| CN114873706A (en) * | 2022-06-02 | 2022-08-09 | 湖南大学 | Amorphous iron oxyhydroxide/polyacrylamide composite flocculant and preparation method and application thereof |
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Cited By (4)
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| CN113842881A (en) * | 2021-09-28 | 2021-12-28 | 厦门大学嘉庚学院 | Oyster shell powder reinforced charcoal for removing micro-plastics in mariculture water body and preparation method and application thereof |
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| CN114873706A (en) * | 2022-06-02 | 2022-08-09 | 湖南大学 | Amorphous iron oxyhydroxide/polyacrylamide composite flocculant and preparation method and application thereof |
| CN114873706B (en) * | 2022-06-02 | 2023-11-21 | 湖南大学 | Amorphous ferric oxide hydroxide/polyacrylamide composite flocculant and preparation method and application thereof |
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Application publication date: 20210423 |