CN110833817A - Dry synthesis method of rice hull biochar loaded nano-iron material - Google Patents
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Abstract
The invention provides a dry synthesis method of a rice hull biochar loaded nano-iron material, which comprises the following preparation steps: 1) soaking the rice hull powder in an acid solution for 24-48 h, then repeatedly washing with distilled water until the pH value is unchanged, and drying for later use; 2) adding the rice hull powder treated in the step 1) into an iron salt solution, sealing, oscillating for 1-6 h, and performing suction filtration and cleaning; preferably, the oscillation time is 2-3 h; 3) drying the product obtained in the step 2), then placing the product in a tubular furnace, introducing nitrogen, and performing pyrolysis; the pyrolysis temperature is 400-1000 ℃, the holding time is 20-180 min, the heating rate is 5-20 ℃/min, and the pressure is 0.04 MPa. The method solves the problems of high cost, low yield and secondary pollution of wet liquid-phase reduction synthesis of nano-iron, and can avoid the risk of hydrogen use in the traditional dry reduction preparation; the material prepared by the invention has lasting and efficient repairing effect on heavy metal Cr (VI) polluted soil, can obviously reduce the bioavailability of heavy metals, and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of material synthesis, and particularly relates to a dry synthesis method of a rice hull biochar loaded nano-iron material.
Background
Cr exists in two valence states in natural environment, namely Cr (VI) and Cr (III), wherein the toxicity of Cr (VI) is 100-1000 times stronger than that of Cr (III), and the Cr (VI) has carcinogenicity and is an environment priority pollutant identified by the United states Environmental Protection Agency (EPA). Because Cr (VI) is not easily adsorbed by soil particles, has stronger mobility, and the pollution problem of hexavalent chromium is particularly severe in the soil with good permeability and lower organic matter content. In recent years, researches show that the nanoscale zero-valent iron has strong reducing capacity, can quickly reduce Cr (VI) into Cr (III), greatly reduces the toxicity and the mobility of Cr (VI), and simultaneously can realize the separation of a reduction product by utilizing ferromagnetism, thereby providing a potential new way for the in-situ repair of Cr (VI) polluted environment.
The nano-iron is zero-valent iron with the scale in the nano level, and the high reaction activity brought by the small-size effect enables the nano-iron to be widely applied in the field of environmental remediation. In recent years, nano-iron is mainly applied to low-oxygen environments such As degradation of chlorine-containing organic pollutants in groundwater, removal of inorganic metal ions (Cr, As, etc.), and the like. The synthesis of the nano-iron mainly comprises a physical method and a chemical method, wherein the most common method is the chemical method which uses borohydride as a reducing agent and reduces iron salt into the nano-iron by a wet method under the oxygen-free condition. However, the method for preparing nano-iron has high cost and low yield, and the use of borohydride and organic reagents easily causes environmental problems such as secondary pollution and the like, so that large-scale industrial production is difficult to realize. Reduction of a-FeOOH or a-Fe with hydrogen in conventional dry chemistry2O3The preparation of nano-iron, however, hydrogen is not easy to store and is easy to explode, so that the application of the method is limited. The nano iron prepared by the physical method is easy to agglomerate and has non-uniform shape, and although the large-scale production can be realized, the activity of the obtained nano iron is lower than that of the obtained nano iron prepared by the chemical method, and in addition, the physical method needs a specific reaction container and has high energy consumption. The nano iron synthesized by the method still has the advantages of easy oxidation,Easy agglomeration, difficult full contact with pollutants and the like, so that the utilization rate of the catalyst is greatly reduced. At present, many researches have been carried out to compound the nano-iron with other materials (such as carbon materials) to obtain relatively stable nano-iron composite materials, and the oxidation resistance of the nano-iron composite materials is improved while the high activity of the nano-iron composite materials is maintained, so that the high-efficiency repairing capability of the nano-iron composite materials on pollutants is fully exerted. However, the carbon material in such research often only plays a role in carrying iron and adsorbing and enriching pollutants, and the generation of nano iron still needs to be realized by a traditional wet method or a dry method.
Disclosure of Invention
In view of the above, the invention aims to provide a dry synthesis method of a rice hull biochar loaded nano-iron material, which is used for preparing the nano-iron material by synchronously reducing a product of a carbonization process while obtaining the biochar material with a soil improvement function by pyrolyzing rice hulls, and aims to provide a method for obtaining the biochar loaded nano-iron material by one-step heat treatment, so as to overcome the defects of the prior art and be used for repairing heavy metal contaminated soil.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a dry synthesis method of a rice hull biochar loaded nano-iron material comprises the following preparation steps:
1) soaking the rice hull powder in an acid solution for 24-48 h, then repeatedly washing with distilled water until the pH value is unchanged, and drying for later use;
2) adding the rice hull powder treated in the step 1) into an iron salt solution, sealing, oscillating for 1-6 h, and performing suction filtration and cleaning; preferably, the oscillation time is 2-3 h;
3) drying the product obtained in the step 2), then placing the product in a tubular furnace, introducing nitrogen, and performing pyrolysis; the pyrolysis temperature is 400-1000 ℃, the holding time is 20-180 min, the heating rate is 5-20 ℃/min, and the pressure is 0.0-0.05 MPa.
Preferably, in the step 1), the acid solution is a hydrochloric acid solution, and the concentration is 0.8-1.2 mol/L; adding 8-18 mL of acid solution into each gram of rice hull powder; the drying temperature is 80-120 ℃, and the drying time is 36-48 h.
Preferably, in step 2), the iron salt isFeCl3、Fe2(SO4)3Or Fe (NO)3)3One or more than two of the above, wherein the mass ratio of the rice hull powder to the iron salt is (3-6): (10-20).
Preferably, in the step 3), the drying temperature is 80-120 ℃, and the drying time is 8-16 h.
Preferably, in the step 3), the pyrolysis temperature is 600-1000 ℃, the holding time is 30-50 min, the heating rate is 5-8 ℃/min, and the pressure is 0.04 MPa.
The invention also provides the application of the rice hull biochar loaded nano-iron material synthesized by the dry synthesis method in the remediation of heavy metal contaminated soil.
The invention also provides application of the rice hull biochar loaded nano-iron material synthesized by the dry synthesis method in removing soil Cr (VI).
According to the invention, the biomass rice hulls are directly used as a reducing agent for carbothermic reduction, and the supported nano iron is obtained by high-temperature synthesis of biochar and in-situ carbon reduction, so that the problems of high cost, low yield and secondary pollution in wet liquid-phase reduction synthesis of nano iron are solved, and the risk of hydrogen use in the traditional dry reduction preparation can be avoided.
Compared with the prior art, the dry synthesis method of the rice hull biochar loaded nano iron material has the following advantages:
1) the biomass-rice hull is directly used as a carrier of ferric salt and a carbon source for carbothermic reduction, the formation of the biological carbon and the nano iron is combined into a whole, and the biological carbon nano iron composite material is obtained by a green, economic, simple and efficient method.
2) The rice hulls are wide in source and low in cost, and the problems of high cost, secondary pollution, safe operation and the like of the traditional synthetic method are solved; the composite material has the capabilities of reducing, magnetism, adsorption, fixation and regulation of soil physicochemical properties, and is a multifunctional material suitable for soil in-situ pollution remediation and improvement.
3) The rice hull biochar loaded nano-iron material obtained by efficiently utilizing biomass and obtaining the high-performance composite nano-material by a simple and low-consumption one-step synthesis method has good thermal stability, oxidation resistance and durable reaction activity, can efficiently reduce Cr (VI) in soil, reduce the toxicity and bioavailability of the Cr (VI), can realize the separation of degradation products from the soil through an external magnetic field, can exert the effect of biochar soil improvement, has a durable and efficient repair effect on the soil polluted by heavy metal Cr (VI), can obviously reduce the bioavailability of the heavy metal, and has wide application prospect.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is an SEM image of the material prepared at 800 ℃ ((a) is rice hull biochar material, and (b) is rice hull biochar loaded nano iron material).
FIG. 2 is an XRD (X-ray diffraction) diagram of rice hull biochar loaded nano iron materials at different preparation temperatures; wherein, 1: Fe3O4，2:Fe2O3，3:α-Fe。
FIG. 3 is a graph showing the effect of different amounts of the prepared material at 800 ℃ on the removal of Cr (VI) in soil (wherein (a) is rice hull biochar material, and (b) is rice hull biochar loaded nano-iron material).
FIG. 4 is a schematic diagram showing the change of Cr morphology before and after preparing a material for soil remediation at 800 ℃.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to examples.
Preparation of a rice hull biochar loaded nano-iron material:
weighing 50g of crushed rice hull powder, soaking in 600ml of hydrochloric acid solution for 48h, repeatedly washing with distilled water until the pH value is unchanged, and drying at 105 ℃ for 48 h. Weighing 10g of iron salt, adding 50ml of deionized water to prepare an iron salt solution, adding 5g of the rice hull powder, sealing, and oscillating for 2.5 h. Filtering, washing rice hull powder for many times, and drying at 105 deg.C for 12 hr.
And (3) pyrolyzing the rice hull powder impregnated with the ferric salt at different temperatures, introducing nitrogen after the tubular furnace is closed, keeping the pressure of the whole pyrolysis process at 0.04MPa for 30 minutes, taking out the sample after pyrolysis is finished, and collecting and storing the sample for later use.
Example 1:
and (3) after the tubular furnace is sealed, introducing nitrogen, keeping the pressure of 0.04MPa in the whole pyrolysis process, and pyrolyzing at 400 ℃ for 30 minutes.
Example 2:
and (3) after the tubular furnace is sealed, introducing nitrogen, keeping the pressure of 0.04MPa in the whole pyrolysis process, and pyrolyzing at 600 ℃ for 30 minutes.
Example 3:
and (3) after the tubular furnace is sealed, introducing nitrogen, and pyrolyzing at 800 ℃ for 30 minutes under the pressure of 0.04MPa in the whole pyrolysis process.
An SEM image of the obtained rice hull biochar loaded nano iron material is shown as a picture 1 (b).
Example 4:
and (3) after the tubular furnace is sealed, introducing nitrogen, and pyrolyzing at 1000 ℃ for 30 minutes under the pressure of 0.04MPa in the whole pyrolysis process.
Example 5:
and (3) after the tubular furnace is sealed, introducing nitrogen, and pyrolyzing at 1200 ℃ for 30 minutes under the pressure of 0.04MPa in the whole pyrolysis process.
Comparative example:
the rice hull powder is directly pyrolyzed without being soaked by iron salt. The pressure of the whole pyrolysis process is kept at 0.04MPa, and the pyrolysis is carried out at 800 ℃ for 30 minutes.
The prepared rice hull biochar loaded nano iron material has the following removal performance on Cr (VI):
soil remediation experiments (conducted in an air environment): 100ml of deionized water is measured and added into a conical flask containing 10g of polluted soil, the mixture is shaken up, then a certain amount of prepared samples are added, the mixture is oscillated in a water bath, and the samples are taken at certain time intervals, wherein the sampling amount is 1ml each time. After filtration through a 0.45 μm filter, the Cr (VI) concentration was measured spectrophotometrically, and the Cr (VI) removal rate was calculated.
The Cr (VI) polluted soil is repaired by using rice hull biochar loaded nano iron materials with different dosages, and the experimental results are shown in the attached figure 3 (4%, 8% and 12% shown in the figure refer to the weight ratio of the rice hull biochar loaded nano iron materials to the polluted soil). The rice hull biochar has no remarkable repairing effect on Cr (VI) polluted soil. And with the increase of the adding amount of the rice hull biochar loaded nano iron material, the removal rate of Cr (VI) in the soil leachate is continuously increased. The material can completely remove Cr (VI) in soil leachate in a short time when the material is added in an amount of 8% and 12%, and Cr (VI) is not found in a monitoring solution for 6 days continuously, which indicates that the material can continuously remove Cr seeped from the soil, and the long-term repair capability of the material on Cr (VI) polluted soil is proved.
After the material is prepared at 800 ℃ to repair the soil, the Cr content of each form is measured to obtain the distribution of Cr forms in the soil, as shown in figure 4. Heavy metals in soil are classified into a weak acid extraction state, a reducible state, an oxidizable state and a residue state according to the ease with which the heavy metals can be dissolved out, and if the heavy metals exist mainly in the weak acid extraction state, the heavy metals pose a great threat to the ecology. After the rice hull biochar and the rice hull biochar loaded nano iron material are repaired, the weak acid extraction state of Cr in soil completely disappears, which shows that the bioavailability of Cr is reduced through the repair. After the rice hull biochar is repaired, Cr in soil mainly exists in a residue state, accounting for 84.9 percent of the total amount, the content of a reducible state is basically kept unchanged (5.5 percent), and the content of an oxidizable state is increased (9.6 percent). After the rice hull biochar loaded nano iron material is repaired, the Cr residue state in soil accounts for 47.5%, the reducible state and the oxidizable state are respectively 24.6% and 27.9%, which are mainly due to the generation of Fe (III)/Cr (III) hydroxide in the process of reducing Cr (VI) by nano iron, so that the reducible, oxidizable and residual states of Cr are increased, and the bioavailability of the Cr is reduced.
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 (7)
1. A dry synthesis method of a rice hull biochar loaded nano-iron material is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
1) soaking the rice hull powder in an acid solution for 24-48 h, then repeatedly washing with distilled water until the pH value is unchanged, and drying for later use;
2) adding the rice hull powder treated in the step 1) into an iron salt solution, sealing, oscillating for 1-6 h, and performing suction filtration and cleaning; preferably, the oscillation time is 2-3 h;
3) drying the product obtained in the step 2), then placing the product in a tubular furnace, introducing nitrogen, and performing pyrolysis; the pyrolysis temperature is 400-1000 ℃, the holding time is 20-180 min, the heating rate is 5-20 ℃/min, and the pressure is 0.03-0.05 MPa.
2. The dry synthesis method of the rice hull biochar loaded nano-iron material according to claim 1, which is characterized in that: in the step 1), the acid solution is a hydrochloric acid solution, and the concentration is 0.8-1.2 mol/L; adding 8-18 mL of acid solution into each gram of rice hull powder; the drying temperature is 80-120 ℃, and the drying time is 36-48 h.
3. The dry synthesis method of the rice hull biochar loaded nano-iron material according to claim 1, which is characterized in that: in step 2), the ferric salt is FeCl3、Fe2(SO4)3Or Fe (NO)3)3One or more than two of the iron salts, wherein the mass ratio of the rice hull powder to the iron salt is (3-6) to (10-20).
4. The dry synthesis method of the rice hull biochar loaded nano-iron material according to claim 1, which is characterized in that: in the step 3), the drying temperature is 80-120 ℃, and the drying time is 8-16 h.
5. The dry synthesis method of the rice hull biochar loaded nano-iron material according to claim 1, which is characterized in that: in the step 3), the pyrolysis temperature is 600-1000 ℃, the holding time is 30-50 min, the heating rate is 5-8 ℃/min, and the pressure is 0.04 MPa.
6. The application of the rice hull biochar loaded nano-iron material synthesized by the dry synthesis method according to any one of claims 1-5 in heavy metal contaminated soil remediation.
7. The application of the rice hull biochar loaded nano-iron material synthesized by the dry synthesis method according to any one of claims 1-5 in removing soil Cr (VI).
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| CN113694883A (en) * | 2020-11-05 | 2021-11-26 | 核工业北京化工冶金研究院 | Preparation method of iron-loaded charcoal with poplar as carrier |
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| CN115337905A (en) * | 2022-08-19 | 2022-11-15 | 重庆大学 | Nano-iron modified biochar composite material and preparation method and application thereof |
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| CN113695588B (en) * | 2021-08-30 | 2023-12-26 | 炭索未来(广东)生态环境科技有限公司 | High-activity zero-valent iron composite material and preparation method and application thereof |
| CN113926845A (en) * | 2021-09-30 | 2022-01-14 | 中山大学 | Application of magnetic biochar-based iron carbide material in heavy metal contaminated soil remediation |
| CN114768761A (en) * | 2022-04-15 | 2022-07-22 | 广东省科学院生态环境与土壤研究所 | Preparation of biochar containing high-durability free radicals and application of biochar in removing heavy metals |
| CN115337905A (en) * | 2022-08-19 | 2022-11-15 | 重庆大学 | Nano-iron modified biochar composite material and preparation method and application thereof |
| CN115337905B (en) * | 2022-08-19 | 2023-09-19 | 重庆大学 | Nano-iron modified biochar composite material and preparation method and application thereof |
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