CN111036174B - Magnetic biochar based on iron-enriched plants and preparation method and application thereof - Google Patents
Magnetic biochar based on iron-enriched plants and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses magnetic biochar based on iron-enriched plants and a preparation method and application thereof. According to the invention, a large amount of iron is accumulated in the iron-enriched plant body, and typical iron-enriched plants such as cogongrass are subjected to high-temperature pyrolysis carbonization or hydrothermal carbonization to obtain the biochar; meanwhile, in the carbonization process, iron enriched in other forms in the plant body is converted into magnetic iron oxide, so that the obtained biochar is magnetic biochar, the magnetization and carbonization can be synchronously completed without additionally adding a magnetizing agent, the preparation process does not produce secondary pollution, and the operation is simple. The magnetic charcoal can effectively remove heavy metal pollutants in underground water, and has wide application prospect in the field of treatment of underground water heavy metal pollution.
Description
Technical Field
The invention belongs to the technical field of biochar, and particularly relates to magnetic biochar based on iron-enriched plants, and a preparation method and application thereof.
Background
Biochar is used as an environment-friendly material and is increasingly widely applied to the fields of waste recycling, soil quality regulation and control and environmental pollution remediation. In recent years, in order to overcome the defects of difficult recovery, difficult regeneration, small adsorption capacity and the like of biochar in the actual utilization process, the preparation and application of Magnetic biochar (Magnetic biochar) draw great attention.
The methods for preparing magnetic biochar are generally classified into the following:
(1) the biomass or the biochar is impregnated by utilizing magnetic endowing agents such as ferric salt and the like, and then the impregnated biomass or biochar is directly pyrolyzed to obtain the magnetic biochar. For example, Mubarak et al (Biomass and Bioenergy,2014,6, 265. sub. 275.) report treating FeCl using microwave pyrolysis (900W, 20 minutes)3The dipped palm oil empty fruit shells are used for preparing magnetic biochar and efficiently removing methylene blue in the water solution; reddy et al utilize Co2+And Fe3+Soaking pine bark biomass (Colloids and Surfaces A,2014,454,96-103.) in the solution, then performing pyrolysis to obtain magnetic biochar, and applying the magnetic biochar to adsorption of lead and cadmium in aqueous solution; wang et al (RSC adv.,2015,5,67971-67978) utilize Mn2+And Fe3+Pine biomass is impregnated and then pyrolyzed to obtain magnetic biochar. Yan et al (ACS Sustainable Chemistry)&Engineering,2015,3(1),125-132.) rice hull charcoal was impregnated with iron acetylacetonate and further pyrolyzed to obtain magnetic charcoal. Chinese patent (201811621104.9) uses ferric chloride solution to impregnate peanut shell biomass, and then pyrolyzes to obtain magnetic biochar. In the Chinese patent (201910064397.3), the mixed solution of straw-based biochar and iron acetylacetonate is placed in a hydrothermal reaction kettle and subjected to hydrothermal treatment to obtain the magnetic biochar.
(2) Directly mixing iron-containing minerals or zero-valent iron with biomass or biochar, and carrying out pyrolysis or drying to prepare the magnetic biochar. For example, Wang et al (Bioresource Technology,2015,175, 391-395) utilize natural α -Fe2O3Mixed with pine biomass, and subjected to electric furnace pyrolysis at 600 ℃ for 1 hour to successfully prepare magnetic biochar and apply to adsorb As (V) in water. Chinese patent (201811622260.7) uses nitric acid to modify peanut shell biochar and nano Fe3O4Mixing, adding ethanol, stirring, and freeze drying to obtain magnetic biochar. Devi et al (Bioresource Technology,2014,169,525-531.) and Chandraiah (Alexandria Engineering Journal,2016,55,619-625.) reported the use of Fe2+And Fe3+Reducing the magnetic carbon into zero-valent iron, combining the zero-valent iron on the surface of the biochar, and drying to obtain the magnetic biochar. Chinese patent (201810855860.1) mixes the sludge with zero-valent iron and persulfate, and then carries out high-temperature pyrolysis to obtain the magnetic sludge biochar. Chinese patent (201810692857.2) magnetic Fe coating a single layer of silica3O4Mixing the nano powder with chicken manure biochar, bentonite, poplar powder and hexadecyl trimethyl ammonium bromide to obtain a suspension, mixing the suspension with polyvinyl alcohol, and drying to obtain the magnetic biochar.
(3) The magnetic biochar is prepared by utilizing coprecipitation reaction, namely, under the existence of biomass or biochar, adding magnetism-imparting agents such as ferric salt and the like, simultaneously adjusting the solution to be alkaline to perform precipitation reaction, and further drying or pyrolyzing the solution to obtain the magnetic biochar. For example, Chen et al (Bioresource Technology,2011,102,716-3+And Fe2+Mixing the solution with orange peel biomass, adjusting to alkalinity to perform precipitation reaction, and further performing pyrolysis to obtain magnetic biochar; zhang et al (Environmental Pollution,2016,216,575-3+And Fe2+Mixing the solutions, adding a strong base solution to perform a precipitation reaction, and further performing pyrolysis to obtain magnetic biochar; similarly, Mohan et al (Chemical Engineering Journal,2014,236,513-2+And Fe3+Mixing the solution with biochar, adding sodium hydroxide to perform coprecipitation reaction, and drying a product to obtain magnetic biochar; zhang et al (Water Science and Technology,2016,74(8):1971-2+And Fe3+Mixing the solution and the biochar under an alkaline condition to perform coprecipitation reaction, and sintering the product at 800 ℃ to obtain magnetic biochar; lai et al (Chemosphere,2019,224,910-2+And Fe3+And mixing the solution with the biochar, adding ammonia water to perform coprecipitation reaction, and drying to obtain the magnetic biochar. Chinese patent (ZL201611024652.4) Fe with pH value of 11-123+And Fe2+Adding plant straw biomass into the mixed solution, stirring, standing to obtain solid, and mixing with calcium carbonate powderMixing, and carrying out anoxic pyrolysis to obtain the magnetic biochar. Chinese patent (201711449364.8) is Fe3+And Fe2+And mixing the solution and the pig manure biochar, adjusting the pH value to 10-11, continuously stirring and boiling the solution, and drying the obtained solid to obtain the magnetic pig manure biochar. Chinese patent (201710303621.0) uses Chinese medicine residue powder treated by sodium carbonate to mix with ferric salt solution, adjusts pH to 10-11, and the solid is pyrolyzed to obtain magnetic biochar. Chinese patent (201711363407.0) is Fe3+And Fe2+Mixing the solution with steam activated biomass charcoal, and adding alkali liquor to generate Fe3O4The magnetic biochar is obtained by loading the magnetic biochar on the surface of the biochar. Chinese patent (201810657102.9) mixing sulfuric acid treated oil tea shell biochar with Fe3+And Fe2+And mixing the solutions, adding urea to adjust the pH value to 10-12, and drying the solid after reaction to obtain the magnetic biochar. Chinese patent (201910058205.8) is Fe3+And Fe2+And mixing the solution with the mulberry tree stalk biochar treated by hydrochloric acid, adding strong base for coprecipitation reaction, and drying the product to obtain the magnetic biochar adsorbent. Chinese patent (201910230934.7) disperses spirulina into ferric nitrate solution, and adds sodium hydroxide solution to generate precipitation reaction, then further pyrolyzes and carbonizes to obtain magnetic charcoal.
The common characteristic of the preparation methods is that exogenous magnetism-imparting substances are required to be added. For example, iron salt, cobalt salt, etc. are added to form ferrite or Fe3O4Or gamma-Fe2O3Adding iron-containing mineral (such as hematite) to convert into magnetic material, or directly adding magnetic material such as zero-valent iron and Fe3O4Or gamma-Fe2O3And the like. However, the above method has disadvantages that the preparation process is complicated and the cost is increased due to the additional introduction of the magnetic-endowing agent, and a few toxic chemical reagents are used in the preparation process, which may cause secondary pollution.
Recently, Chinese patent (ZL201710389611.3) uses excess sludge in urban sewage treatment plants as raw materials, and obtains magnetic sludge biochar by direct high-temperature (400-900 ℃) pyrolysis and carbonization. Because the polyferric sulfate is added into the sewage treatment plant in the flocculation dehydration process, the residual sludge does not need to be added with a magnetizing agent, and the magnetic sludge biochar can be formed through pyrolysis. Chinese patent (201910004100.4) utilizes sludge from sewage treatment plant (containing ferric salt flocculant) to directly pyrolyze and carbonize at high temperature (680-900 ℃) to obtain magnetic sludge biochar, and the magnetic sludge biochar is used for adsorbing fluoroquinolone antibiotics such as ciprofloxacin in water. In the patent, the magnetism-imparting agent is an iron-containing flocculating agent artificially added in the early stage, is retained in the sludge, and pyrolyzes the sludge to obtain the magnetic sludge biochar. Since the sludge itself contains some toxic and harmful substances, the obtained magnetic sludge biochar may contain harmful substances, which limits the practical application thereof. In contrast, biomass resources are very rich, biomass pyrolysis preparation of biochar is beneficial to resource utilization of biomass, and further application of the obtained biochar does not bring secondary risks, so that biomass pyrolysis preparation of biochar is a widely accepted biochar preparation method.
The iron-rich plant is a plant which is commonly found in nature, and typical iron-rich plants include cogongrass rhizome, bermuda grass and the like. The use of jarosite [ KFe ] in vivo has been reported in the literature for Imperata cylindrical3(SO4)2(OH)6]Iron is accumulated in large quantities in the form of ferrihydrite, hematite, ferritin, etc., and the iron content in the rhizome and leaves can reach 23450mg/kg dry weight and 10663mg/kg dry weight, respectively (New Photologist, 2005,165, 781-. Another iron-rich Plant, Bermuda grass (Journal of Plant Nutrition and Soil Science,2013,176,836-842.) has iron contents in its root system, root-like stem and leaves of 63972mg/kg, 1603mg/kg and 3111mg/kg dry weight. However, the preparation of magnetic biochar by direct pyrolysis of iron-enriched plants has not been reported.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the defect that an additional magnetizing agent is needed in the preparation of the magnetic biochar in the prior art, the invention provides the magnetic biochar based on the iron-enriched plant.
The invention also provides a preparation method and application of the magnetic biochar based on the iron-enriched plants.
The technical scheme is as follows: in order to achieve the above object, the present invention provides a magnetic charcoal based on iron-enriched plants, which is characterized in that the magnetic charcoal is obtained by directly subjecting the iron-enriched plants to pyrolysis carbonization or hydrothermal carbonization.
In the process, other forms of iron enriched in the plant body are converted into magnetic iron oxide, and the magnetization and carbonization can be synchronously completed at high temperature without adding an additional magnetizing agent, so that the magnetic biochar is prepared.
Wherein the iron-enriched plant comprises one or more of natural iron-enriched plants or plants artificially induced to have iron-enrichment capacity.
Preferably, the natural iron-rich plant is Imperata cylindrical (L.) P.Beauv.) or Cynodon dactylon (L.) Pers.) and the artificially induced plant having iron-rich ability is Eichhornia crassipes (Mart.) Solms).
The preparation method of the magnetic biochar based on the iron-enriched plants comprises the following steps:
(1) washing the iron-enriched plant with deionized water, naturally drying at room temperature, drying in an oven at 50-105 deg.C for 12-24 hr, pulverizing, and sieving with 50-100 mesh sieve to obtain biomass powder of the iron-enriched plant;
(2) and (2) putting the biomass powder prepared in the step (1) into a carbonization device, carbonizing in a nitrogen atmosphere, cooling to room temperature, taking out, washing and drying to obtain the magnetic biochar.
Preferably, step (1) is dried at 80 ℃ for 15 hours, crushed and sieved through an 80 mesh sieve.
Preferably, the carbonization device in the step (2) is an electric furnace high-temperature pyrolysis carbonization device, the pyrolysis temperature is 300-. The pyrolysis is generally carried out at 500 ℃, the heating rate is 10 ℃/min, and the pyrolysis time is 3 hours for magnetization and carbonization.
As another preferred mode, the carbonizing device in the step (2) is a microwave pyrolysis carbonizing device, the power of microwave pyrolysis carbonization is 600- & gt 1800W, and the pyrolysis time is 5-40 minutes. The magnetization and carbonization are generally carried out at a power of 800W for a pyrolysis time of 30 minutes.
As another optimization, the carbonization device in the step (2) is a hydrothermal carbonization device, the hydrothermal reaction temperature is 200-450 ℃, the hydrothermal reaction time is 30-300 minutes, and the pressure is 4-5 MPa. Generally, the hydrothermal reaction temperature is 300 ℃, the hydrothermal reaction time is 40 minutes, and the pressure is 4.5MPa for magnetization and carbonization.
Preferably, the washing in the step (2) is performed by sequentially adopting deionized water and absolute ethyl alcohol, and the drying temperature is 50-80 ℃. Drying at 60 deg.C.
The invention relates to application of magnetic biochar based on iron-enriched plants in adsorption of heavy metal ions of lead and cadmium in underground water.
The magnetic biochar based on the iron-enriched plants is used in underground water with lead concentration not more than 600mg/L, or hexavalent chromium concentration not more than 500mg/L, or cadmium ion concentration not more than 100mg/L, and the dosage of the magnetic biochar is 0.5-5.0 g/L.
According to the invention, a large amount of iron is accumulated in the iron-enriched plant, and typical iron-enriched plants such as cogongrass are subjected to high-temperature pyrolysis carbonization or hydrothermal carbonization to obtain charcoal; meanwhile, in the carbonization process, iron enriched in other forms in the plant body is converted into magnetic iron oxide, so that the obtained biochar is magnetic biochar, and the magnetization and carbonization can be synchronously completed without additionally adding a magnetizing agent.
The invention directly utilizes iron-enriched plants as biomass, and directly pyrolyzes to realize the synchronous carbonization and magnetization processes without adding magnetizing agents such as ferric salt and the like, thereby obtaining the magnetic biochar. The main principle of the process is as follows: a large amount of iron is accumulated in the iron-enriched plant body in the forms of jarosite, ferrihydrite, hematite, ferritin and the like, and the iron in the forms can be generated in the biomass pyrolysis processCan be converted into magnetic substance such as ferrite, Fe3O4γ-Fe2O3Etc., thus making the obtained charcoal magnetic. When the obtained magnetic biochar is applied to underground water with lead and cadmium concentrations not more than 600mg/L under the condition of the dosage of 0.5-5.0g/L, the adsorption capacity of the magnetic biochar on lead and cadmium pollutants in the underground water can reach 370mg/g and 152mg/g respectively.
Has the advantages that: compared with the prior art, the invention has the following advantages:
(1) the iron-enriched plant used in the invention is a plant commonly existing in the nature, has rich resources, is cheap and easily available, does not contain additional toxic and harmful substances except iron, and compared with other reported sludge and livestock and poultry manure, the iron-enriched plant used as biomass for preparing the magnetic biochar does not bring the risk of secondary pollution in the preparation and application processes.
(2) According to the method, the magnetic biochar can be obtained through direct high-temperature pyrolysis, microwave pyrolysis or hydrothermal pyrolysis carbonization processes without additionally adding a magnetizing agent such as ferric salt and reagents such as strong alkali.
(3) The biochar prepared by the iron-enriched plant shows good application prospect in the field of adsorption of lead and cadmium pollutants in underground water.
Detailed Description
For a better understanding of the present invention, the following examples are included to further illustrate the present invention, but the present invention is not limited to the following examples.
Example 1
Collecting iron-enriched plant cogongrass from the field, washing with deionized water, naturally drying at room temperature, drying in an oven at 50 ℃ for 15 hours, crushing, and sieving with a 80-mesh sieve to obtain biomass powder of the iron-enriched plant. And (2) putting the biomass powder into an electric furnace high-temperature pyrolysis carbonization device, performing high-temperature pyrolysis carbonization in nitrogen atmosphere at the pyrolysis temperature of 500 ℃, at the heating rate of 10 ℃/min for 3 hours, cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
Example 2
Collecting iron-enriched plant imperata from the wild, cleaning with deionized water, naturally drying at room temperature, drying in an oven at 105 ℃ for 15 hours, crushing, and sieving with a 80-mesh sieve to obtain the biomass powder of the iron-enriched plant. And (2) putting the biomass powder into an electric furnace high-temperature pyrolysis carbonization device, performing high-temperature pyrolysis carbonization in nitrogen atmosphere at the pyrolysis temperature of 500 ℃, at the heating rate of 10 ℃/min for 3 hours, cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 50 ℃ to obtain the magnetic biochar.
Example 3
Collecting iron-enriched plant imperata from the wild, cleaning with deionized water, naturally drying at room temperature, drying in an oven at 80 ℃ for 12 hours, crushing, and sieving with a 80-mesh sieve to obtain the biomass powder of the iron-enriched plant. And (2) putting the biomass powder into an electric furnace high-temperature pyrolysis carbonization device, performing high-temperature pyrolysis carbonization in nitrogen atmosphere at the pyrolysis temperature of 500 ℃, at the heating rate of 10 ℃/min for 3 hours, cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 80 ℃ to obtain the magnetic biochar.
Example 4
Collecting iron-enriched plant cogongrass from the field, cleaning with deionized water, naturally air-drying at room temperature, drying in an oven at 80 ℃ for 24 hours, crushing, and sieving with a 80-mesh sieve to obtain biomass powder of the iron-enriched plant. And (2) putting the biomass powder into an electric furnace high-temperature pyrolysis carbonization device, performing high-temperature pyrolysis carbonization in nitrogen atmosphere at the pyrolysis temperature of 500 ℃, at the heating rate of 10 ℃/min for 3 hours, cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
Example 5
Collecting iron-enriched plant cogongrass from the field, cleaning with deionized water, naturally air-drying at room temperature, drying in an oven at 80 ℃ for 15 hours, crushing, and sieving with a 50-mesh sieve to obtain biomass powder of the iron-enriched plant. And (2) putting the biomass powder into an electric furnace high-temperature pyrolysis carbonization device, performing high-temperature pyrolysis carbonization in nitrogen atmosphere at the pyrolysis temperature of 500 ℃, at the heating rate of 10 ℃/min for 3 hours, cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 80 ℃ to obtain the magnetic biochar.
Example 6
Collecting iron-enriched plant cogongrass from the field, cleaning with deionized water, naturally air-drying at room temperature, drying in an oven at 80 ℃ for 15 hours, crushing, and sieving with a 100-mesh sieve to obtain biomass powder of the iron-enriched plant. And (2) putting the biomass powder into an electric furnace high-temperature pyrolysis carbonization device, performing high-temperature pyrolysis carbonization in nitrogen atmosphere at the pyrolysis temperature of 500 ℃, at the heating rate of 10 ℃/min for 3 hours, cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 70 ℃ to obtain the magnetic biochar.
Example 7
Collecting iron-enriched plant cogongrass from the field, cleaning with deionized water, naturally air-drying at room temperature, drying in an oven at 80 ℃ for 15 hours, crushing, and sieving with a 80-mesh sieve to obtain biomass powder of the iron-enriched plant. And (2) putting the biomass powder into an electric furnace high-temperature pyrolysis carbonization device, performing high-temperature pyrolysis carbonization in nitrogen atmosphere at the pyrolysis temperature of 500 ℃, at the heating rate of 15 ℃/min for 1 hour, cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
Example 8
Collecting iron-enriched plant cogongrass from the field, cleaning with deionized water, naturally air-drying at room temperature, drying in an oven at 80 ℃ for 15 hours, crushing, and sieving with a 80-mesh sieve to obtain biomass powder of the iron-enriched plant. And (2) putting the biomass powder into an electric furnace high-temperature pyrolysis carbonization device, performing high-temperature pyrolysis carbonization in nitrogen atmosphere at the pyrolysis temperature of 500 ℃, at the heating rate of 5 ℃/min for 4 hours, cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
Example 9
Collecting iron-enriched plant imperata from the wild, cleaning with deionized water, naturally drying at room temperature, drying in an oven at 80 ℃ for 15 hours, crushing, and sieving with a 80-mesh sieve to obtain the biomass powder of the iron-enriched plant. And (2) putting the biomass powder into an electric furnace high-temperature pyrolysis carbonization device, performing high-temperature pyrolysis carbonization in nitrogen atmosphere at the pyrolysis temperature of 300 ℃, at the heating rate of 10 ℃/min for 3 hours, cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
Example 10
Collecting iron-enriched plant cogongrass from the field, cleaning with deionized water, naturally air-drying at room temperature, drying in an oven at 80 ℃ for 15 hours, crushing, and sieving with a 80-mesh sieve to obtain biomass powder of the iron-enriched plant. And (2) putting the biomass powder into an electric furnace high-temperature pyrolysis carbonization device, performing high-temperature pyrolysis carbonization in nitrogen atmosphere at the pyrolysis temperature of 700 ℃, at the heating rate of 10 ℃/min for 3 hours, cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol sequentially, and drying at 60 ℃ to obtain the magnetic biochar.
Example 11
Collecting iron-enriched plant cogongrass from the field, cleaning with deionized water, naturally air-drying at room temperature, drying in an oven at 80 ℃ for 15 hours, crushing, and sieving with a 80-mesh sieve to obtain biomass powder of the iron-enriched plant. And (2) putting the biomass powder into a microwave pyrolysis carbonization device, performing microwave pyrolysis carbonization in a nitrogen atmosphere with the microwave power of 600W for 30 minutes, cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
Example 12
Collecting iron-enriched plant cogongrass from the field, cleaning with deionized water, naturally air-drying at room temperature, drying in an oven at 80 ℃ for 15 hours, crushing, and sieving with a 80-mesh sieve to obtain biomass powder of the iron-enriched plant. And (2) putting the biomass powder into a microwave pyrolysis carbonization device, performing microwave pyrolysis carbonization in a nitrogen atmosphere with the microwave power of 1800W for 30 minutes, cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
Example 13
Collecting iron-enriched plant cogongrass from the field, cleaning with deionized water, naturally air-drying at room temperature, drying in an oven at 80 ℃ for 15 hours, crushing, and sieving with a 80-mesh sieve to obtain biomass powder of the iron-enriched plant. And (2) putting the biomass powder into a microwave pyrolysis carbonization device, performing microwave pyrolysis carbonization in a nitrogen atmosphere with the microwave power of 800W for 5 minutes, cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
Example 14
Collecting iron-enriched plant cogongrass from the field, cleaning with deionized water, naturally air-drying at room temperature, drying in an oven at 80 ℃ for 15 hours, crushing, and sieving with a 80-mesh sieve to obtain biomass powder of the iron-enriched plant. And (2) putting the biomass powder into a microwave pyrolysis carbonization device, performing microwave pyrolysis carbonization in a nitrogen atmosphere with the microwave power of 800W for 40 minutes, cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
Example 15
Collecting iron-enriched plant cogongrass from the field, cleaning with deionized water, naturally air-drying at room temperature, drying in an oven at 80 ℃ for 15 hours, crushing, and sieving with a 80-mesh sieve to obtain biomass powder of the iron-enriched plant. And (3) putting the biomass powder into a hydrothermal carbonization device, and carrying out hydrothermal carbonization in a nitrogen atmosphere, wherein the hydrothermal reaction temperature is 200 ℃, the hydrothermal reaction time is 40 minutes, and the pressure is 4.5 MPa. And then cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
Example 16
Collecting iron-enriched plant cogongrass from the field, cleaning with deionized water, naturally air-drying at room temperature, drying in an oven at 80 ℃ for 15 hours, crushing, and sieving with a 80-mesh sieve to obtain biomass powder of the iron-enriched plant. And (3) putting the biomass powder into a hydrothermal carbonization device, and carrying out hydrothermal carbonization in a nitrogen atmosphere, wherein the hydrothermal reaction temperature is 450 ℃, the hydrothermal reaction time is 40 minutes, and the pressure is 4.5 MPa. And then cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
Example 17
Collecting iron-enriched plant cogongrass from the field, cleaning with deionized water, naturally air-drying at room temperature, drying in an oven at 80 ℃ for 15 hours, crushing, and sieving with a 80-mesh sieve to obtain biomass powder of the iron-enriched plant. And (3) putting the biomass powder into a hydrothermal carbonization device, and carrying out hydrothermal carbonization in a nitrogen atmosphere, wherein the hydrothermal reaction temperature is 300 ℃, the hydrothermal reaction time is 30 minutes, and the pressure is 4.5 MPa. And then cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
Example 18
Collecting iron-enriched plant cogongrass from the field, cleaning with deionized water, naturally air-drying at room temperature, drying in an oven at 80 ℃ for 15 hours, crushing, and sieving with a 80-mesh sieve to obtain biomass powder of the iron-enriched plant. And (3) putting the biomass powder into a hydrothermal carbonization device, and carrying out hydrothermal carbonization in a nitrogen atmosphere, wherein the hydrothermal reaction temperature is 300 ℃, the hydrothermal reaction time is 300 minutes, and the pressure is 4.5 MPa. And then cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
Example 19
Collecting iron-enriched plant cogongrass from the field, cleaning with deionized water, naturally air-drying at room temperature, drying in an oven at 80 ℃ for 15 hours, crushing, and sieving with a 80-mesh sieve to obtain biomass powder of the iron-enriched plant. And (3) putting the biomass powder into a hydrothermal carbonization device, and carrying out hydrothermal carbonization in a nitrogen atmosphere, wherein the hydrothermal reaction temperature is 300 ℃, the hydrothermal reaction time is 40 minutes, and the pressure is 4 MPa. And then cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
Example 20
Collecting iron-enriched plant cogongrass from the field, cleaning with deionized water, naturally air-drying at room temperature, drying in an oven at 80 ℃ for 15 hours, crushing, and sieving with a 80-mesh sieve to obtain biomass powder of the iron-enriched plant. And (3) putting the biomass powder into a hydrothermal carbonization device, and carrying out hydrothermal carbonization in a nitrogen atmosphere, wherein the hydrothermal reaction temperature is 300 ℃, the hydrothermal reaction time is 40 minutes, and the pressure is 5 MPa. And then cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
Example 21
Collecting iron-enriched plant Bermuda grass from the field, washing with deionized water, naturally drying at room temperature, drying in an oven at 80 deg.C for 15 hr, pulverizing, and sieving with 80 mesh sieve to obtain biomass powder of iron-enriched plant. And (2) putting the biomass powder into an electric furnace high-temperature pyrolysis carbonization device, performing high-temperature pyrolysis carbonization in nitrogen atmosphere at the pyrolysis temperature of 500 ℃, at the heating rate of 10 ℃/min for 3 hours, cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
Example 22
Collecting iron-enriched plants, namely the cogongrass and the bermuda grass, from the field, mixing the collected iron-enriched plants and the cogongrass in any proportion, cleaning the mixture by using deionized water, naturally drying the mixture at room temperature, drying the mixture in an oven for 15 hours at 80 ℃, crushing the dried mixture, and sieving the crushed mixture by using a 80-mesh sieve to obtain biomass powder of the iron-enriched plants. And (2) putting the biomass powder into an electric furnace high-temperature pyrolysis carbonization device, performing high-temperature pyrolysis carbonization in nitrogen atmosphere at the pyrolysis temperature of 500 ℃, at the heating rate of 10 ℃/min for 3 hours, cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
Example 23
Collecting iron-enriched plant cogongrass from the field, cleaning with deionized water, naturally air-drying at room temperature, drying in an oven at 80 ℃ for 15 hours, crushing, and sieving with a 80-mesh sieve to obtain biomass powder of the iron-enriched plant. And (2) putting the biomass powder into an electric furnace high-temperature pyrolysis carbonization device, performing high-temperature pyrolysis carbonization in nitrogen atmosphere at the pyrolysis temperature of 500 ℃, at the heating rate of 10 ℃/min for 3 hours, cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
Example 24
According to literature methods [ AUJ.Technol.2002, 6, 55-60; trends appl.sci.res, 2014,9,485-493 ] collect iron-enriched eichhornia crassipes biomass, wash with deionized water, naturally air-dry at room temperature, dry in an oven at 80 ℃ for 15 hours, pulverize and pass through a 80-mesh sieve to obtain biomass powder of iron-enriched plants. And (2) putting the biomass powder into an electric furnace high-temperature pyrolysis carbonization device, performing high-temperature pyrolysis carbonization in nitrogen atmosphere at the pyrolysis temperature of 500 ℃, at the heating rate of 10 ℃/min for 3 hours, cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
Test examples
The magnetic biochar obtained in example 23 was added to filtered groundwater containing lead ions, cadmium ions, and both lead ions and cadmium ions at a ratio of 0.5 to 5.0g/L, and the mixture was subjected to shaking adsorption for 8 hours, and after adsorption, the magnetic biochar was subjected to solid-liquid separation with strong magnet from water, thereby removing heavy metals of lead and cadmium from groundwater.
1. In the underground water containing lead ions, the adsorption amount of the magnetic biochar to the lead ions is as follows:
according to the using amount of the magnetic biochar of 0.5g/L, the removal rate of underground water with the lead ion concentration of 600mg/L can reach 80% when the pH value is 5.0;
according to the using amount of the magnetic biochar of 5.0g/L, the removal rate of the magnetic biochar in underground water with lead ion concentration of 600mg/L can reach 94% when the pH value is 5.0;
according to the using amount of the magnetic biochar of 0.5g/L, the removal rate of underground water with lead ion concentration of 600mg/L can reach 88% when the pH value is 7.0;
according to the using amount of the magnetic biochar of 5.0g/L, the removal rate can reach 97% in underground water with lead ion concentration of 600mg/L at pH7.0;
according to the using amount of the magnetic biochar of 0.5g/L, the removal rate of the magnetic biochar in underground water with the lead ion concentration of 600mg/L can reach 95% when the pH value is 9.0;
according to the using amount of the magnetic biochar of 5.0g/L, the removal rate can reach 100% in underground water with lead ion concentration of 600mg/L at pH9.0;
2. in the hexavalent chromium-containing underground water, the adsorption capacity of the magnetic biochar to lead ions is as follows:
according to the using amount of the magnetic biochar of 0.5g/L, the removal rate of the magnetic biochar in the groundwater with the chromium (VI) concentration of 500mg/L can reach 82 percent when the pH value is 5.0;
according to the using amount of the magnetic biochar of 5.0g/L, the removal rate of the magnetic biochar in the groundwater with the chromium (VI) concentration of 500mg/L can reach 90 percent when the pH value is 5.0;
according to the using amount of the magnetic biochar of 0.5g/L, the removal rate of the magnetic biochar in the groundwater with the chromium (VI) concentration of 500mg/L can reach 78 percent when the pH value is 7.0;
according to the using amount of the magnetic biochar of 5.0g/L, the removal rate of the magnetic biochar in the groundwater with the chromium (VI) concentration of 500mg/L can reach 85 percent when the pH value is 7.0;
according to the using amount of the magnetic biochar of 0.5g/L, the removal rate of the magnetic biochar in the groundwater with the chromium (VI) concentration of 500mg/L can reach 68 percent when the pH value is 9.0;
according to the using amount of the magnetic biochar of 5.0g/L, the removal rate of the magnetic biochar in the groundwater with the chromium (VI) concentration of 500mg/L can reach 76 percent when the pH value is 9.0;
3. in the underground water containing cadmium ions, the adsorption capacity of the magnetic biochar to lead ions is as follows:
according to the using amount of the magnetic biochar of 0.5g/L, the removal rate of the magnetic biochar in the groundwater with the cadmium ion concentration of 100mg/L can reach 75% when the pH value is 5.0;
according to the using amount of the magnetic biochar of 5.0g/L, the removal rate of the magnetic biochar in the groundwater with the cadmium ion concentration of 100mg/L can reach 79 percent when the pH value is 5.0;
according to the using amount of the magnetic biochar of 0.5g/L, the removal rate of the magnetic biochar in the groundwater with the cadmium ion concentration of 100mg/L can reach 82% when the pH value is 7.0;
according to the using amount of the magnetic biochar of 5.0g/L, the removal rate of the magnetic biochar in the groundwater with the cadmium ion concentration of 100mg/L can reach 88 percent when the pH value is 7.0;
according to the using amount of the magnetic biochar of 0.5g/L, the removal rate of the magnetic biochar in the groundwater with the cadmium ion concentration of 100mg/L can reach 93 percent when the pH value is 9.0;
according to the use amount of the magnetic biochar of 5.0g/L, the removal rate of the underground water with the cadmium ion concentration of 100mg/L can reach 100% when the pH value is 9.0.
Other examples the magnetic biochar prepared in the above examples substantially agreed with the effects of example 23.
Claims (1)
1. The application of the magnetic biochar based on the iron-enriched plant in adsorbing heavy metal ions of lead, chromium and cadmium in underground water is characterized in that the iron-enriched plant is directly pyrolyzed and carbonized at high temperature to obtain the magnetic biochar; the iron-rich plant is a natural iron-rich plant cogongrass;
the application process comprises the following steps: adding magnetic biochar into filtered underground water containing lead ions, cadmium ions and chromium ions according to the proportion of 5.0g/L, carrying out oscillation adsorption for 8 hours, and carrying out solid-liquid separation on the magnetic biochar and the water by using strong magnet after adsorption; the dosage of the magnetic biochar based on the iron-enriched plant is 5.0g/L, the pH value is 9.0, and the lead concentration is 600 mg/L; the dosage of the magnetic biochar based on the iron-enriched plant is 5.0g/L, the pH value is 5.0, and the concentration of hexavalent chromium is 500 mg/L; the dosage of the magnetic biochar based on the iron-enriched plant is 5.0g/L, the pH value is 9.0, and the concentration of cadmium ions is 100 mg/L;
the preparation method of the magnetic biochar based on the iron-enriched plants comprises the following steps:
collecting iron-enriched plant cogongrass from the field, cleaning with deionized water, naturally drying at room temperature, drying in an oven at 80 ℃ for 15 hours, crushing, and sieving with a 80-mesh sieve to obtain biomass powder of the iron-enriched plant; and (2) putting the biomass powder into an electric furnace high-temperature pyrolysis carbonization device, performing high-temperature pyrolysis carbonization in nitrogen atmosphere at the pyrolysis temperature of 500 ℃, at the heating rate of 10 ℃/min for 3 hours, cooling to room temperature, taking out, washing with deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ to obtain the magnetic biochar.
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