CN115041136A - Preparation method and application of aquatic plant-based magnesium modified carbon material - Google Patents
Preparation method and application of aquatic plant-based magnesium modified carbon material Download PDFInfo
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- C02F1/00—Treatment of water, waste water, or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention provides a preparation method and application of an aquatic plant-based magnesium modified carbon material. The method for preparing the magnesium modified carbon material for the aquatic plants in one step through magnesium impregnation-high-temperature micro-oxygen roasting has the characteristics of simple process, low cost, good effect and the like, can provide a resource direction for the treatment of solid waste of water hyacinth, is simple in integral operation, low in cost, green and environment-friendly, and has environmental and economic benefits.
Description
Technical Field
The invention relates to the technical field of waste resource utilization, relates to a preparation method and application of a magnesium modified carbon material based on aquatic plants, and particularly relates to a method for simply preparing a novel magnesium modified carbon material in a micro-aerobic environment by using aquatic plant wastes as main raw materials.
Background
With the rapid development of industry and agriculture, a large amount of pollutants are generated in the environment, and enter the water body in large amount to cause serious water body pollution and harm the ecological environment and human health, wherein heavy metals, nitrogen and phosphorus are the most main pollutants. Eichhornia crassipes, also known as water hyacinth, is a perennial aquatic floating plant and is one of the main invasive species in China. The water channel can be blocked in the breeding season, the traffic is influenced, a large amount of dissolved oxygen in water can be consumed, the activity breeding space of underwater animals is reduced, and a large amount of fishes die. The water hyacinth is generally treated by fishing, but how to treat a large amount of fished water hyacinth becomes a troublesome problem.
With the construction of cities, the development of economy and the increase of population, most of the urban rivers are seriously polluted. The pollution is mostly caused by three wastes discharged from factories along the river bank or domestic sewage and garbage discharged from cities and towns, and the poor and simple treatment facilities and the lack of related management cause a large amount of waste water and waste containing heavy metal pollution to be discharged into the river. Heavy metal and nitrogen and phosphorus pollution are the most serious problem of water body pollution at present, and different physical and chemical methods such as adsorption, chemical precipitation, ion exchange, electrochemical treatment, membrane filtration and the like are generally adopted to treat the water body pollution. The adsorption method is considered to be one of the most effective methods for removing water pollution due to its simple operation, wide material sources, and economy.
Chinese patent with application number CN201810717424.8 discloses a preparation method of magnesium salt modified biochar, which comprises the steps of crushing agricultural and forestry waste into particles with the particle size of less than 5mm, soaking the particles in 0.2-2mol/L sodium hydroxide for 8-24h, washing the particles to be neutral by distilled water, and drying the particles at 105 ℃; then dipping the mixture in magnesium chloride solution for 12 to 14 hours, carrying out ultrasonic treatment, and drying the mixture at the temperature of between 80 and 105 ℃; cracking the mixture in a nitrogen atmosphere to obtain the magnesium salt modified biochar.
Chinese patent application No. CN201710562639.2 discloses a preparation method of magnesium-loaded biochar, which comprises the steps of soaking crushed agricultural and forestry waste in a magnesium chloride solution, carrying out ultrasonic treatment, drying and then firing under anaerobic conditions. The magnesium-loaded biochar can improve the adsorption capacity of the high-purity biochar on cadmium and can effectively adsorb arsenic. Besides purifying the water polluted by cadmium and arsenic, the cadmium and arsenic in the soil can be passivated simultaneously, and the mobility and effectiveness of the cadmium and arsenic are reduced.
The existing preparation method of the magnesium modified biochar has complex effect, the content of magnesium loaded on the magnesium modified biochar is not high, and the adsorption performance of the magnesium modified biochar as an adsorbent needs to be improved. In most processes for preparing the biochar adsorbent by modifying magnesium salts, agricultural and forestry wastes are mostly used as raw materials, and aquatic plants, such as water hyacinth which is abused and disastrous, are subjected to biochar modification and preparation with less research.
The Eichhornia crassipes is used as a raw material for preparing the magnesium modified carbon material, and the functionality of the Eichhornia crassipes can be enhanced through magnesium modification, so that the Eichhornia crassipes has larger specific surface area and increased oxygen-containing functional groups, and the adsorption capacity of the Eichhornia crassipes is improved. The invention solves the problems of low magnesium content load and complicated preparation process of the magnesium-based material, solves the treatment problem of the eichhornia crassipes as an adsorbent, and can treat water pollution to achieve the virtuous cycle of treating waste by waste.
Aiming at the technical problems, the method for preparing the biochar material from the water hyacinth through magnesium modification and removing the water body pollution has environmental benefits, and provides a theoretical basis for the subsequent recycling treatment of the water hyacinth.
Disclosure of Invention
The invention aims to provide a preparation method of a magnesium modified carbon material, which utilizes a one-step method of aquatic plant material pretreatment, magnesium impregnation and high-temperature roasting to prepare an aquatic plant-based carbon material and applies the aquatic plant-based carbon material to the treatment of polluted wastewater. Aiming at the problem of less magnesium loading amount of the magnesium modified biochar, the preparation method of the magnesium modified carbon material provided by the invention can improve the magnesium loading amount and simplify the preparation process of the magnesium loaded biochar material. The adsorbent prepared by the method can effectively remove water body pollution such as nitrogen, phosphorus, heavy metals and the like, and the material can also be used as a stabilizer to be added into the bottom mud of the river channel to slow down the pollution of the bottom mud.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of an aquatic plant-based magnesium modified carbon material comprises the following steps:
1) material pretreatment: drying the collected aquatic plants, crushing, and sieving with a 20-mesh sieve to obtain a biomass raw material;
2) magnesium chloride impregnation: mixing the biomass raw material obtained by the treatment in the step 1) with magnesium chloride, adding pure water, and soaking for a period of time under stirring;
3) dewatering and drying: carrying out suction filtration on the impregnated biomass raw material, drying, and crushing to obtain a crushed material;
4) roasting: placing the crushed material obtained in the step 3) in a muffle furnace, and roasting for a period of time at constant temperature under the micro-oxygen condition to obtain the aquatic plant based magnesium modified carbon material.
Wherein, in the step 2) of magnesium chloride impregnation, the amount of the used magnesium chloride is that the magnesium chloride is mixed with 0.005-0.05mol of magnesium chloride per gram of biomass raw material according to the amount of pure magnesium chloride, the amount of the added pure water is 1:20-50 according to the amount of the biomass raw material, and the impregnation time is 6-20 hours.
Preferably, in step 3), the material is washed with deionized water after suction filtration and before drying.
Further, in the step 3), the drying temperature is 105 ℃, the drying time is 6-12h, and the end point of the drying is that the material becomes a state that can be crushed by hands.
Preferably, in the step 4), the roasting temperature is 300-.
The invention also provides application of the aquatic plant-based magnesium modified carbon material, which comprises the step of using the aquatic plant-based magnesium modified carbon material prepared by the preparation method as an adsorbent for removing phosphorus, ammonia nitrogen and Pb in water 2+ 、Cu 2+ 。
Compared with the prior art, the invention has the beneficial effects that: the aquatic plant magnesium modified carbon material prepared by one-step magnesium impregnation-high-temperature micro-oxygen roasting can effectively improve magnesium loading capacity, has the characteristics of simple process, low cost, good effect and the like, and can provide a recycling direction for the treatment of solid wastes of water hyacinth. The method has the advantages of simple overall operation, low cost, environmental protection and environmental and economic benefits.
Drawings
FIG. 1 is a preparation route and a partial object diagram of an aquatic plant-based magnesium modified carbon material;
FIG. 2 is SEM scanning electron micrographs of an aquatic plant-based magnesium-modified carbon material (a) (b) and a virgin biochar (c) (d);
FIG. 3 is a graph of EDS mapping results for an aquatic plant-based magnesium-modified carbon material, material six, and virgin biochar;
FIG. 4 is a comparison of XPS measurements of aquatic plant-based magnesium-modified carbon material and raw biochar;
FIG. 5 is an XPS spectrum of an aquatic plant-based magnesium modified carbon material and a virgin biochar;
FIG. 6 is XRD spectra of an aquatic plant based magnesium modified carbon material (a) and raw biochar (b);
FIG. 7 is FTIR spectra of the aquatic plant based magnesium modified carbon material (a) and the pristine biochar (b).
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely in the following description with reference to specific embodiments of the present invention and accompanying drawings. 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.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "front", "rear", "both ends", "one end", "the other end", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
Aiming at the current situations of complicated steps and low magnesium content of biochar in the existing magnesium modified biochar preparation process, the invention provides an adsorbent prepared by using aquatic plants such as water hyacinth and the like through one-step preparation method of magnesium modified impregnation and micro-oxygen high-temperature pyrolysis and used for removing nitrogen, phosphorus, lead and copper in water. The method simplifies the preparation process of the magnesium-loaded biochar, improves the magnesium loading capacity of the magnesium modified material, improves the adsorption effect on pollutants in water, and realizes the resource utilization of water hyacinth.
In order to achieve the purpose, the invention provides the following technical ideas: cleaning the salvaged invasive species of water hyacinth, taking the water hyacinth as a carrier, and preparing the aquatic plant-based magnesium modified material by one step through a stirring impregnation-high temperature roasting method. The soaked material is stirred and needs to be cleaned, and magnesium chloride outside the material is removed, so that the prepared material is not a mixture of magnesium oxide and biochar; roasting is carried out by controlling the temperature rise rate to be 10 ℃/min and the micro-oxygen condition, and oxygen-containing functional groups on the surface of the material are increased.
In an exemplary embodiment, the method for preparing the magnesium-modified biochar material for the aquatic plant comprises the following specific steps:
1) the water hyacinth is purchased from a certain aquaculture pond in Hunan, is naturally dried and crushed, and then is sieved by a 20-mesh sieve, so that the water hyacinth is a biomass raw material;
2) taking a certain amount of the material in the step (1), adding magnesium chloride hexahydrate according to the proportion of 0.005-0.05mol per gram of the material, adding pure water according to the solid-liquid ratio of 1:20-50 by mass of the raw materials, and soaking and stirring for 12 hours under a stirrer;
3) carrying out vacuum filtration on the material obtained in the step (2), washing the material with deionized water, drying the material in a drying oven at 105 ℃, and crushing the material after drying;
4) and (4) placing the material obtained in the step (3) in a muffle furnace, roasting at constant temperature for 0.5-2h under the condition of micro-oxygen at the temperature of 300-600 ℃, and controlling the heating rate to be 10 ℃/min to obtain the aquatic plant based magnesium oxide modified material.
And (3) taking the material obtained in the step (1) without adding magnesium chloride, and preparing the reference substance original biochar in the other steps.
The invention also provides an adsorbent prepared by using the water hyacinth for removing phosphorus, ammonia nitrogen and Pb in water 2+ 、Cu 2+ The method uses the adsorbent to remove phosphorus, ammonia nitrogen and Pb in water body 2+ 、Cu 2+ The method comprises the following specific operation steps:
(1) respectively mixing the adsorbent prepared from water hyacinth with phosphorus, ammonia nitrogen and Pb 2+ 、Cu 2+ Mixing the solutions at different solid-to-liquid ratios, carrying out oscillation reaction at 25-45 deg.C in a constant temperature shaker at 140rpm/min for 12h, and extracting supernatant;
(2) collecting the solution after reaction at a set time interval, filtering a water body containing phosphorus and ammonia nitrogen by using rapid filter paper, and respectively measuring the concentrations of the phosphorus and the ammonia nitrogen by a molybdate spectrophotometry and a nano-reagent spectrophotometry; containing Pb 2+ 、Cu 2+ The water body is rapidly filtered by a 0.45 mu m filter, and the concentration of heavy metal in the filtrate is measured by adopting ICP.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments.
The basic preparation and application procedures of the aquatic plant-based magnesium modified carbon material are as follows:
preprocessing water hyacinth: cleaning, naturally drying, and pulverizing;
adding 15.675 g of magnesium chloride hexahydrate in 5g of water hyacinth powder, adding 150 mL of pure water according to the solid-liquid ratio of 1:30, placing the mixture under a stirrer, controlling the rotating speed to be 500 rpm, and soaking and stirring the mixture for 12 hours;
thirdly, carrying out suction filtration on the impregnated powder by using a vacuum pump, washing the material subjected to suction filtration for three times by using pure water, and drying the material in a 105 ℃ drying oven;
putting the obtained biomass into a muffle furnace, setting the heating rate at 10 ℃/min, and roasting at 600 ℃ in a micro-oxygen environment for 2h to obtain the aquatic plant-based magnesium modified carbon material.
Removing pollutants in water: the aquatic plant-based magnesium modified carbon material prepared by the method is used for removing nitrogen, phosphorus and heavy metals in water:
mixing the prepared magnesium-modified carbon material based on aquatic plants with 10-500 mg/L phosphorus solution in a solid-to-liquid ratio of 1:5 (10 mg of adsorbent carbon is added to each 50ml of phosphorus solution), and carrying out oscillation reaction at 25-45 ℃ at 150 rpm/min for 24 hours; after the reaction is finished, measuring the phosphorus content by using a molybdate spectrophotometry;
secondly, mixing the prepared aquatic plant-based magnesium modified carbon material with 5-30 mg/L ammonia nitrogen solution in a solid-to-liquid ratio of 1:1 (10 mg of adsorbent carbon is added to each 10 ml of ammonia nitrogen solution), and carrying out oscillation reaction at 25-60 ℃ at 150 rpm/min for 24 hours; after the reaction is finished, measuring the content of ammonia nitrogen by using a nano reagent spectrophotometry;
mixing the prepared magnesium modified carbon material based on aquatic plants with 10-120 mg/L nitrate nitrogen solution in a solid-to-liquid ratio of 1:1 (10 mg of adsorbent carbon is added to each 10 ml of nitrate nitrogen solution), and carrying out oscillation reaction at 25-45 ℃ at 150 rpm/min for 24 h; after the reaction is finished, measuring the content of nitrate nitrogen by using an ultraviolet spectrophotometry;
mixing the prepared magnesium-based modified carbon material with 20-140 mg/L copper ion solution in a solid-to-liquid ratio of 1:5 (10 mg of adsorbent carbon is added to each 50ml of copper ion solution), and carrying out oscillation reaction at 25-45 ℃ at 150 rpm/min for 24 h; after the reaction is finished, filtering the mixture by using a 0.45-micron filter membrane, and then measuring the content of copper ions by using ICP-OES;
fifthly, mixing the prepared magnesium modified carbon material based on aquatic plants with 50-250 mg/L lead ion solution in a solid-to-liquid ratio of 1:5 (10 mg of adsorbent carbon is added to each 50ml of lead ion solution), and carrying out oscillation reaction at the temperature of 25-45 ℃ and at the speed of 150 rpm/min for 24 hours; after the reaction, the reaction mixture was filtered through a 0.45 μm filter and then the content of lead ions was measured by ICP-OES.
The first embodiment is as follows: aquatic plant based magnesium modified carbon material
The method comprises the following steps: adding 15.675 g magnesium chloride hexahydrate in 5g water hyacinth powder, adding 150 mL pure water according to the solid-to-liquid ratio of 1:30, placing under a stirrer, controlling the rotating speed at 500 rpm, and soaking and stirring for 12 h.
Step two: and (3) carrying out suction filtration on the biomass obtained in the step one by using a vacuum pump, washing the material subjected to suction filtration for three times by using pure water, and drying the material in a drying oven at 105 ℃.
Step three: and (3) placing the biomass obtained in the step two into a muffle furnace, setting the heating rate to be 10 ℃/min, and roasting at 600 ℃ in a micro-oxygen environment for 2h to obtain the aquatic plant-based magnesium modified carbon material.
Scanning electron microscope and XRD show that the magnesium oxide is uniformly loaded in the carbon material. In addition, the X-ray diffraction ratio can correspond to the (111) (200) and (220) crystal faces of magnesium oxide of the aquatic plant-based magnesium modified carbon material, and the FT-IR infrared spectrogram comparison shows that the aquatic plant-based magnesium modified carbon material also contains magnesium hydroxide. The conclusion shows that the magnesium is successfully loaded on the aquatic plant-based magnesium modified carbon material.
FT-IR shows that the oxygen-containing functional groups such as hydroxyl, carboxyl and the like of the magnesium modified carbon material based on the aquatic plants are increased in amount; EDS mapping shows that the weight percentage of oxygen and magnesium elements in the magnesium modified carbon material prepared in the micro-oxygen environment is the largest, the oxygen element is improved by 13.74 percent and 11.63 percent compared with the material six and the original biochar, the weight percentage of the magnesium element is equivalent to that of the material six, but the weight percentage of the magnesium element is improved by 13.04 percent compared with that of the original biochar; by carrying out element semi-quantitative analysis through XPS, compared with the original biochar, the atomic percent of oxygen in the magnesium modified carbon material is increased by 26.16%, and the atomic percent of magnesium is increased by 7.83%.
Example two: raw biochar material based on aquatic plant
The difference between the first embodiment and the second embodiment is that the first and second steps in the above embodiments are eliminated, no magnesium loading is performed, and other conditions are not changed, which is specifically as follows:
5g of water hyacinth powder biomass is put into a muffle furnace, the heating rate is set to be 10 ℃/min, and the water hyacinth powder biomass is roasted at 600 ℃ for 2h at a micro-oxygen environment to obtain the aquatic plant-based original biochar material.
Example three: comparison of adsorption performances of aquatic plant-based original biochar material and magnesium modified carbon material
The adsorption capacity of 0.01g of the aquatic plant-based original biochar material and the adsorption capacity of the magnesium modified carbon material to 100mL of 500mg/L phosphorus solution at 25 ℃ are respectively 18.53 mg/g and 216.23 mg/g;
the adsorption capacity of 0.05g of the aquatic plant-based original biochar material and the magnesium modified carbon material to 50mL of 30mg/L ammonia nitrogen solution at 25 ℃ is 2.06 mg/g and 6.68mg/g respectively; the adsorption capacity of 0.05g of the aquatic plant-based original biochar material and the magnesium modified carbon material to 50mL of 120mg/L nitrate nitrogen solution at 25 ℃ is 14.59 mg/g and 17.96mg/g respectively;
the adsorption capacity of 0.01g of the aquatic plant-based original biochar material and the magnesium modified carbon material to 50mL of 100mg/L lead (II) solution at 25 ℃ is 250.01 mg/g and 410.61mg/g respectively;
the adsorption capacity of 0.01g of the aquatic plant-based original biochar material and the adsorption capacity of the magnesium modified carbon material to 50mL of 100mg/L copper (II) solution at 25 ℃ are 51.42 mg/g and 251.50mg/g respectively.
Example four:
the difference between this example and the first example is that the calcination temperature in the third step of the above example is changed to 300-600 ℃, and the other conditions are not changed, so as to obtain the material four. 0.05g of each of the materials prepared at 300 ℃, 400 ℃, 500 ℃ and 600 ℃ is taken to carry out adsorption experiments, and the adsorption capacity of the materials to 50mL of 20mg/L ammonia nitrogen solution at 25 ℃ is respectively 2.67, 2.88, 3.61 and 6.29 mg/g.
Example five:
the difference between the embodiment and the embodiment I is that the roasting time in the step III of the embodiment is changed to 0.5-2h, and the other conditions are not changed to obtain a material V. Taking 0.05g of each of five materials prepared with roasting time of 0.5, 1, 1.5 and 2h for carrying out adsorption experiments, wherein the adsorption amounts of the five materials to 50mL of 20mg/L ammonia nitrogen solution at 25 ℃ are 3.12, 4.20, 5.43 and 6.29mg/g respectively.
Example six:
the difference between the present embodiment and the first embodiment is that the micro-oxygen environment in the third step of the above embodiment is changed to the oxygen limited environment, and the other conditions are not changed, so that the material is changed to six. The adsorption capacity of 0.01g of the material six and the adsorption capacity of the magnesium modified carbon material to 50mL of 50mg/L phosphorus solution at 25 ℃ are 7.72 mg/g and 60.75 mg/g respectively.
Example seven:
the difference between this example and the first example is that the pure water in the second step of the above example was washed away, and the other conditions were not changed, to obtain material seven. The adsorption capacity of 0.01g of the material seven and the adsorption capacity of the magnesium modified carbon material to 50mL of 50mg/L phosphorus solution at 25 ℃ are 40.16 and 60.75 mg/g respectively.
Example eight:
the difference between this example and the first example is that the third step of the above example is removed, and the other conditions are not changed, so as to obtain material eight. 0.01g of the material VIII and the adsorption capacity of the magnesium modified carbon material to 50mL of 50mg/L phosphorus solution at 25 ℃ are 6.18 and 60.75 mg/g respectively.
Example nine:
the difference between the present embodiment and the first embodiment is that the material nine is obtained by taking the biomass of the water hyacinth powder. The adsorption capacity of 0.01g of the material nine and the adsorption capacity of the magnesium modified carbon material to 50mL of 50mg/L phosphorus solution at 25 ℃ are respectively 1.54 and 60.75 mg/g.
Example ten: application of aquatic plant-based magnesium modified carbon material to adsorption of phosphorus in water
10 mg of the aquatic plant-based magnesium modified carbon material adsorbent is respectively added into 50mL of phosphorus-containing solutions with different concentrations, the concentration range of the solutions is 10-500 mg/L, and the temperature is 25 ℃ and 45 ℃. Shaking for 24 hours ensured that adsorption equilibrium was reached. And taking the supernatant to measure the residual phosphorus concentration of the solution, and obtaining the equilibrium adsorption capacity under different initial phosphorus concentrations. And fitting by adopting an isothermal adsorption model to obtain the aquatic plant-based magnesium modified carbon material, wherein the adsorption of the aquatic plant-based magnesium modified carbon material on phosphorus conforms to a Freundlich isothermal adsorption model. The maximum adsorption capacity is 197.69 mg/g at 25 ℃, and the adsorption capacity can reach 216.23 mg/g at 45 ℃.
Adding 100mg of adsorbent into 250 mL of phosphorus solution with the concentration of 50mg/L, taking supernatant to measure the phosphorus concentration after different time intervals, drawing and fitting the adsorption quantity and time at different time points to obtain that the adsorption of the aquatic plant-based magnesium modified carbon material on phosphorus accords with the quasi-second-order adsorption kinetics, the adsorption rate is high in the first 30 minutes of adsorption, and the adsorption balance can be achieved in 360 minutes.
Example eleven: application of aquatic plant-based magnesium modified carbon material in adsorption of ammonia nitrogen in water
The difference between the embodiment and the implementation is that the phosphorus in the embodiment is changed into ammonia nitrogen, and other conditions are unchanged, specifically as follows:
50mg of the aquatic plant-based magnesium modified carbon material adsorbent is respectively added into 50mL of ammonia nitrogen solutions with different concentrations, the concentration range of the solution is 5-30 mg/L, and the temperature is 25 ℃ and 60 ℃. Shaking for 24 hours ensured that adsorption equilibrium was reached. And taking the supernatant to measure the residual ammonia nitrogen concentration of the solution, so as to obtain the equilibrium adsorption capacity under different initial ammonia nitrogen concentrations. And fitting by adopting an isothermal adsorption model to obtain the aquatic plant-based magnesium modified carbon material, wherein the adsorption of the aquatic plant-based magnesium modified carbon material on ammonia nitrogen conforms to the Freundlich isothermal adsorption model. The maximum adsorption capacity at 25 ℃ is 6.68mg/g, and the adsorption capacity at 60 ℃ can reach 7.13 mg/g.
Adding 50mg of adsorbent into 50mL of phosphorus solution with the concentration of 20mg/L, taking supernatant to measure the phosphorus concentration after different time intervals, drawing and fitting the adsorption quantity and time at different time points to obtain that the adsorption of the aquatic plant-based magnesium modified carbon material on phosphorus accords with the quasi-second-order adsorption kinetics, the adsorption rate is high in the first 30 minutes of adsorption, and the adsorption balance can be achieved in 360 minutes.
Example twelve: application of aquatic plant-based magnesium modified carbon material in adsorption of nitrate nitrogen in water
The present embodiment is different from the embodiment ten in that the phosphorus in the above embodiment is replaced by nitrate nitrogen, and other conditions are not changed, specifically as follows:
50mg of the aquatic plant-based magnesium modified carbon material adsorbent is respectively added into 50mL of nitrate-containing nitrogen solutions with different concentrations, wherein the concentration range of the solutions is 10-120 mg/L, and the temperature is 25 ℃, 35 ℃ and 45 ℃. Shaking for 24 hours ensured that adsorption equilibrium was reached. And taking the supernatant to measure the concentration of the residual nitrate nitrogen in the solution to obtain the equilibrium adsorption capacity under different initial nitrate nitrogen concentrations. And fitting by adopting an isothermal adsorption model to obtain the aquatic plant-based magnesium modified carbon material, wherein the adsorption of the aquatic plant-based magnesium modified carbon material on nitrate nitrogen conforms to the Freundlich isothermal adsorption model. The maximum adsorption capacity at 25 ℃ is 17.96mg/g, the maximum adsorption capacity at 35 ℃ is 18.09 mg/g, and the adsorption capacity at 45 ℃ can reach 19.07 mg/g.
Adding 50mg of adsorbent into 250 mL of nitrate nitrogen solution with the concentration of 20mg/L, taking supernatant to measure the concentration of the nitrate nitrogen after different time intervals, drawing a graph of the adsorption quantity and time at different time points and fitting to obtain that the adsorption of the aquatic plant-based magnesium modified carbon material on the nitrate nitrogen accords with quasi-second-order adsorption kinetics, the adsorption rate is high in the first 120 minutes of adsorption, and the adsorption balance can be achieved in 360 minutes.
Example thirteen: application of aquatic plant-based magnesium modified carbon material in adsorption of copper ions in water
The present embodiment is different from the embodiment ten in that the phosphorus in the above embodiment is replaced by the divalent copper ion, and other conditions are not changed, specifically as follows:
10 mg of the aquatic plant-based magnesium modified carbon material adsorbent is respectively added into 50mL of copper ion-containing solutions with different concentrations, wherein the concentration range of the solutions is 20-140 mg/L, and the temperature is 25 ℃, 35 ℃ and 45 ℃. Shaking for 24 hours ensured that adsorption equilibrium was reached. And taking the supernatant to measure the residual copper ion concentration of the solution, and obtaining the equilibrium adsorption capacity under different initial copper ion concentrations. And fitting by adopting an isothermal adsorption model to obtain the aquatic plant-based magnesium modified carbon material, wherein the adsorption of the aquatic plant-based magnesium modified carbon material on copper ions conforms to the Langmuir isothermal adsorption model. The maximum adsorption capacity at 25 ℃ is 198.05 mg/g, the maximum adsorption capacity at 35 ℃ is 216.53 mg/g, and the adsorption capacity at 45 ℃ can reach 228.51 mg/g.
Adding 10 mg of adsorbent into 50mL of copper ion solution with the concentration of 120mg/L, taking supernatant to measure the concentration of the copper ions after different time intervals, drawing a graph of the adsorption amount and the time at different time points and fitting the graph to obtain the aquatic plant-based magnesium modified carbon material, wherein the adsorption of the aquatic plant-based magnesium modified carbon material on the copper ions accords with the quasi-second-order adsorption kinetics, the adsorption rate is high in the first 60 minutes of adsorption, and the adsorption balance can be achieved in 120 minutes.
Example fourteen: application of aquatic plant-based magnesium modified carbon material in adsorption of lead ions in water
The present example is different from the example ten in that the phosphorus in the above example is replaced by the divalent lead ion, and other conditions are not changed, specifically as follows:
10 mg of the aquatic plant-based magnesium modified carbon material adsorbent is respectively added into 50mL of lead-containing ion solutions with different concentrations, wherein the concentration range of the solution is 50-250 mg/L, and the temperature is 25 ℃, 35 ℃ and 45 ℃. Shaking for 24 hours ensured that adsorption equilibrium was reached. And taking the supernatant to measure the concentration of the residual lead ions in the solution, so as to obtain the equilibrium adsorption capacity under different initial lead ion concentrations. And fitting by adopting an isothermal adsorption model to obtain the aquatic plant-based magnesium modified carbon material, wherein the adsorption of the aquatic plant-based magnesium modified carbon material on lead ions conforms to the Langmuir isothermal adsorption model. The maximum adsorption capacity at 25 ℃ is 619.74 mg/g, the maximum adsorption capacity at 35 ℃ is 737.73 mg/g, and the adsorption capacity at 45 ℃ can reach 764.3 mg/g.
Adding 10 mg of adsorbent into 50mL of lead ion solution with the concentration of 100mg/L, taking supernate to measure the lead ion concentration after different time intervals, drawing and fitting the adsorption quantity and time at different time points to obtain that the adsorption of the aquatic plant-based magnesium modified carbon material on the lead ions accords with the quasi-second-order adsorption kinetics, the adsorption rate is high in the first 60 minutes of adsorption, and the adsorption balance can be achieved in 120 minutes.
According to the embodiment, the water hyacinth is developed into the adsorbent which is feasible to remove heavy metal and nitrogen and phosphorus in water, and a large amount of salvaged water hyacinth can be treated in a recycling manner, so that the water hyacinth has good environmental and economic benefits.
The invention is not described in detail, but is well known to those skilled in the art.
Finally, it is to be noted that: although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (6)
1. The preparation method of the aquatic plant-based magnesium modified carbon material is characterized by comprising the following steps of:
1) material pretreatment: drying the collected aquatic plants, crushing, and sieving with a 20-mesh sieve to obtain a biomass raw material;
2) magnesium chloride impregnation: mixing the biomass raw material obtained by the treatment in the step 1) with magnesium chloride, adding pure water, and soaking for a period of time under stirring;
3) dewatering and drying: carrying out suction filtration on the impregnated biomass raw material, drying, and crushing to obtain a crushed material;
4) roasting: placing the crushed material obtained in the step 3) in a muffle furnace, and roasting for a period of time at constant temperature under the micro-oxygen condition to obtain the aquatic plant based magnesium modified carbon material.
2. The method for preparing an aquatic plant-based magnesium-modified carbon material according to claim 1, wherein in the step 2) of magnesium chloride impregnation, the amount of magnesium chloride used is in a range of 0.005 to 0.05mol per gram of biomass raw material based on the amount of pure magnesium chloride, the amount of pure water added is in a range of 1:20 to 50 in terms of the solid-to-liquid ratio based on the amount of biomass raw material, and the impregnation time is 6 to 20 hours.
3. The method for preparing magnesium-modified charcoal material based on aquatic plants as claimed in claim 1, wherein in step 3), the material is further washed with deionized water after suction filtration and before drying.
4. The method for preparing an aquatic plant based magnesium modified carbon material according to claim 1, wherein in the step 3), the drying temperature is 105 ℃, the drying time is 6-12 hours, and the drying end point is that the material becomes a state that can be crushed by hand.
5. The method for preparing magnesium-modified carbon material based on aquatic plants as claimed in claim 1, wherein in step 4), the calcination temperature is 300-600 ℃, the calcination time is 0.5-2h, the temperature rise rate is 10 ℃/min, and the micro-oxygen condition is that the volume fraction of oxygen is 10-21%.
6. Use of an aquatic plant-based magnesium-modified carbon material, comprising applying the preparation method of any one of claims 1 to 5The aquatic plant-based magnesium modified carbon material prepared by the method is used as an adsorbent for removing phosphorus, ammonia nitrogen and Pb in water 2+ 、Cu 2+ 。
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