CN111672465A - Preparation method and application of ferroferric oxide-manganese dioxide/mulberry stem biochar composite material - Google Patents
Preparation method and application of ferroferric oxide-manganese dioxide/mulberry stem biochar composite material Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0222—Compounds of Mn, Re
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
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Abstract
The invention discloses a preparation method and application of a ferroferric oxide-manganese dioxide/mulberry stem biochar composite material. Carbonizing mulberry stems to prepare mulberry stem biochar; adding ferric chloride and ferrous sulfate solution into the mulberry stalk biochar; adjusting the pH value with an ammonia solution; adding manganese sulfate solid and potassium permanganate solution, and then regulating the pH value by using potassium hydroxide solution; filtering, washing, drying and the like to obtain the ferroferric oxide-manganese dioxide/mulberry stem biomass charcoal composite material. The invention has simple process equipment and easy operation; the prepared ferroferric oxide-manganese dioxide/mulberry stem biomass charcoal composite material has good adsorption effect and can be applied to the treatment of arsenic-containing wastewater and soil.
Description
Technical Field
The invention relates to ferroferric oxide-manganese dioxide (Fe)3O4-MnO2) Preparation method and application of mulberry stalk biomass charcoal composite material.
Background
Nowadays, socio-economic development is rapid, and the environmental problems are more serious. Statistically, 1.5 million people around the world are facing the threat of endemic arsenic poisoning. China is also one of the most severely harmed countries from arsenic poisoning. The problem of farmland pollution in a certain area caused by high-arsenic underground water irrigation also occurs in Taiwan, Xinjiang, inner Mongolia, Shanxi and other provinces. Large-area moderate or severe arsenic pollution of soil is caused by mining, smelting and the like in provinces such as Hunan, Hubei, Guangxi, Yunnan and the like. For example, large-area paddy fields in Hening county of Hunan are polluted by arsenic due to mining and smelting, and the arsenic content of the paddy fields is 92-840 mg/kg. The soil As along the affluent area downstream of the ultra-large tin polymetallic mining field in Guangxi south Dan large-scale factories exceeds the soil environment quality (GB15618-1995) level III standard by 36-276 times.
The nondegradable property of arsenic in water, the accumulation property of arsenic in organisms and the great harm of arsenic after long-term excessive intake into human bodies need to effectively treat the water with the arsenic content exceeding the standard of drinking water and farmland irrigation water. Common treatment methods include physical and chemical techniques such as precipitation, adsorption, ion exchange, reverse osmosis, membrane filtration, and the like; biological methods such as biotransformation, phytoremediation and combinations thereof; an electrochemical method. The adsorption method in the method can remove arsenic in water simply and efficiently, has small interference, and has the advantages of being renewable and low in cost. And thus is widely used.
In recent years, the use of adsorbents at home and abroad to achieve arsenic removal can be classified into the following categories: iron-containing materials, composite materials, nanomaterials, clay materials, active materials. Wherein the application range of the composite material is wider. Common composite materials are mainly composite materials formed by combining iron salts or iron oxides. In the application of removing water pollutants, the biochar has the defects of light weight, small particles and difficult separation, so that a magnetic substance is introduced to facilitate the separation.
The biochar is a carbonaceous material prepared by pyrolyzing biomass under an oxygen-limited condition, and has the advantages of low cost, rich sources and the like. Due to the unique properties (rich functional group content, strong cation exchange capacity, stable chemical properties and the like), the organic metal complex is often used for removing heavy metals and organic pollutants in soil and water, and can reduce the mobility of the pollutants in the soil and reduce the biological effectiveness. In order to obtain better charcoal adsorption effect, there are many studies such as: the biochar is modified by acid/alkali modification, metal or metal oxide modification, inorganic nano material modification, functional group modification and other methods. A large number of researches show that the iron-containing material has the advantages of high arsenic adsorption capacity, high arsenic adsorption kinetics rate and the like, and has small influence on the physical and chemical properties of the soil matrix.
Therefore, the waste mulberry stems are used as raw materials to prepare the biochar, the ferric chloride, the ferrous sulfate, the manganese sulfate and the potassium permanganate are used as modifiers to prepare the Fe3O4-MnO2A biological charcoal composite material for mulberry stems. The composite material combines biochar and Fe3O4And MnO2The method has the advantages of effectively removing arsenic in the arsenic-containing wastewater, effectively fixing arsenic in the arsenic-polluted soil, and remarkably reducing the concentration of soluble arsenic in the soil leaching solution.
Disclosure of Invention
The invention aims to provide a method for preparing Fe by adopting a two-step coprecipitation method under normal pressure and taking mulberry stems as raw materials and ferric chloride, ferrous sulfate, manganese sulfate and potassium permanganate as modifiers3O4-MnO2A method for preparing a mulberry stalk biochar composite material.
The method comprises the following specific steps:
(1) peeling mulberry stems, crushing the mulberry stems into blocks, smashing the mulberry stems into powder by using a universal pulverizer, sieving the powder by using a 20-mesh sieve, and drying the powder in an oven at the temperature of 60-80 ℃ for later use.
(2) And (2) putting the mulberry stem powder obtained in the step (1) into a crucible, then putting the crucible into a muffle furnace, heating to 300-700 ℃ at the speed of 5 ℃/min, keeping for 2 hours, taking out after the temperature is reduced to room temperature, grinding, sieving with a 100-mesh sieve, and sealing for storage.
(3) Weighing 0.1-0.4 g of the mulberry tree stalk biochar obtained in the step (2) into a 500mL beaker, adding 200mL of deionized water, and carrying out ultrasonic treatment for 30 minutes.
(4) Adding 25mL FeCl with the concentration of 0.01-0.04 mol/L into the product obtained in the step (3)3And 25mL of FeSO with the concentration of 0.05 mol/L-0.2 mol/L4The mixed solution is stirred evenly by magnetic force in a magnetic constant-temperature water bath stirrer at the temperature of 30 ℃ to obtain the mixed solution of ferric iron and ferrous iron.
(5) Under the magnetic stirring, NH with the volume percentage concentration of 10-25 percent is dripped into the beaker filled with the mixed solution in the step (4)3·H2And adjusting the pH value of the mixed solution to 9.0-10.0 by using an O solution. The obtained mixed suspension is stirred for 4 hours in a magnetic constant-temperature water bath stirrer at the temperature of 80-90 ℃.
(6) Adding 0.155 g-0.62 g of MnSO into the mixed suspension obtained in the step (5)4·H2O solid, stirred at 80 ℃.
(7) And (4) adding 2.5mL of potassium permanganate solution with the concentration of 0.02-0.08 mol/L into the mixed suspension obtained in the step (6), adjusting the pH value of the mixed solution to 9.0-11 by using potassium hydroxide solution with the concentration of 0.08-0.32 mol/L, and continuing to stir for 1.5-2 hours by magnetic force.
(8) Filtering the mixed suspension obtained in the step (7), washing the mixed suspension with deionized water for multiple times to be neutral, then washing the mixed suspension with absolute ethyl alcohol for two times, and drying the obtained filter cake in a vacuum freeze dryer for 24 to 48 hours at the temperature of minus 50 ℃; taking out, grinding and sieving with a 100-mesh sieve to obtain Fe3O4-MnO2A biological charcoal composite material for mulberry stems.
Produced Fe3O4-MnO2The mulberry stalk biochar composite contains Fe3O4And MnO2: the magnetic material has superparamagnetism, and the saturation magnetization is 1.458 emu/g. The maximum adsorption of arsenic at 25 ℃ was 62.073 mg/g. When the initial total arsenic concentration in the solution is 20mg/L, the removal rate of arsenic is more than 98 percent, the arsenic concentration in the adsorption equilibrium solution is less than 0.5mg/L, and the adsorption equilibrium solutionThe arsenic content in the liquid reaches the national comprehensive sewage discharge standard; when the initial total arsenic concentration in the solution is 2.0mg/L, the removal rate of arsenic is more than 99.5%, and the arsenic concentration in the adsorption equilibrium solution is lower than the limit value of arsenic in the Water quality Standard of Drinking of the world health organization 0.01 mg/L.
Produced Fe3O4-MnO2The mulberry stalk biochar composite material can be applied to the treatment of arsenic-containing waste water and soil.
The invention has simple process equipment and easy operation. Mainly takes waste mulberry stems as raw materials, and reduces the cost. The prepared composite material has higher magnetic saturation strength, can be separated from the solution under the action of an external magnetic field, has good adsorption effect on arsenic in the water solution, and also has good fixing effect on arsenic in soil.
Drawings
FIG. 1 shows Fe obtained by the preparation of the example of the present invention3O4-MnO2Isotherm diagram of adsorption of mulberry stem biomass charcoal composite material on arsenic.
FIG. 2 shows Fe obtained by the preparation of the example of the present invention3O4-MnO2The effect diagram of the mulberry stalk biomass charcoal composite material for fixing arsenic in soil.
FIG. 3 shows Fe obtained by the preparation of the example of the present invention3O4-MnO2Magnetic hysteresis curve of mulberry stem biomass charcoal composite material.
FIG. 4 shows Fe obtained by the preparation of the example of the present invention3O4-MnO2An infrared spectrogram of the mulberry stalk biomass charcoal composite material.
FIG. 5 shows Fe obtained by the preparation of the example of the present invention3O4-MnO2XRD pattern of mulberry stalk biomass charcoal composite material.
FIG. 6 shows Fe obtained by the preparation of the example of the present invention3O4-MnO2SEM image of/mulberry stalk biomass charcoal composite material.
Detailed Description
Example (b):
(1) peeling mulberry stems, crushing into blocks, pulverizing into powder by a universal pulverizer, sieving with a 20-mesh sieve, and drying in an oven at 60 ℃ for later use.
(2) And (2) putting the mulberry stem powder obtained in the step (1) into a crucible, then putting the crucible into a muffle furnace, heating to 600 ℃ at the speed of 5 ℃/min, keeping for 2 hours, taking out when the temperature is reduced to room temperature, grinding, sieving with a 100-mesh sieve, and sealing for storage.
(3) Weighing 0.1g of the mulberry stalk biochar obtained in the step (2) into a 500mL beaker, adding 200mL of deionized water, and carrying out ultrasonic treatment for 30 minutes.
(4) Adding 25mL of FeCl with the concentration of 0.01mol/L into the step (3)3And 25mL of FeSO with a concentration of 0.05mol/L4The mixed solution is stirred evenly in a magnetic constant-temperature water bath stirrer at the temperature of 30 ℃ to obtain the mixed solution.
(5) Dripping NH with the volume percentage concentration of 25 percent into the beaker in the step (4)3·H2O, adjusting the pH value to 10; the resulting mixture was stirred in a magnetic thermostatic water bath at 90 ℃ for 4 hours.
(6) Adding 0.155g of MnSO to the mixed suspension obtained in the step (5)4·H2O solid, stirring at 80 deg.C.
(7) 2.5mL of KMnO with a concentration of 0.02mol/L was added to the product obtained in step (6)4The solution was adjusted to pH 9.5 with 0.08mol/L KOH solution and magnetically stirred for 2 hours.
(8) Filtering the mixed suspension obtained in the step (7), washing the mixed suspension for multiple times by using deionized water to be neutral, then washing the mixed suspension for two times by using absolute ethyl alcohol, and drying the obtained filter cake for 24 hours at the temperature of 50 ℃ below zero in a vacuum freeze dryer; taking out, grinding and sieving with a 100-mesh sieve to obtain Fe3O4-MnO2A biological charcoal composite material for mulberry stems.
Fe obtained in this example3O4-MnO2The mulberry stem biomass charcoal composite material is applied to adsorption removal of arsenic in water.
0.05g of Fe obtained in this example was weighed out3O4-MnO2The mulberry stalk biomass charcoal composite material is put in a 100mL plastic centrifuge tube. Using 0.1mol/L sodium hydroxide solution or salt in advanceThe pH value of the acid solution is adjusted to 5.0, the volume is 25mL, and the arsenic-containing solution with the concentration of 2, 10, 20, 50 and 100mg/L is added into the plastic centrifuge tube. The adsorption was carried out at a temperature of 25 ℃ and a rotation speed of 200 rpm for 48 hours with shaking. Then, the solution was filtered through a 0.22um filter, and the concentration of arsenic remaining in the solution was measured by atomic fluorescence absorption, as shown in FIG. 3.
1g of Fe obtained in this example was weighed3O4-MnO2The mulberry stalk biomass charcoal composite adsorbent and 9g of arsenic-contaminated soil are put in a 50mL plastic centrifuge tube. According to the solid-liquid ratio of 1: 2, adding ultrapure water, adding proclin300 in an amount of 0.02% to limit the biological activity during the culture, and culturing in a constant temperature incubator at 25 ℃. + -. 1 ℃. Samples were taken after 2 days, centrifuged at 8000rpm in a high speed centrifuge and the supernatant was aspirated through a 0.22um filter. The leaching concentration of arsenic in the stabilized soil was analyzed by atomic fluorescence absorption method, and the result is shown in fig. 3.
The results of the arsenic adsorption experiments are shown in FIG. 1. The results of the arsenic fixation experiments in the soil are shown in FIG. 2. The hysteresis diagram is shown in fig. 3. The phase structure and the composition were measured by using an FT-IR Fourier spectrometer and an X-ray diffractometer, and the results are shown in FIGS. 4 and 5. Analysis of Fe by field emission scanning Electron microscopy3O4-MnO2The morphology of the/mulberry stalk biochar composite is shown in figure 6.
Claims (2)
1. A preparation method of a ferroferric oxide-manganese dioxide/mulberry stem biochar composite material is characterized by comprising the following specific steps:
(1) peeling mulberry stems, crushing the mulberry stems into blocks, grinding the mulberry stems into powder by using a universal grinder, sieving the powder by using a 20-mesh sieve, and drying the powder in an oven at the temperature of 60-80 ℃ for later use;
(2) putting the mulberry stem powder obtained in the step (1) into a crucible, then putting the crucible into a muffle furnace, heating to 300-700 ℃ at the speed of 5 ℃/min, keeping for 2 hours, taking out after the temperature is reduced to room temperature, grinding, sieving with a 100-mesh sieve, and sealing for storage;
(3) weighing 0.1-0.4 g of the mulberry tree stalk biochar obtained in the step (2) into a 500mL beaker, adding 200mL of deionized water, and carrying out ultrasonic treatment for 30 minutes;
(4) adding 25mL FeCl with the concentration of 0.01-0.04 mol/L into the product obtained in the step (3)3And 25mL of FeSO with the concentration of 0.05 mol/L-0.2 mol/L4The mixed solution is stirred evenly by magnetic force in a magnetic constant-temperature water bath stirrer at the temperature of 30 ℃ to obtain a mixed solution of ferric iron and ferrous iron;
(5) under the magnetic stirring, NH with the volume percentage concentration of 10-25 percent is dripped into the beaker filled with the mixed solution in the step (4)3·H2O solution, adjusting the pH value of the mixed solution to 9.0-10.0; stirring the obtained mixed suspension in a magnetic constant-temperature water bath stirrer at 80-90 ℃ for 4 hours;
(6) adding 0.155 g-0.62 g of MnSO into the mixed suspension obtained in the step (5)4·H2O solid, stirring at 80 ℃;
(7) adding 2.5mL of potassium permanganate solution with the concentration of 0.02-0.08 mol/L into the mixed suspension obtained in the step (6), adjusting the pH value of the mixed solution to 9.0-11 by using potassium hydroxide solution with the concentration of 0.08-0.32 mol/L, and continuing to stir for 1.5-2 hours by magnetic force;
(8) filtering the mixed suspension obtained in the step (7), washing the mixed suspension with deionized water for multiple times to be neutral, then washing the mixed suspension with absolute ethyl alcohol for two times, and drying the obtained filter cake in a vacuum freeze dryer for 24 to 48 hours at the temperature of minus 50 ℃; taking out, grinding and sieving by a 100-mesh sieve to obtain the ferroferric oxide-manganese dioxide/mulberry stem biochar composite material.
2. The application of the ferroferric oxide-manganese dioxide/mulberry stem biochar composite material prepared by the preparation method according to claim 1 is characterized in that the ferroferric oxide-manganese dioxide/mulberry stem biochar composite material has high magnetic saturation strength, can be separated from a solution under the action of an external magnetic field, has a good adsorption effect on arsenic in an aqueous solution, has a good fixing effect on arsenic in soil, and can be applied to the treatment of arsenic-containing wastewater and soil.
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| CN112774625A (en) * | 2020-12-16 | 2021-05-11 | 西北农林科技大学 | Zirconium oxide doped magnetic high-surface active carbon composite material, preparation method and application |
| CN112958606A (en) * | 2021-02-03 | 2021-06-15 | 中环国投(重庆)环保产业开发有限公司 | Remediation method for organic contaminated soil |
| CN113351153A (en) * | 2021-05-24 | 2021-09-07 | 桂林理工大学 | MgFe-LDO-MnO2Preparation method and application of composite material |
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| CN112756392B (en) * | 2020-12-18 | 2022-03-01 | 广东工业大学 | Remediation agent and remediation method for organic contaminated soil |
| CN112958606A (en) * | 2021-02-03 | 2021-06-15 | 中环国投(重庆)环保产业开发有限公司 | Remediation method for organic contaminated soil |
| CN113351153A (en) * | 2021-05-24 | 2021-09-07 | 桂林理工大学 | MgFe-LDO-MnO2Preparation method and application of composite material |
| CN113351153B (en) * | 2021-05-24 | 2022-08-09 | 桂林理工大学 | MgFe-LDO-MnO 2 Preparation method and application of composite material |
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Application publication date: 20200918 |