CN116272865A - Biochar loaded magnesium ferrite adsorbent and preparation method and application thereof - Google Patents
Biochar loaded magnesium ferrite adsorbent and preparation method and application thereof Download PDFInfo
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 63
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 49
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 48
- 239000011777 magnesium Substances 0.000 title claims abstract description 48
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- 238000001179 sorption measurement Methods 0.000 claims abstract description 40
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- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 13
- 239000012498 ultrapure water Substances 0.000 claims abstract description 13
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 12
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
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- 238000007873 sieving Methods 0.000 claims abstract description 7
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- 238000001354 calcination Methods 0.000 claims abstract description 5
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- 150000003839 salts Chemical class 0.000 claims description 9
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 7
- 230000005291 magnetic effect Effects 0.000 abstract description 5
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910017135 Fe—O Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
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- 150000002500 ions Chemical class 0.000 description 2
- ZTERWYZERRBKHF-UHFFFAOYSA-N magnesium iron(2+) oxygen(2-) Chemical compound [Mg+2].[O-2].[Fe+2].[O-2] ZTERWYZERRBKHF-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
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- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention relates to a biochar loaded magnesium ferrite adsorbent, a preparation method and application thereof, wherein a proper amount of shaddock peel powder is added into ultrapure water under the constant temperature of 25 ℃ water bath, and is stirred uniformly to obtain a mixed solution A, and then a proper amount of MgCl is added 2 ·6H 2 O and FeCl 3 ·6H 2 O, after all solids are completely dissolved, dropwise adding a strong alkali solution until the pH value is=10.0, placing the obtained mixed solution B into an electrothermal constant-temperature blast drying oven, and heating at 60 ℃ for 4 hours to obtainWashing the precipitate A with ultrapure water for multiple times, drying in a drying oven again to constant weight, pouring the obtained solid B into a quartz boat, calcining at constant temperature of 300 ℃ for 1h in a tube furnace filled with inert gas, cooling to room temperature, grinding and sieving with a 100-mesh sieve, washing with ultrapure water to pH=6.5-7.0, and drying at constant temperature of 105 ℃ for 12h to obtain the biochar-loaded magnesium ferrite adsorbent. The preparation method disclosed by the invention is simple in process and short in time consumption, and the produced adsorbent is excellent in magnetic property, good in chemical stability and high in adsorption efficiency, and can be widely used for removing heavy metal water bodies containing antimony and the like.
Description
Technical Field
The invention relates to the field of antimony-containing wastewater treatment, in particular to a biochar-loaded magnesium ferrite adsorbent, and a preparation method and application thereof.
Background
Heavy metal pollution is immeasurable to damage all organisms in the ecological system. In recent years, many researchers have found that the concentration of antimony in soil and water is high, and environmental problems caused by antimony pollution have attracted attention. After Sb enters the soil, pollution stress is formed on the soil ecosystem, the survival of soil organisms is influenced, the diversity of the soil organisms is destroyed, and finally the soil function is reduced. And long-term antimony and its compounds may damage human health and produce acute toxic effects on human organs. There is therefore an urgent need to develop a new technology for antimony pollution.
At present, the method for treating the antimony-containing wastewater mainly comprises an electrochemical method, an adsorption method, a biological oxidation-reduction method, an ion exchange method, a coagulating sedimentation method, a membrane separation method and the like, and is widely used as a promising heavy metal treatment technology due to the characteristics of low operation cost, high adsorption performance, environmental friendliness and the like of the adsorption method. Compared with the traditional adsorption method, the research at the current stage of the adsorption technology mainly focuses on modification or utilizes a synthesis method to prepare the adsorption material with high adsorption performance. The development of a low cost, high performance adsorbent that can replace traditional commercial activated carbon is therefore a challenge that researchers need to face.
Disclosure of Invention
Aiming at the problems, the invention provides the biochar-loaded magnesium ferrite adsorbent with excellent magnetic property, large specific surface area, high surface active site, good chemical stability and high adsorption efficiency, and also provides a preparation method with simple process and short time consumption.
The technical scheme adopted for solving the technical problems is as follows: the preparation method of the biochar loaded magnesium ferrite adsorbent comprises the following steps:
s1, cleaning, drying and crushing shaddock peel, and sieving to obtain shaddock peel powder;
s2, adding a proper amount of ultrapure water into a proper amount of shaddock peel powder at a constant temperature of 25 ℃ in a water bath, and stirring to uniformly disperse the shaddock peel powder to obtain a mixed solution A;
s3, adding a proper amount of MgCl into the mixed solution A obtained in the step S2 2 ·6H 2 O and proper amount of FeCl 3 ·6H 2 O, the shaddock peel powder and MgCl 2 ·6H 2 O and FeCl 3 ·6H 2 O is added dropwise to pH=10.0 after all solids are completely dissolved, so as to obtain a mixed solution B;
s4, placing the mixed solution B obtained in the step S3 into an electrothermal constant-temperature blast drying oven, and heating at 60 ℃ for 4 hours to obtain a precipitate A;
s5, flushing the sediment A obtained in the S4 with ultrapure water for a plurality of times, flushing the unreacted and reacted soluble salt, putting the washed and reacted soluble salt into a blast drying oven again, and drying the washed and reacted soluble salt at 105 ℃ until the weight is constant to obtain a solid B;
s6, pouring the solid B obtained in the S5 into a quartz boat, calcining for 1 hour at the constant temperature of 300 ℃ in a tube furnace filled with inert gas at the heating rate of 5 ℃/min and under the condition of continuously filling the inert gas with 25mL/L, and then cooling;
and S7, cooling to room temperature, grinding with an agate mortar, sieving with a 100-mesh sieve, flushing with ultrapure water to pH=6.5-7.0, and finally baking at a constant temperature of 105 ℃ for 12 hours to obtain the biochar-loaded magnesium ferrite adsorbent.
Preferably, the strong base solution in S3 is 5mol/L sodium hydroxide solution.
Preferably, the MgCl as described in S3 2 ·6H 2 O and FeCl 3 ·6H 2 The concentrations of O were all analytically pure.
Preferably, the inert gas in S6 is nitrogen.
Preferably, the stirring time of the stirring in S2 is 30 minutes.
The invention also provides the biochar-loaded magnesium ferrite adsorbent prepared by the biochar-loaded magnesium ferrite adsorbent preparation method.
The invention also provides an application of the biochar loaded magnesium ferrite adsorbent in removing antimony from Sb-containing wastewater, which comprises the following steps: adding the biochar loaded magnesium ferrite adsorbent into the Sb-containing wastewater solution, controlling the temperature to be 25 ℃ and the pH value to be 2, wherein the concentration ratio of the biochar loaded magnesium ferrite adsorbent to the Sb-containing wastewater solution is 1:1, quantitatively sampling by a disposable syringe after adsorption is finished, filtering by a microporous filter membrane with the diameter of 0.45 mu m, and finally measuring the concentration of the residual Sb solution after adsorption by a flame atomic absorption spectrophotometer to finish the treatment of the Sb-containing wastewater.
Compared with the prior art, the invention has the following beneficial effects:
1. the biochar loaded magnesium ferrite adsorbent has excellent magnetic properties, so that the biochar loaded magnesium ferrite adsorbent can realize rapid separation from a liquid phase by virtue of the action of an external magnetic field after adsorption is finished, avoids inconvenience caused by centrifugation or filtration separation, is convenient to recycle, reduces operation difficulty and cost, and improves adsorption efficiency;
2. the biochar loaded magnesium ferrite adsorbent has a relatively loose and porous structure, obvious particle distribution, high specific surface area, certain water solubility and dispersibility, more active sites, and good adsorption performance on heavy metal ions such as antimony and the like;
3. the preparation method of the biochar loaded magnesium ferrite adsorbent has simple process and low cost, and is suitable for large-scale production and application;
4. the biochar loaded magnesium ferrite adsorbent can adsorb and remove some heavy metal ions in water, has high adsorption efficiency, easily controlled conditions and stable chemical properties, and can be widely used for removing heavy metal water containing antimony and the like.
Drawings
FIG. 1 is a scanning electron microscope image of a biochar-supported magnesium ferrite adsorbent of the present invention;
FIG. 2 is a Fourier infrared spectrum of the biochar-loaded magnesium ferrite adsorbent of the invention;
FIG. 3 is a schematic diagram showing the relationship between the adsorption efficiency of the biochar-loaded magnesium ferrite adsorbent of the invention to Sb in the Sb-containing wastewater solution and the change of pH value;
FIG. 4 is a schematic diagram showing the relationship between the adsorption efficiency of the biochar-loaded magnesium ferrite adsorbent of the invention to Sb in an Sb-containing wastewater solution and the change of the adsorption efficiency with the adsorption time;
FIG. 5 is a schematic diagram showing the relationship between the adsorption efficiency of the biochar-loaded magnesium ferrite adsorbent of the invention to Sb in an Sb-containing wastewater solution and the change of the adsorption amount;
FIG. 6 is a schematic diagram showing the relationship between the adsorption efficiency of the biochar-loaded magnesium ferrite adsorbent of the invention to Sb in an Sb-containing wastewater solution and the change of the adsorption efficiency with temperature.
Detailed Description
The present invention will now be described in detail with reference to fig. 1-6, wherein the exemplary embodiments and descriptions of the present invention are provided for illustration of the present invention and are not intended to be limiting.
The preparation method of the biochar loaded magnesium ferrite adsorbent specifically comprises the following steps:
s1, cleaning, drying and crushing shaddock peel, and sieving to obtain shaddock peel powder;
s2, adding 5.00g of shaddock peel powder into 100mL of ultrapure water at a constant temperature of 25 ℃ in a water bath, stirring for 30 minutes, and uniformly dispersing the shaddock peel powder in 100mL of ultrapure water to obtain a mixed solution A;
s3, adding 4.060g of MgCl into the mixed solution A obtained in the step S2 2 ·6H 2 O and a proper amount of 10.812g FeCl 3 ·6H 2 O, in particular MgCl 2 ·6H 2 O and FeCl 3 ·6H 2 The concentration of O is analytically pure, and the shaddock peel powder and MgCl 2 ·6H 2 O and FeCl 3 ·6H 2 O is added dropwise to a pH value of 10.0 after all solids are completely dissolved, wherein the mass ratio of O is 1:0.8-0.9:2.1-2.3, and a 5mol/L sodium hydroxide solution is added dropwise to obtain a mixed solution B;
s4, placing the mixed solution B obtained in the step S3 into an electrothermal constant-temperature blast drying oven, and heating at 60 ℃ for 4 hours to obtain a precipitate A;
s5, flushing the sediment A obtained in the S4 with ultrapure water for a plurality of times, flushing the unreacted and reacted soluble salt, putting the washed and reacted soluble salt into a blast drying oven again, and drying the washed and reacted soluble salt at 105 ℃ until the weight is constant to obtain a solid B;
s6, pouring the solid B obtained in the S5 into a quartz boat, and calcining for 1h at the constant temperature of 300 ℃ and then cooling under the condition of continuously filling nitrogen into the quartz boat at the heating rate of 5 ℃/min and 25 mL/L;
and S7, cooling to room temperature, grinding with an agate mortar, sieving with a 100-mesh sieve, flushing with ultrapure water to pH=6.5-7.0, and finally baking at a constant temperature of 105 ℃ for 12 hours to obtain the biochar-loaded magnesium ferrite adsorbent.
The application of the biochar loaded magnesium ferrite adsorbent prepared by the preparation method in removing antimony in Sb-containing wastewater comprises the following steps: adding 100mg of the biochar-loaded magnesium ferrite adsorbent into 100mL of Sb-containing wastewater solution, controlling the temperature to 25 ℃ and the pH value to 2, specifically, taking out samples quantitatively by a disposable syringe after the adsorption is finished and filtering by a 0.45 mu m microporous filter membrane, and finally measuring the concentration of the residual Sb solution after adsorption by a flame atomic absorption spectrophotometer to finish the treatment of the Sb-containing wastewater.
The biochar loaded magnesium ferrite adsorbent of the invention utilizes MgCl 2 ·6H 2 O and FeCl 3 ·6H 2 Adding O into mixed shaddock peel powder water,then the precursor is obtained through operations such as drying, water washing and the like, and then the precursor is prepared in N 2 The sediment is put into a tube furnace of a quartz boat at a heating rate of 5 ℃/min for calcination, so that the precursor is completely converted into the biochar, the biochar and the iron-magnesium oxide are well loaded together, the adsorbent has a loose and porous structure, and meanwhile, the adsorbent has a good magnetic effect, the adsorption efficiency is greatly increased, and the application value of the biochar loaded manganese ferrite adsorbent is ensured.
The biochar-supported magnesium ferrite adsorbent prepared by the above preparation method was subjected to the test of the following examples.
Example 1
The charcoal loaded magnesium ferrite adsorbent is observed by a scanning electron microscope, as shown in fig. 1, a plurality of particles are deposited on the shaddock peel charcoal, and the particles are distributed uniformly and have no obvious agglomeration, which indicates that the iron magnesium oxide is successfully dispersed on the shaddock peel charcoal. From the figure, it can be clearly observed that the shaddock peel biochar obtained by pyrolysis presents a relatively uniform three-dimensional network structure and has more pore structures, which is probably caused by the development of the shaddock peel structure. The rich net structure is beneficial to improving the specific surface area of the material, thereby promoting the adsorption of pollutants in the wastewater by the adsorbent. The adsorbent is subjected to Fourier infrared spectrum analysis, and according to the infrared spectrum result, as shown in figure 2, the functional groups on the substance on the surface of the electrode can be judged to comprise O-H bond, C-O bond and Fe-O bond, wherein the specific figure is 3386.13cm -1 Corresponding to O-H bond, 1406.70cm -1 Corresponding to C-O bond, 432.24cm -1 The Fe-O bond is the typical frequency band of the spinel structure, which shows that the spinel magnesium ferrite is successfully prepared, and in conclusion, the biochar loaded magnesium ferrite adsorbent is successfully prepared.
Example 2
The biochar loaded magnesium ferrite adsorbent adsorbs Sb in the Sb-containing wastewater solution:
the biochar loaded magnesium ferrite adsorbent prepared in test example 1 is used for adsorbing heavy metal Sb in aqueous solution, the standard solution of the Sb-containing wastewater solution used in the experiment is 500ppm (500 mg/L), the concentration of the Sb-containing wastewater solution used in the experiment is obtained by diluting the standard solution, and the experiment is carried out in a polyethylene bottle of 100 mL. The test procedure for adsorbing Sb in Sb-containing wastewater solution was as follows:
preparing 10 groups of 100mL Sb-containing wastewater solutions with the concentration of 10mg/L, regulating the initial pH of the solutions to be 2, 4, 6, 8 and 10 respectively by using 0.1mol/L HCl and 0.1mol/L NaOH, adding 100mg of adsorbent into the solutions, fully reacting at about 25 ℃, sampling after 24 hours, filtering the sampled solution by using a 0.45 mu m water system microporous filter membrane, and measuring the concentration of the residual Sb-containing wastewater solution after adsorption by using a flame atomic absorption spectrophotometer. As shown in FIG. 3, the results of the experiment show that the removal rate of Sb was 96.61% when the pH of the solution was 2. When the pH values of the solutions were 4, 6, 8 and 10, the adsorption removal rates for Sb were 87.57%,85.73%,83.63% and 74.60%, respectively. The influence and removal rate of the pH value of the solution on the adsorption capacity of Sb show that the adsorption capacity is reduced from 9.56mg/g to 7.46mg/g along with the increase of the pH value except the same rule.
Three groups of Sb solutions with the concentration of 10mg/L,20mg/L and 30mg/L respectively are prepared, 100mg of adsorbent is added into the Sb solutions, the Sb solutions are carried out at the temperature of about 25 ℃ and the pH value of the Sb solutions is=2, quantitative sampling is carried out by a disposable syringe according to the time intervals of 10min, 30min, 1h, 2h, 4h, 8h, 12h and 24h, and the Sb solutions are filtered by a microporous filter membrane of 0.45 mu m. The content of Sb in the solution was measured with a flame atomic absorption spectrophotometer. As shown in the experimental results in FIG. 4, as shown in FIG. 4, the removal rate of Sb by the biochar-loaded magnesium ferrite adsorbent is faster in all three different concentrations in the first 120min, and especially in the initial concentration of 10mg/L, the removal rate of Sb reaches 55.54% in 120 min. At 240min, the removal rate of the adsorbent to Sb is basically similar at different concentrations and is in the range of 73-76%. The removal rate of Sb is in a slow change trend within 240-720 min, the removal rate of Sb by the adsorbent is basically balanced within 720min, namely 12h, and reaches more than 80%, and then the removal rate of Sb is in a stable state.
Preparing 6 groups of 100mL Sb-containing wastewater solutions with the concentration of 10mg/L, adding 0.005g, 0.01g, 0.02g, 0.05g, 0.1g and 0.2g of adsorbents respectively, fully reacting at the temperature of about 25 ℃ for 24 hours, sampling, filtering the sampled solution by a 0.45 mu m water system microporous filter membrane, and measuring the concentration of the residual Sb-containing wastewater solution after adsorption by a flame atomic absorption spectrophotometer. As shown in fig. 5, it is clear from fig. 5 that the adsorption capacity of the biochar-supported magnesium ferrite adsorbent to Sb gradually decreases with the increase of the amount of the adsorbent added. When the addition amount of the adsorbent is between 0.05g/L and 1g/L, the removal rate of Sb is increased from 23.96% to 81.99% along with the increase of the addition amount of the adsorbent, but when the dosage is between 1g/L and 2g/L along with the increase of the addition amount, the adsorption efficiency is basically unchanged, and the adsorption dynamic balance state is reached.
Preparing 3 groups of 100mL of Sb-containing wastewater solution with the concentration of 10mg/L, adding 100mg of adsorbent into the solution, respectively placing the solution at the temperature of 25 ℃, the temperature of 35 ℃, the temperature of 45 ℃ and the pH=2.0, sampling after the reaction is carried out fully, and the sample is sampled, filtering the sampled solution through a 0.45 mu m water system microporous filter membrane, and measuring the concentration of the residual Sb-containing wastewater solution after adsorption by using a flame atomic absorption spectrophotometer. As shown in fig. 6, the experimental results show that as the reaction temperature increases, the adsorption effect increases, and the adsorption performance analysis was performed at 25 ℃ and room temperature, which is selected from the experimental consideration of the difficulty of temperature increase in the actual removal process, as shown in fig. 6.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above examples, and all technical solutions belonging to the concept of the present invention belong to the protection scope of the present invention. It should be noted that improvements and modifications to the present invention without departing from the principles of the present invention should also be considered as the scope of the present invention for those of ordinary skill in the art.
Claims (7)
1. The preparation method of the biochar-loaded magnesium ferrite adsorbent is characterized by comprising the following steps of:
s1, cleaning, drying and crushing shaddock peel, and sieving to obtain shaddock peel powder;
s2, adding a proper amount of ultrapure water into a proper amount of shaddock peel powder at a constant temperature of 25 ℃ in a water bath, and stirring to uniformly disperse the shaddock peel powder to obtain a mixed solution A;
s3, adding a proper amount of MgCl into the mixed solution A obtained in the step S2 2 ·6H 2 O and proper amount of FeCl 3 ·6H 2 O, the shaddock peel powder and MgCl 2 ·6H 2 O and FeCl 3 ·6H 2 O is added dropwise to pH=10.0 after all solids are completely dissolved, so as to obtain a mixed solution B;
s4, placing the mixed solution B obtained in the step S3 into an electrothermal constant-temperature blast drying oven, and heating at 60 ℃ for 4 hours to obtain a precipitate A;
s5, flushing the sediment A obtained in the S4 with ultrapure water for a plurality of times, flushing the unreacted and reacted soluble salt, putting the washed and reacted soluble salt into a blast drying oven again, and drying the washed and reacted soluble salt at 105 ℃ until the weight is constant to obtain a solid B;
s6, pouring the solid B obtained in the S5 into a quartz boat, calcining for 1 hour at the constant temperature of 300 ℃ in a tube furnace filled with inert gas at the heating rate of 5 ℃/min and under the condition of continuously filling the inert gas with 25mL/L, and then cooling;
and S7, cooling to room temperature, grinding with an agate mortar, sieving with a 100-mesh sieve, flushing with ultrapure water to pH=6.5-7.0, and finally baking at a constant temperature of 105 ℃ for 12 hours to obtain the biochar-loaded magnesium ferrite adsorbent.
2. The method for preparing the biochar-supported magnesium ferrite adsorbent according to claim 1, wherein the method comprises the following steps: the strong alkali solution in S3 is 5mol/L sodium hydroxide solution.
3. The method for preparing the biochar-supported magnesium ferrite adsorbent according to claim 1, wherein the method comprises the following steps: mgCl as described in S3 2 ·6H 2 O and FeCl 3 ·6H 2 The concentrations of O were all analytically pure.
4. The method for preparing the biochar-supported magnesium ferrite adsorbent according to claim 1, wherein the method comprises the following steps: the inert gas in S6 is nitrogen.
5. The method for preparing the biochar-supported magnesium ferrite adsorbent according to claim 1, wherein the method comprises the following steps: the stirring time of the stirring in S2 was 30 minutes.
6. The biochar-supported magnesium ferrite adsorbent manufactured by the biochar-supported magnesium ferrite adsorbent manufacturing method according to any one of claims 1 to 5.
7. The use of the biochar-supported magnesium ferrite adsorbent for removing antimony from Sb-containing wastewater according to claim 6, comprising the steps of: adding the biochar loaded magnesium ferrite adsorbent into the Sb-containing wastewater solution, controlling the temperature to be 25 ℃ and the pH value to be 2, wherein the concentration ratio of the biochar loaded magnesium ferrite adsorbent to the Sb-containing wastewater solution is 1:1, quantitatively sampling by a disposable syringe after adsorption is finished, filtering by a microporous filter membrane with the diameter of 0.45 mu m, and finally measuring the concentration of the residual Sb solution after adsorption by a flame atomic absorption spectrophotometer to finish the treatment of the Sb-containing wastewater.
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