CN114433227A - Modified peat-magnetite composite magnetic Fenton material and preparation method and application thereof - Google Patents
Modified peat-magnetite composite magnetic Fenton material and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of Fenton materials, and particularly relates to a modified peat-magnetite composite magnetic Fenton material as well as a preparation method and application thereof. The preparation method comprises the following steps: ball-milling woody peat and natural magnetite particles to obtain uniform mixed powder, carrying out hydrothermal reaction on the obtained mixed powder to obtain a slurry product, drying, grinding, crushing and sieving to obtain the modified peat-magnetite composite magnetic Fenton material; the wood peat and natural magnetite particles which are widely distributed and have low price are used as raw materials, and the particle size of the materials is reduced to nano/micron grade by a high-energy ball milling method, so that the mass transfer process of the materials in the catalytic reaction is promoted. And then, carrying out hydrothermal reaction on the ball-milled materials, and modifying the hydrophobic woody peat under the conditions of higher temperature and the pressure of the reaction kettle, so that the hydrophilicity of the peat is improved, and the Fenton reactivity of the peat is enhanced.
Description
Technical Field
The invention belongs to the technical field of Fenton materials, and particularly relates to a modified peat-magnetite composite magnetic Fenton material as well as a preparation method and application thereof.
Background
The conventional heterogeneous Fenton catalytic method or catalytic wet hydrogen peroxide oxidation (CWPO) and other advanced oxidation technologies are mostly carried out by preparing the catalyst into a powder material, which makes the recovery of the catalyst difficult. Therefore, a magnetic fenton catalyst that can be recovered by a simple and efficient magnetic separation method has received much attention. Most of the existing magnetic Fenton catalysts are artificially synthesized magnetite (Fe)3O4) The preparation cost is high, the process is complex, the saturation magnetic susceptibility is generally lower than that of natural magnetite, and the magnetic separation performance is lower.
The natural magnetite has wide distribution and low price, and the common crystal lattice has the doping of Al, Ti, Ni and other elements, which is beneficial to improving the reactivity of the natural magnetite and is an ideal magnetic Fenton catalyst. In addition, Fe (II) may react with H in Fenton's reaction2O2The reaction generates highly active hydroxyl free radical (. OH), while Fe (III) is reacted with H2O2Reduction to Fe (II), but at a low reaction rate, and H2O2Is decomposed into low-activity superoxide radical (O)2 ·-) Further generating oxygen gas, resulting in H2O2The inefficiency of (c) is broken down. The lattice structure of magnetite contains Fe (II), so that the magnetite is compared with maghemite (gamma-Fe) which has the same magnetism but does not contain Fe (II)2O3) Has more value for Fenton reaction. However, natural magnetite is mostly in the form of dense block or granular aggregate, and even after the natural magnetite is subjected to procedures such as jaw crushing and the like, the particle size of the natural magnetite is still as high as 0.5-2 cm, which is not beneficial to the mass transfer process of catalytic reaction. In addition, for the Fenton reaction, Fe (II) in the magnetite lattice after the decomposition part is H2O2Oxidized to fe (iii). Therefore, the re-reduction of fe (iii) in magnetite is the key rate-limiting step limiting its fenton reactivity.
Due to the characteristics of abundant functional groups, high specific surface area, good electron transfer property and the like, many researchers use the carbon material to compound with magnetite and further promote the reduction of Fe (III) in the magnetite. Most of the common carbon materials are high-cost materials such as graphene oxide, carbon nanotubes and fullerol, which limits the application prospect of the carbon materials as environmental catalysts. Hydrothermal carbon is generally synthesized from glucose, starch, and the like, and is widely used in heterogeneous fenton reactions because of mild synthesis conditions. In addition, the hydrothermal carbon can generate abundant carbon center Persistent Free Radicals (PFRs) in the hydrothermal process, and can be used as an electron donor to promote the reduction of Fe (III) in the magnetite. However, the hydrothermal carbon using glucose and the like as raw materials still has the limitations of low yield, high raw material cost and the like, and the application value of the hydrothermal carbon material in the actual environment is limited.
Therefore, in order to solve the above problems, the present invention provides a fenton material with excellent performance by hydrothermally modifying a woody peat and loading magnetite thereon.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a modified peat-magnetite composite magnetic fenton material, a preparation method and an application thereof, so that the modified peat-magnetite composite magnetic fenton material can be used for treating water and soil pollution.
The technical content of the invention is as follows:
the invention provides a preparation method of a modified peat-magnetite composite magnetic Fenton material, which comprises the following steps:
ball-milling woody peat and natural magnetite particles to obtain uniform mixed powder, carrying out hydrothermal reaction on the obtained mixed powder to obtain a slurry product, drying, grinding, crushing and sieving to obtain the modified peat-magnetite composite magnetic Fenton material;
the carbon content of the woody peat is about 30-80%;
the mass ratio of the woody peat to the natural magnetite is 1: 1-9: 1;
the rotation speed of the ball milling is 300-900 rpm, and the ball milling is carried out until the particle size of the mixed powder is concentrated to 0.1-10 mu m;
the temperature of the hydrothermal reaction is 140-220 ℃, the time is 2-16 h, and the pressure in the hydrothermal conversion process comes from the self-pressure of the reaction kettle body;
the adopted woody peat substances are obtained by depositing and converting the remains of ancient higher plants in the crustal, and the original substances of lignin, cellulose and the like of the plants are converted into humus substances, quinones substances and the like with higher fenton activity under the influence of geological action, so that the method has a prospect of being applied to catalytic fenton reaction compared with the traditional hydrothermal carbon material.
The invention also provides the modified peat-magnetite composite magnetic Fenton material prepared by the method.
The invention also provides a modified peat-magnetite composite magnetic Fenton material applied to treatment of water and soil pollution.
The invention has the following beneficial effects:
according to the modified peat-magnetite composite magnetic Fenton material and the preparation method thereof, the widely distributed and low-cost woody peat and natural magnetite particles are used as raw materials, and the particle size of the material is reduced to nano/micron level by a high-energy ball milling method, so that the mass transfer process of the material in a catalytic reaction is promoted. And then, carrying out hydrothermal reaction on the ball-milled material, modifying the woody peat under the conditions of higher temperature and self pressure of the reaction kettle, so that the originally hydrophobic woody peat is changed into hydrophilic woody peat, and meanwhile, rich surface functional groups such as hydroxyl, carboxyl and the like are obtained, so that the Fenton reactivity of the woody peat is improved, binding sites with magnetite are increased, and meanwhile, the internal structure of the woody peat is gradually graphitized in the hydrothermal reaction, thereby being beneficial to the rapid transfer of electrons. In the Fenton reaction, the hydrothermal woody peat not only can utilize active substances such as PFRs which are rich in electrons per se to enable Fe (III) in the magnetite to be rapidly reduced, but also can directly participate in H2O2The efficiency of the fenton reaction is further improved. Compared with the traditional Fenton catalyst, the catalyst material has the advantages of low cost, high yield and easy recovery, also embodies the characteristics of good catalytic effect, low hydrogen peroxide consumption, high stability and favorable recovery in practical application, is used for the advanced treatment of water and soil pollution, and has the advantages of high treatment efficiency, simple operation and comprehensive costLow cost and the like.
Drawings
FIG. 1 is a graph comparing the efficiency of degrading bisphenol A by Fenton material and natural magnetite according to different proportions;
FIG. 2 is a graph comparing the efficiency of degrading bisphenol A by a sample of inventive woody peat, 50% Mag-HTP, 50% Mag-woody peat, HTP;
FIG. 3 is a graph showing the results of cyclic degradation of bisphenol A by the composite magnetic Fenton material of example 3;
FIG. 4 is a graph comparing the degradation rate of bisphenol A by Fenton's material of the present invention and the material prepared by comparative example;
fig. 5 is a Fe 2p characterization spectrum of X-ray photoelectron spectroscopy (XPS) after 8 reactions of the fenton material of the present invention.
Detailed Description
The present invention is described in further detail in the following description of specific embodiments and the accompanying drawings, it is to be understood that these embodiments are merely illustrative of the present invention and are not intended to limit the scope of the invention, which is defined by the appended claims, and modifications thereof by those skilled in the art after reading this disclosure that are equivalent to the above described embodiments.
All the raw materials and reagents of the invention are conventional market raw materials and reagents unless otherwise specified.
Example 1
Preparation of modified peat-magnetite composite magnetic Fenton material
The method comprises the following steps of (1) mixing woody peat and natural magnetite particles according to a mass ratio of 9:1, ball milling at the rotation speed of 900 rpm to obtain uniform mixed powder, carrying out hydrothermal reaction on the obtained mixed powder at 220 ℃ to obtain a slurry-like product, drying, grinding, crushing and sieving to obtain the 10% Mag-HTP hydrothermal woody peat-magnetite composite magnetic Fenton material.
Example 2
Preparation of modified peat-magnetite composite magnetic Fenton material
Mixing the woody peat and the natural magnetite particles according to the mass ratio of 3:7, carrying out ball milling at the rotating speed of 600 rpm to obtain uniform mixed powder, carrying out hydrothermal reaction on the obtained mixed powder at 180 ℃ to obtain a slurry-like product, drying, grinding, crushing and sieving to obtain the 30% Mag-HTP hydrothermal woody peat-magnetite composite magnetic Fenton material.
Example 3
Preparation of modified peat-magnetite composite magnetic Fenton material
Mixing the woody peat and the natural magnetite particles according to the mass ratio of 1:1, mixing, carrying out ball milling at the rotation speed of 300 rpm to obtain uniform mixed powder, carrying out hydrothermal reaction on the obtained mixed powder at 140 ℃ to obtain a slurry-like product, drying, grinding, crushing and sieving to obtain the 50% Mag-HTP hydrothermal woody peat-magnetite composite magnetic Fenton material.
As shown in fig. 1, the degradation efficiency of the natural magnetite and the degradation efficiency of the Mag-HTP prepared in examples 1 to 3 to bisphenol a are compared, and it can be seen that the degradation efficiency of the composite magnetic fenton material prepared in the embodiment of the present invention to bisphenol a is higher and the difference is more obvious.
Test examples
Soil remediation application of modified peat-magnetite composite magnetic Fenton material
The composite magnetic fenton material prepared in example 3 is used for an experiment of degrading a contaminated soil leachate, and the reaction conditions are as follows: the organic contaminated soil is taken from the vicinity of a chemical plant in Guangdong province, the solid-liquid ratio of the contaminated soil sample is 2:1, the concentration of hydrogen peroxide is 2 mmol/L, the adding amount of the catalyst is 0.2 g/L, the initial pH of the reaction is =3, the catalyst material is recovered through a magnetic rod after the experiment is finished, then the residual soil sample is centrifugally separated, the content of residual total organic carbon in the soil is measured, and the experiment result shows that more than 70% of the Total Organic Carbon (TOC) value of the contaminated soil sample is degraded.
Comparative example 1
Preparing Mag-woody peat: mixing the woody peat and the natural magnetite particles according to the mass ratio of 1:1, mixing, and performing ball milling at the rotating speed of 600-800 rpm to obtain uniform mixed powder, thereby obtaining the Mag-woody peat material.
As shown in fig. 2, which is a comparison of the degradation efficiency of the wood peat, the composite magnetic fenton material of example 3, the comparative example 1 and the HTP to bisphenol a, it can be seen that the degradation efficiency of the composite magnetic fenton material prepared by the example of the present invention to bisphenol a is higher and the difference is more obvious.
As shown in fig. 3, the experimental results of cyclic degradation of bisphenol a by the composite magnetic fenton material of example 3 are shown, and the reaction conditions are as follows: initial bisphenol A concentration of 30 mg/L, hydrogen peroxide concentration of 2 mmol/L, catalyst dosage of 0.2 g/L, initial reaction pH = 3. Therefore, the composite magnetic Fenton material prepared by the invention can still achieve better degradation effect on bisphenol A after 8 cycles, and the XPS characterization spectrogram of FIG. 5 finds Fe of magnetite in the catalyst material before and after reaction2+/Fe3+The proportion is not changed greatly, which shows that rich electrons contained in the hydrothermalized woody peat are continuously transferred to the magnetite to promote Fe in the magnetite3+Thereby ensuring the Fenton reaction.
Comparative example 2
Synthesis of magnetic Nanoparticles (NMP): 15mg of sodium citrate and 15mg of FeCl2·4H2O (synthetic magnetite) was added to 30 mL of deionized water, followed by 0.5mL of 25% NH3·H2And O. Oil bath at 80 ℃ for 4 hours, separated using a magnet, washed centrifugally and then freeze-dried (see paper Song et al, ACS appl. Nano mater, 2019).
Comparative example 3
Preparation of 50% NMP-HTP: weighing equal amount of woody peat powder and NMP powder, mixing and ball-milling (ball-material ratio is 10:1, rotation speed is 600 rpm, time is 2 h), then adding 3 g of ball-milled mixed powder into a reaction kettle, adding 40 mL of water, carrying out hydrothermal reaction at 180 ℃ for 4 h, cooling, taking out, washing and drying to obtain the product.
Comparative example 4
Mag-HTCglucoseThe preparation of (1): 20 g of glucose is weighed and dissolved in 400 mL of deionized water, and then an appropriate amount of ball-milled magnetite particles are added to the solution, and the mixture is placed into a reaction kettle and subjected to hydrothermal reaction at 180 ℃ for 8 hours. The obtained mixture is centrifuged, washed and dried to obtain the product.
Comparative example 5
Preparation of 50% Mag-PBC: putting the woody peat into a tube furnace, introducing nitrogen for protection, heating to 500 ℃ at the heating rate of 10 ℃/min, keeping for 1 hour, cooling, taking out, mixing natural magnetite, and then carrying out ball milling for 2 hours (ball-to-material ratio 10:1, rotating speed 600 rpm) to obtain a Mag-PBC sample (refer to the paper Zhang et al, Sci. Total environ, 2021).
As shown in FIG. 4, the adsorption effect of the 50% NMP-HTP material was slightly higher than that of the composite magnetic Fenton material of example 3, due to artificially synthesized magnetite (Fe)3O4) The aging time of the particles in the synthesis process is greatly shortened compared with that of natural magnetite, so that the crystallinity is weak, and the grain sizes are all in the nanometer level, thereby slightly increasing the specific surface area of the material and enhancing the adsorption effect of the material on BPA. However, the 50% NMP-HTP material had a less than adequate BPA degradation rate than the composite magnetic Fenton material of example 3 (50% Mag-HTP), again due to the synthesized Fe3O4The crystallinity is weaker, and the material is compared with solid-phase Fe of natural magnetite2+The content is insufficient, and thus the reactivity is insufficient. The 50% Mag-PBC material has an increased adsorption rate to BPA compared to the composite magnetic fenton material of example 3, which indicates that the specific surface area of Mag-PBC may increase after heat treatment, which is consistent with the conclusion that the specific surface area of the biochar material obtained by heat treatment at 500 ℃ or higher is significantly increased as mentioned in the literature (Li et al, sci. Total environ, 2021).
Another reason for enhancing the adsorption capacity of 50% Mag-PBC to BPA is that the graphitization degree of the biochar is increased due to high-temperature heating of the material, so that the hydrophobicity of the biochar is increased, and the adsorption performance to organic matters is enhanced. However, it can be seen that the degradation effect of 50% Mag-PBC on BPA is rather lagged behind that of other materials, because some of the fenton-reactive substances contained in the woody peat (such as quinones, humus and some persistent radical PFRs) can be retained by hydrothermal processes, and the structure of the woody peat is destroyed by the high-temperature pyrolysis process, and the materials as a whole exhibit characteristics similar to those of ordinary graphite or activated carbon, so that the reactivity of 50% Mag-PBC material is lower than that of 50% Mag-HTP material. And Mag-HTC synthesized by taking glucose as precursorglucoseMaterialActive functional groups and PFRs with abundant electrons are formed, but do not contain the ability to directly promote H2O2Decomposed species or functional groups, and thus the fenton reactivity of the material is reduced compared to the 50% Mag-HTP material.
Claims (6)
1. A preparation method of a modified peat-magnetite composite magnetic Fenton material is characterized by comprising the following steps:
ball-milling woody peat and natural magnetite particles to obtain uniform mixed powder, carrying out hydrothermal reaction on the obtained mixed powder to obtain a slurry product, drying, grinding, crushing and sieving to obtain the modified peat-magnetite composite magnetic Fenton material;
the carbon content of the woody peat is 50-80%.
2. The method for preparing a composite magnetic Fenton material according to claim 1, wherein the mass ratio of the woody peat to the natural magnetite is 1: 1-9: 1.
3. The method for preparing a composite magnetic Fenton material according to claim 1, wherein the rotation speed of the ball mill is 300-900 rpm.
4. The method for preparing a composite magnetic Fenton material according to claim 1, wherein the temperature of the hydrothermal reaction is 140-220 ℃.
5. A modified peat-magnetite composite magnetic Fenton material prepared by the method of any one of claims 1 to 4.
6. The modified peat-magnetite composite magnetic Fenton material according to claim 5, which is applied to the treatment of water and soil pollution.
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