CN109019699B - Preparation method of rod-like ferroferric oxide particle-loaded biochar composite material - Google Patents
Preparation method of rod-like ferroferric oxide particle-loaded biochar composite material Download PDFInfo
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- C01G49/00—Compounds of iron
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- C01G49/08—Ferroso-ferric oxide (Fe3O4)
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- 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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Abstract
A preparation method of a rod-shaped ferroferric oxide particle-loaded biochar composite material relates to a preparation method of a biochar composite material. The method aims to solve the problems that the existing preparation method for the biochar surface loaded with the metal oxide particles consumes long time and the particles are easy to agglomerate. The method comprises the following steps: firstly, modifying and electrolyzing the mixture solution by electrochemical assistance: shearing, crushing, washing, drying and sieving the biomass material to obtain fine biomass material powder; mixing the biomass material fine powder with a metal salt solution, applying voltage to the mixed solution by using a direct-current voltage-stabilizing power supply, stirring for reaction to obtain a solid-liquid mixture, and drying; and secondly, placing the dried mixture in a tubular furnace, heating and pyrolyzing to obtain the ferroferric oxide particle-loaded biochar composite material. The method reduces the reaction time and enhances the adsorption capacity and absorption rate of the material. The invention is used for removing heavy metal ions in sewage.
Description
Technical Field
The invention relates to a preparation method of a biochar composite material.
Background
Fe3O4The particles, as one of the representative magnetic materials, are widely used in the field of removing heavy metals from water bodies due to their characteristics of large specific surface area, high surface energy, easy preparation and the like. However, in general Fe3O4Severe agglomeration of the particles can occur, further resulting in larger particles being formed, thereby significantly reducing reactivity and mobility. Thus, Fe3O4The range of applications of the particles is limited.
Biochar is used as a sustainable carbon source, and is widely used as an effective adsorbent for removing organic pollutants and heavy metal ions in water and soil environment due to wide sources, low price and easy availability of preparation raw materials. Among them, the hierarchical porous structure is often considered as a main factor that the biochar has a strong adsorption affinity for various contaminants. In practical application, the simple separation of the powdered biochar from the aqueous solution can effectively capture heavy metal ions, which has great significance and draws great attention.
The existing preparation method of the biochar surface loaded metal oxide particles has long consumption time and the particles are easy to agglomerate.
Disclosure of Invention
The invention provides a preparation method of a rod-shaped ferroferric oxide particle-loaded biochar composite material, aiming at solving the problems of long consumption time and easy agglomeration of particles in the existing preparation method of biochar surface-loaded metal oxide particles.
The preparation method of the rod-shaped ferroferric oxide particle-loaded biochar composite material comprises the following steps:
firstly, modifying and electrolyzing the mixture solution by electrochemical assistance:
shearing and crushing the biomass material, washing the biomass material for 3 to 10 times by using distilled water, drying the biomass material at the temperature of between 60 and 90 ℃, and sieving the dried biomass material by using a 20-100-mesh sieve to obtain fine biomass material powder;
mixing the biomass material fine powder with a metal salt solution to obtain a mixed solution, applying voltage to the mixed solution by using a direct current stabilized voltage supply (Agilent E3646A DC), stirring and reacting for 3-15 min at a stirring speed of 500-1500 r/min to obtain a solid-liquid mixture, and finally drying the solid-liquid mixture at 70-100 ℃ under a vacuum condition to obtain a dried mixture;
the concentration of the metal salt solution in the first step is 0.1-2 mol/L;
the volume ratio of the mass of the biomass material fine powder to the metal salt solution in the step one is (1-5) g (1-50) mL;
and secondly, placing the dried mixture in a tubular furnace, introducing inert gas into the tubular furnace, heating the tubular furnace to 500-700 ℃ under the protection of the inert gas, and pyrolyzing at the temperature of 500-700 ℃ under the protection of inert gas atmosphere to obtain the ferroferric oxide particle-loaded biochar composite material.
Further, the biomass material in the step one is one or a mixture of more of corn straw, rice hull, wood dust and bamboo.
Further, the metal salt solution in the step one is an iron salt solution.
Further, the ferric salt in the ferric salt solution is FeCl3·6H2O、Fe2(SO4)3Or Fe (NO)3)3·9H2O。
Further, in the first step, the applied voltage is 0-60V.
Further, the inert gas in the second step is nitrogen or argon.
Further, in the second step, the temperature rise rate of the tubular furnace is 3-10 ℃/min when the temperature is raised to 500-700 ℃ under the protection of inert gas.
Further, the pyrolysis time in the second step is 0.5-2 h.
The invention has the beneficial effects that:
1. the invention takes biomass materials as raw materials, and prepares the rod-shaped ferroferric oxide particle-loaded biochar composite material by a method combining electrochemical assistance and pyrolysis activation. The composite material has larger specific surface area, and the specific surface area of the rod-like ferroferric oxide particle-loaded biochar composite material prepared by the invention is 100.02m2The rod-shaped ferroferric oxide particles are uniformly dispersed on the surface of the charcoal material, so that the dispersion degree of the rod-shaped ferroferric oxide particles is improved;
2. the biomass material and the metal salt solution are mixed, then a voltage is applied to the mixed solution by using a direct current stabilized voltage supply (Agilent E3646ADC), electrochemical modification plays a role in activating the biomass to a certain extent, and the surface functional groups of the biomass material can be effectively increased. In addition, the use of ferric chloride as the electrolyte generates strong oxidants (i.e., HOCl and OCl) in solution by electrochemical reaction within a few minutes-) The time for soaking iron ions into biomass is obviously shortened (only 10 minutes is needed), and binding sites of the rod-shaped ferroferric oxide particles loaded with the biochar composite material are provided. Thereby enhancing the adsorption capacity of the material andthe rate of absorption.
3. Biomass materials (such as corn stalks, wood chips and bamboo poles) are used as agricultural wastes, and the economic cost of synthetic materials is reduced due to wide material sources, low price and easy obtainment;
4. according to the invention, the rod-shaped ferroferric oxide magnetic material and the agricultural waste biomass material are combined to prepare the composite material, and the utilization efficiency of the composite material in the environment is improved due to the synergistic effect of the rod-shaped ferroferric oxide magnetic material and the agricultural waste biomass material; the rod-like ferroferric oxide particle loaded biochar composite material prepared by the invention removes heavy metal Pb2+The adsorption amount of the adsorbent is 118.998-119.248 mg/g.
5. The invention uses electrochemistry assistance, the preparation method is rapid and efficient, the raw materials are cheap and easy to obtain, and the synthetic materials are easy to separate, thus being suitable for large-scale synthesis preparation.
Drawings
FIG. 1 is a scanning electron microscope photograph of a charcoal composite material loaded with rod-shaped ferroferric oxide particles prepared in example 1;
FIG. 2 is a scanning electron micrograph of the ferroferric oxide particle-supported biochar composite prepared in example 2;
FIG. 3 is a transmission electron micrograph of the ferroferric oxide particle-supported biochar composite prepared in example 1;
FIG. 4 is an XRD spectrum of a biological carbon composite material loaded with rod-shaped ferroferric oxide particles prepared in example 1;
fig. 5 is a nitrogen adsorption-desorption spectrum of the biological carbon composite material loaded with the rod-shaped ferroferric oxide particles prepared in example 1.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
The first embodiment is as follows: the preparation method of the rod-shaped ferroferric oxide particle-loaded biochar composite material comprises the following steps:
firstly, modifying and electrolyzing the mixture solution by electrochemical assistance:
shearing and crushing the biomass material, washing the biomass material for 3 to 10 times by using distilled water, drying the biomass material at the temperature of between 60 and 90 ℃, and sieving the dried biomass material by using a 20-100-mesh sieve to obtain fine biomass material powder;
mixing the biomass material fine powder with a metal salt solution to obtain a mixed solution, applying voltage to the mixed solution by using a direct-current voltage stabilization power supply, stirring and reacting for 3-15 min at a stirring speed of 500-1500 r/min to obtain a solid-liquid mixture, and finally drying the solid-liquid mixture under a vacuum condition at 70-100 ℃ to obtain a dried mixture;
wherein the concentration of the metal salt solution is 0.1-2 mol/L;
the volume ratio of the mass of the biomass material fine powder to the metal salt solution is (1-5) g (1-50) mL;
and secondly, placing the dried mixture in a tubular furnace, introducing inert gas into the tubular furnace, heating the tubular furnace to 500-700 ℃ under the protection of the inert gas, and pyrolyzing at the temperature of 500-700 ℃ under the protection of inert gas atmosphere to obtain the ferroferric oxide particle-loaded biochar composite material.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the biomass material in the step one is one or a mixture of more of corn straw, rice hull, wood dust and bamboo. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the metal salt solution in the step one is an iron salt solution. The other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the ferric salt in the ferric salt solution is FeCl3·6H2O、Fe2(SO4)3Or Fe (NO)3)3·9H2And O. The others are the same as in one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: in the first step, the applied voltage is 0-60V. The other is the same as one of the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: and the inert gas in the second step is nitrogen or argon. The other is the same as one of the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: in the second step, the temperature of the tubular furnace is raised to 500-700 ℃ under the protection of inert gas, and the heating rate is 3-10 ℃/min. The other is the same as one of the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: and the pyrolysis time in the second step is 0.5-2 h. The other is the same as one of the first to seventh embodiments.
The following examples are given to illustrate the present invention, and the following examples are carried out on the premise of the technical solution of the present invention, and give detailed embodiments and specific procedures, but the scope of the present invention is not limited to the following examples.
Example 1:
the preparation method of the rod-shaped ferroferric oxide particle-loaded biochar composite material comprises the following steps:
firstly, preparing a mixture composite material:
firstly, shearing and crushing corn straws, washing the corn straws for 5 times by using distilled water, drying the corn straws at the temperature of 80 ℃, and sieving the corn straws by using a 50-mesh sieve to obtain biomass material fine powder; (ii) a
And secondly, mixing the biomass material fine powder with 1.2mol/L ferric salt solution, applying 20V voltage to the mixed solution by using a direct current stabilized power supply (Agilent E3646A DC), and stirring and reacting for 10min at a stirring speed of 1000r/min to obtain a solid-liquid mixture. Finally, drying the solid-liquid mixture at 80 ℃ under a vacuum condition to obtain a dried mixture;
the ferric salt in the first step ② is FeCl3·6H2O；
The mass ratio of the biomass material fine powder to the ferric salt solution in the first step is 1g to 10 mL;
and secondly, placing the dried mixture in a tubular furnace, introducing nitrogen gas into the tubular furnace, heating the tubular furnace to 600 ℃ at the heating rate of 10 ℃/min under the protection of the nitrogen gas, and pyrolyzing the tubular furnace at the temperature of 600 ℃ for 1h under the protection of nitrogen gas atmosphere to obtain the rod-shaped ferroferric oxide particle-loaded biochar composite material.
The rod-like ferroferric oxide particle-loaded biochar composite material prepared in the embodiment is subjected to Langmuir model fitting at 55 ℃ and then heavy metal Pb is removed2+The maximum adsorption capacity of the adsorbent is up to 126.2mg/g, and the kinetic rate constant k2It was 0.054 g/mg. multidot.h.
The voltage-applying reaction time in this example is only 10min, and the rod-like ferroferric oxide particle-supported biochar composite material prepared in this example actually removes heavy metal Pb2+The adsorbed amount of (A) was 119.12 mg/g.
The scanning electron micrograph of the rod-shaped ferroferric oxide particle-supported biochar composite material prepared in the example is shown in fig. 1. From the low magnification scanning electron microscope image, it can be seen that a large number of layered structures are stacked together to form a carbon support with a complex structure after electrochemical pretreatment.
FIG. 3 shows a transmission electron microscope photograph of the rod-shaped ferroferric oxide particle-supported biochar composite material. Fe can be seen from the transmission electron micrograph3O4The rods have a diameter of about 7-8nm and a length of up to several hundred nanometers uniformly dispersed on the charcoal surface.
FIG. 4 shows an XRD spectrum of the biological carbon composite material loaded by the rod-shaped ferroferric oxide particles. The crystal structure can be confirmed by XRD spectrogram. For the rod-shaped ferroferric oxide particle-loaded biochar composite material, the amorphous phase of the biochar leads to a wide diffraction peak with a small angle, and an XRD (X-ray diffraction) pattern and Fe after electrochemical modification3O4(JCPDS No.88-0866) the characteristic peaks are perfectly matched, indicating Fe3O4The particles had a high degree of crystallinity and were deposited uniformly on the surface of the biochar, corresponding to SEM and TEM results.
FIG. 5 shows nitrogen absorption of a rod-shaped ferroferric oxide particle-loaded biochar composite materialAdsorption-desorption spectra. According to the IUPAC classification, the adsorption isotherm of a sample of the biochar composite loaded with rod-shaped ferroferric oxide particles is an isotherm belonging to type IV with a hysteresis loop of H4, which means that mesopores are present in the three composites. The specific surface area of the rod-shaped ferroferric oxide particle-loaded biochar composite material is 100.0m2/g。
Example 2:
the preparation method of the rod-shaped ferroferric oxide particle-loaded biochar composite material comprises the following steps:
firstly, preparing a mixture composite material:
firstly, shearing and crushing corn straws, washing the corn straws for 5 times by using distilled water, drying the corn straws at the temperature of 80 ℃, and sieving the corn straws by using a 50-mesh sieve to obtain biomass material fine powder;
② mixing the biomass material fine powder with 1.2mol/L ferric salt solution, stirring and reacting for 30min at the stirring speed of 1000 r/min. Finally, drying the solid-liquid mixture at 80 ℃ under a vacuum condition to obtain a dried mixture;
the ferric salt in the first step ② is FeCl3·6H2O；
The mass of finely divided biomass material powder and FeCl described in step one ②3The volume ratio of the solution is 1g to 10 mL;
and secondly, placing the dried mixture in a tubular furnace, introducing nitrogen gas into the tubular furnace, heating the tubular furnace to 600 ℃ at the heating rate of 10 ℃/min under the protection of the nitrogen gas, and pyrolyzing the tubular furnace at the temperature of 600 ℃ for 1h under the protection of nitrogen gas atmosphere to obtain the rod-shaped ferroferric oxide particle-loaded biochar composite material.
The rod-like ferroferric oxide particle-loaded biochar composite material prepared in the embodiment is subjected to Langmuir model fitting at 55 ℃ and then heavy metal Pb is removed2+The maximum adsorption capacity of the adsorbent is up to 87.4mg/g, and the kinetic rate constant k2The concentration was 0.068 g/mg. multidot.h.
The reaction time without voltage application in this example was 30min, which is longer. The heavy metal adsorption device is used for a long time, and the heavy metal adsorption effect is poor, so that the efficiency is low.
FIG. 2 shows a scanning electron micrograph of the ferroferric oxide particle-loaded biochar composite. Fe can be seen from scanning electron micrographs3O4There is an accumulation of irregular fragments and lumps with the biochar.
Claims (7)
1. A preparation method of a rod-shaped ferroferric oxide particle-loaded biochar composite material is characterized by comprising the following steps:
firstly, modifying and electrolyzing the mixture solution by electrochemical assistance:
shearing and crushing the biomass material, washing the biomass material with distilled water for 3-10 times, drying the biomass material at the temperature of 60-90 ℃, and screening the dried biomass material with a 20-100-mesh sieve to obtain fine biomass material powder;
mixing the biomass material fine powder with a metal salt solution to obtain a mixed solution, applying voltage to the mixed solution by using a direct-current voltage-stabilizing power supply, stirring and reacting for 3-15 min at a stirring speed of 500-1500 r/min to obtain a solid-liquid mixture, and finally drying the solid-liquid mixture at 70-100 ℃ under a vacuum condition to obtain a dried mixture;
wherein the concentration of the metal salt solution is 0.1-2 mol/L; the metal salt solution is an iron salt solution;
the volume ratio of the mass of the biomass material fine powder to the metal salt solution is (1-5) g (1-50) mL;
placing the dried mixture in a tubular furnace, introducing inert gas into the tubular furnace, heating the tubular furnace to 500-700 ℃ under the protection of the inert gas, and then pyrolyzing at 500-700 ℃ under the protection of the inert gas atmosphere to obtain the ferroferric oxide particle-loaded biochar composite material.
2. The preparation method of the rod-like ferroferric oxide particle-supported biochar composite material according to claim 1, characterized by comprising the following steps: the biomass material in the step one is one or a mixture of more of corn straw, rice hull, wood dust and bamboo.
3. The preparation method of the rod-like ferroferric oxide particle-supported biochar composite material according to claim 1 or 2, characterized by comprising the following steps: the ferric salt in the ferric salt solution is FeCl3·6H2O、Fe2(SO4)3Or Fe (NO)3)3·9H2O。
4. The preparation method of the rod-like ferroferric oxide particle-supported biochar composite material according to claim 3, characterized by comprising the following steps: in the first step, the applied voltage is 20-60V.
5. The preparation method of the rod-like ferroferric oxide particle-supported biochar composite material according to claim 4, characterized by comprising the following steps: and the inert gas in the second step is nitrogen or argon.
6. The preparation method of the rod-like ferroferric oxide particle-supported biochar composite material according to claim 5, characterized by comprising the following steps: and in the second step, the temperature rise rate of the tubular furnace is 3-10 ℃/min when the temperature of the tubular furnace is raised to 500-700 ℃ under the protection of inert gas.
7. The preparation method of the rod-like ferroferric oxide particle-supported biochar composite material according to claim 6, characterized by comprising the following steps: and the pyrolysis time in the second step is 0.5-2 h.
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