CN112295543A - A kind of preparation method and application of biochar with high-efficiency heavy metal adsorption performance - Google Patents
A kind of preparation method and application of biochar with high-efficiency heavy metal adsorption performance Download PDFInfo
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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
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- 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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- 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
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
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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
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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
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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Abstract
A preparation method and application of biochar with efficient heavy metal adsorption performance belong to the field of resource utilization of environment functional materials and biomass. The method comprises the following steps: drying, grinding and sieving the municipal sludge, and calcining the municipal sludge at high temperature in a tubular furnace to obtain the sludge-based biochar BC. Two 50mL mixed solutions of ethanol and water (volume ratio 1:1) were prepared and named as A, B solution, 2g of calcined sludge biochar BC was added to solution A, and 20.75g of FeCl was added to solution B36H2O and 2g of cetyltrimethylammonium bromide (CTAB), stirring, standing, centrifuging, and freeze-dryingDrying to obtain the modified sludge biochar nZVI-BC. The method has the advantages of simple process, stable preparation raw material source, low cost and the like, can efficiently and quickly remove heavy metal pollutants, and simultaneously provides a new way for resource utilization of sludge.
Description
Technical Field
The invention belongs to the field of environment functional materials and biomass resource utilization, and particularly relates to a modified sludge biochar material as well as a preparation method and application thereof.
Background
Heavy metals have been widely used in various industries including mining, leather tanning, electroplating, ferrous metallurgy or pigment synthesis and dyeing, etc., which results in the inevitable eventual release of heavy metals into the aqueous environment with the sewer line. It is characterized by high toxicity and non-biodegradability, which if not properly treated would pose a serious threat to aquatic life and human health. Research shows that lead as one of the highly toxic heavy metals threatens human health, mainly affects the central nervous system of human body, and causes diseases such as hepatitis, nephrotic syndrome and the like; cr (chromium) component6+Usually in the form of more mobile, easily soluble and toxic oxyanions, and direct skin contact with chromium compounds can cause skin damage and also affect respiratory tract, eyes, ears, gastrointestinal tract, etc.; excessive copper causes cirrhosis, diarrhea, vomiting, dyskinesia, and sensorineural disorder, etc. Therefore, people pay attention to the popularization of a more efficient and secondary pollution-free method for removing heavy metal ions in water.
The traditional heavy metal sewage treatment method has certain disadvantages, such as high cost and easy secondary pollution caused by a physical and chemical method; biological processes can only handle relatively low concentrations and are lengthy. Many studies have reported biochar as an adsorbent for removing heavy metals. Because the structure is stable, the specific surface area and the pore volume are large, the active functional groups are rich, and the biochar has wide application prospects in environmental remediation, soil improvement and wastewater treatment. Although biochar is inexpensive and readily available, its adsorption capacity is limited. In addition, biochar lacks stability and reusability, and its small particle size makes it difficult to recover from wastewater. The above factors limit the application of the biochar in the actual wastewater treatment, and the biochar has limited adsorption capacity to some heavy metal pollutants, and in order to obtain the biochar with stronger adsorption property, the biochar needs to be modified to enhance the physicochemical properties related to the adsorption capacity. Therefore, the invention adopts the method that the high-efficiency green environmental material, namely the nano zero-valent iron is loaded on the biological carbon to improve the adsorption capacity of the biological carbon to the heavy metals. The common zero-valent iron has certain effect on certain pollutants, but has slow degradation speed and is possible to generate extremely toxic byproducts, and the nano zero-valent iron has extremely high specific surface area, can realize reduction reaction on most heavy metals, and shows excellent performance in the aspect of removing organic pollutants and heavy metals in water. Studies have shown that the incorporation of nZVI into a biochar matrix enhances its adsorption properties. Therefore, the modified biochar (nZVI-BC) is prepared by taking municipal sludge as a raw material and compounding the nano zero-valent iron through a high-temperature slow pyrolysis method, is applied to the adsorption removal of heavy metals of chromium (Cr), copper (Cu) and lead (Pb), provides a new way for improving the preparation of biochar for adsorption removal of heavy metals in water, and realizes the resource utilization of sludge.
Disclosure of Invention
In view of the problems and technical analysis, the invention aims to provide a preparation method of a modified sludge biochar material, which is simple to operate and easy to obtain raw materials, and the prepared nZVI-BC has larger specific surface area and reducibility. The invention also aims to realize resource utilization of the sludge.
In order to achieve the first object, the invention adopts the following technical scheme:
a preparation method of biochar with high-efficiency heavy metal adsorption performance comprises the following steps:
(1) drying the sludge in a drying oven at 100 ℃ to constant weight, taking out, grinding and sieving by a 100-mesh sieve;
(2) putting the sludge obtained in the step (1) into a tube furnace, and introducing N2Heating to 700 ℃ at the speed of 10 ℃/min, staying for two hours, and then cooling to room temperature to obtain sludge-based biochar BC;
(3) preparing two 50mL mixed solutions of ethanol and water, namely A, B solution, wherein the volume ratio of the ethanol to the water is 1: 1; adding 2g of the sludge-based biochar BC prepared in the step (2) into the solution A, and simultaneously adding 20.75g of FeCl into the solution B3·6H2O and 2g cetyltrimethylammonium bromide (CTAB), wherein the CTAB functions to prevent nanoparticles produced in subsequent reactions from agglomerating;
(4) adding the two solutions prepared in step (3) into a three-neck flask, stirring for 30min, and then using one neck of the three-neck flask for supplying inert N2Gas to drive air into the flask to prevent oxidation of ZVI. 150mL of 0.6mol/L KBH added dropwise from another neck4Stirring for 6h at 25 ℃, standing and aging for 3 d;
(5) and (4) centrifuging the mixed solution in the step (4) at 15000rpm for 15min, washing the solid with 200mL of ethanol for five times, and carrying out vacuum freeze drying at-50 ℃ to obtain the biochar nZVI-BC with the performance of efficiently adsorbing heavy metals.
In order to achieve another purpose, the invention adopts the following technical scheme:
an application of a modified sludge biochar material as an adsorbent for heavy metals Cr, Cu and Pb, and used for efficiently adsorbing the heavy metals Cr, Cu and Pb.
The invention has the beneficial effects that: the modified sludge biochar (nZVI-BC) is successfully prepared by a high-temperature slow pyrolysis method and used for adsorbing and removing heavy metals in water, and the material has the advantages of good reducibility, large specific surface area and the like. The invention has simple process, stable preparation raw materials, low cost and the like, provides a new way for resource utilization of sludge, and has good environmental effect and social effect.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) of a modified sludge biochar material of the invention.
FIG. 2 is an XRD spectrum of the modified sludge biochar material of the invention.
FIG. 3 is a dynamic study diagram of the modified sludge biochar material of the invention for adsorbing and removing heavy metals Cr, Cu and Pb.
Detailed Description
The present invention will be described in detail below with reference to examples to enable those skilled in the art to better understand the present invention, but the present invention is not limited to the following examples.
Example 1:
modified sludge biochar material: taking a small amount of municipal sludge, placing the sludge in a drying oven to dry the sludge at 100 ℃ to constant weight, taking out the sludge, grinding the sludge, sieving the sludge with a 100-mesh sieve, placing the ground sludge in a tubular furnace, introducing N2Heating to 700 ℃ at the speed of 10 ℃/min, staying for two hours, and then cooling to room temperature to obtain sludge-based biochar BC; two 50mL mixed solutions of ethanol and water (v: v is 1:1) were prepared and named as A, B solution, and 2g of the prepared sludge-based biochar BC was added to solution A, while 20.75g of FeCl was added to solution B3·6H2O and 2g of cetyltrimethylammonium bromide (CTAB), and the two solutions prepared were again added to a three-necked flask and stirred for 30min, after which one neck of the three-necked flask was used for supplying inert N2Gas to drive air into the flask to prevent oxidation of ZVI. 150mL of 0.6mol/L KBH added dropwise from another neck4Stirring for 6h at 25 ℃, standing and aging for 3 d; and finally, centrifuging the mixed solution at 15000rpm for 15min, washing the solid with 200mL of ethanol for 5 times, and carrying out vacuum freeze drying at-50 ℃ to obtain the biochar nZVI-BC with the performance of efficiently adsorbing heavy metals.
SEM analysis results (FIG. 1) of the nZVI-BC adsorbent material showed the morphology of coarse and irregularly shaped microaggregates. Part of the pore structure present in BC was blocked by nZVI particles after modification. Coverage of nZVI on the modified biochar surface was further confirmed by EDS analysis. As shown in fig. 2, the material had only peaks of silica and calcium carbonate, while the main peak near 35 ° after modification confirmed the presence of nZVI, indicating that nano zero-valent iron particles were successfully loaded on the surface of the sludge-based biomass.
Example 2:
kinetic study of the nZVI-BC prepared in example 1 for the adsorption removal of the heavy metal chromium (Cr): dissolving an appropriate amount of Cr (VI) in a volumetric flask to prepare a stock solution of 1000mg/L, and then using 10mM NaNO3Diluted to the desired concentration. Adjusting the pH of the solution to 2-12 with 0.1M HCl and NaOH at intervals of 1, finally adjusting the pH of the solution to 3, then placing the reaction flask in a constant temperature oscillator at a temperature of 298K, shaking for 360min, taking supernatant at different time periods (1min, 5min, 10min, 30min, 60min, 180min, 360min, 540min, 720min and 1440min), filtering with a 0.45 mu M filter membrane, and determining the residual content of heavy metal Cr in the sample by a liquid chromatograph. As shown in FIG. 3, the adsorption rate was faster before 180min, then the adsorption rate began to decrease, and finally the equilibrium was reached around 540min, at which the adsorption amount of BC to Cr was only 54.39mg/g (FIG. 3), while the adsorption amount of nZVI-BC to Cr reached 174.6mg/g (FIG. 3).
Example 3:
kinetic study of the nZVI-BC prepared in example 1 for the adsorption removal of the heavy metal copper (Cu): a stock solution of 1000mg/L was prepared by dissolving an appropriate amount of copper (Cu) in a volumetric flask, followed by 10mM NaNO3Diluted to the desired concentration. Adjusting the pH of the solution to 2-12 with 0.1M HCl and NaOH at intervals of 1, finally adjusting the pH of the solution to 4, then placing the reaction flask in a constant temperature oscillator at a temperature of 298K, shaking for 360min, taking supernatant at different time periods (1min, 5min, 10min, 30min, 60min, 180min, 360min, 540min, 720min and 1440min), filtering with a 0.45 μ M filter membrane, and determining the residual content of Cu in the sample by liquid chromatography. As shown in FIG. 3, the adsorption rate was faster before 180min, then the adsorption rate began to decrease, and finally the equilibrium was reached around 540min, and the adsorption amount of BC to Cu was only 58.39mg/g (FIG. 3) at the equilibrium, while the adsorption amount of nZVI-BC to Cu was 209.5mg/g (FIG. 3), respectively.
Example 4:
kinetic study of the nZVI-BC prepared in example 1 for the adsorption removal of the heavy metal lead (Pb): a stock solution of 1000mg/L was prepared by dissolving an appropriate amount of lead (Pb) in a volumetric flask, followed by 10mM NaNO3Diluted to the desired concentration. The solution pH was adjusted to 2-12 with 0.1M HCl and NaOH at 1 intervals, finally adjusted to 4, then the reaction flask was placed in a constant temperature shaker at 298K and shaken for 360min, and the supernatant was taken at different time periods (1min, 5min, 10min, 30min, 60min, 180min, 360min, 540min, 720min, and 1440min), filtered with a 0.45 μ M filter, and the remaining content of Pb in the sample was determined by liquid chromatography. As shown in FIG. 3, the adsorption rate was faster before 180min, then the adsorption rate began to decrease, and finally the equilibrium was reached around 540min, at which the adsorption amount of BC to Pb was only 164.12mg/g (FIG. 3), while the adsorption amount of nZVI-BC to Pb was 598.8mg/g (FIG. 3).
Claims (2)
1. A preparation method of biochar with high-efficiency heavy metal adsorption performance is characterized by comprising the following steps:
(1) drying the sludge in a drying oven at 100 ℃ to constant weight, taking out, grinding and sieving by a 100-mesh sieve;
(2) putting the sludge obtained in the step (1) into a tube furnace, and introducing N2Heating to 700 ℃ at the speed of 10 ℃/min, staying for two hours, and then cooling to room temperature to obtain sludge-based biochar BC;
(3) two 50mL portions of a mixed solution of ethanol and water at a volume ratio of 1:1, named as A, B solution, were prepared, and 2g of the sludge-based biochar BC prepared in step (2) was added to the A solution, while 20.75g of FeCl was added to the B solution3·6H2O and 2g of cetyltrimethylammonium bromide CTAB, wherein the CTAB functions to prevent nanoparticles generated in subsequent reactions from condensing;
(4) adding the two solutions prepared in step (3) into a three-neck flask, stirring for 30min, and then using one neck of the three-neck flask for supplying inert N2Gas to drive air into the flask to prevent oxidation of ZVI; 150mL of 0.6mol/L KBH added dropwise from another neck4Stirring for 6h at 25 ℃, standing and aging for 3 d;
(5) and (4) centrifuging the mixed solution in the step (4) at 15000rpm for 15min, washing the solid with 200mL of ethanol for five times, and performing vacuum freeze drying at-50 ℃ to obtain the biochar nZVI-BC with the performance of efficiently adsorbing heavy metals.
2. The application of the biochar prepared by the preparation method of claim 1 is characterized in that the prepared biochar nZVI-BC is used as a heavy metal adsorbent for efficiently adsorbing heavy metals.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114149023A (en) * | 2021-12-02 | 2022-03-08 | 南京工程学院 | High-value conversion and reuse method for tobacco waste |
| CN115948169A (en) * | 2022-11-24 | 2023-04-11 | 生态环境部土壤与农业农村生态环境监管技术中心 | Preparation method and application of a biochar-loaded modified nano-zero-valent iron material |
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| CN114149023A (en) * | 2021-12-02 | 2022-03-08 | 南京工程学院 | High-value conversion and reuse method for tobacco waste |
| CN114149023B (en) * | 2021-12-02 | 2024-01-26 | 南京工程学院 | Method for high-value conversion and reutilization of tobacco waste |
| CN115948169A (en) * | 2022-11-24 | 2023-04-11 | 生态环境部土壤与农业农村生态环境监管技术中心 | Preparation method and application of a biochar-loaded modified nano-zero-valent iron material |
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