CN118719003A - Sludge-based magnetic biochar, preparation method and application - Google Patents
Sludge-based magnetic biochar, preparation method and application Download PDFInfo
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- 239000012528 membrane Substances 0.000 claims description 4
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- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
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- KVGZZAHHUNAVKZ-UHFFFAOYSA-N 1,4-Dioxin Chemical compound O1C=COC=C1 KVGZZAHHUNAVKZ-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/40—Valorisation of by-products of wastewater, sewage or sludge processing
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- Treatment Of Sludge (AREA)
Abstract
The invention relates to a sludge-based magnetic biochar, a preparation method and application thereof. The preparation method of the sludge-based magnetic biochar comprises the following steps: mixing the residual sludge and the residual biogas residue in an inert atmosphere, then heating to a target temperature, and performing pyrolysis treatment to obtain an intermediate; soaking the intermediate in an acid solution, and performing ultrasonic treatment to obtain sludge-based magnetic biochar; the surplus sludge is sludge treated by a dehydrating agent; the residual biogas residue is the biogas residue treated by the dehydrating agent. The invention also provides the sludge-based magnetic biochar prepared by the preparation method. The invention also provides application of the sludge-based magnetic biochar prepared by the preparation method, and application of the sludge-based magnetic biochar in adsorbing organic pollutants in water. The invention provides a novel biochar adsorbent and realizes the efficient removal of perfluoroalkyl and polyfluoroalkyl substances (PFAS) pollutants in water.
Description
Technical Field
The invention relates to the technical field of sewage treatment, in particular to sludge-based magnetic biochar, a preparation method and application.
Background
Perfluoroalkyl and polyfluoroalkyl materials (PFAS), which are a class of organic compounds having unique carbon-fluorine bonds, are widely used in numerous industrial and consumer product manufacturing fields such as coatings, tarpaulins, inks, food packaging, fire fighting foams, and the like, due to their excellent water, oil, corrosion resistance, and the like. However, these characteristics of PFAS lead to its long-term presence and accumulation in the environment, causing serious environmental hazards, becoming a global environmental pollution problem. PFAS is not only difficult to biodegrade, but also has high bioaccumulation, can be transmitted through food chains and food nets and accumulated in organisms, constitutes a potential threat to the ecosystem and human health, and can cause chronic toxicity and even cause serious diseases such as cancers.
In order to cope with PFAS pollution problems, various treatment technologies including chemical oxidation, biodegradation, membrane separation, etc. have been developed at present. However, these aspects generally face limitations such as low efficiency, high cost, complex operation, etc., and are difficult to meet increasingly stringent environmental standards and governance requirements. Under the background, the adsorption technology is an important research direction for treating PFAS pollution as a simple, efficient and economical treatment method.
Adsorption techniques transfer contaminants from solution to the adsorbent by physical or chemical interactions between the adsorbent and the target contaminant, thereby effecting removal of the contaminant. Compared with the traditional treatment technology, the adsorption technology has the advantages of low treatment cost, simple and convenient operation, no secondary pollution and the like. In water, PFAS exists mainly in the form of anions, and the interaction between the hydrophilic head and the surface of the adsorbent is the key to the adsorption process. Therefore, finding adsorbents with high affinity is critical for PFAS removal.
Although the traditional adsorbents such as activated carbon, ferric oxide, aluminum oxide and the like are used for removing PFAS, the problems of low adsorption efficiency, limited selectivity, high preparation cost and the like exist. Biochar is an emerging adsorbent, and is of great interest because of its wide source, simple preparation and low cost. The biochar is prepared by pyrolyzing biomass materials (such as wood, straw, plant residues and the like) at high temperature, has rich pore structures and surface functional groups, and shows good adsorption performance on organic substances. However, the conventional biochar still has the problems of unstable adsorption performance, limited adsorption capacity and the like when adsorbing PFAS. To solve these problems, it is necessary to modify biochar to improve its adsorption performance.
In recent years, researchers have been working on improving the adsorption capacity of the biochar to PFAS by optimizing the preparation method of the biochar, such as by using a pyrolysis method, to effectively control the pore structure thereof, and to increase the specific surface area and the porosity thereof. Inorganic substances and ash in the biochar are removed by acid washing and other methods, so that the surface adsorption sites of the biochar are increased. In addition, the biomass materials such as sludge are used as raw materials for preparing the biochar, so that the waste recycling can be realized, and the adsorption performance of the biochar can be improved.
Sludge is a byproduct of sewage treatment by water treatment plants and sewage treatment facilities, and a large amount of sludge treatment and disposal is a huge environmental and economic burden. By converting the sludge into biochar, the burden of sludge treatment can be reduced, and PFAS pollutants in the water body can be effectively treated. The magnetic biochar disclosed in CN202310930768.8, a preparation method and application thereof, has larger specific surface area, pore volume and saturation magnetization intensity, and has the adsorption efficiency of dioxin for flue gas treatment of 99.8 percent. A method for preparing a sludge biochar material as disclosed in CN202311551684.X and application thereof in wastewater treatment. And loading manganese element on the product after anaerobic carbonization treatment by using a chemical precipitation method to obtain the required sludge biochar material. However, the preparation method has the problems of low adsorption efficiency, difficult regeneration, high raw material cost, poor environmental friendliness, single function, insufficient technical innovation and the like. Therefore, the development of an improved biochar adsorbent and a preparation method thereof has important significance for efficiently removing PFAS pollutants in water and realizing the effective utilization of waste resources.
Disclosure of Invention
In view of the above, the invention aims to provide a sludge-based magnetic biochar, a preparation method and application thereof, so as to provide a novel biochar adsorbent and realize efficient removal of PFAS pollutants in a water body.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the sludge-based magnetic biochar comprises the following steps:
Step 1, mixing residual sludge and residual biogas residues in an inert atmosphere, and then heating to a target temperature for pyrolysis treatment to obtain an intermediate;
Step 2, soaking the intermediate in an acid solution, and performing ultrasonic treatment to obtain sludge-based magnetic biochar;
The surplus sludge is sludge treated by a dehydrating agent;
The residual biogas residue is biogas residue treated by a dehydrating agent;
the dehydrating agent is selected from polyaluminum ferric chloride and/or polyaluminum ferric sulfate.
According to the technical means, the prepared sludge-based magnetic biochar has a larger specific surface area and a pore structure through treatments such as carbonization and modification after mixing the residual sludge and the residual biogas residues, the adsorption performance of the sludge-based magnetic biochar is remarkably improved, the dehydrating agent is decomposed into magnetic substances in the pyrolysis treatment process through the treatment of the sludge and the biogas residues, so that the biochar is endowed with magnetism, the recycling is facilitated, and the experimental results show that the F-53B has excellent removal capacity and regeneration cycle adsorption capacity under the condition of relative concentration of a natural water environment when the F-53B is used as an adsorbent, so that the water purification aim is effectively realized. The sludge-based magnetic biochar can not only efficiently remove PFAS pollutants in water, but also realize the recycling of sludge.
Preferably, in the step 1, the pretreatment of the residual sludge and the pretreatment of the residual biogas residue are included;
the pretreatment of the excess sludge comprises the following steps: heating, drying, crushing and screening the residual sludge of the domestic sewage treatment plant;
The pretreatment of the residual biogas residues comprises the following steps: and (3) performing freeze drying, crushing and screening treatment on the residual biogas residues after anaerobic fermentation of the kitchen waste.
The magnetic sludge-based biochar prepared by adopting a pyrolysis method effectively regulates and controls the pore structure and the specific surface area, removes inorganic substances and ash by acid washing and other methods, and obviously improves the adsorption performance; meanwhile, in the pyrolysis process, the dehydrating agent is decomposed into magnetic substances, so that the biochar is endowed with magnetism, and the recycling and cyclic utilization are facilitated.
Preferably, the pretreatment of the residual sludge specifically comprises: obtaining surplus sludge (dehydrated by a dehydrating agent) of a domestic sewage treatment plant, measuring the water content, carrying out forced air heating drying at the temperature of 80-150 ℃ to remove a large amount of water, drying to constant weight, crushing the dried sludge by adopting a mechanical crushing mode with the rotating speed of 100-150r/min, and screening the crushed sludge by adopting a 100-mesh screen to obtain screened sludge for later use.
Preferably, the pretreatment of the residual biogas residue specifically comprises: obtaining residual biogas residues (dehydrated by a dehydrating agent) of anaerobic fermentation in a kitchen waste treatment plant, measuring the water content, freeze-drying the biogas residues at the temperature of-10 ℃ to-50 ℃, removing a large amount of water, drying to constant weight, crushing the dried biogas residues by adopting a mechanical crushing mode with the rotating speed of 100 r/min-150 r/min, screening the crushed biogas residues by adopting a 100-mesh screen, and obtaining screened biogas residues for later use.
Preferably, the temperature of the heating and drying is 80-150 ℃.
Preferably, the temperature of the freeze drying is-10 ℃ to-50 ℃.
Preferably, the crushing mode is mechanical crushing, and the rotating speed of the mechanical crushing is 100r/min-150r/min.
Preferably, the sieving treatment is a 100 mesh screen.
Preferably, the mass ratio of the excess sludge to the excess biogas residue is 3:1-1:3.
Preferably, the heating mode is temperature programming, and the temperature programming speed is 3 ℃/min-10 ℃/min.
Preferably, the target temperature is 500-1100 ℃.
Preferably, the pyrolysis treatment time is 30-180 min.
Preferably, electric heating is used to raise the temperature.
Preferably, in step 1, the method specifically includes: completely and uniformly mixing the screened sludge and the screened biogas residues according to the mass ratio of 3:1-1:3 to obtain a mixture; placing the mixture into a two-section tube furnace, heating to a target temperature in a temperature programming mode under the protection of inert gas, performing pyrolysis treatment in an electric heating mode, carbonizing organic matters in the mixture, cooling at room temperature, grinding and screening to obtain an intermediate of the sludge-based magnetic biochar; wherein the temperature-programmed heating rate is 3-10 ℃/min, the target temperature is 500-900 ℃, and the pyrolysis treatment time is 30-180 min; and cooling the pyrolyzed mixture to room temperature, and then sieving the mixture with a 100-mesh sieve to obtain the intermediate of the sludge-based magnetic biochar.
Preferably, the acidic solution is a sulfuric acid solution;
The concentration of the acid in the acid solution is 2M;
The ultrasonic treatment time is 60-120 min.
Preferably, after the ultrasonic treatment, the method further comprises filtering, heating, drying and sieving treatment to obtain the sludge-based magnetic biochar.
Preferably, the filtration is vacuum filtration, and the vacuum filtration membrane is 0.22 μm.
Preferably, the filtration is followed by washing with ethanol and then with ultrapure water.
Preferably, the temperature of the heating and drying is 80-150 ℃.
Preferably, the sieving treatment is a 200 mesh screen.
Preferably, in step 2, the method specifically includes: soaking the sieved intermediate in 2M sulfuric acid solution, performing ultrasonic treatment for 60-120 min, performing vacuum suction filtration by adopting a filter membrane of 0.22 mu M, then flushing with ethanol and ultrapure water for 3 times or more respectively, performing forced air heating and drying at the temperature of 80-150 ℃ to remove a large amount of water, drying to constant weight, crushing, and sieving with a 200-mesh sieve to obtain the finished sludge-based magnetic biochar.
The invention also provides the sludge-based magnetic biochar prepared by the preparation method.
The invention also provides application of the sludge-based magnetic biochar prepared by the preparation method, and application of the sludge-based magnetic biochar in adsorbing organic pollutants in water.
Preferably, the sludge-based magnetic biochar is used for adsorbing perfluoroalkyl and polyfluoroalkyl substances in a water body.
Preferably, the sludge-based magnetic biochar is used for adsorbing chloropolyfluoroalkyl ether sulfonate (F-53B) in a water body.
The invention has the beneficial effects that:
According to the sludge-based magnetic biochar, through the treatment of carbonization, modification and the like after mixing the residual sludge and the residual biogas residues, the prepared sludge-based magnetic biochar has a larger specific surface area and a pore structure, and the adsorption performance of the sludge-based magnetic biochar is remarkably improved; the sludge and the biogas residues are treated by adopting the dehydrating agent, and the dehydrating agent is decomposed into magnetic substances in the pyrolysis treatment process, so that the biochar is endowed with magnetism, and the recycling is facilitated; and the experimental result shows that when the water purifying agent is used as an adsorbent, the water purifying agent has excellent removing capacity and regeneration cycle adsorption capacity for F-53B under the condition of the relevant concentration of the natural water environment, and the aim of water body purification is effectively realized. The sludge-based magnetic biochar can not only efficiently remove PFAS pollutants in water, but also realize the recycling of sludge and the recycling of the sludge-based magnetic biochar, and has popularization and application values in the technical field of sewage treatment.
Drawings
FIG. 1 is a graph showing the adsorption efficiency of different doses of sludge-based magnetic biochar to F-53B;
FIG. 2 is a graph showing the adsorption rate of F-53B by different doses of sludge-based magnetic biochar;
FIG. 3 is a graph showing the adsorption efficiency of the sludge-based magnetic biochar to F-53B under different temperature conditions;
FIG. 4 is a graph showing the adsorption rate of the sludge-based magnetic biochar to F-53B under different temperature conditions;
FIG. 5 is a graph showing the adsorption efficiency of the sludge-based magnetic biochar to F-53B under different initial pH values;
FIG. 6 is a graph showing the adsorption rate of the sludge-based magnetic biochar to F-53B under different initial pH values;
FIG. 7 is a graph showing the adsorption efficiency of the sludge-based magnetic biochar to F-53B in the presence of different anions and cations;
FIG. 8 is a graph showing the adsorption rate of F-53B by sludge-based magnetic biochar in the presence of different anions and cations;
FIG. 9 is a graph of the cyclic adsorption result of the sludge-based magnetic biochar on F-53B;
FIG. 10 is a graph showing the adsorption efficiency of F-53B by sludge-based biochar prepared under different temperature conditions.
Detailed Description
The embodiments of the present invention will be described with reference to preferred embodiments, and other advantages and effects of the present invention will be readily apparent to those skilled in the art from the disclosure herein. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention. It should be understood that the preferred embodiments are presented by way of illustration only and not by way of limitation.
Specific techniques or conditions are not noted in the specific examples and are described in the literature or are in accordance with the product specifications. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
A sludge-based magnetic biochar comprising the steps of:
S1, placing surplus sludge (dehydrated by polyaluminium ferric chloride) retrieved from a domestic sewage treatment plant in an oven at 105 ℃, drying to constant weight, crushing by a crusher, and sieving by a 100-mesh screen to obtain sludge powder for later use;
residual biogas residue (dehydrated by polyaluminium ferric chloride) after anaerobic fermentation of the kitchen waste is freeze-dried at the temperature of minus 30 ℃, crushed by a crusher and filtered by a 100-mesh screen to obtain biogas residue powder for later use;
S2, mixing the sludge powder in the S1 with biogas residue powder according to a mass ratio of 1:1, and then placing the mixture in an inert gas environment for pyrolysis. In the pyrolysis process, firstly, keeping inert atmosphere through ventilation, then heating to 700 ℃ at the speed of 10 ℃/min, keeping 60 min, and cooling to obtain an intermediate;
S3, soaking the intermediate obtained in the step S2 in 2M sulfuric acid, performing ultrasonic treatment on the intermediate 120 min, and filtering; then, washing the filter cake with ethanol for three times to remove impurities such as residual inorganic salts and the like; and then, washing the filter cake to be neutral by ultrapure water, placing the filter cake in a baking oven at 105 ℃ for drying, and passing through a 200-mesh screen after grinding treatment to obtain the sludge-based magnetic biochar.
Example 2
A sludge-based magnetic biochar comprising the steps of:
S1, placing surplus sludge (dehydrated by polymeric ferric chloride) retrieved from a domestic sewage treatment plant in an oven at 105 ℃, drying to constant weight, crushing by a crusher, and sieving by a 100-mesh screen to obtain sludge powder for later use;
freeze-drying the residual biogas residue (dehydrated by polymeric ferric chloride) after anaerobic fermentation of the kitchen waste at-30deg.C, crushing with a crusher, and sieving with 100 mesh sieve to obtain biogas residue powder;
S2, mixing the sludge powder in the S1 with biogas residue powder according to a mass ratio of 1:1, and then placing the mixture in an inert gas environment for pyrolysis. In the pyrolysis process, firstly, keeping inert atmosphere through ventilation, then heating to 600 ℃ at the speed of 10 ℃/min, keeping the temperature at 60 min, and cooling to obtain an intermediate;
S3, soaking the intermediate obtained in the step S2 in 2M sulfuric acid, performing ultrasonic treatment on the intermediate 120 min, and filtering; then, washing the filter cake with ethanol for three times to remove impurities such as residual inorganic salts and the like; and then, washing the filter cake to be neutral by ultrapure water, placing the filter cake in a baking oven at 105 ℃ for drying, and passing through a 200-mesh screen after grinding treatment to obtain the sludge-based magnetic biochar.
Example 3
A sludge-based magnetic biochar comprising the steps of:
S1, placing surplus sludge (dehydrated by polymeric ferric chloride) retrieved from a domestic sewage treatment plant in an oven at 105 ℃, drying to constant weight, crushing by a crusher, and sieving by a 100-mesh screen to obtain sludge powder for later use;
Freeze-drying the residual biogas residue (dehydrated by polyaluminium chloride) after anaerobic fermentation of the kitchen waste at the temperature of minus 30 ℃, crushing by a crusher, and sieving by a 100-mesh screen to obtain biogas residue powder for later use;
S2, mixing the sludge powder in the S1 with biogas residue powder according to a mass ratio of 1:1, and then placing the mixture in an inert gas environment for pyrolysis. In the pyrolysis process, firstly, keeping inert atmosphere through ventilation, then heating to 500 ℃ at the speed of 10 ℃/min, keeping 60 min, and cooling to obtain an intermediate;
S3, soaking the intermediate obtained in the step S2 in 2M sulfuric acid, performing ultrasonic treatment on the intermediate 120 min, and filtering; then, washing the filter cake with ethanol for three times to remove impurities such as residual inorganic salts and the like; and then, washing the filter cake to be neutral by ultrapure water, placing the filter cake in a baking oven at 105 ℃ for drying, and passing through a 200-mesh screen after grinding treatment to obtain the sludge-based magnetic biochar.
Example 4
A sludge-based magnetic biochar comprising the steps of:
S1, placing surplus sludge (dehydrated by polymeric ferric chloride) retrieved from a domestic sewage treatment plant in an oven at 105 ℃, drying to constant weight, crushing by a crusher, and sieving by a 100-mesh screen to obtain sludge powder for later use;
Freeze-drying the residual biogas residue (dehydrated by polyaluminium chloride) after anaerobic fermentation of the kitchen waste at the temperature of minus 30 ℃, crushing by a crusher, and sieving by a 100-mesh screen to obtain biogas residue powder for later use;
S2, mixing the sludge powder in the S1 with biogas residue powder according to a mass ratio of 1:1, and then placing the mixture in an inert gas environment for pyrolysis. In the pyrolysis process, firstly, keeping inert atmosphere through ventilation, then heating to 900 ℃ at the speed of 10 ℃/min, keeping 60 min, and cooling to obtain an intermediate;
S3, soaking the intermediate obtained in the step S2 in 2M sulfuric acid, performing ultrasonic treatment on the intermediate 120 min, and filtering; then, washing the filter cake with ethanol for three times to remove impurities such as residual inorganic salts and the like; and then, washing the filter cake to be neutral by ultrapure water, placing the filter cake in a baking oven at 105 ℃ for drying, and passing through a 200-mesh screen after grinding treatment to obtain the sludge-based magnetic biochar.
Example 5
A sludge-based magnetic biochar comprising the steps of:
S1, placing surplus sludge (dehydrated by polymeric ferric chloride) retrieved from a domestic sewage treatment plant in an oven at 105 ℃, drying to constant weight, crushing by a crusher, and sieving by a 100-mesh screen to obtain sludge powder for later use;
Freeze-drying the residual biogas residue (dehydrated by polyaluminium chloride) after anaerobic fermentation of the kitchen waste at the temperature of minus 30 ℃, crushing by a crusher, and sieving by a 100-mesh screen to obtain biogas residue powder for later use;
S2, mixing the sludge powder in the S1 with biogas residue powder according to a mass ratio of 1:1, and then placing the mixture in an inert gas environment for pyrolysis. In the pyrolysis process, firstly, keeping inert atmosphere through ventilation, then heating to 1100 ℃ at the speed of 10 ℃/min, keeping 60 min, and cooling to obtain an intermediate;
S3, soaking the intermediate obtained in the step S2 in 2M sulfuric acid, performing ultrasonic treatment on the intermediate 120 min, and filtering; then, washing the filter cake with ethanol for three times to remove impurities such as residual inorganic salts and the like; and then, washing the filter cake to be neutral by ultrapure water, placing the filter cake in a baking oven at 105 ℃ for drying, and passing through a 200-mesh screen after grinding treatment to obtain the sludge-based magnetic biochar.
Detection analysis
1) Adsorption of F-53B by different doses of sludge-based magnetic biochar
The experimental conditions were that the biochar dosage was in the range of 0.1-1.0 g/L and the initial concentration of chloropolyfluoroalkyl ether sulfonate (F-53B) was 1 mg/L at a temperature of 25 ℃. In a constant temperature and constant speed device, different doses of the sludge-based magnetic biochar prepared in example 1 were mixed with F-53B solution for a reaction time of 12 min. Samples were taken at regular intervals and the contaminant concentration was measured using a high performance liquid chromatograph. The results are shown in fig. 1 and 2.
From the analysis in FIG. 1, it is found that even at a lower dose (0.2 g/L) the sludge-based magnetic biochar can achieve F-53B adsorption efficiency of 70% or more in a shorter time. And the adsorption efficiency is gradually improved along with the increase of the dosage of the sludge-based magnetic biochar, and the adsorption efficiency can reach more than 98% in 12 min. Thus, the sludge-based magnetic biochar has excellent adsorption performance on F-53B.
From the analysis in FIG. 2, the adsorption rate of F-53B was significantly faster with increasing biochar dosage. Wherein, when the biochar dosage is increased from 0.6 g/L to 0.8 g/L, the rate of adsorption rate increase becomes slower, and is only increased from 0.00264 s -1 to 0.00267 s -1. The increase in adsorption rate demonstrates that higher doses of biochar accelerate the adsorption process of F-53B, thus demonstrating the rapid adsorption kinetics of the sludge-based magnetic biochar of the present invention to F-53B.
2) Adsorption of F-53B by sludge-based magnetic biochar under different temperature conditions
Under the temperature conditions of different temperatures, the adsorption experiment of the sludge-based magnetic biochar on F-53B is carried out. Wherein the temperature setting range is 15-45 ℃, and the concentration of F-53B is 1 mg/L. Adding 0.8 g/L sludge-based magnetic biochar adsorbent into the reaction system, reacting 12. 12 min in constant temperature and constant speed equipment, sampling and filtering at fixed time intervals, and detecting the concentration of pollutants in a high performance liquid chromatograph. The results are shown in fig. 3 and 4.
As can be seen from the analysis in FIG. 3, the temperature has a small influence on the adsorption efficiency of F-53B, and an adsorption effect of 80% or more is achieved at 10 s and an adsorption efficiency of 98% or more is achieved at 12 min even at 15 ℃.
As can be seen from the analysis in FIG. 4, the temperature has a smaller effect on the adsorption rate of F-53B, wherein the adsorption rate reaches a maximum value of 0.00314 s -1 at 45 ℃. The higher reaction temperature can accelerate the adsorption of the sludge-based magnetic biochar to F-53B.
3) Adsorption of F-53B by sludge-based magnetic biochar under different pH values
The adsorption experiments of the sludge-based magnetic biochar prepared in example 1 under different initial solution pH conditions on F-53B were performed at a temperature of 25 ℃. Wherein the dosage of the sludge-based magnetic biochar is 0.8 g/L, and the F-53B concentration is 1 mg/L. And adjusting the pH value in the reaction system to 3-11. The reaction 12 min was carried out in a constant temperature and constant speed apparatus, and the concentration of the contaminants was measured in a high performance liquid chromatograph after sampling and filtering at fixed time intervals. The results are shown in fig. 5 and 6.
As can be seen from the analysis in FIG. 5, the pH has an important effect on the adsorption of F-53B, and F-53B can achieve 99% adsorption efficiency in an acidic environment. Even when the pH reached 11, the adsorption efficiency of F-53B was still significant, with about 71.76%.
From the analysis in FIG. 6, it can be seen that the sludge-based magnetic biochar can exhibit good adsorption rates over a wide range of solution pH values (3-9). Wherein, when the pH value reaches 11, the adsorption rate is obviously inhibited, which is only 7.53 multiplied by 10 -4s-1. From the results, the adsorption of F-53B by the sludge-based magnetic biochar can be implemented under a wider pH value of the solution, and the adsorption rate of the solution with strong alkalinity is inhibited.
4) Adsorption of F-53B by sludge-based magnetic biochar in the presence of different anions and cations
The ion concentration and the adsorption of F-53B by the biochar prepared in example 1 was affected by the presence of anions and cations in the solution. The effect of anions and cations was studied in this study using salts such as Na 2SO4、NaCl、Na2CO3、KCl、CaCl2 and MgCl 2. In the adsorption process, the influence of the inorganic salt concentration on the adsorption performance is inspected by utilizing the salt concentration range of 0-60 mg/L. The results are shown in fig. 7 and 8.
From the analysis in fig. 7, it is seen that the presence of anions and cations in the solution has less effect on the adsorption of the sludge-based magnetic biochar. The changes induced by CO 3 2- are notable. With the increase of Na 2CO3 concentration, the adsorption capacity of the sludge-based biochar is obviously hindered, which is probably due to the increase of pH value caused by the hydrolysis of CO 3 2-, so that the electrostatic repulsive force between F-53B and the biochar is enhanced, and is probably due to the fact that CO 3 2- is more easily adsorbed on the surface of the biochar and occupies available binding sites.
From the analysis in fig. 8, it is seen that the presence of anions and cations in the solution has less effect on the adsorption of the sludge-based magnetic biochar. It was observed that only the adsorption rates of CO 3 2- and Mg + showed a significant decrease with ion concentration from 20 Mg/L to 60 Mg/L. The adsorption rates were reduced from 0.0073 s -1 and 0.0075 s -1 to 0.0019 s -1 and 0.0031 s -1, respectively. From the results, the adsorption of F-53B by the sludge-based magnetic biochar provided by the invention can be slightly inhibited in the water body rich in CO 3 2-.
5) Circulating adsorption of F-53B by sludge-based magnetic biochar
The specific operation is as follows: in a multiple cycle adsorption experiment, 1.0 mg/L of F-53B solution was treated with the sludge-based magnetic biochar of example 1. First, sludge-based magnetic biochar was mixed with 1.0 mg/L of F-53B solution and subjected to primary adsorption for half an hour. The sludge-based magnetic biochar was then separated from the solution and dried 24 h in an oven at 40 ℃. Next, the dried adsorbent was mixed with fresh F-53B solution and subjected to the next round of cyclical adsorption experiments. The above steps were repeated 6 times, and the specific results are shown in fig. 9.
From the analysis in FIG. 9, the adsorption rate of F-53B by the primary use of the sludge-based magnetic biochar is as high as 99.10%. As the number of cycles increases, the adsorption efficiency and rate of the biochar to F-53B gradually decrease. After six cycles, the removal efficiency remained at 72.46%. The decrease in adsorption efficiency is mainly due to the gradual decrease in available binding sites and the loss of adsorbent during collection.
6) Adsorption of F-53B by preparing sludge-based magnetic biochar under different temperature conditions
The experimental conditions were that the biochar dose was 0.8 g/L and the initial concentration of chloropolyfluoroalkyl ether sulfonate (F-53B) was 1 mg/L at a temperature of 25 ℃. In a constant temperature and constant speed apparatus, sludge-based biochar prepared at different temperatures (i.e., the sludge-based biochar prepared in examples 1 to 5) was mixed with the F-53B solution for a reaction time of 12 min. The contaminant concentration was detected using a high performance liquid chromatograph. The results are shown in FIG. 10.
From the analysis in FIG. 10, it is known that the preparation temperature is an important influencing factor influencing the adsorption performance of the sludge-based magnetic biochar, and the adsorption effect of F-53B is remarkably improved as the preparation temperature is increased from 500 ℃ to 700 ℃. The removal rate is improved from the original 21.04% to 99.77%. However, as the preparation temperature was further raised to 900℃and 1100℃the adsorption effect of F-53B could still be maintained at 99.90%. From this, it was found that when the preparation temperature reached 700℃and above, the obtained sludge-based magnetic biochar almost completely adsorbed F-53B.
In conclusion, the sludge-based magnetic biochar is prepared by skillfully mixing the sludge and the biogas residues, and the sludge and the biogas residues are synergistically modified, so that the problems of low reusable efficiency and difficult recovery of the biochar prepared by singly adopting the sludge are solved, the problem of low adsorption efficiency of the biochar prepared by singly adopting the biogas residues on organic pollutants is solved, and the defect of F-53B adsorption of the sludge and the biogas residues is effectively overcome.
According to the preparation method of the sludge-based magnetic biochar, the steps of pretreatment, pyrolysis treatment, acid modification treatment and the like are combined, organic substances in sludge and biogas residues are converted into the biochar, and magnetism is endowed to the biochar for subsequent recycling, so that the prepared sludge-based magnetic biochar can effectively treat organic pollutants in wastewater, can realize recycling of organic waste resources, has dual benefits of environment and economy, and has popularization and application values in the technical field of sewage treatment.
The above embodiments are merely preferred embodiments for fully explaining the present invention, and the scope of the present invention is not limited thereto. Equivalent substitutions and modifications will occur to those skilled in the art based on the present invention, and are intended to be within the scope of the present invention.
Claims (10)
1. The preparation method of the sludge-based magnetic biochar is characterized by comprising the following steps of:
Step 1, mixing residual sludge and residual biogas residues in an inert atmosphere, and then heating to a target temperature for pyrolysis treatment to obtain an intermediate;
Step 2, soaking the intermediate in an acid solution, and performing ultrasonic treatment to obtain sludge-based magnetic biochar;
The surplus sludge is sludge treated by a dehydrating agent;
The residual biogas residue is biogas residue treated by a dehydrating agent;
the dehydrating agent is selected from polyaluminum ferric chloride and/or polyaluminum ferric sulfate.
2. The method for preparing sludge-based magnetic biochar according to claim 1, wherein the method comprises pretreatment of excess sludge and pretreatment of excess biogas residue before the step 1;
the pretreatment of the excess sludge comprises the following steps: heating, drying, crushing and screening the residual sludge of the domestic sewage treatment plant;
The pretreatment of the residual biogas residues comprises the following steps: and (3) performing freeze drying, crushing and screening treatment on the residual biogas residues after anaerobic fermentation of the kitchen waste.
3. The method for preparing sludge-based magnetic biochar according to claim 2, wherein the temperature of the heating and drying is 80-150 ℃;
and/or the freeze-drying temperature is-10 ℃ to-50 ℃;
And/or the crushing mode is mechanical crushing, and the rotating speed of the mechanical crushing is 100 r/min-150 r/min;
And/or, the screening treatment is a 100 mesh screen.
4. The method for preparing sludge-based magnetic biochar according to claim 1, wherein the mass ratio of the excess sludge to the excess biogas residue is 3:1-1:3.
5. The method for preparing the sludge-based magnetic biochar according to claim 1, wherein the heating mode is temperature programming, and the temperature programming rate is 3-10 ℃/min;
and/or the target temperature is 500-1100 ℃;
and/or the pyrolysis treatment time is 30-180 min.
6. The method for producing sludge-based magnetic biochar according to claim 1, wherein the acidic solution is a sulfuric acid solution;
The concentration of the acid in the acid solution is 2M;
The ultrasonic treatment time is 60-120 min.
7. The method for producing sludge-based magnetic biochar according to claim 1, further comprising filtration, heat drying and sieving treatment after the ultrasonic treatment, to obtain the sludge-based magnetic biochar.
8. The method for preparing sludge-based magnetic biochar according to claim 7, wherein the filtration is vacuum filtration, and the membrane of the vacuum filtration is 0.22 μm;
And/or, further comprising, after said filtering, washing with ethanol and ultra-pure water in sequence;
and/or the temperature of the heating and drying is 80-150 ℃;
And/or, the sieving treatment is that of passing through a 200-mesh screen.
9. A sludge-based magnetic biochar produced by the production method of any one of claims 1 to 8.
10. Use of the sludge-based magnetic biochar produced by the production method according to any one of claims 1 to 8 for adsorbing organic pollutants in a body of water;
or the sludge-based magnetic biochar is applied to adsorbing perfluoroalkyl and polyfluoroalkyl substances in a water body;
or the application of the sludge-based magnetic biochar in water body for adsorbing chloro-polyfluoroalkyl ether sulfonate.
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