CN110801814A - Preparation method of magnetic amino walnut shell biochar novel adsorbent - Google Patents
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- 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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- 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
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- 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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- 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
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- 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
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses a preparation method of a novel magnetic amino walnut shell biochar adsorbent, which is applied to adsorption of heavy metal cadmium in water, wherein walnut shells are used as raw materials in the preparation process, and are firstly placed in a muffle furnace to prepare walnut shell biochar; then loading the nano Fe3O4 particles on the magnetic carrier to make the walnut shell biochar have magnetism; and finally, crosslinking chitosan on the surface of the magnetic walnut shell biochar by using sodium tripolyphosphate buffer solution as a crosslinking agent to prepare the magnetic amino walnut shell biochar. Compared with the effect of removing cadmium in water by adsorption of original walnut shell biochar, the adsorbent prepared by the invention has the advantages of high removal rate, large adsorption capacity and the like, and is high in recycling property. The preparation raw materials of the invention have wide sources, low cost and higher economic benefit, and can achieve the effect of treating waste by waste in the aspect of environmental protection, and the application of the prepared novel adsorbent in the cadmium-containing wastewater purification treatment provides a certain theoretical basis for the treatment of heavy metal wastewater in the future.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a preparation method of a novel magnetic amino walnut shell biochar adsorbent.
Background
In recent years, with the rapid development of economy in China, industrial wastewater discharged by industries such as electrolysis, electroplating and metallurgy contains a large amount of cadmium ions every year. Once discharged into the environment, these heavy metal pollutants which cannot be effectively degraded and destroyed become permanent pollutants. If the water body is polluted by heavy metal cadmium once, the content of the cadmium is low, but the pollution hazard is very obvious, and the cadmium can finally enter a human body through the transmission effect of a food chain and generate a biological amplification or biological enrichment phenomenon, so that the health of the human body and the environment are seriously damaged. For removing heavy metals in water, currently, common methods include ion exchange, chemical precipitation, membrane separation, electrochemistry, biological methods, adsorption and the like. Compared with other technologies, adsorption has received much attention due to its advantages such as easy operation, economy and efficiency. The existing adsorbent generally has the defects of high cost, low recycling performance and the like, wherein the original walnut shell biochar has small adsorption capacity on heavy metal ions and low regeneration utilization rate, so that a novel adsorbent needs to be researched.
Disclosure of Invention
The invention aims to overcome the technical defects and provides a preparation method of a novel magnetic amino walnut shell biochar adsorbent, which can solve the problems of small adsorption capacity of original walnut shell biochar on heavy metal ions, low regeneration utilization rate and the like.
In order to achieve the purpose of the invention, the invention adopts the technical scheme that: a preparation method of a novel magnetic amino walnut shell biochar adsorbent comprises the following preparation steps,
the method comprises the following steps: selecting walnut shells with the particle size of 0.8-1.2mm, washing with deionized water, removing surface impurities, drying at 80 ℃, then cracking in a muffle furnace at 600 ℃ under the protection of nitrogen atmosphere to generate walnut shell biochar, grinding the walnut shell biochar through an 80-mesh screen, and marking the walnut shell biochar as BC;
step two: ultrasonically dispersing 1.2g of powdered walnut shell biochar in 120ml of ethylene glycol for 2h, and then carrying out ultrasonic dispersion on 1.32gCH3COONa and 1.25g FeCl3·6H2Adding O into the solution, stirring for 30min, transferring the mixed solution into a stainless steel autoclave with a Teflon lining, heating at 200 deg.C for 10h, centrifuging to obtain black precipitate, washing with water and ethanol for three times, and vacuum drying at 60 deg.C for 24h to obtain the final product3O4The walnut shell biochar of (1) is marked as MBC;
step three: diluting 10ml HAC with distilled water to 500ml to obtain 2% HAC, dissolving 2g chitosan in 60ml HAC solution to obtain chitosan solution, then weighing 2g MBC, ultrasonically dispersing in the chitosan solution, measuring 100ml 0.05 mol.L-1Sodium tripolyphosphate solution of 0.1 mol.L-1Adjusting the pH value to 8 by HCl, adding the mixture into the mixture, fully stirring the mixture at room temperature for 12 hours, finally washing the mixture for a plurality of times by deionized water until the mixture is neutral, and obtaining the chitosan-stabilized magnetic nano-Fe-loaded material3O4The walnut shell biochar of (1) is denoted as CMBC.
Step four: and after the modified walnut shell biochar adsorbing material is subjected to adsorption treatment, desorbing and regenerating the adsorbent by using a desorbent.
Further, according to mass-to-volume ratio MBC: and (3) chitosan: 2% acetic acid: 0.05 mol. L-1Sodium tripolyphosphate is 1:1:30: 50.
Furthermore, the particle size of the magnetic amino walnut shell biochar adsorbent is 0.8-1.2 mm.
Further, 10ml of HAC was taken in the third step, and diluted with distilled water to 500ml to obtain a 2% HAC solution, and 2g of chitosan was sufficiently dissolved in 60ml of the HAC solution to obtain the chitosan solution used.
Further, in the fourth step, 0.1 mol.L of desorbent is adopted-1Soaking in HCl solution, shaking for 4 hr, washing the adsorbent to neutrality, oven drying, and repeating the process for 20 mg. L-1And adsorbing the wastewater containing Cd.
Further, the magnetic amino walnut shell biochar adsorbent is used for treating heavy metal wastewater, and comprises the preparation method of the magnetic amino walnut shell biochar adsorbent in any one of claims 1 to 5.
The invention also aims to provide a chemical wastewater treatment process, which comprises the novel magnetic amino walnut shell biochar adsorbent with high adsorption performance prepared by the preparation method of the novel magnetic amino walnut shell biochar adsorbent with high adsorption performance.
The invention also aims to provide an electroplating wastewater treatment process, which comprises the novel magnetic amino walnut shell biochar adsorbent with high adsorption performance prepared by the preparation method of the novel magnetic amino walnut shell biochar adsorbent with high adsorption performance.
The invention has the beneficial effects that: the invention provides a novel magnetic walnut shell biochar adsorbent with high-efficiency adsorption performance and a preparation method thereof3O4The particles are loaded on the magnetic walnut shell biochar to enable the magnetic walnut shell biochar to have magnetism, and finally chitosan is crosslinked on the surface of the magnetic walnut shell biochar, so that the magnetic amino walnut shell biochar is prepared, and the effect of changing waste into valuable by using waste is achieved. The lignocellulose waste has the advantages of wide source, low price, short regeneration period, biodegradability, environmental friendliness and the like, is an important biomass resource, has become a new trend of current research in the aspect of environmental protection, and particularly has become an ideal choice for treating heavy metal wastewater. The novel magnetic walnut shell biochar adsorbing material is prepared by chemically modifying a natural walnut shell biochar adsorbent and adding nano Fe3O4Amino functional group is introduced into walnut shellThe novel adsorbent is prepared on the surface of the biochar. Compared with natural walnut shell biochar, the magnetic amino walnut shell biochar has the characteristics of high separability, high reusability and the like, and the adsorption capacity is greatly improved. Therefore, the method has a good application prospect in the treatment of the wastewater polluted by the heavy metal cadmium. The adsorbent prepared by the invention can reduce the cost in the aspect of economy and can realize the purpose of treating wastes with processes of wastes against one another in the aspect of environmental protection. The preparation raw materials of the invention have wide sources, and the application of the prepared novel adsorbent in the purification treatment of heavy metal wastewater provides a theoretical basis for relevant wastewater treatment technologies.
Drawings
FIG. 1 is a flow chart of the preparation method of the novel magnetic amino walnut shell adsorbent.
Figure 2 is an XRD pattern of the adsorbent of example 1 provided by practice of the present invention.
FIG. 3 is a scanning electron micrograph of the adsorbent of example 1 provided by the practice of the present invention.
FIG. 4 is a graph showing the effect of the addition of the adsorbent in example 1 on the removal of Cd (II) in accordance with the practice of the present invention.
FIG. 5 is a graph showing the effect of the adsorbent of example 1 on Cd (II) removal at different pH values.
FIG. 6 is a graph showing the effect of the adsorbent of example 1 on Cd (II) removal at different ion concentrations.
FIG. 7 is a graph showing the effect of regenerating the adsorbent of example 1 in accordance with the practice of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
As shown in figure 1, the preparation method of the novel magnetic walnut shell biochar adsorbent with high-efficiency adsorption performance comprises the following steps:
s101: selecting walnut shells with the particle size of 0.8-1.2mm, washing with deionized water, removing surface impurities, drying at 80 ℃, then cracking in a muffle furnace at 600 ℃ under the protection of nitrogen atmosphere to generate walnut shell biochar, grinding the walnut shell biochar through an 80-mesh screen, and marking the walnut shell biochar as BC;
s102: ultrasonically dispersing 1.2g of powdered walnut shell biochar in 120ml of ethylene glycol for 2h, and then carrying out ultrasonic dispersion on 1.32gCH3COONa and 1.25gFeCl3·6H2Adding O into the solution, stirring for 30min, transferring the mixed solution into a stainless steel autoclave with a Teflon lining, heating at 200 deg.C for 10h, centrifuging to obtain black precipitate, washing with water and ethanol for three times, and vacuum drying at 60 deg.C for 24h to obtain the final product3O4The walnut shell biochar of (1) is marked as MBC;
s103: diluting 10ml HAC with distilled water to 500ml to obtain 2% HAC, dissolving 2g chitosan in 60ml HAC solution to obtain chitosan solution, then weighing 2g MBC, ultrasonically dispersing in the chitosan solution, measuring 100ml 0.05 mol.L-1Sodium tripolyphosphate solution of 0.1 mol.L-1Adjusting the pH value to 8 by HCl, adding the mixture into the mixture, fully stirring the mixture at room temperature for 12 hours, finally washing the mixture for a plurality of times by deionized water until the mixture is neutral, and obtaining the chitosan-stabilized magnetic nano-Fe-loaded material3O4The walnut shell biochar of (1) is denoted as CMBC.
S104: and after the modified walnut shell biochar adsorbing material is subjected to adsorption treatment, desorbing and regenerating the adsorbent by using a desorbent.
The present invention will be further described below in connection with the experiments of wastewater treatment.
Experimental part
(1) To determine the optimum amount of adsorbent, 40mL of 20 mg.L was added at pH 6-1The Cd (II) is put into a 50mL centrifuge tube, and the addition amounts of the adsorbent are respectively 1, 2, 5, 8, 10, 12, 15, 20 and 25 g.L-1Oscillating at constant temperature for 24h (25 ℃, 180 r)·min-1) An adsorption test was performed to examine the effect of the amount of adsorbent added on the removal rate of Cd (II), as shown in FIG. 4.
(2) Investigating the effect of the adsorbent on removing Cd (II) under different pH values, weighing 0.48g of the adsorbent in a 50mL plastic centrifuge tube, adding 40mL of the adsorbent with the concentration of 20 mg.L-1Respectively adjusting the pH value of the Cd (II) to 3, 4, 5, 6, 7 and 8, and oscillating at constant temperature for 24h (25 ℃, 180 r.min)-1) Adsorption experiments were performed as shown in fig. 5.
(3) Investigating the removal effect of the adsorbent on Cd (II) under different ion concentrations, weighing 0.48g of the adsorbent into a 50mL plastic centrifuge tube, adding 40mL of Cd (II), and setting the initial concentration gradient of Cd (II) to be 0, 5, 10, 20, 40, 60, 80, 100 mg.L-1Oscillating at constant temperature for 24h (25 ℃, 180 r.min)-1) Adsorption experiments were performed as shown in fig. 6.
(4) The magnetic amino walnut shell prepared in the example 1 is desorbed and regenerated, and 0.1 mol.L of desorbent is selected-1Soaking and shaking the HCl solution for 4h, washing the adsorbent with deionized water to neutrality, drying, and repeating the process for 20 mg.L-1The wastewater containing Cd (II) is subjected to adsorption treatment, and the recycling effect diagram is shown in FIG. 7.
Experiments show that: when the pH of the solution is equal to 6, the dosage of the adsorbent is 12 g.L-1The initial concentration of Cd (II) is 40 mg.L-1In time, the adsorption rate of the adsorbent to Cd (II) is as high as 99.36 percent; in fig. 7, after the magnetic amino walnut shell biochar is reused for 5 times, the effect can still reach more than 90%.
The present invention and the embodiments thereof have been described above, but the description is not limited to the embodiments, but only one of the embodiments of the present invention, and the actual embodiments are not limited thereto. In summary, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. A preparation method of a novel magnetic amino walnut shell biochar adsorbent is characterized by comprising the following steps: comprises the following preparation steps of the following steps of,
the method comprises the following steps: selecting walnut shells with the particle size of 0.8-1.2mm, washing with deionized water, removing surface impurities, drying at 80 ℃, then cracking in a muffle furnace at 600 ℃ under the protection of nitrogen atmosphere to generate walnut shell biochar, grinding the walnut shell biochar through an 80-mesh screen, and marking the walnut shell biochar as BC;
step two: ultrasonically dispersing 1.2g of powdered walnut shell biochar in 120ml of ethylene glycol for 2h, and then carrying out ultrasonic dispersion on 1.32gCH3COONa and 1.25g FeCl3·6H2Adding O into the solution, stirring for 30min, transferring the mixed solution into a stainless steel autoclave with a Teflon lining, heating at 200 deg.C for 10h, centrifuging to obtain black precipitate, washing with water and ethanol for three times, and vacuum drying at 60 deg.C for 24h to obtain the final product3O4The walnut shell biochar of (1) is marked as MBC;
step three: diluting 10ml HAC with distilled water to 500ml to obtain 2% HAC, dissolving 2g chitosan in 60ml HAC solution to obtain chitosan solution, then weighing 2g MBC, ultrasonically dispersing in the chitosan solution, measuring 100ml 0.05 mol.L-1Sodium tripolyphosphate solution of 0.1 mol.L-1Adjusting the pH value to 8 by HCl, adding the mixture into the mixture, fully stirring the mixture at room temperature for 12 hours, finally washing the mixture for a plurality of times by deionized water until the mixture is neutral, and obtaining the chitosan-stabilized magnetic nano-Fe-loaded material3O4The walnut shell biochar of (1) is denoted as CMBC.
Step four: and after the modified walnut shell biochar adsorbing material is subjected to adsorption treatment, desorbing and regenerating the adsorbent by using a desorbent.
2. The preparation method of the magnetic amino walnut shell biochar adsorbent according to claim 1, which is characterized in that: according to mass-to-volume ratio MBC: and (3) chitosan: 2% acetic acid: 0.05 mol. L-1Sodium tripolyphosphate is 1:1:30: 50.
3. The preparation method of the magnetic amino walnut shell biochar adsorbent according to claim 1, which is characterized in that: the particle size of the magnetic amino walnut shell biochar adsorbent is 0.8-1.2 mm.
4. The preparation method of the magnetic amino walnut shell biochar adsorbent according to claim 1, which is characterized in that: diluting 10ml HAC with distilled water to 500ml in step three to obtain 2% HAC solution, and dissolving 2g chitosan in 60ml HAC solution to obtain chitosan solution.
5. The preparation method of the magnetic amino walnut shell biochar adsorbent according to claim 1, which is characterized in that: in the fourth step, 0.1 mol.L of desorbent is adopted-1Soaking in HCl solution, shaking for 4 hr, washing the adsorbent to neutrality, oven drying, and repeating the process for 20 mg. L-1And adsorbing the wastewater containing Cd.
6. The preparation method of the magnetic amino walnut shell biochar adsorbent according to claim 1, which is characterized in that: the magnetic amino walnut shell biochar adsorbent is used for treating heavy metal wastewater, and comprises the preparation method of the magnetic amino walnut shell biochar adsorbent in any one of claims 1 to 5.
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Application publication date: 20200218 |