CN111760552A - Preparation method and application of magnetic biochar capable of synchronously adsorbing nitrogen and phosphorus - Google Patents
Preparation method and application of magnetic biochar capable of synchronously adsorbing nitrogen and phosphorus Download PDFInfo
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- CN111760552A CN111760552A CN202010711295.9A CN202010711295A CN111760552A CN 111760552 A CN111760552 A CN 111760552A CN 202010711295 A CN202010711295 A CN 202010711295A CN 111760552 A CN111760552 A CN 111760552A
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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
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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
- B01J20/28—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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- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
- C02F2101/105—Phosphorus 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
- C02F2101/16—Nitrogen compounds, e.g. ammonia
Abstract
A preparation method and application of magnetic biochar capable of synchronously adsorbing nitrogen and phosphorus belong to the field of resource utilization of environment functional materials and biomass. Adding dried sludge powder to FeSO4·7H2Soaking in O solution and shaking. Then the vibrated sludge/FeSO4And putting the mixed solution into an oven for drying. Grinding and sieving the dried material, and adding MgCl into the material2·6H2In O solution, and performing magnetic stirringAnd (4) stirring. The NaOH solution was then slowly added to the mixed solution and magnetically stirred, followed by aging. And then repeatedly washing the precipitate obtained by filtering with deionized water to be neutral and drying. And finally, placing the obtained dry precipitate in a tubular furnace for continuous calcination to obtain the magnetic sludge biochar. When the adsorbent is used in aqueous solution of ammonia nitrogen and phosphate, the equilibrium adsorption capacity of the adsorbent to the ammonia nitrogen and the phosphate is 103.12mg g respectively when the pH is 9‑1And 205.07mg g‑1。
Description
Technical Field
The invention belongs to the field of resource utilization of environmental functional materials and biomass, and particularly relates to a preparation method and application of magnetic biochar capable of synchronously adsorbing nitrogen and phosphorus.
Background
At present, the eutrophication phenomenon of water bodies is more and more serious due to the discharge of high-nitrogen and phosphorus wastewater, and nitrogen and phosphorus are indispensable nutrient elements in agricultural production. Therefore, the method has important practical significance on how to efficiently recover the nitrogen and phosphorus resources in the wastewater. Because ammonia nitrogen and phosphate carry opposite charges, it is generally difficult to recover them simultaneously.
Struvite precipitation is considered to be an effective method for synchronously recovering ammonia nitrogen and phosphate in water, and has been widely applied to the treatment of various water containing ammonia nitrogen and phosphate, including urine, sludge supernatant, livestock wastewater, leachate and the like. The struvite precipitation method can synchronously remove ammonia nitrogen and phosphate, and the recovered product can be used as a slow release fertilizer to improve the soil property and promote the growth of crops. However, the use of this method has the disadvantages of high cost of magnesium source, high alkalinity conditions and difficult recovery of the reacted material.
Aiming at the problems, the invention aims to develop a novel magnetic sludge-based biochar composite material which has the advantages of targeted supply of magnesium ions, strong alkaline regulation and control performance, low cost and easy recovery, can synchronously recover nitrogen and phosphorus in wastewater, and realizes resource utilization of sludge.
Disclosure of Invention
Aiming at the problems and technical analysis, the invention aims to provide a preparation method of magnetic sludge biochar (MF-SBC) capable of synchronously adsorbing nitrogen and phosphorus, which is simple to operate and easy to obtain raw materials.
A preparation method of magnetic biochar capable of synchronously adsorbing nitrogen and phosphorus comprises the following steps:
(1) adding dried powdered sludge to FeSO4·7H2Soaking in the O solution and shaking to obtain a mixed solution.
(2) And (3) putting the mixed solution obtained in the step (1) into an oven to dry to constant weight.
(3) Grinding and sieving the dried material obtained in the step (2), and adding the ground material into MgCl2·6H2O solution, and performing magnetic stirring.
(4) And (4) slowly adding a NaOH solution into the solution after the magnetic stirring in the step (3) and carrying out magnetic stirring, and then aging.
(5) And (4) filtering the aged solution in the step (4), repeatedly washing the obtained precipitate with deionized water to be neutral, and drying to constant weight.
(6) And (4) placing the dried precipitate obtained in the step (5) into a tubular furnace for continuous calcination to obtain the MF-SBC.
Further, in the step (1), FeSO4·7H2The concentration of the O solution is 0.2mol/L, and the powdered sludge and the FeSO are mixed4·7H2The O solution was added at a ratio of 1g to 20 mL. The soaking and shaking time was 6 h.
Further, in the step (2), the drying temperature is 75-85 ℃.
Further, in the step (3), MgCl2·6H2The concentration of the O solution is 1.25mol/L, MgCl2·6H2The addition amount of the O solution is equal to that of FeSO in the step (1)4·7H2The amount of O solution added. GrindingThe aperture size of the sieve in the sieving is 200 meshes; the magnetic stirring time is 30 min.
Further, in the step (4), the concentration of the NaOH solution is 2.5mol/L, and the addition amount of the NaOH solution is equal to that of the FeSO in the step (1)4·7H2The amount of O solution added. The magnetic stirring time is 12h, and the aging time is 24 h.
Further, in the step (5), the drying temperature is 75-85 ℃.
Further, in the step (6), the temperature rise rate of the calcination is 5 ℃/min; the temperature of continuous calcination was 450 ℃ and the time of continuous calcination was 2 hours.
The magnetic sludge biochar material MF-SBC prepared based on the steps can be used for synchronously removing or recycling ammonia nitrogen and phosphate in water.
The invention has the beneficial effects that: the magnetic sludge biochar (MF-SBC) is successfully prepared by a calcining method, has the advantages of good chemical stability, large specific surface area and the like, and can be used for synchronously removing or recycling ammonia nitrogen and phosphate in water. 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 field emission Scanning Electron Microscope (SEM) image of the MF-SBC adsorbent material of the present invention.
Figure 2 is an XRD pattern of the MF-SBC adsorbent material of the present invention.
FIG. 3 is a diagram of the synchronous adsorption effect of the MF-SBC adsorbent material on nitrogen and phosphorus under different initial pH values.
FIG. 4 is a diagram of the simultaneous adsorption kinetics of nitrogen and phosphorus by the MF-SBC adsorbent material of the present invention.
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:
preparing magnetic sludge biochar: firstly, accurately weighing 25g of dried sludge powder to 50mL0.2M of FeSO4·7H2Soaking in O solution and shaking for 6 h. Then the vibrated sludge/FeSO4The mixed solution is put into an oven to be dried at 80 ℃, the dried material is ground and sieved by a 200-mesh sieve, and then 50mL of 1.25M MgCl is added2·6H2And O solution, and performing magnetic stirring for 30 min. Subsequently, 50mL of a 2.5M NaOH solution was slowly added to the above mixed solution and magnetically stirred for 12 hours, followed by aging for 24 hours. Repeatedly cleaning the precipitate obtained by filtering the solution with deionized water to neutrality, drying at 80 ℃, finally placing the obtained dried precipitate in a tubular furnace, slowly heating to 450 ℃ at a speed of 5 ℃/min, and continuously calcining for 2h at the temperature to obtain the sample, namely the magnetic sludge biochar (MF-SBC).
SEM analysis results (FIG. 1) of MF-SBC materials show that the MF-SBC surface has irregular morphology with densely grown agglomerated particles. XRD analysis of MF-SBC the results are shown in FIG. 2, with one corresponding to Fe at 35.66 ° 2 θ3O4Shows that the MF-SBC material contains Fe3O4The reason why the MF-SBC has magnetic properties is explained. Diffraction peaks exist at positions with the 2 theta of 42.94 degrees, 62.30 degrees, 74.67 degrees and 78.64 degrees, the diffraction peaks are highly matched with an MgO standard card (PDF #45-0946), the biological carbon can be judged to contain MgO components, and the surface MF-SBC is magnetic sludge biological carbon rich in MgO particles.
Example 2:
the influence of different pH values on the synchronous adsorption and nitrogen and phosphorus removal of MF-SBC in the embodiment 1 is as follows: 0.3g of MF-SBC was weighed into conical flasks containing 100mL of ammonia nitrogen and phosphate at concentrations of 160mg/L and 80mg/L, respectively, the pH of the solution was adjusted to 3-11 with 0.1M HCl and NaOH at an interval of 1, and the conical flasks were then placed in a constant temperature shaker at 298K and shaken for 720 min. After the reaction is finished, taking supernatant, filtering by using a 0.45-micron membrane, and detecting the concentrations of phosphate and ammonia nitrogen by using a UV-vis spectrophotometer. As a result, as shown in FIG. 3, in the range of initial pH 3.0-9.0, the adsorption amounts of ammonia nitrogen and phosphate both increased with increasing pH, in the range of pH 9.0-11.0, the adsorption amounts of ammonia nitrogen and phosphate decreased with increasing pH, and the maximum adsorption amount was reached at pH 9,respectively 85.8mg g-1And 209.95mg g-1。
Example 3:
the kinetic study of the MF-SBC prepared in example 1 for simultaneous adsorption of nitrogen and phosphorus removal: weighing 0.3gMF-SBC, adding the SBC into a conical flask containing 100mL of ammonia nitrogen and phosphate with the concentration of 160mg/L and 80mg/L respectively, adjusting the pH value of the solution to 9, placing the conical flask in a constant temperature oscillator with the temperature of 298K, oscillating for 720min, taking supernatant at different time periods, filtering by using a 0.45 mu m membrane, and detecting the concentrations of the phosphate and the ammonia nitrogen by using a UV-vis spectrophotometer. The results are shown in FIG. 4, the adsorption capacity of MF-SBC to ammonia nitrogen and phosphate rapidly increases within 0-60min, and then slowly increases to 120min to reach the adsorption equilibrium state, at which the adsorption capacity of ammonia nitrogen and phosphate reaches 103.12mg g-1And 205.07mg g-1。
Claims (10)
1. The preparation method of the magnetic biochar capable of synchronously adsorbing nitrogen and phosphorus is characterized by comprising the following steps of:
(1) adding dried powdered sludge to FeSO4·7H2Soaking in the O solution and oscillating to obtain a mixed solution;
(2) putting the mixed solution obtained in the step (1) into an oven to dry to constant weight;
(3) grinding and sieving the dried material obtained in the step (2), and adding the ground material into MgCl2·6H2In the O solution, performing magnetic stirring;
(4) slowly adding a NaOH solution into the solution obtained after the magnetic stirring in the step (3), magnetically stirring, and then aging;
(5) filtering the solution aged in the step (4), repeatedly washing the obtained precipitate with deionized water to be neutral, and drying to constant weight;
(6) and (4) placing the dried precipitate obtained in the step (5) into a tubular furnace for continuous calcination to obtain the MF-SBC.
2. The method for preparing the magnetic biochar capable of synchronously adsorbing nitrogen and phosphorus according to claim 1, wherein the method is characterized in thatIn step (1), FeSO4·7H2The concentration of the O solution is 0.2mol/L, and the powdered sludge and the FeSO are mixed4·7H2The O solution was added at a ratio of 1g to 20 mL.
3. The method for preparing magnetic biochar capable of synchronously adsorbing nitrogen and phosphorus according to claim 1, wherein in the step (3), MgCl is adopted2·6H2The concentration of the O solution is 1.25mol/L, MgCl2·6H2The addition amount of the O solution is equal to that of FeSO in the step (1)4·7H2The amount of O solution added.
4. The method for preparing magnetic biochar capable of synchronously adsorbing nitrogen and phosphorus according to claim 1, wherein in the step (4), the concentration of NaOH solution is 2.5mol/L, and the addition amount of NaOH solution is equal to that of FeSO in the step (1)4·7H2The amount of O solution added.
5. The method for preparing magnetic biochar capable of synchronously adsorbing nitrogen and phosphorus according to claim 1, wherein in the step (6), the temperature rise rate of calcination is 5 ℃/min; the temperature of continuous calcination was 450 ℃ and the time of continuous calcination was 2 hours.
6. The method for preparing magnetic biochar capable of synchronously adsorbing nitrogen and phosphorus according to claim 1, wherein in the step (1), the soaking and shaking time is 6 hours.
7. The method for preparing the magnetic biochar capable of synchronously adsorbing nitrogen and phosphorus according to claim 1, wherein the drying temperature in the step (2) and the step (5) is 75-85 ℃.
8. The method for preparing magnetic biochar capable of synchronously adsorbing nitrogen and phosphorus according to claim 1, wherein in the step (3), the size of the aperture of a sieve in a grinding and sieving process is 200 meshes; the magnetic stirring time is 30 min.
9. The method for preparing magnetic biochar capable of synchronously adsorbing nitrogen and phosphorus according to claim 1, wherein in the step (4), the magnetic stirring time is 12 hours, and the aging time is 24 hours.
10. The application of the magnetic biochar MF-SBC capable of synchronously adsorbing nitrogen and phosphorus is characterized in that the magnetic biochar MF-SBC prepared by the preparation method according to any one of claims 1 to 9 is used for synchronously removing or recycling ammonia nitrogen and phosphate in water.
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Application publication date: 20201013 |