CN106390927B - Preparation method of biological carbon composite adsorption material for removing phosphate from surface water - Google Patents
Preparation method of biological carbon composite adsorption material for removing phosphate from surface water Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- C02F1/00—Treatment of water, waste water, or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
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- 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
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Abstract
The invention discloses a preparation method of a biological carbon composite adsorption material for removing phosphate from surface water, which belongs to the field of biological carbon adsorption materials and specifically comprises the following steps of (1) cleaning, air-drying and cutting shaddock peel and orange peel, (2) heating, pyrolyzing, cooling and crushing the granular solid to prepare carbonized shaddock peel and carbonized orange peel, (3) modifying the pyrolyzed substances, and respectively modifying ferrous sulfate, sodium thiosulfate and hexadecyl trimethyl ammonium bromide, (4) cleaning and drying with deionized water to obtain the modified biological carbon adsorption material, wherein after surface sewage with the phosphate concentration of 10 mg/L is treated by the adsorption material, the content of the phosphate in the water reaches the surface water environmental quality standard (GB 3838 and 2002) V (less than or equal to 0.4 mg/L).
Description
Technical Field
The invention belongs to the field of biological carbonaceous adsorption materials, particularly relates to preparation of a phosphate sewage treatment adsorption material, and particularly relates to a biological carbonaceous composite adsorption material and a preparation method thereof.
Background
China is a country with a shortage of water resources, and the problem of eutrophication is one of the serious water pollution problems faced by China. According to statistics, the eutrophication of the main lakes in China caused by nitrogen and phosphorus pollution accounts for more than 56% of the lakes in statistics. The eutrophication of the water body is mainly caused by the fact that the water body contains too many nutrient substances such as nitrogen, phosphorus and the like which can be utilized by algae, wherein the phosphorus is a limiting factor of the proliferation of the algae and is a key nutrient substance causing the eutrophication of the water body. How to remove the phosphorus in the water with high efficiency and low cost and solve the eutrophication of the water body becomes the key point of the current research work.
At present, the commonly used wastewater dephosphorization methods at home and abroad mainly comprise a dredging method, a biological method, a chemical method and an adsorption method. The dredging method has high cost and complex management, and is not beneficial to the treatment of urban rivers, lakes and reservoirs; the biological method is greatly influenced by water quality fluctuation, has unstable dephosphorization effect and is easily influenced by external factors such as temperature, dissolved oxygen, pH value and the like; although the chemical method has a high phosphorus removal rate, the chemical method has a high operation cost, and easily generates a large amount of sludge which is difficult to treat, thereby causing secondary pollution. In comparison, the adsorption method has the advantages of low energy consumption, fast removal, stable phosphorus removal performance, no secondary pollution and the like. The key point of the application of the method lies in the selection of the excellent adsorbent, so that the method meets the requirements of strong adsorption capacity, easily available materials, reusability and low cost as much as possible.
However, the inorganic and organic fillers widely used in the market at present are difficult to satisfy the requirement of environmental friendliness. For example, the ceramsite filler which is widely applied in the inorganic filler needs a large amount of clay in the preparation process, conflicts with the current tense agricultural production land, and a large amount of energy is consumed in the sintering preparation process; most of raw materials for preparing the organic filler come from petroleum derivatives and belong to non-renewable resources. In addition, the fillers are difficult to biodegrade in the environment after being discarded, thus not only threatening the survival of the living organisms in the surrounding environment, but also limiting the reutilization of the discarded fillers.
In the prior art, some technologies for preparing environment-friendly fillers by using biomass as a raw material exist. For example, chinese patent No. 201610271844.9, published 2016, 06, 22, discloses a preparation method and an application of a nanoparticle-loaded expanded granular carbon dephosphorizing adsorbent, which is prepared by modifying lignocellulosic biomass with a surfactant, an amino starch binder and the like, and has high phosphorus adsorption efficiency, but the preparation process of the adsorbent is complex and is difficult to realize industrial application; for another example: chinese patent application No.: 201210100733.3, published as 8.1.2012, discloses a composite ecological filler and its preparation method, which comprises mixing steel slag particles with anthracite and zeolite at a ratio of 1:1:1 to obtain aggregate, mixing the aggregate, high-strength aluminate cement, ferric oxide and water at a certain ratio, and air drying in a well-ventilated place to obtain the final product. The preparation method of the filler realizes the purpose of treating wastes with wastes, but has a great problem on the secondary utilization of the adsorption saturated filler. For another example, chinese patent application No. 201410430743.2, application publication No. 2014, 12/24. This patent discloses a patent document entitled "modified shaddock peel adsorbent and method for producing the same" which is specifically modified based on the adsorption characteristics of metal ions in a cationic state and is not suitable for adsorption of phosphate in an anionic state. Other patents such as chinese patent No. 200710118941.5, published on 2007, 11/7/a, disclose a patent document entitled preparation of a novel biofilm carrier and its use in industrial wastewater treatment, chinese patent application no: 200510014992.4, published 2006, 5.31.a patent application document entitled controllable degradable cellulose-based microbial carrier filler for water treatment and a preparation method thereof is disclosed, as well as chinese patent nos.: 200510019894.X, published 2006, 6 and 28, is named as an application technology of a natural plant towel gourd hollow fiber material, the research results are poor in phosphorus adsorption effect, organic matters in the fillers are unstable in nature and are easily and rapidly degraded by microorganisms in water, so that the fillers are frequently replaced, and the load of the organic matters in the water is increased.
In the phosphorus removal adsorbent modification technology, some modification methods with better phosphorus removal effect exist. For example, chinese patent No. 201310327020.5, published 2013, 10 and 23, discloses a patent document entitled biocarbon composite porous filler and a preparation method thereof, which is obtained by carbonizing biomass such as rice straw, peanut shell, etc., loading iron oxide, and performing microwave modification, and although an iron adsorbent has a good adsorption and phosphorus removal effect, the adsorption effect is easily affected by ambient environmental factors because the direct adsorption process is reversible. For another example: chinese patent No. 201610234529.9, published 2016, month 07, and day 20, discloses a phosphorus removal adsorbent named expanded graphite supported composite metal and a patent document of a preparation method thereof, wherein the patent document is that composite metal lanthanum and iron are supported and modified on expanded graphite, so that although the adsorption efficiency of the expanded graphite on phosphorus is improved, the utilization rate of metal ions is low, rare earth lanthanum is not easily available, and the price is high. And the ferric salt is rich in resources and low in price, and has very important practical significance for deeply exploring a modification method of the loaded iron to improve the phosphorus removal efficiency and relieve the eutrophication degree of the water body.
Disclosure of Invention
Aiming at the defects of high operation cost, difficult operation and easy secondary pollution in the existing technology for removing water phosphate, the invention provides a preparation method of a biological carbon composite adsorption material for removing water phosphate, so that the purposes of simple preparation process and low operation cost can be realized, the adsorption capacity of phosphate is improved, and an effective way is provided for the resource utilization of wastes.
In order to solve the above problems, the present invention adopts the following technical solutions.
The invention relates to a preparation method of a biological carbon composite adsorption material for removing water phosphate, which comprises the following specific steps:
(1) cutting and drying the shaddock peel and the orange peel to obtain biomass solid;
(2) heating and pyrolyzing the biomass solid in oxygen deficiency or oxygen-free environment;
(3) cooling the biomass solid after pyrolysis in the step (2), and then adding 1.2-1.5 mol/L FeSO4Shaking the solution, filtering and collecting biochar solid, adding 0.1-0.3 mol/L Na2S2O3In the solution, filtering and collecting the biochar solid after oscillation; cleaning living thingsAdding the carbon solid into 0.01-0.03 mol/L CTMAB solution, oscillating, filtering, washing with deionized water to neutrality, and drying at 80-100 deg.C for 5-6 hr;
(4) and (4) cleaning the mixture obtained in the step (3) with clear water, and drying to obtain the biological carbon composite adsorption material.
Preferably, in the step (1), the mass ratio of the shaddock peel to the orange peel is 1-9: 1. The biological carbon composite porous filler prepared in the range has high porosity and high adsorption efficiency.
Preferably, in the step (2), the pyrolysis temperature is 350-450 ℃. The adsorption efficiency is obviously reduced when the pyrolysis temperature is too high or too low. The pyrolysis time is selected for 20-30 minutes through multiple optimization experiments, biomass solids can be fully carbonized in the time period, and carbonized products are convenient to collect.
Preferably, in step (3), the shaking is carried out in a water bath at 25-45 ℃.
Preferably, the biocarbon composite adsorbent obtained by the above-described production method.
The biological carbon composite adsorption material is obtained by carbonizing biomass, loading nano iron and grafting functional groups. The invention utilizes the characteristics that the biological carbonaceous composite adsorption material has large specific surface area, is easy to disperse in aqueous solution and has a large number of active point sites on the surface to adsorb phosphate in water, and the specific principle is presumed as follows:
the carbonized shaddock peel and the carbonized orange peel have larger specific surface area, and have the adsorption characteristics of high reduction potential and high reaction rate after being loaded with nano iron; continuously adding CTMAB for modification, wherein the ammonium terminal of the CTMAB and the K of the biochar+、Mg2+And ion exchange is carried out, so that carbon long chain molecules of the surfactant are introduced, and the long chain has more hydrophobic active sites, so that the nano iron particles can be better adsorbed on the surface.
The existing form of phosphate in water is easily influenced by the pH value of the environment. Phosphorus in wastewater is usually present in the form of orthophosphate, polyphosphate and organophosphorus, and polyphosphate can be hydrolyzed into orthophosphate under acidic conditionsA phosphate salt. Therefore, in the process of adsorbing and removing phosphorus from wastewater, orthophosphate is mainly concerned. Orthophosphates are ionized in water with H2PO4 -、HPO4 2-And PO4 3-Three existing forms, H when the pH value of the water environment is 3.0-9.02PO4 -、HPO4 2-Is the predominant form of presence. When the phosphate reaches the inner ring layer of the surface of the adsorbent, the phosphate can be directly connected with metal ions through coordination bonds (shown in formulas 1 and 2); when the phosphate cannot reach the adsorption site and is coordinated with the adsorption site, the phosphate anions and the biochar composite adsorption material with positive charges can generate electrostatic attraction (shown in formulas 3 and 4) in the solution, so that the comprehensive adsorption capacity of the biochar composite adsorption material on the phosphate ions is promoted, and the aim of removing the phosphate in the water body is fulfilled.
Fe—OH-+H2PO4 -→Fe—H2PO4 -+OH-(1)
Fe—OH-+HPO4 2-→Fe—HPO4 2-+OH-(2)
Fe—OH2 ++H2PO4 -→Fe—OH2 +—H2PO4 -(3)
Fe—OH2 ++HPO4 2-→Fe—OH2 +—HPO4 2-(4)
Compared with the prior art, the invention has the beneficial effects that:
(1) the biological carbon composite adsorption material has certain pore structure and surface chemical characteristics, has higher removal rate (the removal rate can reach 95.50 percent when the concentration of P is 10.0 mg/L) to water phosphate (orthophosphate and pyrophosphate). after surface sewage with the concentration of phosphate of 10 mg/L is treated by the adsorption material, the content of the water phosphate reaches the surface water environment quality standard (GB 3838 and 2002) V (less than or equal to 0.4 mg/L).
(2) The invention comprehensively considers the economic cost and the carbonization effect of carbonization, obtains the optimum carbonization temperature of 350-450 ℃ and the carbonization time of 20-30 minutes through orthogonal optimization experiments of different carbonization parameters, improves the carbonization efficiency and saves the economic cost.
(3) The biomass solids adopted in the method are shaddock peel and orange peel, and the biomass raw materials are common substances in daily life, are wide in source and low in cost. The material with saturated adsorption can be used as phosphorus resource for secondary utilization after being filtered and collected. Not only realizes the resource utilization of the waste, but also brings good social and economic benefits.
Drawings
FIG. 1 is a schematic view of the preparation process of the present invention.
FIG. 2 is a scanning electron microscope image of the product of shaddock peel after biomass carbonization in example 1 of the present invention before modification.
FIG. 3 is a scanning electron microscope image of the modified product of carbonized shaddock peel biomass in example 1 of the present invention;
as can be seen from the figure, the surface structure of the modified composite adsorbing material is more dispersed, mainly due to the fact that CTMAB is inserted into the carbonized material layers.
FIG. 4 is a graph showing the energy spectrum analysis of the biomass of shaddock peel before modification after carbonization in example 1 of the present invention;
as can be seen from the figure, the main constituent elements of the carbonized product are C and O, and the carbonized product also contains trace elements such as Mg, Si, Cl, Ca and the like.
FIG. 5 is a diagram showing the modified energy spectrum of the biomass of shaddock peel in example 1 of the present invention;
as can be seen from the figure, the main elements of the modified carbonized product are C, O and Fe, wherein w (Fe) is 18.44%, which indicates that the surface of the modified adsorbing material is loaded with iron oxide and also contains trace elements such as Na, Al and S.
Detailed Description
The present invention will be described in further detail below with reference to the accompanying drawings, but the present invention is not limited thereto.
In the preparation of biomass materials in the present preparation method, the common property of two biomass solids is utilized in each step, so the preparation is described in the examples by taking only part of the materials and parameters as examples, and the preparation flow is shown in fig. 1.
Example 1
Cleaning pericarpium Citri Grandis, air drying, cutting, heating and pyrolyzing in muffle furnace at 350 deg.C in anoxic environment for 30 min, cooling, and adding 1.2 mol/L FeSO4Oscillating the solution for 60 minutes, filtering and collecting the carbonized biomass solid, and adding the cleaned carbonized biomass solid into Na containing 0.1 mol/L2S2O3And oscillating for 40 minutes, filtering and collecting the solid, adding the solid into a CTMAB solution containing 0.03 mol/L, oscillating for 50 minutes, filtering, washing with deionized water to be neutral, and drying at 80 ℃ for 6 hours to obtain the biological carbonaceous composite adsorption material 1.
Example 2
Cleaning pericarpium Citri Tangerinae, air drying, cutting, heating and pyrolyzing in muffle furnace in anoxic environment at 350 deg.C for 30 min, cooling, and adding 1.2 mol/L FeSO4Oscillating the solution for 60 minutes, filtering and collecting the carbonized biomass solid, and adding the cleaned carbonized biomass solid into Na containing 0.1 mol/L2S2O3And oscillating for 40 minutes, filtering and collecting the solid, adding the solid into a CTMAB solution containing 0.03 mol/L, oscillating for 50 minutes, filtering, washing with deionized water to be neutral, and drying at 100 ℃ for 5 hours to obtain the biological carbonaceous composite adsorption material 2.
Example 3
Cleaning and air-drying the shaddock peel and the orange peel, heating and pyrolyzing the shaddock peel and the orange peel in a muffle furnace in an oxygen-free environment at the pyrolysis temperature of 450 ℃ for 20 minutes, cooling the pyrolyzed material, mixing the shaddock peel and the orange peel according to the mass ratio of 9:1, and adding 1.5 mol/L of FeSO4Oscillating the solution for 60 minutes, filtering and collecting the carbonized biomass solid, and adding the cleaned carbonized biomass solid into Na containing 0.3 mol/L2S2O3After the solid is collected by filtration, the solid is added into a CTMAB solution containing 0.03 mol/L, shaken for 50 minutes, filtered and washed with deionized water untilAnd (4) neutralizing, and drying for 5 hours at 100 ℃ to obtain the biological carbonaceous composite adsorption material 3.
Example 4
The same as in example 3, except that the pyrolysis time was 30 minutes.
Example 5
The same as example 3, except that the mass ratio of the shaddock peel to the orange peel was 1: 1.
Comparative example
Cleaning and air-drying the shaddock peel, and then heating and pyrolyzing the shaddock peel in a muffle furnace at 350 ℃ for 30 minutes. And cooling the pyrolyzed material, collecting carbonized biomass solids, and directly using the carbonized biomass solids as a phosphorus adsorption material after air drying.
The biological carbonaceous adsorption materials prepared in the above examples 1 to 5 and comparative example were respectively tested for phosphorus removal adsorption, and sodium dihydrogen phosphate (NaH) was used for the experiment2PO4) The phosphate concentration of the self-prepared phosphorus wastewater is 5 mg/L and 10 mg/L, the adsorption time is 15 hours, the water temperature is 35 ℃, and the oscillation speed is 150 rpm.
The test data shows that the adsorbing materials obtained in examples 1-5 of the present invention have very significant removal efficiency for phosphate in sewage (as shown in table 1). at phosphate concentrations of 5.0 mg/L and 10 mg/L, the removal rate of phosphorus by the adsorbing materials 1-5 is significantly higher than that of the comparative adsorbing material.
TABLE 1 phosphorus removal test results of various examples
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example | |
| Removal ratio at initial concentration of phosphorus of 5 mg/L (%) | 96.20 | 92.40 | 97.80 | 98.20 | 94.60 | 51.00 |
| Removal ratio at initial concentration of phosphorus of 10 mg/L (%) | 93.70 | 90.20 | 94.50 | 96.30 | 92.70 | 46.50 |
Claims (5)
1. A preparation method of a biological carbonaceous composite adsorption material for removing phosphate from surface water is characterized by comprising the following steps:
(1) cutting and drying the shaddock peel and the orange peel to obtain biomass solid;
(2) heating and pyrolyzing the biomass solid in oxygen deficiency or oxygen-free environment;
(3) cooling the biomass solid after pyrolysis in the step (2), and then adding 1.2-1.5 mol/L FeSO4Shaking the solution, filtering and collecting biochar solid, adding 0.1-0.3 mol/L Na2S2O3Adding the cleaned biological carbon solid into 0.01-0.03 mol/L CTMAB solution, vibrating, filtering, washing with deionized water to neutrality, and oven drying at 80-100 deg.C for 5-6 hr;
(4) and (4) cleaning the mixture obtained in the step (3) with clear water, and drying to obtain the biological carbon composite adsorption material.
2. The preparation method of the biological carbon composite adsorption material for removing phosphate from the surface water body according to claim 1, wherein in the step (1), the mass ratio of the shaddock peel to the orange peel is 1-9: 1.
3. The preparation method of the biological carbonaceous composite adsorption material for removing phosphate from the surface water body as claimed in claim 1, wherein in the step (2), the pyrolysis temperature is 350-.
4. The method for preparing the biological carbonaceous composite adsorption material for removing the phosphate from the surface water body according to claim 1, wherein in the step (3), the oscillation is carried out in a water bath at the temperature of 25-45 ℃.
5. The biological carbon composite adsorption material obtained by the preparation method of the biological carbon composite adsorption material for removing phosphate from surface water according to any one of claims 1 to 4.
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| CN109647337A (en) * | 2019-01-21 | 2019-04-19 | 河南永泽环境科技有限公司 | A kind of composite adsorbing material of denitrogenation dephosphorizing and preparation method thereof |
| CN110026156B (en) * | 2019-04-09 | 2022-03-04 | 华侨大学 | Preparation method and application of zirconium oxide loaded shaddock peel adsorbent |
| CN110302750B (en) * | 2019-05-16 | 2020-04-28 | 东莞理工学院 | Efficient phosphorus removal biochar and preparation method and application thereof |
| CN110180498A (en) * | 2019-05-23 | 2019-08-30 | 江苏省农业科学院 | Carry the preparation method and application of lanthanum magnetism hydro-thermal charcoal adsorbent |
| CN111302482B (en) * | 2020-03-03 | 2022-04-05 | 北京林业大学 | Biological retention material for synchronously removing nitrogen, phosphorus and pesticides in rainwater runoff and application method |
| CN115106063B (en) * | 2022-07-06 | 2023-08-15 | 重庆大学 | Porous biochar prepared from eggshells and orange peels and application of porous biochar in dephosphorization |
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