CN114560548B - Method for removing dye in water body by activating persulfate through loofah sponge biochar catalyst - Google Patents
Method for removing dye in water body by activating persulfate through loofah sponge biochar catalyst Download PDFInfo
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- CN114560548B CN114560548B CN202210118471.7A CN202210118471A CN114560548B CN 114560548 B CN114560548 B CN 114560548B CN 202210118471 A CN202210118471 A CN 202210118471A CN 114560548 B CN114560548 B CN 114560548B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 134
- 244000280244 Luffa acutangula Species 0.000 title claims abstract description 121
- 235000009814 Luffa aegyptiaca Nutrition 0.000 title claims abstract description 121
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 66
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 230000003213 activating effect Effects 0.000 title claims abstract description 7
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- 238000006731 degradation reaction Methods 0.000 claims description 52
- CQPFMGBJSMSXLP-UHFFFAOYSA-M acid orange 7 Chemical compound [Na+].OC1=CC=C2C=CC=CC2=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 CQPFMGBJSMSXLP-UHFFFAOYSA-M 0.000 claims description 47
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- 229940043267 rhodamine b Drugs 0.000 claims description 10
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 9
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- 238000002360 preparation method Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical group NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 claims description 4
- 229940107698 malachite green Drugs 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 18
- 230000003197 catalytic effect Effects 0.000 abstract description 16
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- 238000005087 graphitization Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 239000000975 dye Substances 0.000 description 57
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 10
- 239000010802 sludge Substances 0.000 description 9
- 239000003344 environmental pollutant Substances 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- GSDSWSVVBLHKDQ-JTQLQIEISA-N Levofloxacin Chemical compound C([C@@H](N1C2=C(C(C(C(O)=O)=C1)=O)C=C1F)C)OC2=C1N1CCN(C)CC1 GSDSWSVVBLHKDQ-JTQLQIEISA-N 0.000 description 6
- XMEVHPAGJVLHIG-FMZCEJRJSA-N chembl454950 Chemical compound [Cl-].C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H]([NH+](C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O XMEVHPAGJVLHIG-FMZCEJRJSA-N 0.000 description 6
- 229960003376 levofloxacin Drugs 0.000 description 6
- 231100000719 pollutant Toxicity 0.000 description 6
- 150000003254 radicals Chemical class 0.000 description 6
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- 230000004913 activation Effects 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000002023 wood Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 241000209094 Oryza Species 0.000 description 4
- 235000007164 Oryza sativa Nutrition 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
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- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
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- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000000987 azo dye Substances 0.000 description 2
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- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 2
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- 229920002488 Hemicellulose Polymers 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
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- 150000001450 anions Chemical class 0.000 description 1
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- 230000007547 defect Effects 0.000 description 1
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- 230000018109 developmental process Effects 0.000 description 1
- 125000000664 diazo group Chemical group [N-]=[N+]=[*] 0.000 description 1
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- 229910002804 graphite Inorganic materials 0.000 description 1
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- 239000010903 husk Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
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- 238000011068 loading method Methods 0.000 description 1
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- 239000012528 membrane Substances 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 230000001089 mineralizing effect Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
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- 239000000843 powder Substances 0.000 description 1
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- 239000002243 precursor Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
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- 229910001428 transition metal ion Inorganic materials 0.000 description 1
Classifications
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/084—Decomposition of carbon-containing compounds into carbon
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The application discloses a method for removing dye in water by using a loofah sponge charcoal catalyst to activate persulfate, which is characterized in that the loofah sponge charcoal catalyst is used for degrading dye wastewater, wherein the loofah sponge charcoal catalyst is prepared by calcining loofah sponge and modifying the loofah sponge by acid, and the calcining temperature is 750-850 ℃. The loofah sponge biochar catalyst adopted in the application has the advantages of high graphitization degree, ordered whole structure, thin tube wall, rich micropore structure, large specific surface area, excellent catalytic activity and the like, and has the advantages of simplicity in operation, no need of large-scale equipment, low cost, wide application range, small use amount, high treatment efficiency, good treatment effect, strong reusability, environmental friendliness and the like when being used for activating persulfate to degrade the dye in the water body, can efficiently degrade the dye in the water body, and has good application value.
Description
Technical Field
The application belongs to the field of luffa recycling and advanced oxidation treatment of environmental pollutants, and particularly relates to a method for removing dyes in water by using luffa biochar catalyst to activate persulfate.
Background
Along with the development of the printing and dyeing industry and the intermediate chemical industry production industry, a large amount of dye wastewater is discharged into water bodies, particularly azo dye wastewater, which can occupy more than two thirds of the printing and dyeing wastewater, and serious harm is caused to water bodies and water body organisms, and azo dyes become research important and difficult points due to the characteristics of high chromaticity, poor biodegradability, complex components, high toxicity and the like. In order to achieve decolorization and mineralization of dyes in wastewater, more and more researchers are working to find efficient, energy-saving, environment-friendly and lower-cost dye treatment methods.
At present, main treatment technical methods of dye wastewater can be classified into destructive methods and non-destructive methods. Non-destructive methods include adsorption, precipitation filtration, membrane separation, etc., which can directly remove dye molecules, but cannot degrade or mineralize them; destructive methods are mainly advanced oxidation and biological methods, and such treatments can directly destroy the structure of dye molecules or mineralize them. Biological methods are widely used because of their economical efficiency and good effect; however, the method is complex in operation, has high requirements on the quality of the inlet water, and is not suitable for dye wastewater with high toxicity and poor biodegradability. Therefore, finding a treatment method capable of degrading dyes with high efficiency and environment-friendly is a great problem facing the society today.
The advanced oxidation method is most widely applied in the field of water treatment, and the method adopts an oxidant to react with organic pollutants in a water body to destroy the molecular structure of the pollutants, so that the pollutants are converted into other small molecular substances and even thoroughly mineralized, and the aim of removing the pollutants is fulfilled. Advanced oxidation techniques based on persulfates (e.g., sodium persulfate, PS) are considered to be an efficient method of eliminating dyes, and the sulfate radical (SO 4. Cndot. -) generated by persulfates has a higher redox potential, a wider PH application range, a stronger target contaminant selectivity, a longer half-life, and thus is able to mineralize dyes in water to a higher extent than advanced oxidation techniques based on hydroxyl radicals (OH-). From the point of view of the radical-based degradation mechanism, the hyperactive radicals may react with dye molecules by addition or other reactions, thereby breaking chemical bonds of the dye molecules, or mineralizing them directly into carbon dioxide and water.
Since persulfates are very stable at room temperature, activators become critical to the persulfate system, and many studies have focused on the activation of persulfates. In the existing persulfate activation method, methods such as heat, ultraviolet light, ultrasonic wave and the like need high energy and strict reaction conditions; transition metal ion activation requires complex post-treatments to remain clean; alkali activation requires adjustment of the pH of the system and may increase the risk of corrosion to the equipment. Therefore, the carbon-rich material biochar becomes a popular high-efficiency green catalyst with the advantages of good pore structure, large specific surface area, low cost, wide sources and the like. Waste biomass such as wood, sludge, manure, pesticide residues, etc. can be used to produce biochar by a thermochemical process, and the resulting biochar will be used to activate persulfates to produce Reactive Oxygen Species (ROS) to degrade organic pollutants. However, the present inventors found in previous studies that: the existing biochar prepared from waste biomass such as wood, sludge, manure, pesticide residues and the like is usually used as an adsorbent for adsorbing organic pollutants in a water body, the thorough removal of the organic pollutants is not realized, and the problems of complex subsequent recovery treatment, complex steps and the like exist; in addition, even if the catalyst is used as a catalyst for activating persulfate, the problems of poor activation effect, large catalyst consumption, long treatment time, low dye removal rate in water body and the like exist, and the aim of efficiently degrading the dye in the water body is difficult to achieve.
Therefore, the loofah sponge biochar catalyst with high graphitization degree, ordered integral structure, thin tube wall, rich micropore structure, large specific surface area and excellent catalytic activity is obtained, and has important significance for effectively activating persulfate and realizing effective degradation of dye.
Disclosure of Invention
The application aims to overcome the defects of the prior art and provide the method for removing the dye in the water body by using the loofah sponge biochar catalyst to activate the persulfate, which has the advantages of simple operation, no need of large-scale equipment, low cost, wide application range, small use amount, high treatment efficiency, good treatment effect, strong reusability and environmental friendliness.
In order to solve the technical problems, the application adopts the following technical scheme.
A method for removing dye in water by using loofah sponge charcoal catalyst activated persulfate comprises the steps of degrading dye wastewater by using loofah sponge charcoal catalyst activated persulfate; the loofah sponge biochar catalyst is prepared by calcining loofah sponge and modifying the loofah sponge with acid; the calcining temperature is 750-850 ℃.
The method is further improved, and the preparation method of the loofah sponge biochar catalyst comprises the following steps of:
s1, calcining loofah sponge under the protection of inert gas to obtain a calcined product;
s2, mixing the calcined product obtained in the step S1 with an acid solution, standing, washing and drying to obtain the loofah sponge biochar catalyst.
In the above method, further improved, in step S1, the temperature rising rate in the calcining process is 5 ℃/min, and the calcining time is 2h.
In the above method, further improved, in step S2, the concentration of the acid solution is 6mol/L, the acid solution is nitric acid, and the standing time is 12 hours.
In the above method, further improved, in step S1, the inert gas is nitrogen, and the retinervus luffae fructus further includes the following pretreatment before calcining: washing and drying retinervus Luffae fructus; the temperature of the drying was 60 ℃.
In the above method, further improved, in step S2, the drying temperature is 110 ℃, and the drying time is 12 hours; the drying process further comprises the following steps: grinding the dried product, and sieving with a 100-mesh sieve.
The method is further improved, and the degradation treatment is as follows: mixing the loofah sponge biochar catalyst with dye wastewater, stirring, adding persulfate to perform degradation reaction, and finishing degradation of the dye in the wastewater.
According to the method, the addition amount of the loofah sponge charcoal catalyst is 0.05-0.2 g of the loofah sponge charcoal catalyst added into each liter of dye wastewater.
The method is further improved, the initial concentration of the dye wastewater is 0.1 mg/L-20 mg/L, the initial pH value of the dye wastewater is 3-10, and the dye in the dye wastewater comprises at least one of rhodamine B, acid orange, methyl orange and malachite green; the adding amount of the persulfate is 5-15 mmol of persulfate per liter of dye wastewater, and the persulfate is sodium persulfate.
According to the method, the stirring time is 30min, and the degradation reaction time is 30-60 min.
Compared with the prior art, the application has the advantages that:
(1) The application provides a method for removing dye in water by using a loofah sponge charcoal catalyst to activate persulfate, which is used for degrading dye wastewater, wherein the adopted loofah sponge charcoal catalyst is prepared by calcining loofah sponge and modifying the loofah sponge by acid, and the calcining temperature is 750-800 ℃. Compared with the conventional biochar catalyst, the loofah sponge is selected as a precursor of the biochar, the loofah sponge has an obvious three-dimensional network tube bundle structure, and meanwhile, the components of the loofah sponge mainly contain cellulose, hemicellulose and lignin, wherein the cellulose and the lignin are beneficial to preparing the porous biochar material with developed pore structures, and the porous biochar catalyst has the advantages which are not possessed by the conventional biochar catalyst. Therefore, the loofah sponge biochar catalyst prepared by the method has a rich honeycomb porous structure, can provide more active sites in the degradation reaction process, is easier to generate multiple electron transfer, and improves the catalytic activity; moreover, the research shows that the catalytic mechanism and the deactivation of the catalyst are closely related to the swelling effect, the porous structure of the loofah sponge biochar catalyst is more beneficial to adsorbing reactants on the surface or in pores of the catalyst, the formed swelling effect can enable the reactants to better contact with active groups, the catalytic efficiency is further improved, and finally, the efficient removal of the dye in the water body is realized. Taking acid orange as an example, the degradation principle is shown in formulas (1) to (11), and specifically comprises the following steps: catalytic site on the surface of loofah sponge biochar catalyst activates persulfate to generate SO 4 ·- (OH) and (O) 2 – Isoradical and method of preparing the same 1 O 2 The persulfate can react with water to form SO 4 ·- Free radicals 1 O 2 These groups react with contaminants adsorbed on the catalyst surface to degrade the dye (acid orange) into small molecular substances until finally into water and carbon dioxide, thereby realizing efficient degradation of the dye. In the degradation reaction process of the application, besides the effect of free radicals, electrochemical characterization means are utilized to prove a non-free radical path mainly based on charge transferNamely, the loofah sponge biochar catalyst and Persulfate (PS) form an LSB-PS complex, and electrons are transferred from pollutants to the LSB-PS complex, so that the decomposition of the persulfate and the degradation of acid orange are accelerated. The method can be carried out at normal temperature and normal pressure, can mineralize various dyes (such as acid orange, methyl orange, rhodamine B, malachite green and the like) into water and carbon dioxide, can effectively carry out solid-liquid separation, has no secondary pollution, has the advantages of simple operation, no need of large-scale equipment, low cost, wide application range, small use amount, high treatment efficiency, good treatment effect, strong reusability, environmental friendliness and the like, can efficiently degrade the dyes in the water body, and has good application value.
S 2 O 8 2- +2H 2 O→HO 2 - +2SO 4 2- +3H + (1)
S 2 O 8 2- +HO 2 - →SO 4 ·- +SO 4 2- +·O 2 - +H + (2)
SO 4 ·- +OH – →SO 4 2- +HO· (3)
SO 4 ·- +H 2 O→HSO 4 - +HO· (4)
2·O 2 - +2H 2 O→H 2 O 2 +2OH – + 1 O 2 (5)
LSB surface -OOH+S 2 O 8 2- →LSB surface -OO ·- +SO 4 ·- +HSO 4 - (6)
LSB surface -OH+S 2 O 8 2- →LSB surface -O ·- +SO 4 ·- +HSO 4 - (7)
AO7+SO 4 ·- /HO·/·O 2 – / 1 O 2 →intermediates+CO 2 +H 2 O (8)
LSB+S 2 O 8 2- →[LSB-PS*] (9)
[LSB-PS*]+AO7→2SO 4 2- +LSB+AO7 OX (10)
S 2 O 8 2- +2e - →2SO 4 2- (11)
(2) Compared with other biochar catalysts prepared from waste biomasses such as wood, sludge, manure, pesticide residues and the like, the addition amount of the loofah sponge biochar catalyst is 0.05-0.2 g per liter of dye wastewater, and the loofah sponge biochar catalyst has the advantages of small catalyst usage amount, high degradation efficiency, short degradation time and the like from the aspects of catalyst usage amount, degradation reaction time and removal rate, can effectively activate persulfate, and achieves the aim of efficiently degrading dyes in water.
(3) The loofah sponge biochar catalyst is prepared from the loofah sponge serving as a raw material through simple pretreatment, calcination and acid modification, is a green, environment-friendly and economic heterogeneous catalytic material, and has the advantages of high graphitization degree, ordered integral structure, thin tube wall, abundant micropore structure, large specific surface area, excellent catalytic activity and the like; the preparation raw materials have wide sources and low price, and more accords with the standard of modern scientific technology of environmental protection, high quality and low price; the preparation method has the advantages of simple process, mild reaction condition, convenient operation, cleanness, no pollution and the like, is suitable for large-scale preparation and is convenient for industrial utilization.
(4) In the application, the crystallinity of the loofah sponge biochar catalyst is not obviously changed after the loofah sponge biochar catalyst is reused for four times, the catalyst recovery method after the loofah sponge biochar catalyst is simple, most of the catalyst can be obtained only through suction filtration, and the loss rate of the catalyst is low. Therefore, the loofah sponge biochar catalyst has the advantages of stable structure, simple recovery, high recovery rate and the like.
(5) In the application, the loofah sponge biochar catalyst also can show higher catalytic activity when degrading dye under the existence of a plurality of anions; meanwhile, the catalyst can degrade dye wastewater in the pH value of 3-10, can show higher catalytic activity, and has the advantage of wide application range. In addition, the loofah sponge charcoal catalyst disclosed by the application not only can realize high-efficiency degradation of conventional dye wastewater (such as rhodamine B, malachite green and the like) but also can realize high-efficiency degradation of diazo dye wastewater (such as acid orange, methyl orange and the like), so that the degradation system constructed by the loofah sponge charcoal catalyst and persulfate can effectively degrade the dye in the wastewater, and the removal rate can reach more than 95%.
(6) In the application, the loofah sponge biochar catalyst still can show higher catalytic activity in actual water bodies (tap water, river water and lake water), and can well operate in high-concentration and low-concentration dye wastewater (0.1 mg/L-20 mg/L).
Drawings
FIG. 1 is an SEM image of a loofah sponge biochar catalyst (LSB-800) prepared in example 1 of the present application.
FIG. 2 is an XRD pattern of the loofah sponge biochar catalyst (LSB-400, LSB-600, LSB-800) prepared in example 1 of the present application.
FIG. 3 is a graph showing the degradation effect of the loofah sponge charcoal catalyst prepared under the different calcination temperature conditions in example 1 of the present application on acid orange.
FIG. 4 is a graph showing the degradation effect of the loofah sponge biochar catalyst (LSB-800) of example 3 of the present application on acid orange under different pH conditions.
FIG. 5 is a graph showing the degradation effect of the loofah sponge biochar catalyst (LSB-800) on rhodamine B, acid orange, methyl orange, tetracycline hydrochloride and levofloxacin in example 4 of the present application.
FIG. 6 is a graph showing the degradation effect of the loofah sponge biochar catalyst (LSB-800) of example 5 of the present application on acid orange under different water conditions.
Detailed Description
The application is further described below in connection with the drawings and the specific preferred embodiments, but the scope of protection of the application is not limited thereby. The materials and instruments used in the examples below are all commercially available.
Example 1:
a method for removing dye in water by using loofah sponge charcoal catalyst to activate persulfate, specifically, the method for degrading acid orange wastewater by using loofah sponge charcoal catalyst to activate persulfate comprises the following steps:
weighing 20mg of loofah sponge biochar catalyst (LSB-400, LSB-600 and LSB-800) prepared under different calcining temperature conditions, respectively adding the loofah sponge biochar catalyst into 100mL of acid orange (AO 7) solution with the initial pH value of 3.42 and 20mg/L, magnetically stirring for 30min to ensure that adsorption balance is achieved, then adding 10mM sodium Persulfate (PS), and carrying out degradation reaction for 60min to finish the removal of the acid orange in the water body.
PS group: no catalyst was added and the other conditions were the same.
LSB-800 group: the persulfate was not added, and the other conditions were the same.
In the embodiment, the loofah sponge biochar catalyst (LSB-800) is prepared by calcining loofah sponge and modifying the loofah sponge with acid, and comprises the following steps:
(1) The collected retinervus Luffae fructus is removed seed, and then washed with deionized water to remove dust thereon, and then dried at 60deg.C in a forced air dryer, and stored in a sealed container after completely drying. And (3) placing the dried luffa into a tube furnace, heating to 800 ℃ according to a heating rate of 5 ℃/min under the protection of nitrogen atmosphere, calcining, and carbonizing for 2 hours to obtain a calcined product.
(2) Calcining the product at 100mL and 6M HNO 3 After soaking for 12 hours, washing with deionized water to neutrality and drying at 110 deg.c for 12 hours. Grinding the dried solid sample into powder, sieving with 100 mesh sieve (particle size<0.15 mm) to obtain the loofah sponge biochar catalyst, which is marked as LSB-800.
In this embodiment, the preparation method of the loofah sponge biochar catalyst (LSB-400) is basically the same as that of the loofah sponge biochar catalyst (LSB-800), and the difference is that: the calcination temperature for preparing LSB-400 was 400 ℃.
In this embodiment, the preparation method of the loofah sponge biochar catalyst (LSB-600) is basically the same as that of the loofah sponge biochar catalyst (LSB-800), and the difference is that: the calcination temperature for preparing LSB-600 was 600 ℃.
Characterization of loofah sponge biochar catalysts (LSB-400, LSB-600, LSB-800) prepared under different calcination temperature conditions prepared in example 1 of the present application: phase composition XRD, micro morphology SEM.
FIG. 1 is an SEM image of a loofah sponge biochar catalyst (LSB-800) prepared in example 1 of the present application. As can be seen from fig. 1, the loofah sponge biochar catalyst (LSB-800) has a significant honeycomb structure, which provides more catalytic active sites during the subsequent degradation reaction and provides electron transfer channels, which is beneficial to improve the catalytic activity of the loofah sponge biochar catalyst. Meanwhile, the network framework structure widely connected with LSB-800 provides conditions for dye adhesion, so that a good channel for electron mass transfer can be provided. In addition, compared with LSB-400 and LSB-600, the LSB-800 of the application has higher graphitization degree, more orderly overall structure, thinnest tube wall, more favorable electron transfer, larger specific area of the LSB-800 and abundant micropores, thereby providing more active sites in the degradation catalytic reaction process and finally realizing the efficient removal of dye in water.
FIG. 2 is an XRD pattern of the loofah sponge biochar catalyst (LSB-400, LSB-600, LSB-800) prepared in example 1 of the present application. As can be seen from fig. 2, the characteristic peak of the loofah sponge biochar catalyst corresponds to the characteristic peak of C, and the main phase composition of the loofah sponge biochar catalyst is graphite carbon.
In the degradation reaction process, 2mL samples are respectively taken by a syringe at 5min, 10min, 20min, 30min and 60min and placed in a 5mL centrifuge tube (0.5 mL of methanol quencher is added in advance to terminate the reaction), and then the concentration of the sample is measured at 485nm wavelength by ultraviolet, so that the removal rate of the different loofah sponge biochar catalysts on acid orange is obtained.
FIG. 3 is a graph showing the degradation effect of the loofah sponge charcoal catalyst prepared under the different calcination temperature conditions in example 1 of the present application on acid orange. As can be seen from fig. 3, the removal rate of acid orange was only 10% when PS was used alone (PS group); when LSB-800 is used alone (LSB-800 group), the removal rate of acid orange is less than 25% in one hour due to the adsorption of LSB-800 itself. When the loofah sponge biochar catalyst and PS are combined, the removal rates of the LSB-400, the LSB-600 and the LSB-800 on acid oranges are 11%, 12% and 100% in sequence, and the reasons of low removal rates of the LSB-400 and the LSB-600 are as follows: on one hand, the calcination temperature is too low, so that the graphitization degree of the loofah sponge biochar catalyst is too low, and an orderly integral structure cannot be obtained; on the other hand, the calcination temperature is too low, the specific surface area of the prepared loofah sponge charcoal catalyst is too small, the adsorption of the catalyst to dye is poor, more catalytic active sites cannot be provided in the degradation reaction process, and finally the removal effect of the loofah sponge charcoal catalyst to the dye is affected. Therefore, the loofah sponge biochar catalyst (LSB-800) prepared by the method has the advantages that the degradation efficiency of the loofah sponge biochar catalyst on the acid orange is greatly improved, the removal rate of the acid orange can reach 100%, the acid orange can be completely degraded and removed, and the loofah sponge biochar catalyst also shows very excellent catalytic performance, and the loofah sponge biochar charcoal catalyst can efficiently activate PS. As can be seen, LSB-800 showed the best catalytic performance at an initial pH of 3.42, a PS concentration of 10mM and a catalyst loading of 0.2g/L, with a removal rate of 100% for acid orange in one hour.
Example 2:
a method for removing dye in water by using catalyst activated persulfate, specifically, degrading acid orange wastewater by using different catalyst activated persulfate, comprises the following steps:
sludge biochar, magnetic sludge biochar, iron-doped sludge biochar, rice bran biochar, rice husk biochar, wood dust biochar and the loofah sponge biochar catalyst (LSB-800) prepared in example 1 are respectively added into an acid orange solution (AO 7), stirred, persulfate is added for degradation reaction, and removal of acid orange in water is completed.
The catalyst, the pollutants, the technological parameters of the catalyst and the removal rate of acid orange are shown in table 1 (the sludge biochar, the magnetic sludge biochar, the iron-doped sludge biochar, the rice bran biochar, the rice hull biochar and the wood chip biochar in table 1 are all prepared by the prior art).
TABLE 1 degradation effects of different catalysts on acid orange
As can be seen from Table 1, compared with other biochar catalysts, the loofah sponge biochar catalyst provided by the application can realize efficient degradation of dye pollutants under the condition of relatively small dosage, is a novel Fenton catalyst with excellent performance, has the advantages of small catalyst dosage, high degradation efficiency, short degradation time and the like, can be widely used for degrading dyes in water, and has high use value and good application prospect.
Example 3:
a method for removing dye in water by using loofah sponge charcoal catalyst to activate persulfate, specifically, the method for degrading acid orange wastewater by using loofah sponge charcoal catalyst to activate persulfate comprises the following steps:
6 parts of 100mL and 20mg/L acid orange solution are taken, the pH values are respectively adjusted to 3, 3.42, 5, 7, 9 and 11, 20mg of the loofah sponge biochar catalyst (LSB-800) prepared in the example 1 is added, magnetic stirring is carried out for 30min, adsorption balance is achieved, then 10mM PS is added, degradation reaction is carried out for 30min, and removal of acid orange in the water body is completed.
In the degradation reaction process, 2mL of samples are respectively taken by a syringe at 5min, 10min, 20min and 30min and placed in a 5mL centrifuge tube (0.5 mL of methanol quencher is added in advance to terminate the reaction), and then the concentration of the samples is measured by ultraviolet at 485nm wavelength, so that the removal rate of the different loofah sponge biochar catalysts on acid oranges is obtained.
FIG. 4 is a graph showing the degradation effect of the loofah sponge biochar catalyst (LSB-800) of example 3 of the present application on acid orange under different pH conditions. As can be seen from FIG. 4, the LSB-800 of the present application has a removal rate of 87.6%,96%,83.9%,91.1% and 82.2% for acid orange at pH values of 3, 3.42, 5, 7 and 9; and the removal rate of LSB-800 to acid orange is less than 70% under the condition of pH value of 11. It can be seen that the loofah sponge biochar catalyst can achieve high-efficiency removal rate of acid orange in the pH value range of 3-10, which indicates that the loofah sponge biochar catalyst is prepared from the loofahThe application range of the pH value of the degradation system constructed by the complex biological carbon catalyst and PS is wider. In the degradation process of the acid orange, when the initial pH value of the acid orange solution is 3.0-9.0, the pH value in a reaction system is gradually changed into acidity or neutrality; however, when the initial pH of the acid orange solution is 11.0, the reaction system remains strongly basic. Thus, when the initial pH of the acid orange solution=11.0, the pH is at>In the heterogeneous system of pHpzc, the electrostatic repulsion of the acid orange is increased, and thus the removal efficiency of the acid orange is remarkably reduced; at the same time, at higher pH, PS will break down itself into SO via a non-radical pathway 4 2- ，O 2 And H 2 O, thereby inhibiting the active group SO 4 ·- Is generated; furthermore, under alkaline conditions, the reactive group SO 4 ·- Will be with OH - The reaction generates OH (hydroxyl radical), but the hydroxyl radical is quenched by byproducts generated by PS self-decomposition, thereby reducing the rate of degradation reaction.
Example 4:
a method for removing dye in water by using loofah sponge charcoal catalyst to activate persulfate, specifically, the method for degrading rhodamine B wastewater, acid orange wastewater, methyl orange wastewater, tetracycline hydrochloride and levofloxacin by using loofah sponge charcoal catalyst to activate persulfate comprises the following steps:
weighing 5 parts of the loofah sponge biochar catalyst (LSB-800) prepared in the example 1, respectively adding 20mg of the loofah sponge biochar catalyst into 100mL of a rhodamine B solution, 20mg/L of a lime solution, a methyl orange solution, tetracycline hydrochloride and levofloxacin (the initial pH values of the solutions are 3.42), magnetically stirring for 30min to ensure that adsorption balance is achieved, then adding 10mM of PS, and carrying out degradation reaction for 60min to remove rhodamine B, lime, methyl orange, tetracycline hydrochloride and levofloxacin in a water body.
In the degradation reaction process, 2mL samples are taken by a syringe respectively at 5min, 10min, 20min, 30min and 60min and placed in a 5mL centrifuge tube (0.5 mL of methanol quencher is added in advance to terminate the reaction), and then the concentration of the sample is measured at 485nm wavelength by ultraviolet, so that the removal rate of the loofah sponge charcoal catalyst on different dye wastewater is obtained.
FIG. 5 is a graph showing the degradation effect of the loofah sponge biochar catalyst (LSB-800) on rhodamine B, acid orange, methyl orange, tetracycline hydrochloride and levofloxacin in example 4 of the present application. As can be seen from FIG. 5, the removal rate of LSB-800 of the present application was 100%, 70%,58% for rhodamine B, acid orange, methyl orange, tetracycline hydrochloride, and levofloxacin. Therefore, the loofah sponge charcoal catalyst has a general degradation effect on the antibiotic wastewater, and has an excellent degradation effect on different dye wastewater, which indicates that a degradation system constructed by the loofah sponge charcoal catalyst and PS can degrade the dye in the wastewater, and the removal rate can reach 100%.
Example 5:
a method for removing dye in water by using loofah sponge charcoal catalyst to activate persulfate, specifically, the method for degrading acid orange wastewater by using loofah sponge charcoal catalyst to activate persulfate comprises the following steps:
4 parts of the loofah sponge biochar catalyst (LSB-800) prepared in the example 1 are weighed, 20mg of the loofah sponge biochar catalyst is respectively added into deionized water containing acidic orange, tap water, river water and lake water (the parameters of the waste water are 100mL, 20mg/L and the initial pH value is 3.42), magnetic stirring is carried out for 30min, adsorption balance is ensured, 10mM PS is added, degradation reaction is carried out for 30min, and removal of the acidic orange in the water body is completed.
In the degradation reaction process, 2mL of samples are respectively taken by a syringe at 5min, 10min, 20min and 30min and placed in a 5mL centrifuge tube (0.5 mL of methanol quencher is added in advance to terminate the reaction), and then the concentration of the sample is measured by ultraviolet at 485nm wavelength, so that the removal rate of the loofah sponge biochar catalyst on acid orange under different water conditions is obtained.
FIG. 6 is a graph showing the degradation effect of the loofah sponge biochar catalyst (LSB-800) of example 5 of the present application on acid orange under different water conditions. As can be seen from FIG. 6, the removal rate of the LSB-800 of the present application to acid orange in deionized water, tap water, river water and lake water is 96%,98.4%,91.6% and 95.4% in this order. Therefore, the loofah sponge biochar catalyst disclosed by the application works well in actual water bodies, and acid oranges in different water bodies are effectively degraded.
The above description is only of the preferred embodiment of the present application, and is not intended to limit the present application in any way. While the application has been described in terms of preferred embodiments, it is not intended to be limiting. Any person skilled in the art can make many possible variations and modifications to the technical solution of the present application or equivalent embodiments using the method and technical solution disclosed above without departing from the spirit and technical solution of the present application. Therefore, any simple modification, equivalent substitution, equivalent variation and modification of the above embodiments according to the technical substance of the present application, which do not depart from the technical solution of the present application, still fall within the scope of the technical solution of the present application.
Claims (7)
1. A method for removing dye in water by using a loofah sponge charcoal catalyst to activate persulfate is characterized in that the method is to degrade dye wastewater by using the loofah sponge charcoal catalyst to activate persulfate; the loofah sponge biochar catalyst is prepared by calcining loofah sponge and modifying the loofah sponge with acid; the calcining temperature is 750-850 ℃; the degradation treatment is as follows: mixing the loofah sponge biochar catalyst with dye wastewater, stirring, adding persulfate to perform degradation reaction, and finishing degradation of the dye in the wastewater; the addition amount of the loofah sponge charcoal catalyst is 0.2g of the loofah sponge charcoal catalyst added into each liter of dye wastewater, and the degradation reaction time is 60 minutes; the initial concentration of the dye wastewater is 0.1 mg/L-20 mg/L, the initial pH value of the dye wastewater is 3.42, and the dye in the dye wastewater comprises at least one of rhodamine B, acid orange, methyl orange and malachite green; the adding amount of the persulfate is 5-15 mmol of persulfate per liter of dye wastewater, and the persulfate is sodium persulfate.
2. The method for removing dye in water by using the loofah sponge charcoal catalyst to activate persulfate according to claim 1, wherein the preparation method of the loofah sponge charcoal catalyst comprises the following steps:
s1, calcining loofah sponge under the protection of inert gas to obtain a calcined product;
s2, mixing the calcined product obtained in the step S1 with an acid solution, standing, washing and drying to obtain the loofah sponge biochar catalyst.
3. The method for removing dye from water by using the loofah sponge charcoal catalyst to activate persulfate according to claim 2, wherein in the step S1, the temperature rising rate in the calcination process is 5 ℃/min, and the calcination time is 2h.
4. The method for removing dye from water by using the loofah sponge charcoal catalyst to activate persulfate according to claim 3, wherein in the step S2, the concentration of the acid solution is 6mol/L, the acid solution is nitric acid, and the standing time is 12 hours.
5. The method for removing dye from water by activating persulfate through a loofah sponge charcoal catalyst according to any one of claims 2 to 4, wherein in step S1, the inert gas is nitrogen, and the loofah sponge further comprises the following pretreatment before calcination: washing and drying retinervus Luffae fructus; the temperature of the drying was 60 ℃.
6. The method for removing dye from water by using the loofah sponge charcoal catalyst to activate persulfate according to any one of claims 2 to 4, wherein in the step S2, the drying temperature is 110 ℃, and the drying time is 12 hours; the drying process further comprises the following steps: grinding the dried product, and sieving with a 100-mesh sieve.
7. The method for removing dye from water by activating persulfate through loofah sponge charcoal catalyst according to claim 1, wherein the stirring time is 30min.
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