CN115318238A - Adsorbent for adsorbing Congo red dye in water and preparation method and application thereof - Google Patents
Adsorbent for adsorbing Congo red dye in water and preparation method and application thereof Download PDFInfo
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 104
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 title claims abstract description 74
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000001044 red dye Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000001179 sorption measurement Methods 0.000 claims abstract description 51
- 238000003756 stirring Methods 0.000 claims abstract description 35
- 239000002351 wastewater Substances 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 23
- 239000002131 composite material Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 abstract description 17
- 239000011259 mixed solution Substances 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 5
- 235000019441 ethanol Nutrition 0.000 description 12
- 239000000975 dye Substances 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000002835 absorbance Methods 0.000 description 6
- 239000000706 filtrate Substances 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002070 nanowire Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- -1 (azo) diamino Chemical group 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 239000002060 nanoflake Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- 239000013178 MIL-101(Cr) Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000987 azo dye Substances 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000012621 metal-organic framework Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000299 mutagenicity Toxicity 0.000 description 1
- 230000007886 mutagenicity Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0259—Compounds of N, P, As, Sb, Bi
-
- 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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- B01J2220/42—Materials comprising a mixture of inorganic materials
-
- 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
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
-
- 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
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention relates to an adsorbent for adsorbing Congo red dye in water, and a preparation method and application thereof. In a reaction kettle, WCl 6 Mixing with solvent anhydrous ethanol, and stirring to obtain light blue solution. Adding g-C to the light blue solution 3 N 4 After stirring, the temperature of the mixed solution is raised to 170-185 ℃, the pressure is raised to 2-2.5MPa, and the time lasts for 10-12h. Cooling, centrifuging, washing with distilled water and ethanol, and drying to obtain yellowish powder adsorbent g-C 3 N 4 ‑W 18 O 49 . Adding 100-120mg/L adsorbent g-C into wastewater containing Congo red dye 3 N 4 ‑W 18 O 49 Adsorption time of 3-4h, filtering and separating the adsorbent g-C 3 N 4 ‑W 18 O 49 . The adsorption amount of the adsorption material prepared by the invention to Congo red dye in wastewater is large and can reach 1452mg/g; the prepared adsorbing material can be recycled and can be quickly resolved under alkaline conditions.
Description
Technical Field
The invention belongs to the technical field of preparation of water treatment adsorbents, and particularly relates to a prepared efficient adsorbent for adsorption separation of Congo red dye in water. An adsorbent for adsorbing Congo red dye in water, a preparation method and application thereof.
Background
Due to the rapid development of modern industrialization, more and more organic dye wastewater comes from industries such as food, textile, leather, plastics, cosmetics, rubber, paper making, printing, electroplating and the like, and the organic dye wastewater is discharged into water environment without being fully treated, so that huge pollution risk is caused to the environment. Such as producing significant coloration, increasing the chemical oxygen demand of the water body, blocking light from entering the water system, and threatening the aquatic ecosystem. Wherein congo red (1-naphthalenesulfonic acid-3, 3- (4, 4-biphenylbis (azo) diamino) disodium salt) is a typical benzidine anionic azo dye, has inherent toxicity, mutagenicity and carcinogenicity, and has certain threat to aquatic organisms and human bodies. Meanwhile, congo red dye molecules have a complex aromatic structure and good physicochemical and thermo-optical stability, so that the Congo red dye molecules are difficult to biodegrade. Dye wastewater is often high in chroma and high in pollutant concentration and is difficult to purify. Therefore, how to reasonably and effectively treat the wastewater containing the Congo red becomes one of important and urgent environmental problems.
At present, there are various physical and chemical methods for removing congo red dye in water systems, such as filtration, adsorption, ion exchange, photocatalysis, biodegradation, electrochemical methods, etc. Among them, the adsorption method is considered to be a promising, effective and versatile technique because of its simple operation, high efficiency, no secondary pollution and reusable adsorbent. To date, a large number of adsorbents have been reported, such as clay, ash, activated carbon, molecular sieves, metal-organic frameworks, silicon nanomaterials, and metal oxides, among others. However, many adsorbents have disadvantages of small adsorption capacity and difficult analysis treatment, which limits their practical applications. For example, the adsorption capacity of the carbonated hydroxyapatite after adsorbing Congo red for 60min is 24.59mg/g, the adsorption capacity of the MIL-101 (Cr) after adsorbing Congo red for 180min is about 115mg/g andMgFe 2 O 4 -NH 2 the adsorption capacity after adsorbing Congo red for 180min is 71.4mg/g. (chemical research and application, 2020, 32 (4): 600-608, sep.Purif.Technol.2017, 177, 272-280, ACS appl.Nano Mater.2019,2 5329-5341; therefore, designing an adsorbent with high adsorption performance, eco-friendliness and good cycle performance for wastewater treatment remains a great challenge.
Disclosure of Invention
In order to reasonably and effectively treat the wastewater containing the Congo red dye and efficiently adsorb and separate the Congo red dye from the Congo red wastewater, the research finds that the nano oxide has large specific surface area and has higher active sites due to quantum effect, so the nano oxide has important application prospect in the aspect of adsorbing and removing organic pollutants in water environment, such as Ba 5 Si 8 O 21 ZnO, mgO and WO 3 And the like. The simultaneous study found that the defect W 18 O 49 Perfect WO 3 Has better adsorption capacity. Defect state W therein 18 O 49 Deeply attracts our attention, though a single W 18 O 49 The adsorbent has certain adsorption capacity, but cannot meet the adsorption requirement of people, so that through careful analysis and detailed research, people apply W 18 O 49 And g-C 3 N 4 The composite adsorbent has better adsorption capacity, wider application range and more stability. Calcining urea as precursor to obtain g-C with uniform porous structure 3 N 4 The nano-flake has certain adsorption capacity and can be used as a carrier. Then W is mixed 18 O 49 The nano-wire grows on the surface in situ to prepare the nano-adsorbent with a three-dimensional network structure (g-C for short in the invention) 3 N 4 -W 18 O 49 ) And the adsorption treatment method is applied to the adsorption treatment process of Congo red dye wastewater, and has very strong adsorption capacity on the Congo red dye.
The invention designs and synthesizes a novel, high-efficiency and reusable adsorbentCongo red dye in the adsorption water. The adsorbent of the present invention is g-C 3 N 4 And W 18 O 49 Composite of compositions, hereinafter abbreviated to g-C 3 N 4 -W 18 O 49 。
The technical scheme adopted by the invention is as follows:
an adsorbent for adsorbing Congo red dye in water; the adsorbent is g-C 3 N 4 And W 18 O 49 A composite of the components.
A preparation method of an adsorbent for adsorbing Congo red dye in water comprises the following steps:
1) In a reaction kettle, WCl 6 Mixing with solvent anhydrous ethanol, and stirring to obtain light blue solution;
2) Adding g-C to the light blue solution 3 N 4 After stirring, heating the mixed solution to 170-185 ℃, and increasing the pressure to 2-2.5MPa for 10-12h;
3) Cooling, centrifuging, washing with distilled water and ethanol, and drying to obtain yellowish powder adsorbent g-C 3 N 4 -W 18 O 49 。
The mass of the ethanol and the WCl 6 The mass ratio is (150-170): 1.
the WCl 6 Mixing with ethanol, and stirring for 20-30min.
Said g-C 3 N 4 Mass and WCl 6 The mass ratio is (0.2-0.4): 1.
said addition of g to C 3 N 4 Then stirring for 30-40min.
The method for adsorbing Congo red in water by using the adsorbent provided by the invention is characterized in that 100-120mg/L adsorbent g-C is added into wastewater containing Congo red dye 3 N 4 -W 18 O 49 The adsorption time is 3 to 4 hours, and the adsorbent g-C is separated by filtration 3 N 4 -W 18 O 49 。
Preferably, the adsorption temperature is from 25 to 45 ℃.
The Congo red desorption experiment is realized through a simple and easy operation mode. Washing with aqueous sodium hydroxide solutionThe operations of ultrasonic treatment, ethanol washing, ultrasonic treatment, separation, drying and the like are carried out, and then 4 times of cyclic adsorption experiments are carried out repeatedly, and the result shows that the g-C 3 N 4 -W 18 O 49 The performance of the composite adsorbent for adsorbing Congo red still keeps a higher level (1210 mg/g).
The invention adopts an in-situ solvothermal method to mix g-C 3 N 4 And W 18 O 49 Compounding to prepare g-C 3 N 4 And W 18 O 49 Composite adsorbents, abbreviated as g-C 3 N 4 -W 18 O 49 。
In a reaction kettle, WCl 6 Mixing with anhydrous ethanol, and stirring for a certain time to obtain light blue solution. To this solution was added g-C 3 N 4 After stirring for a certain time, the mixed solution is heated and pressurized, and is kept for a certain time under the high-temperature and high-pressure state. Finally, obtaining light yellow powder after cooling, centrifuging, washing by distilled water and ethanol and drying, thus obtaining the efficient adsorbent g-C of the invention 3 N 4 -W 18 O 49 . In the preparation of the adsorbents g to C of the invention 3 N 4 -W 18 O 49 In this case, the preparation process conditions are very important and should be well controlled. For preparing efficient Congo red adsorbent g-C 3 N 4 -W 18 O 49 The key conditions for the preparation we used and defined.
The basic process of adsorbing Congo red dye in waste water by using the adsorbent prepared by the invention is as follows:
adding the adsorbent g-C of the invention into wastewater containing Congo red dye 3 N 4 -W 18 O 49 Stirring for adsorption, keeping at a certain temperature for a period of time, and filtering to separate out adsorbent g-C 3 N 4 -W 18 O 49 . The adsorbed wastewater is colorless.
Adsorbent g-C 3 N 4 -W 18 O 49 The proper addition amount in the waste water is 100-120mg/L. The addition amount of the adsorbent is too small, the adsorption capacity is insufficient, and the addition amount of the adsorbent is too much, so that the better adsorption effect cannot be reflected, but the adsorption effect can be reflectedResulting in waste of the adsorbent.
Adsorbents g to C of the invention 3 N 4 -W 18 O 49 The adsorbent is prepared by a solvent method, the preparation process is simple, and the pollution is less when the adsorbent is prepared. The adsorbent has high adsorption capacity on Congo red dye, and the adsorption capacity is higher than that of common adsorbents such as activated carbon and molecular sieve. The Congo red dye adsorbed by analysis is simple in process, the adsorbent can be recycled for multiple times, and the adsorption capacity can reach 1210mg/g after 4 adsorption cycles.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments in order to more clearly describe the objects and advantages of the present invention. The specific embodiments described herein are merely illustrative of the present invention and do not delimit the technology.
Preparation examples 1 and 2 below prepare materials g to C, respectively 3 N 4 And material W 18 O 49 Or g-C purchased or otherwise 3 N 4 And material W 18 O 49 The present invention can be implemented.
Preparation example 1
g-C 3 N 4 Preparing nano flakes:
yellow g-C was prepared using literature methods (appl. Catal. B: environ, 2017, 217 3 N 4 And (3) powder. 2.0g of urea was placed in a crucible with a lid and calcined in a muffle furnace under air conditions. Calcining at 400 deg.C for 1h at a heating rate of 2.0 deg.C/min. The resulting powder was then thoroughly ground and dispersed in 0.5M HNO 3 In aqueous solution, sonicated for 3h and heated in a water bath at 80 ℃ for 3h. Finally, centrifugal separation, washing to neutrality and drying are carried out.
Preparation example 2
W 18 O 49 Preparing the nano wire:
w was prepared using the method of literature (j.colloid inter.sci., 2020, 579 18 O 49 A nanowire.
In a 80mL reaction vessel, 0.2g WCl 6 Mixing with 40mL of absolute ethyl alcohol, and stirring for 20-30min to form a light blue solution. Then the reaction kettle is closed, the temperature and the pressure of the mixed solution are raised, the temperature is maintained at 178-181 ℃, and the pressure is maintained at 2-2.5MPa for 10-12h. Finally cooling, centrifugally separating, washing with distilled water and ethanol, and drying to obtain light yellow powder, namely W 18 O 49 。
Example 1
g-C 3 N 4 -W 18 O 49 Preparing a Congo red adsorbent:
wherein the mass of ethanol and WCl 6 The mass ratio is 160:1.
the blue solution was prepared with stirring for 25min.
g-C 3 N 4 Mass and WCl 6 The mass ratio is 0.3:1.
adding g-C 3 N 4 After that, stirring was required for 35min.
The temperature is maintained at 180 ℃ and the pressure is 2MPa. The heat preservation time is 11h.
In a 80mL reaction vessel, 0.2g WCl 6 Mixing with 32g of absolute ethanol, stirring for 25min to form a light blue solution. To this solution was added 0.06g of g-C obtained in preparation example 1 3 N 4 After stirring for 35min, the mixed solution is heated and pressurized, the temperature is maintained at 180 ℃, and the pressure is maintained at 2MPa for 11h. Finally, obtaining light yellow powder after cooling, centrifugal separation, washing by distilled water and ethanol and drying, thus obtaining the efficient adsorbent g-C of the invention 3 N 4 -W 18 O 49 . Designated as adsorbent 1.
Example 2
g-C 3 N 4 -W 18 O 49 Preparing a Congo red adsorbent:
wherein the mass of ethanol is equal to WCl 6 The mass ratio is 170:1.
the blue solution was prepared with stirring for 30min.
g-C 3 N 4 Mass and WCl 6 The mass ratio is 0.2:1.
adding g-C 3 N 4 After that, stirring is required40min。
The temperature is maintained at 170 ℃ and the pressure is preferably 2.5MPa. The incubation time required 12h.
In a 80mL reaction vessel, 0.2g WCl 6 Mixing with 34g of absolute ethanol, and stirring for 30min to form a light blue solution. To this solution was added 0.04g of g-C obtained in preparation example 1 3 N 4 After stirring for 40min, the mixed solution is heated and pressurized, the temperature is maintained at 170 ℃, and the pressure is maintained at 2.5MPa for 12h. Finally, obtaining light yellow powder after cooling, centrifugal separation, washing by distilled water and ethanol and drying, thus obtaining the efficient adsorbent g-C of the invention 3 N 4 -W 18 O 49 . Designated as adsorbent 2.
Example 3
g-C 3 N 4 -W 18 O 49 Preparing a Congo red adsorbent:
wherein the mass of ethanol is equal to WCl 6 The mass ratio is 150:1.
stirring for a certain time to prepare a blue solution, and stirring for 20min.
g-C 3 N 4 Mass and WCl 6 The mass ratio is 0.4:1.
adding g-C 3 N 4 After that, stirring was required for 30min.
The temperature was maintained at 185 ℃ and the pressure at 2.5MPa. The holding time required 10h.
In an 80mL reaction kettle, 0.2g WCl 6 Mixing with 30g of anhydrous ethanol, and stirring for 20min to form a light blue solution. To this solution was added 0.08g of g-C obtained in preparation example 1 3 N 4 And after stirring for 30min, raising the temperature and the pressure of the mixed solution, keeping the temperature at 170 ℃ and keeping the pressure at 2.5MPa for 10h. Finally cooling, centrifugally separating, washing by distilled water and ethanol, and drying to obtain light yellow powder, namely the high-efficiency adsorbent g-C of the invention 3 N 4 -W 18 O 49 . Designated as adsorbent 3.
Example 4
With adsorbents g-C 3 N 4 -W 18 O 49 (adsorbent 1) Congo Red adsorbing WaterA dye.
To 100mL of Congo Red in water, the dye Congo Red concentration was 150mg/L, and 10mg of the adsorbents g-C prepared in example 1 were added 3 N 4 -W 18 O 49 I.e., adsorbent 1, was adsorbed at 45 ℃ for 3 hours with stirring. Filtering out the adsorbent, testing the change of Congo red absorbance of the filtrate by using an ultraviolet-visible spectrophotometer, and finally calculating the adsorption quantity, wherein the Congo red adsorption quantity is 1452.75mg/g adsorbent.
Example 5
With adsorbent g-C 3 N 4 -W 18 O 49 (adsorbent 2) adsorbs Congo red dye in water.
To 100mL of Congo Red in water, the dye Congo Red concentration was 150mg/L, and 10mg of the adsorbents g-C prepared in example 1 were added 3 N 4 -W 18 O 49 I.e., adsorbent 1, was adsorbed at 45 ℃ for 3 hours with stirring. Filtering out the adsorbent, testing the change of Congo red absorbance of the filtrate by using an ultraviolet-visible spectrophotometer, and finally calculating the adsorption amount, wherein the Congo red adsorption amount is 1442.66mg/g of the adsorbent.
Example 6
With adsorbents g-C 3 N 4 -W 18 O 49 (adsorbent 3) adsorbs congo red dye in water.
To 100mL of Congo Red in water, the dye Congo Red concentration was 150mg/L, and 10mg of the adsorbents g-C prepared in example 1 were added 3 N 4 -W 18 O 49 I.e., adsorbent 1, was adsorbed at 45 ℃ for 3 hours with stirring. Filtering the adsorbent, testing the change of Congo red absorbance of the filtrate by using an ultraviolet-visible spectrophotometer, and finally calculating the adsorption quantity, wherein the Congo red adsorption quantity is 1403.17mg/g of the adsorbent.
Example 7
With adsorbents g-C 3 N 4 -W 18 O 49 (adsorbent 1) adsorbs congo red dye in water.
To 100mL of Congo Red in water, the dye Congo Red concentration was 150mg/L, and 10mg of the adsorbents g-C prepared in example 1 were added 3 N 4 -W 18 O 49 I.e., adsorbent 1, was adsorbed at 35 ℃ for 3 hours with stirring. Filtering the adsorbent, testing the change of Congo red absorbance of the filtrate by using an ultraviolet-visible spectrophotometer, and finally calculating the adsorption capacity, wherein the Congo red adsorption capacity is 1360.26mg/g of the adsorbent.
Example 8
With adsorbents g-C 3 N 4 -W 18 O 49 (adsorbent 1) adsorbs Congo red dye in water.
To 100mL of Congo Red in water, the dye Congo Red concentration was 150mg/L, and 10mg of the adsorbents g-C prepared in example 1 were added 3 N 4 -W 18 O 49 I.e., adsorbent 1, was adsorbed at 25 ℃ for 3 hours with stirring. Filtering the adsorbent, testing the change of Congo red absorbance of the filtrate by using an ultraviolet-visible spectrophotometer, and finally calculating the adsorption quantity, wherein the Congo red adsorption quantity is 1109.94mg/g of the adsorbent.
Example 9
With adsorbents g-C 3 N 4 -W 18 O 49 (adsorbent 1) adsorbs Congo red dye in water.
In 100mL of Congo red aqueous solution, the dye Congo red concentration was 150mg/L, and 10mg of the adsorbents g to C prepared in example 1 were added 3 N 4 -W 18 O 49 I.e., adsorbent 1, was adsorbed at 45 ℃ for 2 hours with stirring. Filtering out the adsorbent, testing the change of Congo red absorbance of the filtrate by using an ultraviolet-visible spectrophotometer, and finally calculating the adsorption amount, wherein the Congo red adsorption amount is 1095.42mg/g adsorbent.
Example 10
Adsorbent g-C 3 N 4 -W 18 O 49 (adsorbent 1) Congo red dye was desorbed.
In 500mL of Congo red aqueous solution having a Congo red concentration of 150mg/L, 50mg of the adsorbents g to C prepared in example 1 of the present invention were added 3 N 4 -W 18 O 49 I.e., adsorbent 1, was adsorbed at 45 ℃ for 3 hours with stirring. Adding the filtered adsorbent into sodium hydroxide aqueous solution with certain concentration, stirring for 50-60 min, performing ultrasonic treatment for 2-3 min, washing and drying the adsorbent, and performing next adsorption experimentAfter repeating the reaction for four times, the adsorption quantity of the Congo red obtained is about 1210mg/g.
The invention belongs to the technical field of preparation of water treatment adsorbents, and provides a high-efficiency composite adsorbent g-C 3 N 4 -W 18 O 49 And is used for adsorption separation of Congo red dye in water. As can be seen from the above data, the composite adsorbent g-C prepared by the present patent 3 N 4 -W 18 O 49 The Congo red dye has quite excellent adsorption performance, and the adsorption capacity reaches 1452.75mg/g after 3-4h, which is 7-10 times of that of most reported adsorbents. Meanwhile, the solution can be quickly resolved under alkaline conditions, and the adsorption quantity of 1210mg/g can be still maintained after four times of circulation. The method has potential application in adsorbing organic pollutants in various wastewater in the future.
While the methods and techniques of the present invention have been described in terms of preferred embodiments, it will be apparent to those of skill in the art that variations and modifications of the methods and techniques described herein may be practiced without departing from the spirit and scope of the invention. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the spirit, scope and content of the invention.
Claims (8)
1. An adsorbent for adsorbing Congo red dye in water; characterized in that the adsorbent is g-C 3 N 4 And W 18 O 49 A composite of components.
2. The method for preparing an adsorbent for adsorbing congo red dye in water according to claim 1, comprising the steps of:
1) In a reaction kettle, WCl 6 Mixing with solvent anhydrous ethanol, and stirring to obtain light blue solution;
2) Adding g-C to the light blue solution 3 N 4 After stirring, mixingHeating the solution to 170-185 ℃, and boosting the pressure to 2-2.5MPa for 10-12h;
3) Cooling, centrifuging, washing with distilled water and ethanol, and drying to obtain yellowish powder adsorbent g-C 3 N 4 -W 18 O 49 。
3. The process according to claim 2, wherein the ethanol mass and WCl are 6 The mass ratio is (150-170): 1.
4. the method of claim 2, wherein WCl is used 6 Mixing with ethanol, and stirring for 20-30min.
5. The process according to claim 2, wherein g-C is 3 N 4 Mass and WCl 6 The mass ratio is (0.2-0.4): 1.
6. the process according to claim 2, wherein g-C is added 3 N 4 Then stirring for 30-40min.
7. The method for adsorbing Congo red in water by using the adsorbent of claim 1, wherein 100-120mg/L of adsorbent g-C is added to wastewater containing Congo red dye 3 N 4 -W 18 O 49 The adsorption time is 3 to 4 hours, and the adsorbent g-C is separated by filtration 3 N 4 -W 18 O 49 。
8. The process as claimed in claim 7, wherein the adsorption temperature is from 25 to 45 ℃.
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