CN114455664A - Visible light illumination enhanced type sterilization and decoloration dual-function water treatment agent - Google Patents
Visible light illumination enhanced type sterilization and decoloration dual-function water treatment agent Download PDFInfo
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- CN114455664A CN114455664A CN202110820596.XA CN202110820596A CN114455664A CN 114455664 A CN114455664 A CN 114455664A CN 202110820596 A CN202110820596 A CN 202110820596A CN 114455664 A CN114455664 A CN 114455664A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 35
- 230000001954 sterilising effect Effects 0.000 title claims abstract description 18
- 238000004659 sterilization and disinfection Methods 0.000 title claims abstract description 18
- 238000005286 illumination Methods 0.000 title description 6
- 239000000084 colloidal system Substances 0.000 claims abstract description 25
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 241000894006 Bacteria Species 0.000 claims abstract description 5
- 229910052709 silver Inorganic materials 0.000 claims abstract description 4
- 238000001179 sorption measurement Methods 0.000 claims abstract description 4
- 239000000470 constituent Substances 0.000 claims abstract description 3
- 239000003344 environmental pollutant Substances 0.000 claims abstract description 3
- 239000011941 photocatalyst Substances 0.000 claims abstract description 3
- 231100000719 pollutant Toxicity 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 31
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 22
- 238000001354 calcination Methods 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 14
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 14
- 229910021649 silver-doped titanium dioxide Inorganic materials 0.000 claims description 14
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 9
- 239000004202 carbamide Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 7
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 7
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 7
- BJAARRARQJZURR-UHFFFAOYSA-N trimethylazanium;hydroxide Chemical compound O.CN(C)C BJAARRARQJZURR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 5
- 230000007547 defect Effects 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 229910019792 NbO4 Inorganic materials 0.000 claims description 3
- 230000002950 deficient Effects 0.000 claims description 3
- 230000001788 irregular Effects 0.000 claims description 3
- 230000031700 light absorption Effects 0.000 claims description 3
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 230000009471 action Effects 0.000 claims description 2
- 230000001588 bifunctional effect Effects 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 230000020477 pH reduction Effects 0.000 claims 2
- 125000004433 nitrogen atom Chemical group N* 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 238000009825 accumulation Methods 0.000 abstract description 3
- 239000004408 titanium dioxide Substances 0.000 abstract description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract 3
- BFRGSJVXBIWTCF-UHFFFAOYSA-N niobium monoxide Chemical compound [Nb]=O BFRGSJVXBIWTCF-UHFFFAOYSA-N 0.000 abstract 3
- 229910001923 silver oxide Inorganic materials 0.000 abstract 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Substances [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 abstract 2
- 239000011148 porous material Substances 0.000 abstract 1
- 239000004332 silver Substances 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 13
- 230000000844 anti-bacterial effect Effects 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000003899 bactericide agent Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 238000004042 decolorization Methods 0.000 description 2
- 230000009977 dual effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000000703 high-speed centrifugation Methods 0.000 description 1
- -1 hydroxyl free radical Chemical class 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000002648 laminated material Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
-
- 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
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
-
- 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
-
- 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)
- Water Supply & Treatment (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The invention provides visible light irradiation enhanced sterilization and decoloration dual-function water treatment and a preparation method thereof, namely silver/titanium dioxide and nitrogen-doped niobium-oxygen colloid are self-assembled in the form of nano sol to form a novel sterilization and decoloration dual-function layered water treatment agent. When no visible light is emitted, the water is used as a common water treatment agent, and silver sterilization and niobium-oxygen laminate pore accumulation adsorption decoloration are carried out; the water treatment agent can be used as a photocatalyst under visible light, and the constituent units of the water treatment agent, namely the silver/titanium dioxide and the nitrogen-doped niobium-oxygen laminate, can excite hydroxyl radicals (OH), oxidize and mineralize bacteria and colored pollutants in water, so that the sterilization and decoloration capabilities of the water treatment agent are enhanced, and the water treatment agent is suitable for being used in all-weather environments.
Description
Technical Field
The invention relates to a novel water treatment agent and a preparation method thereof, in particular to an illumination-enhanced sterilization and decoloration dual-function water treatment agent.
Background
A large amount of colored and bacteria-containing wastewater generated in the production process of industries such as papermaking, spinning, chemical engineering, medicine and the like. In recent years, as environmental protection policies are tightened, water treatment in the industries becomes a research hotspot. Ag. Cu, Zn and the like are widely applied as classical bactericides. Generally, the sterilization efficiency of the antibacterial material is improved by dispersing the sterilization ions such as Ag, Cu, Zn and the like on a molecular sieve, alumina, titanium dioxide, activated carbon and the like, and then forming a composite structure with other carriers.
The layered material is a three-dimensional structure material consisting of 2D laminates, has the advantages that the composition of the 2D laminates can be designed, the interlayer distance can be adjusted, the layer-by-layer accumulation can be controlled, and the like, and can form new acid sites, accumulation holes and larger specific surface area after the layered material is self-assembled, which are favorable for adsorption and catalytic reaction. Therefore, in recent years, attention has been paid to applications in the fields of materials, environmental protection, and the like. The traditional Nb-containing layered material has absorption in an ultraviolet region and weak absorption in a visible region, and can expand the absorption of the material to the visible region by doping nonmetal and metal to form vacancies.
In view of the above, the invention aims to construct a 2D laminate material and Ag/TiO with absorption in visible light region through a double-colloid self-assembly process2The composite material of the material is prepared by loading the traditional bactericide Ag in TiO in a highly dispersed manner2So as to realize different path treatment of the colored and bacteria-containing sewage under the conventional and illumination conditions.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the visible light illumination enhanced type Ag/TiO with double functions of sterilization and decoloration2-N/Nb2.89O10.89A water treatment agent and a preparation method thereof.
Ag/TiO2-N/Nb2.89O10.89A water treatment agent comprising: N/Nb2.89O10.89Structure and position in N/Nb2.89O10.89Internal Ag/TiO structure2(ii) a The N/Nb2.89O10.89The structure is composed of regular NbO4Tetrahedral and irregular defective N-NbO doped with N atoms4-xThe tetrahedra are connected through oxygen atoms and are orderly arranged into a layered structure, the doped defect structure can expand the light absorption to a visible region, and Ag/TiO2Ag is uniformly loaded on nano TiO2The particle clusters formed on the surface are integrally positioned among the layers of the laminated structure.
Ag/TiO2-N/Nb2.89O10.89The preparation method of the water treatment agent comprises the following steps:
Step 4, mixing the white sol Ag/TiO obtained in the step 12Slowly adding the colloid N-Nb in the step 32.89O10.89Stirring, centrifuging to obtain lower layer, washing, drying and calcining to obtain the final product Ag/TiO2-N/Nb2.89O10.89A water treatment agent.
Preferably, in the step 1, the ratio of titanium isopropoxide: water: ethanol volume ratio 20: 2: 80, stirring temperature of 60 ℃, stirring time of 12h, silver nitrate addition of 5ml and stirring time of 2 h.
Preferably, the nitrogen source in the step 2 adopts urea, K2CO3、Nb2O5And urea species in a ratio of 1.1: 3: 0.1.
preferably, the layer N/HNb in the step 3 is2.89O10.89The mass ratio of trimethyl ammonium hydroxide to water is 1:0.3:100, the stirring time is 7 days at room temperature, and the centrifugal speed is 10000 rpm.
Preferably, the white sol Ag/TiO in the step 42: colloidal N/Nb2.89O10.89The volume ratio is 1:1, the centrifugal rotation speed is 10000rpm, the drying temperature is 80 ℃, the drying time is 12h, the calcining temperature is 400 ℃, and the calcining time is 3 h.
The beneficial effects of the invention are: Ag/TiO 22Nb doped with nitrogen in the form of nanosol2.89O10.89The colloid is self-assembled to form a novel bactericidal and decolor bifunctional layered water treatment agent: Ag/TiO in the absence of visible light2-N/Nb2.89O10.89As a conventional water treatment agent, Ag and N/Nb2.89O10.89The laminated plate has double functions of sterilization and physical adsorption decoloration due to the stacked gaps; under visible light, Ag/TiO2-N/Nb2.89O10.89As a photocatalyst, its constituent unit Ag/TiO2And N/Nb2.89O10.89The water treatment agent can excite strong oxidant namely hydroxyl free radical (OH), bacteria and colored pollutants in water are oxidized and mineralized under the action of the OH, and on the basis of conventional degerming and decoloring, the sterilization and decoloring capacity of the water treatment agent can be enhanced by visible light illumination, so that the water treatment agent is suitable for being used in all-weather environments.
Drawings
FIG. 1 shows Ag/TiO2-N/Nb2.89O10.89A water treatment agent structure diagram; in the figure, 1 is N/Nb2.89O10.89Layer board 2 is TiO2Colloid, 3 is Ag nano-particles.
Detailed Description
The present invention will be further described with reference to the following examples. The following examples are set forth merely to aid in the understanding of the invention. It should be noted that, for a person skilled in the art, several modifications can be made to the invention without departing from the principle of the invention, and these modifications and modifications also fall within the protection scope of the claims of the present invention.
The Ag/TiO of the invention2-N/Nb2.89O10.89The water treatment agent comprises N/Nb2.89O10.89Structure and position in N/Nb2.89O10.89Internal Ag/TiO structure2A nanoparticle; N/Nb2.89O10.89From regular NbO4Tetrahedral and irregular defective N-NbO doped with N atoms4-xThe tetrahedra are connected via oxygen atoms and are arranged in an ordered manner to form a layered structure, the doped defect structure being such thatThe light absorption extends to the visible region; Ag/TiO 22Ag is uniformly loaded on nano TiO2The particle clusters formed on the surface are integrally positioned among the layers of the laminated structure. The preparation method comprises the following steps: adding a certain amount of Ag/TiO2Colloid and nitrogen-doped Nb2.89O10.89Forming self-assembly system with nano colloid, centrifuging, drying and calcining to obtain layered Ag/TiO2-N/Nb2.89O10.89A water treatment agent.
Example 1:
dispersing 20ml of titanium isopropoxide into 80ml of ethanol solution, adding 2ml of deionized water, and stirring and refluxing for 12 hours at 60 ℃ to form white colloid; cooling to room temperature, adding 0.01M silver nitrate solution 5ml into the colloid, and stirring for 2h to obtain colloid Ag/TiO2。
Will K2CO3、Nb2O5And urea in a mass ratio of 1.1: 3: 0.1, adding the mixture into an agate mortar for full grinding, calcining at 600 ℃ for 2h, and then calcining at 900 ℃ for 3h to obtain layered N/KNb2.89O10.89(ii) a Will be layered N/KNb2.89O10.89And 6mol/L hydrochloric acid is dispersed in deionized water solution according to the volume ratio of 1:100, after stirring for 7 days at room temperature, high-speed centrifugation is carried out, the lower layer solid is taken out, washed until no chloride ion is contained (ICP detection), and dried to obtain the layered N/HNb2.89O10.89。
Mixing N/HNb2.89O10.89Mixing trimethyl ammonium hydroxide and water according to the mass ratio of 1g: 0.3 g:100 g, stirring at room temperature for 7 days, centrifuging at 10000rpm, taking the upper layer colloidal liquid, and recording as colloid N/Nb2.89O10.89。
50ml of colloidal Ag/TiO2Slowly adding dropwise to 50ml of colloid N/Nb2.89O10.89Stirring, centrifuging at 10000rpm, drying at 80 deg.C for 12h, calcining at 400 deg.C for 3h to obtain visible light irradiation enhanced type Ag/TiO with dual functions of sterilization and decolorization2-N/Nb2.89O10.89A water treatment agent.
Example 2:
dispersing 20ml titanium isopropoxide into 80ml ethanol solution, adding 4ml deionized water, stirring and refluxing at 40 deg.C for 24 hr to obtain white pigmentColor colloid; cooling to room temperature, adding 8ml of 0.01M silver nitrate solution into the colloid, and continuously stirring for 2h to obtain colloid Ag/TiO2。
Will K2CO3、Nb2O5And urea in a mass ratio of 1.1: 3: 0.1, adding the mixture into an agate mortar for full grinding, calcining at 600 ℃ for 2h, and then calcining at 900 ℃ for 3h to obtain layered N/KNb2.89O10.89(ii) a Will be layered N/KNb2.89O10.89Dispersing 6mol/L hydrochloric acid in deionized water solution according to the volume ratio of 1:100, stirring at room temperature for 7 days, centrifuging at high speed, taking out lower layer solid, washing until no chloride ion is contained (ICP detection), and drying to obtain layered N/HNb2.89O10.89。
Mixing N/HNb2.89O10.89Mixing trimethyl ammonium hydroxide and water according to the mass ratio of 1g: 0.5 g:100 g, stirring at room temperature for 7 days, centrifuging at 12000rpm, taking the upper layer colloidal liquid, and recording as colloid N/Nb2.89O10.89。
50ml of colloidal Ag/TiO2Slowly adding dropwise to 50ml of colloid N/Nb2.89O10.89Stirring, centrifuging at 9000rpm, drying at 80 deg.C for 12 hr, calcining at 450 deg.C for 3 hr to obtain visible light irradiation enhanced antibacterial and decolorizing dual-functional Ag/TiO2-N/Nb2.89O10.89A water treatment agent.
Example 3:
dispersing 20ml of titanium isopropoxide into 80ml of ethanol solution, adding 1ml of deionized water, and stirring and refluxing for 12 hours at 70 ℃ to form white colloid; cooling to room temperature, adding 2ml of 0.01M silver nitrate solution into the colloid, and continuously stirring for 2h to obtain colloid Ag/TiO2。
Will K2CO3、Nb2O5And urea in a mass ratio of 1.1: 3: 0.1, adding the mixture into an agate mortar for full grinding, calcining at 600 ℃ for 2h, and then calcining at 900 ℃ for 3h to obtain layered N/KNb2.89O10.89(ii) a Will be layered N/KNb2.89O10.89And 6mol/L hydrochloric acid are dispersed in deionized water solution according to the volume ratio of 1:100, stirred for 7 days at room temperature, centrifuged at high speed, and the lower solid is taken out and washed until no chloride ion is contained (ICP detection)Measuring), drying to obtain layered N/HNb2.89O10.89。
Mixing N/HNb2.89O10.89Mixing trimethyl ammonium hydroxide and water according to the mass ratio of 1g:0.1 g:100 g, stirring at room temperature for 7 days, centrifuging at 9000rpm, taking the upper layer colloidal liquid, and recording as colloid N/Nb2.89O10.89。
50ml of colloidal Ag/TiO2Slowly adding dropwise to 50ml of colloid N/Nb2.89O10.89Stirring, centrifuging at 10000rpm, drying at 80 deg.C for 12h, calcining at 400 deg.C for 5h to obtain visible light irradiation enhanced type Ag/TiO with dual functions of sterilization and decolorization2-N/Nb2.89O10.89A water treatment agent.
Claims (7)
1. A visible light irradiation enhanced type sterilization and decoloration dual-function water treatment agent is characterized by comprising: N/Nb2.89O10.89Two-dimensional laminate structure and N/Nb-site2.89O10.89Internal Ag/TiO structure2(ii) a The N/Nb2.89O10.89The structure is composed of regular NbO4Tetrahedral and N atom doped irregular defective N/NbO4-xThe tetrahedra are connected through oxygen atoms and are orderly arranged into a layered structure, the doped defect structure can expand the light absorption to a visible region, and Ag/TiO2Ag is uniformly loaded on nano TiO2The particle clusters formed on the surface are integrally positioned among the layers of the laminated structure.
2. The Ag/TiO of claim 12-N/Nb2.89O10.89The preparation method of the water treatment agent is characterized by comprising the following steps:
step 1, adding a certain amount of titanium isopropoxide into a mixed solution of deionized water and ethanol, stirring at a certain temperature, cooling after white sol is formed, then adding a certain amount of silver nitrate with the concentration of 0.01M into the sol, fully stirring at room temperature for a certain time, and dissolving to obtain white sol Ag/TiO2;
Step 2, adding K2CO3、Nb2O5And urea according to a certain proportionCalcining at 600 deg.C for 2 hr and 900 deg.C for 3 hr to obtain layered N/KNb2.89O10.89(ii) a Will be layered N/KNb2.89O10.89Dispersing 6mol/L hydrochloric acid in deionized water solution according to the volume ratio of 1:100, stirring at room temperature for 7 days, centrifuging at high speed, taking out lower layer solid, washing until no chloride ion is contained, and drying to obtain layered N/HNb2.89O10.89;
Step 3, adding N/HNb2.89O10.89Mixing trimethyl ammonium hydroxide and water at a certain ratio, stirring at room temperature for a certain time, centrifuging at high speed to obtain upper layer colloidal liquid, and recording as colloid N/Nb2.89O10.89;
Step 4, mixing the white sol Ag/TiO obtained in the step 12Slowly adding the colloid N-Nb in the step 32.89O10.89Stirring, centrifuging to obtain lower layer, washing, drying and calcining to obtain the final product Ag/TiO2-N/Nb2.89O10.89A water treatment agent.
3. Ag/TiO according to claim 22-N/Nb2.89O10.89The preparation method of the water treatment agent is characterized by comprising the following steps: titanium isopropoxide in the step 1: water: ethanol volume ratio 20: and (1-5) stirring at 40-70 ℃ for 1-24h, adding 1-10ml of silver nitrate and stirring for 1-6 h.
4. Ag/TiO according to claim 22-N/Nb2.89O10.89The preparation method of the water treatment agent is characterized by comprising the following steps: in the step 2, the nitrogen source adopts urea K2CO3、Nb2O5And urea substance in a ratio of (1-1.3) to 3: 0.1; further characterized in that: nitrogen is doped in the K-type layered structure to form a doped defect structure, and then acidification treatment is carried out to reach the H-type layered structure, so that secondary calcination of doping N after acidification is avoided, and the stability of the layered structure is maintained.
5. Ag/TiO according to claim 22-N/Nb2.89O10.89Water treatment agentThe preparation method is characterized by comprising the following steps: in the step 3, layered N/HNb2.89O10.89The mass ratio of trimethyl ammonium hydroxide to water is 1 (0.1-0.5): 100, the stirring time at room temperature is 1-7 days, and the centrifugal rotation speed is 9000-.
6. Ag/TiO according to claim 22-N/Nb2.89O10.89The preparation method of the water treatment agent is characterized by comprising the following steps: in the step 4, white sol Ag/TiO2: colloidal N/Nb2.89O10.89The volume ratio is 1:1, the centrifugal rotation speed is 9000-.
7. The visible light irradiation enhanced type sterilization and decoloration bifunctional Ag/TiO material as claimed in claim 12-N/Nb2.89O10.89A water treatment agent characterized by: Ag/TiO in the absence of visible light2-N/Nb2.89O10.89As a conventional water treatment agent, Ag and N/Nb2.89O10.89The laminated plate has double functions of sterilization and physical adsorption decoloration due to the stacked gaps; under visible light, Ag/TiO2-N/Nb2.89O10.89As a photocatalyst, its constituent unit Ag/TiO2And N/Nb2.89O10.89Can excite strong oxidant-hydroxyl free radical (OH), oxidize and mineralize bacteria and colored pollutants in water under the action of OH, and visible light can enhance the sterilization and decoloration capacity of the water treatment agent, so that the water treatment agent is suitable for being used in all-weather environments.
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