CN109158122A - A kind of preparation method and application of nitrogen-doped nanometer silica photocatalysts - Google Patents
A kind of preparation method and application of nitrogen-doped nanometer silica photocatalysts Download PDFInfo
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- CN109158122A CN109158122A CN201810970605.1A CN201810970605A CN109158122A CN 109158122 A CN109158122 A CN 109158122A CN 201810970605 A CN201810970605 A CN 201810970605A CN 109158122 A CN109158122 A CN 109158122A
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- nitrogen
- photocatalysts
- doped nanometer
- silica
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 119
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 56
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000003054 catalyst Substances 0.000 claims abstract description 31
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002253 acid Substances 0.000 claims abstract description 12
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 10
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 10
- 230000032683 aging Effects 0.000 claims abstract description 6
- 239000007790 solid phase Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 28
- 230000015556 catabolic process Effects 0.000 claims description 21
- 238000006731 degradation reaction Methods 0.000 claims description 21
- 239000003344 environmental pollutant Substances 0.000 claims description 16
- 231100000719 pollutant Toxicity 0.000 claims description 15
- 229910052724 xenon Inorganic materials 0.000 claims description 10
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 10
- IZUPBVBPLAPZRR-UHFFFAOYSA-N pentachloro-phenol Natural products OC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl IZUPBVBPLAPZRR-UHFFFAOYSA-N 0.000 claims description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 7
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical group OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- WHHGLZMJPXIBIX-UHFFFAOYSA-N decabromodiphenyl ether Chemical compound BrC1=C(Br)C(Br)=C(Br)C(Br)=C1OC1=C(Br)C(Br)=C(Br)C(Br)=C1Br WHHGLZMJPXIBIX-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000012544 monitoring process Methods 0.000 claims description 5
- LAXBNTIAOJWAOP-UHFFFAOYSA-N 2-chlorobiphenyl Chemical group ClC1=CC=CC=C1C1=CC=CC=C1 LAXBNTIAOJWAOP-UHFFFAOYSA-N 0.000 claims description 4
- VEORPZCZECFIRK-UHFFFAOYSA-N 3,3',5,5'-tetrabromobisphenol A Chemical compound C=1C(Br)=C(O)C(Br)=CC=1C(C)(C)C1=CC(Br)=C(O)C(Br)=C1 VEORPZCZECFIRK-UHFFFAOYSA-N 0.000 claims description 4
- DVFKPXJNRSFHJY-UHFFFAOYSA-N C1(=CC=CC=C1)O.C(C1=CC=CC=C1)Cl Chemical compound C1(=CC=CC=C1)O.C(C1=CC=CC=C1)Cl DVFKPXJNRSFHJY-UHFFFAOYSA-N 0.000 claims description 4
- XEFQLINVKFYRCS-UHFFFAOYSA-N Triclosan Chemical compound OC1=CC(Cl)=CC=C1OC1=CC=C(Cl)C=C1Cl XEFQLINVKFYRCS-UHFFFAOYSA-N 0.000 claims description 4
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 238000004817 gas chromatography Methods 0.000 claims description 4
- 229960003500 triclosan Drugs 0.000 claims description 4
- BZQKBFHEWDPQHD-UHFFFAOYSA-N 1,2,3,4,5-pentabromo-6-[2-(2,3,4,5,6-pentabromophenyl)ethyl]benzene Chemical compound BrC1=C(Br)C(Br)=C(Br)C(Br)=C1CCC1=C(Br)C(Br)=C(Br)C(Br)=C1Br BZQKBFHEWDPQHD-UHFFFAOYSA-N 0.000 claims description 3
- XBNGYFFABRKICK-UHFFFAOYSA-N 2,3,4,5,6-pentafluorophenol Chemical compound OC1=C(F)C(F)=C(F)C(F)=C1F XBNGYFFABRKICK-UHFFFAOYSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 239000003708 ampul Substances 0.000 claims description 3
- CAYGQBVSOZLICD-UHFFFAOYSA-N hexabromobenzene Chemical compound BrC1=C(Br)C(Br)=C(Br)C(Br)=C1Br CAYGQBVSOZLICD-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- SVHOVVJFOWGYJO-UHFFFAOYSA-N pentabromophenol Chemical compound OC1=C(Br)C(Br)=C(Br)C(Br)=C1Br SVHOVVJFOWGYJO-UHFFFAOYSA-N 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 150000003071 polychlorinated biphenyls Chemical class 0.000 claims description 2
- 241000790917 Dioxys <bee> Species 0.000 claims 1
- 229910003978 SiClx Inorganic materials 0.000 claims 1
- 238000004128 high performance liquid chromatography Methods 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 12
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- 239000007789 gas Substances 0.000 abstract description 3
- 239000005543 nano-size silicon particle Substances 0.000 abstract description 3
- 239000012071 phase Substances 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 230000004044 response Effects 0.000 abstract description 2
- 230000001376 precipitating effect Effects 0.000 abstract 2
- 239000004115 Sodium Silicate Substances 0.000 abstract 1
- 125000004429 atom Chemical group 0.000 abstract 1
- 238000010348 incorporation Methods 0.000 abstract 1
- 125000004433 nitrogen atom Chemical group N* 0.000 abstract 1
- 239000012429 reaction media Substances 0.000 abstract 1
- 238000004088 simulation Methods 0.000 abstract 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 11
- -1 pyrene radical cation Chemical class 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 239000000356 contaminant Substances 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002210 silicon-based material Substances 0.000 description 4
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 description 2
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N carbon dioxide Natural products O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthrene Natural products C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N CHCl3 Substances ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910020489 SiO3 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- VZGDMQKNWNREIO-UHFFFAOYSA-N carbon tetrachloride Substances ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000007210 heterogeneous catalysis Methods 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-N hydroperoxyl Chemical compound O[O] OUUQCZGPVNCOIJ-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 1
- 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 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 230000005298 paramagnetic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 description 1
- 238000007539 photo-oxidation reaction Methods 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 230000000192 social effect Effects 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000009777 vacuum freeze-drying Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation method and applications of nitrogen-doped nanometer silica photocatalysts, belong to photocatalysis technology field.The preparation method is as follows: acid adding forms it into precipitating after nitrogen source is mixed with sodium silicate solution, precipitating obtains nitrogen-doped nanometer silica photocatalysts after aging, washing, drying, roasting, grinding.The catalyst has spherical morphology, and partial size accounts for about the 5-6% of total atom number in 100-200 nm, the incorporation of nitrogen-atoms.The invention also includes application of the catalyst in terms of the organic pollutant in photocatalytic degradation solid phase surface, feature includes that reaction medium can be water phase or gas phase, using simulation natural light irradiation as light source.The present invention uses precipitation method synthetic nitrogen mixed with nano-silicon dioxide photochemical catalyst, and method is simple, reproducible, yield is high, and uses simulated solar Photic driving response, has good catalytic effect to a plurality of types of organic pollutants.
Description
Technical field
A kind of photocatalysis technology field of the present invention, and in particular to preparation method of nitrogen-doped nanometer silica photocatalysts
And application.
Background technique
Photocatalysis is a kind of high-level oxidation technology that pollutant is effectively treated, and photochemical catalyst is that light-catalyzed reaction is able to efficiently
The key gone on smoothly.Metal-oxide semiconductor (MOS) photochemical catalyst such as TiO2、ZnO、Fe2O3、ZrO2、V2O5、WO3And Bi2O3Deng one
As need 400 nm of wavelength ultraviolet excitation below that could generate catalytic effect, to using being concentrated mainly on visible region
Sunlight wave, it is necessary to change the electronic structure of material to improve its visible light catalytic performance.A kind of important and effective method
It is element doping, in the lattice that dopant is mixed to original catalysis material, changes the element composition and Atomic Arrangement of material, from
And change the electronic structure of material, improve photocatalyst activity.Element doping can be divided into two kinds, first is that metal or transition metal member
The doping of element, for example, 21 kinds of transition metal element doped TiO of the system evaluations such as Choi2Colloidal sol aoxidizes CHCl3And reduction
CCl4Ability, find Fe3+、Mo5+、Ru3+、Os3+、Re5+、V4+And Rh3+Doping significantly improves TiO2Photocatalytic redox
Activity.Estrellan etc. prepares Fe-Nb/TiO2The efficiency of material, degradation PFOA increases about 6.4 times.Second is that nonmetallic
The doping of element, such as N, S, C, B, P, I, F.To analyze F, N, C, S and P etc. comprehensively non-from experiment and point of theory by Asahi etc.
Metallic element adulterates TiO2Feasibility and superiority, discovery N doping is the visible light-responded TiO of design2Catalyst it is most effective
A kind of doping method, N-TiO2There is a more obvious absorption in wavelength < 500 nm visible region, and to methyl blue and acetaldehyde
Photocatalytic degradation efficiency is higher.Existing research is mostly focused on modified TiO2Photochemical catalyst, for other after element doping
The activity change situation of type photochemical catalyst is also known little about it.
Earth silicon material is from a wealth of sources, cheap, and chemical property is stablized, and has high temperature resistant, anticorrosive, good insulating
Etc. excellent characteristics, thus be concerned in Material Field.With the development of nanotechnology, nano SiO 2 particle is opened
Hair and application are significant.Currently, silica nano material is mainly reflected in two in the application of field of environment pollution control
A aspect: first is that the absorption property excellent using silica nano material, carries out Adsorption to environmental pollutants, for example,
Polyethyleneimine-nanometer silicon dioxide composite material of synthesis is successfully used to adsorb capture CO by Li et al. people2Gas.Second is that will
Silica nano material is as the carrier of catalyst or by surface modification, degradation removal pollutant, for example, Dong et al. will
Silver nano-grain is fixed on fibrous nano silica as recyclable efficient heterogeneous catalysis, for restoring pollution
Object.The drop that composite material is used for methyl orange is made in the nano silica extracted in titanium dioxide and rice husk by Sarkar et al.
Solution.Under normal conditions, it the surface modification of silica, modification and composite Nano silicon materials is prepared as carrier each contributes to mention
High catalytic efficiency.So, whether silica itself has catalytic activity；
Silica is the main component part of atmosphere mine dust, is often used as model particulate matter to simulate organic pollutant especially
It is the atmospheric photochemistry behavior of polycyclic aromatic hydrocarbon (PAHs).For example, Mao etc. has found, the light reaction of pyrene/silica sample is related to three
A main intermediate species, there is pyrene radical cation, ultra-oxygen anion free radical (O2•–) and hydroperoxyl radical, wherein O2•–It is by O2
The electronics for capturing silica surface generates.It has been demonstrated that there are various active free radicals, such as silicon on silica surface
Base free radical, ultra-oxygen anion free radical (O2•–), oxygen radical, carbon dioxide free radical (CO2) and hydroxyl radical free radical (
OH).Accordingly, it is presumed that, the light of the organic pollutant adsorbed in silica particles can also occur for OH photooxidation reaction
In chemical conversion process.However, people are also knows about the effect played in silica surface light reaction of OH free radical at present
It obtains less.
In recent years, it has been found that commercially available silica gel (silica, the granularity that electron microscope analysis obtains is in nanoscale) is in simulating sun
Light irradiation is lower to generate hydroxyl radical free radical, can effectively oxidative degradation decabromodiphenyl oxide, and pass through paramagnetic resonance technology and degradation
The structural analysis of product demonstrates the generation of hydroxyl radical free radical, research work be published in 2017 "Water Research》
On.So, if whether be modified (element doping) to nano silica can improve the catalytic degradation efficiency to pollutant, urges
Changing mechanism is what；
The catalytic degradation of pollutant is imitated therefore, it is necessary to further investigate nano silica and its modification (element doping) material
Rate and its catalytic mechanism.
Currently, obtained production, the photochemical catalyst of application is titania nanoparticles, which is only capable of using wavelength
Ultraviolet light less than 385nm, it is lower to Solar use.In the prior art it is also reported that some utilization efficiency for improving visible light
Method, such as by adulterate nonmetallic or transition metal ions, surface fuel sensitization or modification have surface plasma body resonant vibration
The noble metal nano particles etc. of effect, catalyst system made from these methods is unstable, high production cost and is difficult to scale
Production.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method and application models of nitrogen-doped nanometer silica photocatalysts
It encloses, catalyst production cost produced by the present invention is low, high catalytic efficiency, can be catalyzed the light degradation of Some Organic Pollutants.
The present invention adopts the following technical scheme:
A kind of preparation method of nitrogen-doped nanometer silica photocatalysts, steps are as follows: by a certain amount of Na2SiO3•9H2O is molten
It is spare in deionized water；A certain amount of nitrogen source aqueous solution is added dropwise into solution, and is stirred on magnetic stirring apparatus, then
With acid solution tune pH to 7-9 or so, stop acid adding；After being sufficiently stirred, aging 2-4h, is washed with deionized at 30-80 DEG C
3-5 times, 10h or more is dried in vacuo under conditions of 30-80 DEG C, cooling to guarantee that solid is sufficiently dry, grinding；Then exist
6-10h is roasted under the conditions of 200-900 DEG C, grinding obtains nitrogen-doped nanometer silica photocatalysts.
Further, the nitrogen source is ammonium nitrate or ammonium chloride, concentration 0.5-2mol/L.
Further, the acid solution is hydrochloric acid or nitric acid, concentration 0.5-2mol/L.
Further, the calcination atmosphere is air.
Further, the Na of addition2SiO3•9H2O, nitrogen source, the molar ratio of acid solution are 1:0.5:1.5.
The present invention also provides N dopings made from the preparation method of the nitrogen-doped nanometer silica photocatalysts to receive
Application of the rice silica photocatalysts in the organic pollutant in degradation solid phase surface, steps are as follows: by target contaminant
Be dissolved in corresponding solvent, after container is added in the catalyst of the pollutant solution and corresponding amount of suitable concentration and volume together
In, make solvent volatilization completely, weighs the mixture of a certain amount of pollutant and catalyst in reaction vessel, there is water or nothing
It is reacted under the conditions of water, room temperature, uses xenon lamp as light source, the variation of monitoring pollution object concentration calculates its degradation rate.
Further, the target contaminant be decabromodiphenyl oxide, it is hexabromobenzene, Polychlorinated biphenyls, decabromodiphenylethane, more
Chloro diphenyl sulfide, polyfluoro for dibenzo to dioxin, Pentafluorophenol, pentachlorophenol, pentabromophenol, benzyl chloride phenol, triclosan or
Tetrabromobisphenol A.
Further, the concentration of the pollutant solution is 1.0 × 10-4mol/kg；The pollutant and catalyst
Molar ratio is 10-6-10-2: 1；The catalyst is the nitrogen-doped nanometer silica photocatalysts of 300-500 DEG C of roasting.
Further, the reaction vessel is quartz ampoule, and the xenon lamp is 500W xenon lamp, utilizes gas-chromatography or height
The variation of effect liquid phase chromatogram monitoring pollution object concentration.
In the method for the invention, after obtaining the suspension comprising N doping silica, conventional solid-liquid can be used
Separate mode handle suspension, resulting solid product is separated with solution, preferably, be separated by solid-liquid separation mode for from
Heart separation.After separation of solid and liquid, gained N doping silica is washed and dried as needed, is obtained more with removing impurity
High purity.Preferred drying mode is a kind of in vacuum freeze drying or vacuum drying.
Compared with the prior art, the present invention has the following beneficial effects:
First, the present invention uses precipitation method synthetic nitrogen mixed with nano-silicon dioxide photochemical catalyst, and method is simple, low in cost, both
It can be used for the operation of laboratory small range, and can be used for large-scale industrial production；
Second, the present invention uses simulated solar Photic driving response, is a kind of environmental-friendly sustainable environmental improvement method, tool
There is important social effect；
Third, nitrogen-doped nanometer silica photocatalysts produced by the present invention to decabromodiphenyl oxide, hexabromobenzene, ten chlordiphenyls,
Decabromodiphenylethane, more chloro diphenyl sulfides, octafluoro for dibenzo to dioxin, Pentafluorophenol, pentachlorophenol, pentabromophenol,
Benzyl chloride phenol, triclosan and tetrabromobisphenol A all have preferable degradation rate, wherein to decabromodiphenyl oxide, ten chlordiphenyls, tetrabromobisphenol
A, the removal rate of the 6h of more chloro diphenyl sulfides, benzyl chloride phenol and triclosan has reached 100%(Fig. 1).
Detailed description of the invention
Fig. 1 is the nitrogen-doped nanometer silica photocatalysts (2 gained of embodiment) under 300 DEG C of roastings, in gas phase condition
The schematic diagram of lower catalytic degradation plurality of target pollutant；
Fig. 2 is the transmission electron microscope picture of non-impurity-doped (a) and (b) and N doping (c), (d) nanometer silicon dioxide material (300 DEG C of roastings)
(TEM), wherein (b) and (d) is high power transmission electron microscope picture (HRTEM), wherein a, b are to roast at 300 DEG C to obtain in embodiment 1
Pure nano silica, c, d be embodiment 2 made from catalyst；
Fig. 3-a is non-impurity-doped (a) nano silica (pure nano silica obtained by 1 300 DEG C of roastings of embodiment) photochemical catalyst
X-ray photoelectron spectroscopy figure (XPS) full spectrum；
Fig. 3-b is the X-ray photoelectron of N doping (b) nano silica photochemical catalyst (2 300 DEG C of embodiment roasting gained)
The full spectrum of energy spectrum diagram (XPS)；
Fig. 3-c is the XPS spectrum figure of the N1s of 2 300 DEG C of the embodiment resulting nitrogen-doped nanometer silica photocatalysts of roasting；
Fig. 4 is that (N-300) (3 gained of embodiment) and non-impurity-doped (Si-300) nano silica material are adulterated by nitrogen source of ammonium nitrate
Material (300 DEG C of roastings) ten chlordiphenyl degradation efficiency curve comparisons of catalysis, after doping, 4h catalytic degradation efficiency is increased to 97% from 21%
(4.6 times) show that ammonium nitrate is the photocatalysis efficiency that nano silica can also greatly improved in nitrogen source doping.
Specific embodiment
Below by specific embodiment, invention is further described in detail, but those skilled in the art will manage
Solution, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.
Implementation 1: the preparation of pure nanometer silicon dioxide material
Take 1 part of Na2SiO3•9H2O is dissolved in 2 parts of deionized water, spare；To Na2SiO3It is added dropwise 2 mol/L's in solution
Hydrochloric acid, while being stirred on magnetic stirring apparatus, it adjusts pH value of solution to 9 or so, stops acid adding；Then it is stirred for 0.5h, at 50 DEG C
Aging 2h is washed with deionized 3 times, sufficiently washes away excess ions in solution；Then it is dried in vacuo under conditions of 80 DEG C
10h or more, cooling to guarantee that solid sufficiently removes water, simple grinding obtains white solid；Then it roasts, roasts in air atmosphere
Burning temperature is 200,300,500,700,900 DEG C, calcining time 6h；It is cooling, pure nanometer silicon dioxide material is obtained after grinding.
Embodiment 2: using ammonium chloride as nitrogen source
Take 1 part of Na2SiO3•9H2O is dissolved in 2 parts of deionized water, spare；To Na2SiO30.5 part is added dropwise in solution
2mol/L ammonium chloride solution, while being stirred on magnetic stirring apparatus, then instilled dropwise with the hydrochloric acid solution of 0.5 mol/L, it adjusts molten
Liquid pH to 9 or so stops acid adding；Then it is stirred for 0.5h, the aging 2h at 50 DEG C is washed with deionized 3 times, sufficiently washes
Remove excess ions in solution；Then it is dried in vacuo 12h under conditions of 80 DEG C, it is cooling to guarantee that solid sufficiently removes water, simply grind
Mill obtains white solid；Then it is roasted in air atmosphere, maturing temperature is respectively 200,300,500,700,900 DEG C, roasting
Time is 6h；It is cooling, nitrogen-doped nanometer earth silicon material is obtained after grinding.
The catalyst of the roasting of different temperatures obtained by Examples 1 and 2 ten chlordiphenyl (PCB- after 500 W xenon lamps irradiate 4 hours
209) removal rate is as shown in table 1 below:
The catalyst of the roasting of different temperatures obtained by 1 Examples 1 and 2 of table ten chlordiphenyl (PCB- after 500 W xenon lamps irradiate 4 hours
209) removal rate
Embodiment 3: using ammonium nitrate as nitrogen source
Take 1 part of Na2SiO3•9H2O is dissolved in 2 parts of deionized water, spare；To Na2SiO3The 2 of 0.5 part are added dropwise in solution
Mol/L ammonium nitrate solution, while being stirred on magnetic stirring apparatus, then instilled dropwise with the nitric acid solution of 0.5 mol/L, adjust solution
PH to 9 or so stops acid adding；Then it is stirred for 0.5h, the aging 2h at 50 DEG C is washed with deionized 3 times, sufficiently washes away
Excess ions in solution；Then 10h or more is dried in vacuo under conditions of 80 DEG C, it is cooling to guarantee that solid sufficiently removes water, simply
Grinding obtains white solid；Then it is roasted in air atmosphere, maturing temperature is 300 DEG C, calcining time 6h；It is cooling, grinding
After obtain nitrogen-doped nanometer earth silicon material.
Embodiment 4: whether there is or not nitrogen-doped nanometer earth silicon materials to be catalyzed ten chlordiphenyl degradation experiments
Ten chlordiphenyl solution, 1g embodiment 1 and the embodiment 2 of 26 μm of ol/L of 2 mL is taken to distinguish resulting two kinds of catalyst point
It is not added to the container, makes solvent volatilization completely, weigh ten chlordiphenyls of 0.05g and the mixture of different catalysts respectively in 50
In mL quartz ampoule, 40 mL deionized waters are added, use 500W xenon lamp as light irradiation, room temperature monitors ten chlorine with gas-chromatography
The variation of biphenyl concentration calculates its degradation rate, studies the catalytic efficiency (table 1) of two kinds of materials.
Embodiment 5: nitrogen-doped nanometer silica photocatalysts catalytic degradation target contaminant experiment
Target contaminant is dissolved in corresponding solvent, after by 2 institute of the pollutant solution of 26 μm of ol/L of 2 mL and 1g embodiment
Catalyst (300 DEG C roasting) be added to the container together, make solvent volatilization completely, weigh 0.05g pollutant and catalyst
Mixture reacts, room temperature in reaction vessel in the case where having water or anhydrous condition, uses 500W xenon lamp as light source, with efficient
The variation of liquid chromatogram or gas-chromatography monitoring pollution object concentration calculates its degradation rate (Fig. 1).
Embodiment described above is only to absolutely prove preferred embodiment that is of the invention and being lifted, and protection scope is unlimited
In this.Those skilled in the art's made equivalent substitute or transformation on the basis of the present invention, in protection of the invention
Within the scope of, protection scope of the present invention is subject to claims.
Claims (9)
1. a kind of preparation method of nitrogen-doped nanometer silica photocatalysts, which is characterized in that steps are as follows: will be a certain amount of
Na2SiO3•9H2O is dissolved in deionized water, spare；A certain amount of nitrogen source aqueous solution is added dropwise into solution, and is stirred in magnetic force
It mixes and is stirred on device, then with acid solution tune pH to 7-9 or so, stop acid adding；After being sufficiently stirred, the aging 2-4h at 30-80 DEG C is used
Deionized water is washed 3-5 times, and 10h or more is dried in vacuo under conditions of 30-80 DEG C, cooling, grinding；Then at 200-900 DEG C
Under the conditions of roast 6-10h, grinding obtains nitrogen-doped nanometer silica photocatalysts.
2. the preparation method of nitrogen-doped nanometer silica photocatalysts according to claim 1, which is characterized in that described
Nitrogen source is ammonium nitrate or ammonium chloride, concentration 0.5-2mol/L.
3. the preparation method of nitrogen-doped nanometer silica photocatalysts according to claim 1, which is characterized in that described
Acid solution is hydrochloric acid or nitric acid, concentration 0.5-2mol/L.
4. the preparation method of nitrogen-doped nanometer silica photocatalysts according to claim 1, which is characterized in that described
Calcination atmosphere is air.
5. the preparation method of nitrogen-doped nanometer silica photocatalysts according to claim 1, which is characterized in that be added
Na2SiO3•9H2O, nitrogen source, the molar ratio of acid solution are 1:0.5:1.5.
6. nitrogen-doped nanometer dioxy made from the preparation method of nitrogen-doped nanometer silica photocatalysts described in claim 1
Application of the SiClx photochemical catalyst in the organic pollutant in degradation solid phase surface, which is characterized in that steps are as follows: by target dirt
Dye object is dissolved in corresponding solvent, after appearance is added in the catalyst of the pollutant solution and corresponding amount of suitable concentration and volume together
In device, make solvent volatilization completely, weigh the mixture of a certain amount of pollutant and catalyst in reaction vessel, have water or
It is reacted under anhydrous condition, room temperature, uses xenon lamp as light source, the variation of monitoring pollution object concentration calculates its degradation rate.
7. nitrogen-doped nanometer made from the preparation method of nitrogen-doped nanometer silica photocatalysts according to claim 6
Application of the silica photocatalysts in the organic pollutant in degradation solid phase surface, which is characterized in that the target stains
Object is that decabromodiphenyl oxide, hexabromobenzene, Polychlorinated biphenyls, decabromodiphenylethane, more chloro diphenyl sulfides, polyfluoro are disliked for dibenzo to two
English, Pentafluorophenol, pentachlorophenol, pentabromophenol, benzyl chloride phenol, triclosan or tetrabromobisphenol A.
8. nitrogen-doped nanometer made from the preparation method of nitrogen-doped nanometer silica photocatalysts according to claim 6
Application of the silica photocatalysts in the organic pollutant in degradation solid phase surface, which is characterized in that the pollutant is molten
The concentration of liquid is 1.0 × 10-4mol/kg；The molar ratio of the pollutant and catalyst is 10-6-10-2: 1；The catalyst is
The nitrogen-doped nanometer silica photocatalysts of 300-500 DEG C of roasting.
9. nitrogen-doped nanometer made from the preparation method of nitrogen-doped nanometer silica photocatalysts according to claim 6
Application of the silica photocatalysts in the organic pollutant in degradation solid phase surface, which is characterized in that the reaction vessel
For quartz ampoule, the xenon lamp is 500W xenon lamp, utilizes the variation of gas-chromatography or high performance liquid chromatography monitoring pollution object concentration.
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