CN110193372A - A kind of photochemical catalyst, preparation method and application - Google Patents
A kind of photochemical catalyst, preparation method and application Download PDFInfo
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- CN110193372A CN110193372A CN201810159150.5A CN201810159150A CN110193372A CN 110193372 A CN110193372 A CN 110193372A CN 201810159150 A CN201810159150 A CN 201810159150A CN 110193372 A CN110193372 A CN 110193372A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 63
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000012986 modification Methods 0.000 claims abstract description 6
- 230000004048 modification Effects 0.000 claims abstract description 6
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 5
- 229910052789 astatine Inorganic materials 0.000 claims abstract description 4
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 4
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 4
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 4
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 39
- 229910052736 halogen Inorganic materials 0.000 claims description 24
- 150000002367 halogens Chemical class 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 24
- 239000002994 raw material Substances 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 18
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 17
- 239000002904 solvent Substances 0.000 claims description 16
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 15
- 229910052797 bismuth Inorganic materials 0.000 claims description 13
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 13
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims description 6
- 239000002957 persistent organic pollutant Substances 0.000 claims description 6
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 6
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims description 6
- 239000001509 sodium citrate Substances 0.000 claims description 6
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 5
- -1 alcohol compound Chemical class 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000001508 potassium citrate Substances 0.000 claims description 5
- 229960002635 potassium citrate Drugs 0.000 claims description 5
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 claims description 5
- 235000011082 potassium citrates Nutrition 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 235000009518 sodium iodide Nutrition 0.000 claims description 5
- 239000003814 drug Substances 0.000 claims description 4
- 150000004820 halides Chemical class 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 4
- 238000007626 photothermal therapy Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- TXKAQZRUJUNDHI-UHFFFAOYSA-K bismuth tribromide Chemical compound Br[Bi](Br)Br TXKAQZRUJUNDHI-UHFFFAOYSA-K 0.000 claims description 3
- 238000013170 computed tomography imaging Methods 0.000 claims description 3
- 235000011187 glycerol Nutrition 0.000 claims description 3
- 238000003384 imaging method Methods 0.000 claims description 3
- 239000001103 potassium chloride Substances 0.000 claims description 3
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 2
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 2
- 229930195725 Mannitol Natural products 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000000594 mannitol Substances 0.000 claims description 2
- 235000010355 mannitol Nutrition 0.000 claims description 2
- 230000003287 optical effect Effects 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 238000002560 therapeutic procedure Methods 0.000 claims description 2
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 2
- KOECRLKKXSXCPB-UHFFFAOYSA-K triiodobismuthane Chemical compound I[Bi](I)I KOECRLKKXSXCPB-UHFFFAOYSA-K 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 1
- 239000002202 Polyethylene glycol Substances 0.000 claims 1
- 239000011575 calcium Substances 0.000 claims 1
- 229910052791 calcium Inorganic materials 0.000 claims 1
- 238000005660 chlorination reaction Methods 0.000 claims 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 1
- 229920001223 polyethylene glycol Polymers 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 13
- 238000007146 photocatalysis Methods 0.000 abstract description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 abstract description 7
- 239000001301 oxygen Substances 0.000 abstract description 7
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 238000001228 spectrum Methods 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 94
- 239000000463 material Substances 0.000 description 17
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 14
- 238000012512 characterization method Methods 0.000 description 11
- 239000000243 solution Substances 0.000 description 10
- 210000004881 tumor cell Anatomy 0.000 description 10
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 7
- 229960000907 methylthioninium chloride Drugs 0.000 description 7
- 238000000862 absorption spectrum Methods 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000012488 sample solution Substances 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 230000002779 inactivation Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000007810 chemical reaction solvent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000009849 deactivation Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000013467 fragmentation Methods 0.000 description 2
- 238000006062 fragmentation reaction Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 230000004083 survival effect Effects 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000012930 cell culture fluid Substances 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
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- 239000010453 quartz Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001931 thermography Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K41/00—Medicinal preparations obtained by treating materials with wave energy or particle radiation ; Therapies using these preparations
- A61K41/0057—Photodynamic therapy with a photosensitizer, i.e. agent able to produce reactive oxygen species upon exposure to light or radiation, e.g. UV or visible light; photocleavage of nucleic acids with an agent
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/04—X-ray contrast preparations
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/22—Echographic preparations; Ultrasound imaging preparations ; Optoacoustic imaging preparations
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- 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
- B01J27/06—Halogens; Compounds thereof
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/04—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing carboxylic acids or their salts
-
- 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
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
-
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/345—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of ultraviolet wave energy
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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
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Optics & Photonics (AREA)
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- Catalysts (AREA)
Abstract
This application discloses a kind of photochemical catalyst, preparation method and application, the photochemical catalyst includes citric acid and BiOX, and the citric acid modification is in the BiOX surface；The chemical formula of the BiOX is BiOX；Wherein, X is selected from least one of F, Cl, Br, I, At；The color of the photochemical catalyst is black.The Lacking oxygen energy level being stabilized between conduction band and valence band in the band structure of the photochemical catalyst, make it have the wide spectrum absorption for extending to visible-range, to significantly improve its photocatalysis performance, and there is certain oxidation resistance, it can thus keep black to stablize in oxygen atmosphere environment and hot elevated temp, guarantee the long period stability of its efficient visible light catalytic performance.
Description
Technical field
This application involves a kind of black BiOX photochemical catalyst, preparation method and its in photocatalysis environmental improvement, photothermal conversion
The application of device etc. belongs to nano material, photocatalysis field.
Background technique
With the development and the improvement of people's living standards of modern industrial or agricultural, more and more trade wastes, life rubbish
The organic pollutants such as rubbish, remains of pesticide and chemical fertilizer enter by all means in water body for the survival of mankind, and photocatalysis is dropped
Solution technology is then to solve the problems, such as that organic pollutant provides a green, reliable approach, and wherein semiconductor light-catalyst is
Key link in Photocatalyst.
BiOX (X=F, Cl, Br, I, At) is a kind of novel lamellar semiconducting compound, sheet, flower ball-shaped, meso-hole structure
BiOX show good photocatalysis performance.It is micro- that the patent document of Publication No. CN102910673A discloses a kind of BiOCl
The preparation method of flower nano-photocatalyst material.The patent document of Publication No. CN103920509A discloses a kind of mesoporous BiOX light
The preparation method of catalyst.
The forbidden bandwidth of BiOX is gradually reduced with the increase of halogen atomic number, and photocatalysis performance also gradually mentions
It rises, how further to promote the photocatalysis performance of BiOX is that numerous researchers are of interest.It is prepared by ad hoc approach
The black BiOX material for increasing a Lacking oxygen defect level newly between conduction band and valence band is a kind of emerging method, and this method can
To realize that BiOX material in the absorption of visible region, greatly expands the spectral absorption range of material, to further increase it
Photocatalysis performance.Such as Liqun Ye (Liqun Ye, Xiaoli Jin, Yumin Leng, et al.Synthesis of black
ultrathin BiOCl nanosheets for efficient photocatalytic H2production under
Visible light irradiation, Journal of Power Sources, 2015,293:409-415) disclose one
The kind black BiOCl material with good visible light catalysis activity, but its oxygen atmosphere stability and thermal stability are bad.
Summary of the invention
According to the one aspect of the application, a kind of stable photochemical catalyst is provided, in the band structure of the photochemical catalyst
The Lacking oxygen energy level being stabilized between conduction band and valence band makes it have the wide spectrum absorption for extending to visible-range, thus
Its photocatalysis performance is significantly improved, and there is certain oxidation resistance, thus can be in oxygen atmosphere environment and heat heating
It keeps black to stablize in environment, guarantees the long period stability of its efficient visible light catalytic performance.
The photochemical catalyst includes citric acid and BiOX, and the citric acid modification is in the BiOX surface；
The chemical formula of the BiOX is BiOX；Wherein, X is selected from least one of F, Cl, Br, I, At；
The color of the photochemical catalyst is black.
Optionally, the size of the photochemical catalyst is 1~200nm.Preferably, the size of the photochemical catalyst be 20nm~
100nm.It is further preferred that the size of the photochemical catalyst is 20nm~80nm.
Optionally, the pattern of the photochemical catalyst is sheet.
According to further aspect of the application, the preparation method of above-mentioned photochemical catalyst is provided, which is characterized in that the side
Method at least includes the following steps:
A) raw material containing bismuth element and halogen is obtained into presoma I by hydro-thermal reaction or solvent thermal reaction；
B) presoma I is contacted with the solution containing citrate, after being surface modified, obtains the photochemical catalyst.
Optionally, in the raw material containing bismuth element and halogen described in step a), the molar ratio of bismuth element and halogen X are as follows:
Bi:X=1:0.5~5.
Optionally, the temperature of solvent thermal reaction described in step a) is 150~180 DEG C, and the reaction time is 10~15 hours；
The temperature of hydro-thermal reaction described in step a) is 150~180 DEG C, and the reaction time is 10~15 hours.
Optionally, solvent employed in solvent heat described in step a) is selected from alcohol compound, ketone compounds, ethers
At least one of compound.
Optionally, solvent employed in solvent heat described in step a) is selected from ethyl alcohol, ethylene glycol, diethylene glycol, poly- second
At least one of glycol, glycerine, ethylene glycol monomethyl ether, diethylene glycol (DEG) and mannitol.
Optionally, in the raw material containing bismuth element and halogen described in step a), bismuth element comes from bismuth nitrate, bismuth chloride, bromine
Change at least one of bismuth, bismuth iodide；
The halogen comes from least one of alkali halide, alkaline-earth halide.
Optionally, described in step a) in the raw material containing bismuth element and halogen, the halogen from sodium chloride, potassium chloride,
At least one of calcium chloride, sodium bromide, potassium bromide, sodium iodide, potassium iodide, bismuth chloride.
Optionally, the mass ratio of presoma I described in step b) and citrate in the solution containing citrate are as follows:
Presoma I: citrate=1:10~20；
The concentration of citrate is 50~200mg/mL in the solution containing citrate.
Optionally, method used by surface modification described in step b) is lighting process.
The single line light source of any wavelength or the multi-thread light source of any wave-length coverage can be used in the light source of the lighting process.
Optionally, the lighting process condition is that the mixture of presoma I and the solution containing citrate is placed in wave
It is irradiated 1~5 hour under the long light no more than 420nm.
Preferably, the lighting process condition is that the mixture of presoma I and the solution containing citrate is placed in wave
It is irradiated 2~5 hours under the light of long 100~420nm.
Optionally, citrate described in step b) in sodium citrate, potassium citrate, ammonium citrate at least one
Kind.
According to the another aspect of the application, provides any of the above-described photochemical catalyst or any of the above-described method is prepared
Photochemical catalyst is in photocatalytic degradation organic pollutants in water body, the application of the field of environmental improvement of air cleaning.
According to the another aspect of the application, provides any of the above-described photochemical catalyst or any of the above-described method is prepared
Application of the photochemical catalyst in photothermal conversion device.
According to the another aspect of the application, provides any of the above-described photochemical catalyst or any of the above-described method is prepared
Application of the photochemical catalyst in photoacoustic imaging, CT imaging, the preparation of optical dynamic therapy medicament, the preparation of photo-thermal therapy medicament.
The beneficial effect that the application can generate includes at least:
1) black BiOX photochemical catalyst provided herein, extends the spectral absorption range of photochemical catalyst, thus aobvious
The catalytic capability for improving photochemical catalyst is write, autonomous visible light catalytic is especially realized, can be effectively applied to photocatalytic degradation
Organic pollutants in water body and photocatalysis water restore hydrogen manufacturing.
2) black BiOX photochemical catalyst provided herein has certain oxidation resistance, thus can be in oxygen atmosphere
It keeps black to stablize in collarette border and hot elevated temp, guarantees the long period stability of its efficient visible light catalytic performance.
3) black BiOX photochemical catalyst provided herein has CT imaging and photoacoustic imaging performance, and has well
Photothermal conversion effect can be used for the Clinics and Practices field of photothermal conversion device field and disease.
Detailed description of the invention
Fig. 1 is sample 1#TEM map.
Fig. 2 is sample 1#UV-visible absorption spectrum.
Fig. 3 is sample 1#、D1#And D2#Visible light photocatalytic degradation methylene blue experimental result comparison diagram.
Fig. 4 is sample 1#Photo-thermal heat up experimental result picture.
Fig. 5 is sample 1#Tumour cell photo-thermal therapy experimental result picture.
Fig. 6 is sample 1#XRD characterization map.
Specific embodiment
The application is described in detail below with reference to embodiment, but the application is not limited to these embodiments.
Unless otherwise instructed, the raw material in embodiments herein is bought by commercial sources.
Analysis method is as follows in embodiments herein:
In embodiment, characterized using structure of the X-ray powder diffraction to photochemical catalyst sample, X-ray powder diffraction
Using 600 powder diffractometer of Rigaku company MiniFlex, Cu K α radiation source is used
In embodiment, the transmission electron microscope of sample is characterized using the 20 type transmission electron microscope of Tecnai F of FEI Co., the U.S..
In embodiment, the uv-visible absorption spectra of sample is using Beijing Puxi General Instrument Co., Ltd
T10CS type ultraviolet-visible spectrophotometer characterization.
In embodiment, light processing is irradiated using the 500W Hg lamp+420nm ultraviolet cut-off filter of Xujiang Electromechanical Plant, Nanjing, China.
1 black BiOCl photochemical catalyst sample 1 of embodiment#~15#Preparation
Sample 1#Preparation
By the Bi (NO of 486mg3)3·5H2O is dissolved in the diethylene glycol (DEG) (DEG) of 20mL, and the BiCl of 455mg is then added3,
Obtain mixed solution.Then, above-mentioned mixed solution is transferred to progress solvent thermal reaction 15h, reaction temperature 150 in reaction kettle
℃.After reaction, it is cooled to room temperature, collects sediment, cleaned with ethyl alcohol and deionized water.Finally, place the product in 80 DEG C
Lower drying 6 hours, obtains intermediate powder sample.It is by the concentration that the above-mentioned gained powder sample of 100 μ g is dispersed to 20mL
In the sodium citrate aqueous solution of 50mg/mL, lighting process 3h, removes supernatant in the UV lamp, and the BiOCl light for collecting black is urged
Agent sediment, is cleaned with deionized water, is subsequently dried, and product black BiOCl photochemical catalyst can be obtained, be denoted as sample 1#。
Sample 2#Preparation
Preparation step and raw material proportioning are the same as sample 1#Preparation, the difference is that, by the BiCl of halogen source3NaCl is changed to,
The temperature of solvent thermal reaction is 180 DEG C, time 10h；Gained black BiOCl photochemical catalyst is denoted as sample 2#。
Sample 3#Preparation
Preparation step and raw material proportioning are the same as sample 1#Preparation, the difference is that, by the BiCl of halogen source3KCl is changed to,
Ultraviolet lamp irradiation time is 1h, and gained black BiOCl photochemical catalyst is denoted as sample 3#。
Sample 4#Preparation
Preparation step and raw material proportioning are the same as sample 1#Preparation, the difference is that, by the BiCl of halogen source3It is changed to
BiBr3, ultraviolet lamp irradiation time is 5h, and gained black BiOBr photochemical catalyst is denoted as sample 4#。
Sample 5#Preparation
Preparation step and raw material proportioning are the same as sample 1#Preparation, the difference is that, by the BiCl of halogen source3It is changed to NaBr.
Gained black BiOBr photochemical catalyst is denoted as sample 5#。
Sample 6#Preparation
Preparation step and raw material proportioning are the same as sample 1#Preparation, the difference is that, by the BiCl of halogen source3It is changed to KBr.
Gained black BiOBr photochemical catalyst is denoted as sample 6#。
Sample 7#Preparation
Preparation step and raw material proportioning are the same as sample 1#Preparation, the difference is that, by the BiCl of halogen source3It is changed to NaI.
Gained black BiOI photochemical catalyst is denoted as sample 7#。
Sample 8#Preparation
Preparation step and raw material proportioning are the same as sample 1#Preparation, the difference is that, by the BiCl of halogen source3It is changed to KI.Institute
It obtains black BiOI photochemical catalyst and is denoted as sample 8#。
Sample 9#Preparation
Preparation step and raw material proportioning are the same as sample 1#Preparation, the difference is that, coating material sodium citrate is changed
For potassium citrate.Gained black BiOCl photochemical catalyst is denoted as sample 9#。
Sample 10#Preparation
Preparation step and raw material proportioning are the same as sample 4#Preparation, the difference is that, coating material sodium citrate is changed
For potassium citrate.Gained black BiOBr photochemical catalyst is denoted as sample 10#。
Sample 11#Preparation
Preparation step and raw material proportioning are the same as sample 7#Preparation, the difference is that, coating material sodium citrate is changed
For potassium citrate.Gained black BiOI photochemical catalyst is denoted as sample 11#。
Sample 12#Preparation
Preparation step and raw material proportioning are the same as sample 1#Preparation, the difference is that, by solvent thermal reaction solvent for use DEG
It is changed to diethylene glycol.Gained black BiOCl photochemical catalyst is denoted as sample 12#。
Sample 13#Preparation
Preparation step and raw material proportioning are the same as sample 1#Preparation, the difference is that, by solvent thermal reaction solvent for use DEG
It is changed to glycerine.Gained black BiOCl photochemical catalyst is denoted as sample 13#。
Sample 14#Preparation
Preparation step and raw material proportioning are the same as sample 1#Preparation, the difference is that, by the BiCl of halogen source3It is changed to BiCl3
And BiBr3Mixture, mixing molar ratio are BiCl3: BiBr3=1:1.Gained black BiOCl0.5Br0.5Photochemical catalyst is denoted as sample
14#。
Sample 15#Preparation
Preparation step and raw material proportioning are the same as sample 1#Preparation, the difference is that, by the BiCl of halogen source3Be changed to NaCl,
The mixture of NaBr and NaI three, the mixing molar ratio of three are NaCl:NaBr:NaI=1:1:1.Gained black BiOCl1/ 3Br1/3I1/3Photochemical catalyst is denoted as sample 15#。
1 sample D1 of comparative example#And D2#Preparation
Sample D1#Preparation
According to document Nanoscale, record in 2016,8,12715-12722 is prepared the BiOCl of white, is denoted as
Sample D1#。
Sample D2#Preparation
According to 34 (2014) 107e112 of document Y.Li et al./Solid State Sciences) in method, system
It is standby to obtain black BiOCl, it is denoted as sample D2#。
2 sample 1 of embodiment#~15#TEM characterization and XRD characterization
Respectively to sample 1#~15#Carry out TEM characterization and XRD characterization.The results show that sample 1#~15#Particle size range point
For cloth in 1~200nm, the particle size range of most of sample is distributed in 20nm~100nm, and concentrates on 20nm~80nm；Sample
Rule or irregular sheet pattern is presented.
With sample 1#For Typical Representative, TEM photo is as shown in Figure 1, XRD spectrum is as shown in Figure 6.As seen from Figure 1,
For the black BiOCl photochemical catalyst for using herein described method to be prepared for sheet layer material, size is distributed in 1-200nm, collection
In in 20nm~80nm, particle diameter distribution is uniform.The sample size and TEM characterization result converted by XRD characterization result in Fig. 6
Unanimously.
Sample 2#~15#TEM characterization result and XRD spectrum and sample 1#Characterization result it is similar, be sheet layer material,
Size is in 1-200nm.
3 sample 1 of embodiment#~15#Uv-visible absorption spectra analysis
Sample 1 is investigated respectively#~15#Uv-visible absorption spectra analyzed.The results show that sample 1#~15#?
In the wave-length coverage of 200~900nm, absorbance is between 0.36~0.46.Typical Representative such as sample 1#, ultraviolet-visible
Absorption spectrum is as shown in Figure 2.
The reactivity worth of the visible light photocatalytic degradation methylene blue of 4 sample of embodiment is tested
Respectively to sample 1#~15#、D1#And D2#As catalyst, the catalytic performance for degradation of methylene blue is carried out
Characterization.
Specific experiment step and condition are as follows:
The aqueous solution of methylene blue that the concentration of 100mL is 10mg/mL is put into quartz beaker, 20mg photocatalysis is added
Agent, ultrasonic 10min, magnetic agitation 30min reaches absorption-desorption balance under dark condition, and light is carried out in photochemical reactor
According to.Magnetic agitation is carried out in whole process.By certain time interval, 4mL sample solution is extracted, 10000rpm, 15min are centrifuged,
Remove particle, the maximum absorption band of test record supernatant and the uv-visible absorption spectra of dye solution.
The results show that sample 1#~15#Preferably degradation of methylene blue, photocatalysis performance it can be substantially better than D1#And D2#。
With sample 1#For Typical Representative, degradation process Methylene Blue concentration changes with time as shown in Figure 3.As seen from the figure,
Using photochemical catalyst sample 1 described herein#, the degradation rate and palliating degradation degree of methylene blue be substantially better than D1#And D2#。
The light thermal property of 5 sample of embodiment is tested
Respectively to sample 1#~15#Light thermal property tested.
Specific experiment step and condition are as follows:
It takes 50mg sample to be dissolved in ultrapure water, is diluted to various concentration, such as 100,200,300,400,500 micrograms/milli
It rises, 1mL sample solution is taken to be placed in cuvette, with 808nm near infrared light laser light source irradiating sample solution, used in irradiation process
Thermal imaging system records the temperature change of sample solution in real time.By recording certain time some strength (such as 5min, 2W/cm2) swash
The temperature variations of sample solution determine the photothermal conversion performance of material after radiant irradiation.
The results show that sample 1#~15#There is good photothermal conversion efficiency under 808nm near infrared light, and rising
It will not albefaction during temperature.With sample 1#For Typical Representative, test results are shown in figure 4 for light thermal property.It can be seen by Fig. 4
Out, when sample concentration is 300 mcg/mls or more, sample temperature can increase 20 degrees Celsius, i.e. room after 10min illumination
Sample actual temperature can reach 45 degrees Celsius or more in warm environment, have good photothermal conversion performance, and photothermal conversion performance
It is not influenced by ambient temperature.
Inactivation performance test of 6 sample of embodiment for tumour cell
Respectively by sample 1#~15#Test can be carried out to the deactivation of tumour cell.
Specific experiment step and condition are as follows:
Typically, it is inoculated with MCF-7 tumour cell in 96 orifice plates, is cultivated 24 hours in cell incubator, pastes cell
Wall.Next day, the cell culture fluid in 96 orifice plates was sucked out, and was substituted for the culture solution containing various concentration specimen material, co-cultured 4
After hour, upper solution is replaced with pure culture solution again.Then tissue culture plate is placed under near-infrared laser and is irradiated, if
Set the control group of different materials concentration, different illumination intensity and different light application times.After irradiation) cell plates are put back to carefully
Continue culture 20 hours in born of the same parents' incubator, MTT is then added dropwise into culture plate, measure absorbance with microplate reader, is calculated thin
Born of the same parents' survival rate.To obtain material to the inactivation performance of tumour cell.
The results show that sample 1#~15#Under 808nm near infrared light, there is excellent deactivation to tumour cell
Energy.With sample 1#For Typical Representative, to the inactivation performance of tumour cell, test results are shown in figure 5.As seen from Figure 5,
Under our experiment condition, simple near infrared light does not have apparent fragmentation effect to tumour cell.And for containing sample
The experimental group of material, under near infrared light, specimen material has significant fragmentation effect for tumour cell, and kills effect
Fruit enhances with the increase of sample concentration, and in the case where sample concentration is 400 mcg/ml, after 5min illumination, tumour is thin
Born of the same parents' inactivation ratio reaches 90% or more.As it can be seen that there is our material good near-infrared to induce photo-thermal therapy tumour cell performance.
The above is only several embodiments of the application, not does any type of limitation to the application, although this Shen
Please disclosed as above with preferred embodiment, however not to limit the application, any person skilled in the art is not taking off
In the range of technical scheme, a little variation or modification are made using the technology contents of the disclosure above and is equal to
Case study on implementation is imitated, is belonged in technical proposal scope.
Claims (10)
1. a kind of photochemical catalyst, which is characterized in that the photochemical catalyst includes citric acid and BiOX, the citric acid modification
In the BiOX surface；
The chemical formula of the BiOX is BiOX；Wherein, X is selected from least one of F, Cl, Br, I, At；
The color of the photochemical catalyst is black.
2. photochemical catalyst according to claim 1, which is characterized in that the size of the photochemical catalyst is 1~200nm；
Preferably, the size of the photochemical catalyst is 20nm~100nm；
It is further preferred that the size of the photochemical catalyst is 20nm~80nm；
Preferably, the pattern of the photochemical catalyst is sheet.
3. the preparation method of any one of claim 1 to 2 photochemical catalyst, which is characterized in that the method include at least with
Lower step:
A) raw material containing bismuth element and halogen is obtained into presoma I by hydro-thermal reaction or solvent thermal reaction；
B) presoma I is contacted with the solution containing citrate, after being surface modified, obtains the photochemical catalyst；
Preferably, in the raw material containing bismuth element and halogen described in step a), the molar ratio of bismuth element and halogen X are as follows:
Bi:X=1:0.5~5；
Preferably, the temperature of solvent thermal reaction described in step a) is 150~180 DEG C, and the reaction time is 10~15 hours；Step
A) temperature of hydro-thermal reaction described in is 150~180 DEG C, and the reaction time is 10~15 hours.
4. the preparation method of photochemical catalyst according to claim 3, which is characterized in that adopted in solvent heat described in step a)
Solvent is selected from least one of alcohol compound, ketone compounds, ether compound；
Preferably, solvent employed in solvent heat described in step a) be selected from ethyl alcohol, ethylene glycol, diethylene glycol, polyethylene glycol,
At least one of glycerine, ethylene glycol monomethyl ether, diethylene glycol (DEG) and mannitol.
5. the preparation method of photochemical catalyst according to claim 3, which is characterized in that step a) is described to contain bismuth element and halogen
In the raw material of element, bismuth element comes from least one of bismuth nitrate, bismuth chloride, bismuth bromide, bismuth iodide；
The halogen comes from least one of alkali halide, alkaline-earth halide；
Preferably, in the raw material containing bismuth element and halogen described in step a), the halogen comes from sodium chloride, potassium chloride, chlorination
At least one of calcium, sodium bromide, potassium bromide, sodium iodide, potassium iodide, bismuth chloride.
6. the preparation method of photochemical catalyst according to claim 3, which is characterized in that presoma I described in step b) with contain
There is the mass ratio of citrate in the solution of citrate are as follows:
Presoma I: citrate=1:10~20；
The concentration of citrate is 50~200mg/mL in the solution containing citrate.
7. the preparation method of photochemical catalyst according to claim 3, which is characterized in that surface modification described in step b) is adopted
Method is lighting process；
Preferably, the lighting process condition is that the mixture of presoma I and the solution containing citrate is placed in wavelength not
It is irradiated 1~5 hour under light more than 420nm；
Preferably, citrate described in step b) is selected from least one of sodium citrate, potassium citrate, ammonium citrate.
8. the described in any item photochemical catalysts of claim 1 to 2 are prepared into according to the described in any item methods of claim 3 to 7
To at least one of photochemical catalyst in photocatalytic degradation organic pollutants in water body, photocatalytic degradation air organic pollutant
In application.
9. the described in any item photochemical catalysts of claim 1 to 2 are prepared into according to the described in any item methods of claim 3 to 7
To the application in photothermal conversion device of at least one of photochemical catalyst.
10. the described in any item photochemical catalysts of claim 1 to 2 are prepared according to the described in any item methods of claim 3 to 7
At least one of obtained photochemical catalyst is in photoacoustic imaging, CT imaging, the preparation of optical dynamic therapy medicament, photo-thermal therapy medicament
Preparation in application.
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