CN106944153A - A kind of sandwich construction nano-complex and its application - Google Patents
A kind of sandwich construction nano-complex and its application Download PDFInfo
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- CN106944153A CN106944153A CN201710148966.3A CN201710148966A CN106944153A CN 106944153 A CN106944153 A CN 106944153A CN 201710148966 A CN201710148966 A CN 201710148966A CN 106944153 A CN106944153 A CN 106944153A
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- 238000010276 construction Methods 0.000 title claims abstract description 25
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 47
- OVBPIULPVIDEAO-LBPRGKRZSA-N folic acid Chemical compound C=1N=C2NC(N)=NC(=O)C2=NC=1CNC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 OVBPIULPVIDEAO-LBPRGKRZSA-N 0.000 claims abstract description 40
- 230000001699 photocatalysis Effects 0.000 claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 235000019152 folic acid Nutrition 0.000 claims abstract description 21
- 239000011724 folic acid Substances 0.000 claims abstract description 21
- 238000007146 photocatalysis Methods 0.000 claims abstract description 20
- OVBPIULPVIDEAO-UHFFFAOYSA-N N-Pteroyl-L-glutaminsaeure Natural products C=1N=C2NC(N)=NC(=O)C2=NC=1CNC1=CC=C(C(=O)NC(CCC(O)=O)C(O)=O)C=C1 OVBPIULPVIDEAO-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229960000304 folic acid Drugs 0.000 claims abstract description 19
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 17
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 17
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 17
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 17
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 17
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 3
- 229910052684 Cerium Inorganic materials 0.000 claims abstract 2
- 229910052725 zinc Inorganic materials 0.000 claims abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 235000019441 ethanol Nutrition 0.000 claims description 17
- 239000012153 distilled water Substances 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- -1 alcohol ester Chemical class 0.000 claims description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910020442 SiO2—TiO2 Inorganic materials 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- 238000009938 salting Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- 239000004246 zinc acetate Substances 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- ODPUKHWKHYKMRK-UHFFFAOYSA-N cerium;nitric acid Chemical compound [Ce].O[N+]([O-])=O ODPUKHWKHYKMRK-UHFFFAOYSA-N 0.000 claims 1
- 238000004513 sizing Methods 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 239000010410 layer Substances 0.000 abstract description 14
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000002346 layers by function Substances 0.000 abstract 2
- 239000000047 product Substances 0.000 description 23
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- 238000004458 analytical method Methods 0.000 description 12
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- 235000011167 hydrochloric acid Nutrition 0.000 description 8
- 210000004881 tumor cell Anatomy 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 7
- 230000004083 survival effect Effects 0.000 description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 125000005909 ethyl alcohol group Chemical group 0.000 description 6
- 206010028980 Neoplasm Diseases 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000002428 photodynamic therapy Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 201000011510 cancer Diseases 0.000 description 4
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- 239000002351 wastewater Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 3
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000000502 dialysis Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 3
- 230000002147 killing effect Effects 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 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 3
- 229940012189 methyl orange Drugs 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 3
- 235000015497 potassium bicarbonate Nutrition 0.000 description 3
- 239000011736 potassium bicarbonate Substances 0.000 description 3
- IWZKICVEHNUQTL-UHFFFAOYSA-M potassium hydrogen phthalate Chemical compound [K+].OC(=O)C1=CC=CC=C1C([O-])=O IWZKICVEHNUQTL-UHFFFAOYSA-M 0.000 description 3
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XPFJYKARVSSRHE-UHFFFAOYSA-K trisodium;2-hydroxypropane-1,2,3-tricarboxylate;2-hydroxypropane-1,2,3-tricarboxylic acid Chemical compound [Na+].[Na+].[Na+].OC(=O)CC(O)(C(O)=O)CC(O)=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O XPFJYKARVSSRHE-UHFFFAOYSA-K 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000006285 cell suspension Substances 0.000 description 2
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 229940064302 folacin Drugs 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
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- 239000012808 vapor phase Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 238000002965 ELISA Methods 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 229910001308 Zinc ferrite Inorganic materials 0.000 description 1
- 230000001464 adherent effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005880 cancer cell killing Effects 0.000 description 1
- 208000035269 cancer or benign tumor Diseases 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002512 chemotherapy Methods 0.000 description 1
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- 239000011248 coating agent Substances 0.000 description 1
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- 239000000356 contaminant Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
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- 230000008878 coupling Effects 0.000 description 1
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- HJUFTIJOISQSKQ-UHFFFAOYSA-N fenoxycarb Chemical compound C1=CC(OCCNC(=O)OCC)=CC=C1OC1=CC=CC=C1 HJUFTIJOISQSKQ-UHFFFAOYSA-N 0.000 description 1
- 102000006815 folate receptor Human genes 0.000 description 1
- 108020005243 folate receptor Proteins 0.000 description 1
- NNGHIEIYUJKFQS-UHFFFAOYSA-L hydroxy(oxo)iron;zinc Chemical compound [Zn].O[Fe]=O.O[Fe]=O NNGHIEIYUJKFQS-UHFFFAOYSA-L 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000000415 inactivating effect Effects 0.000 description 1
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- 229910052742 iron Inorganic materials 0.000 description 1
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- 239000006249 magnetic particle Substances 0.000 description 1
- 230000029052 metamorphosis Effects 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 231100000252 nontoxic Toxicity 0.000 description 1
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- 235000015097 nutrients Nutrition 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
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- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000886 photobiology Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000003504 photosensitizing agent Substances 0.000 description 1
- 229910021650 platinized titanium dioxide Inorganic materials 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
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- 238000006862 quantum yield reaction Methods 0.000 description 1
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- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
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- 239000000725 suspension Substances 0.000 description 1
- 238000002626 targeted therapy Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 230000010415 tropism Effects 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
Classifications
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- 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
-
- 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
-
- 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
- B01J35/396—Distribution of the active metal ingredient
- B01J35/397—Egg shell like
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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
- 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
- B01J35/396—Distribution of the active metal ingredient
- B01J35/398—Egg yolk like
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Epidemiology (AREA)
- Veterinary Medicine (AREA)
- Molecular Biology (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Inorganic Chemistry (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Biochemistry (AREA)
- Toxicology (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Cosmetics (AREA)
- Catalysts (AREA)
- Medicines That Contain Protein Lipid Enzymes And Other Medicines (AREA)
Abstract
The present invention provides a kind of sandwich construction nano-complex and its application.The sandwich construction nano-complex includes the sandwich construction that inner nuclear layer, separation layer, functional layer and double modified layers from inside to outside are constituted, and the sandwich construction nano-complex formula is FeaOb–SiO2–TiO2–<X+FA>, wherein inner nuclear layer FeaObFor magnetic Fe3O4Or magnetic Fe2O3Or both formed mixture, separation layer is SiO2, functional layer is TiO2, double modified layers<X+FA>Middle X takes a kind of its element for Zn, La, Ce, and FA is folic acid.The nano-complex of the special construction has magnetic, visible light-responded property, biologic specificity and enhanced photocatalytic activity.The nano-complex can be applied to photocatalysis field.Step is simple and convenient to operate, practical.
Description
Technical field
The invention belongs to magnetic material, nano material and photocatalysis technology field, more particularly to a kind of sandwich construction nanometer
Compound and its application.
Background technology
Since the nanometers such as Pd, Cu, Fe are successfully made with inert gases agglomeration method first in 1980s Gleiter et al.
Since particulate, nano material is increasingly becoming the emphasis of countries in the world research and development as a kind of new material.Because nano material is obvious not
Body material and individual molecule are same as, thus with unique skin effect, small-size effect, quantum size effect and tunnel effect
Should, show many distinctive physics and chemical property, electronics, optics, life science, information Store, papermaking, ceramics,
The fields such as cosmetics, catalysis, medicine, environmental protection show wide application prospect.
Wherein, the semi-conducting material TiO of nanostructured2It is considered as most having one of catalysis material of application prospect at present.
TiO2There is the low advantage of nontoxic, stable chemical nature, cost as photochemical catalyst, can be produced under light action has Strong oxdiative
The hole of ability and hydroxyl radical free radical, can finally make organic substance complete oxidation generate the nothings such as carbon dioxide, water and sulfate radical
Machine ion, can carry out advanced treating to the organic pollution in waste water, environment is repaired, photochemical catalytic oxidation is also acted as and kills
Bacterium.Medically, with the development of optical fiber technology, endoscopic technic and laser medicine, TiO2In theory may be used as medical photosensitive agent
All kinds of tumour cells are killed in photochemical catalytic oxidation under light action, so that optical dynamic therapy (photodynamic therapy, PDT)
Malignant tumour；Compared with the traditional remedies such as operation, chemotherapy, radiotherapy, its great advantage be by tumour cell be enriched with and to
Tumor tissues orientation imports light source realization to the selective killing of cancer cell, without performing surgical operation, and avoids biography
To the shortcoming of a large amount of infringements of normal cell in therapy of uniting.
TiO2In liquid phase photocatalysis, although with making us satisfied catalytic activity, but because its broad-band gap causes
It could only trigger light-catalyzed reaction under ultraviolet light, it is impossible to sufficiently respond to visible ray, and this just greatly limit making for it
With efficiency, and ultraviolet light has very big injury to human body.In addition, TiO2Light produces electronics after exciting and hole life is very short,
(quantum yield is low) easily is combined, there is the low problem of catalytic efficiency.
To solve the above problems, various countries researcher is from different perspectives to TiO2Following modified measures are carried out.In order to drop
Low TiO2The band gap of photochemical catalyst, raising electronics separate with hole, its response wave length scope is extended to visible region, improve it
Photocatalytic activity and efficiency, the means taken have semiconductors coupling, ion doping, super-strong acidified, noble metal loading, photosensitizer
Deng.For example：Ha Sung Park etc. are prepared for 2.5wt%Cu/TiO2Visible-light response type catalyst, makes absorbing boundary from ultraviolet
Area extends to 480-490nm, and photocatalysis efficiency (Ha Sung Park, Dong Hyun Kim, Sun are improved to a certain extent
Jae Kim,Kyung Sub Lee,Journal of Alloys and Compounds,2006,415:51–55).In order to just
In separation TiO2, patent 201410187192.1 discloses a kind of magnetic nanometer photocatalyst ZnFe2O4/TiO2, the photochemical catalyst
For handling waste water from dyestuff and oily waste water and energy Magnetic Isolation.For PDT, Liu etc. is prepared for Pt/TiO2Nano combined material
Material, and for PDT suppress tumour cell increment (Lei Liu, Peng Miao, Yuanyuan Xu, Zhipeng Tian,
Zhigang Zou,Genxi Li,Journal of Photochemistry and Photobiology B:Biology,
2010,98:207–210)。
Although these measures are to TiO2The problem present in liquid phase photocatalysis proposes some improvement projects, to a certain degree
On improve TiO2Efficiency, but still TiO can not be overcome completely2Whole defects, it is impossible to really meet practical application request.
Particularly in accurate medical science oncotherapy, also require that it has targeting to tumour cell.Folic acid (folic acid, FA) is
A kind of soluble small molecular vitamin, it can specifically bind with folacin receptor (folate receptor, FR).Leaf
Acid acceptor altimeter in tumour cell reaches, and is hardly expressed in normal cell, based on folacin receptor in tumour cell and just
Differential expression in normal cell, can be achieved the active targeting conveying of folic acid nano-complex, has in neoplasm targeted therapy only
Special advantage, if revesting magnetic, can produce actively and passively targeted double function.
By the literature search discovery to prior art, " vapor phase hydrolysis method prepares magnetic photocatalyst Fe to document3O4/
SiO2/TiO2And its photocatalysis performance " report using vapor phase hydrolysis method, with Fe3O4Nano magnetic particle is magnetic core, at it
One layer of SiO of Surface coating2To prevent photoetch, nano-titanium oxide is then deposited on Fe3O4/SiO2Particle surface, so as to prepare
The Fe of core shell structure3O4/SiO2/TiO2Composite, for photocatalysis degradation organic contaminant；Though its composite reported
Magnetic is introduced, but it is different from the preparation method and process route of the present invention, and be not further introduced into other ornamental equivalents to increase
Strong visible light-responded property and biologic specificity (Guo Dongxue, ancestor Helen, Wu Yihong, Zhang Qinghong, Chinese science and technology paper, 2014,9,6:
637-641)。
Document " photocatalysis folic acid nano-TiO2Compound target killing cancer cell effect and and interaction of biomacromolecules
Research " proposes folic acid nano-TiO2Compound targeting photocatalysis killing cancer cell, although the compound of its report has folic acid
Targeting, but be not further introduced into other ornamental equivalents to realize visible light-responded property and magnetic target tropism (Gao Xiaoya, Shanxi medical courses in general
University, Master's thesis, 2012).
The content of the invention
In order to overcome above-mentioned deficiency, the present invention provides a kind of sandwich construction nano-TiO gathered multi -function in integral whole2Compound
And its application.The sandwich construction nano-TiO2Compound energy responding to visible light, suppresses electronics and hole-recombination, enhancing photocatalysis are lived
Property and with biologic specificity.The sandwich construction nano-TiO2Compound can be applied to photocatalysis, particularly liquid phase photocatalysis
Field.
To achieve these goals, the present invention is adopted the following technical scheme that：
A kind of sandwich construction nano-complex, the sandwich construction nano-complex formula is FeaOb–SiO2–TiO2–<X+
FA>, with FeaObFor kernel, SiO is coated with successively in its outer layer2Layer, TiO2Layer and<X+FA>Double modified layers, wherein, X be Zn,
La or Ce, FA are folic acid, and a, b are the natural number more than zero.
It is preferred that, the FeaObFor magnetic Fe3O4Or magnetic Fe2O3Or both formed mixture.
It is preferred that, the FeaObContent be 0.0001-95wt%, SiO2Content be 0.0001-95wt%, TiO2's
Content is 1-95wt%, and X content is 0.01-0.5wt%, and surplus is FA.
It is preferred that, the Fe2O3Crystal formation be γ types, SiO2Structure be unformed, TiO2Crystal formation be Anatase.
It is preferred that, FeaObMean particle dia is 0.0001-30nm, SiO2Thickness is 0.0001-50nm, TiO2Thickness is
0.0001-50nm, nano-complex overall dimensions are no more than 150nm.
Present invention also offers a kind of preparation method of sandwich construction nano-complex, including：
By FeaObIt is well mixed with distilled water, absolute ethyl alcohol, concentrated ammonia liquor, then tetraethyl orthosilicate is added dropwise and reacted, is reacted
Finish, magnetic settlement, wash, heat treatment obtains FeaOb–SiO2；
By above-mentioned FeaOb–SiO2It is well mixed with absolute ethyl alcohol, metatitanic acid alcohol ester, ultrasonic disperse, adds absolute ethyl alcohol, steaming
Distilled water and concentrated hydrochloric acid mixed liquor, water-bath are aged, and are heat-treated, and roasting produces FeaOb–SiO2–TiO2；
By above-mentioned FeaOb–SiO2–TiO2Add in salting liquid, be well mixed, dry, roasting obtains FeaOb–SiO2–TiO2–
X；
By above-mentioned FeaOb–SiO2–TiO2- X water dispersion solution is mixed with the folic acid solution of saliferous, is dialysed, and is dried, i.e.,
.
It is preferred that, the salt in the salting liquid is zinc acetate, lanthanum nitrate or cerous nitrate.
It is preferred that, the salt in the folic acid solution of the saliferous is sodium acid carbonate, sodium carbonate, saleratus or potassium carbonate.
Present invention also offers sandwich construction nano-complex prepared by any above-mentioned method.
Present invention also offers application of the above-mentioned sandwich construction nano-complex of any one in photocatalysis field.
Beneficial effects of the present invention
(1) the sandwich construction nano-complex gathers multi -function in integral whole, and overcomes TiO2Asked present in photocatalysis
Topic.TiO can be reduced2Band gap, widen TiO2Absorbing boundary, responding to visible light, suppression electronics and hole-recombination are so as to strengthen photocatalysis
Activity, can respond externally-applied magnetic field, with magnetic, can by externally-applied magnetic field realize transmit or separate, additionally with biospecific
Property.It can be applied to photocatalysis field, such as PDT, sterilizing, degradation of organic substances.
(2) preparation method of the present invention is simple, efficiency high, practical, it is easy to promote.
Embodiment
It is noted that described further below is all exemplary, it is intended to provide further instruction to the application.Unless another
Indicate, all technologies used herein and scientific terminology are with usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
Embodiment 1：Prepare sandwich construction nano-complex
Step (1)：Prepare 0.24molL-1Iron chloride and 0.12molL-1Frerrous chloride mixed solution, adds several drops
Watery hydrochloric acid, is passed through under nitrogen bubble 40min, stirring condition and adds ammoniacal liquor (6-7wt%) to pH=9, reacts 4h, Magneto separate, according to
It is secondary to be washed with distilled water, ethanol 3 times, 30 DEG C of heat treatment 4h.It is added into citric acid-sodium citrate solution that (citrate is dense
Spend for 0.2molL-1), ultrasonic disperse is uniform, centrifuges and is washed with ethanol 3 times, is dried in vacuo.Products therefrom is counted as S1。
Step (2)：Product made from 40mg steps (1) is weighed, is continued under stirring condition, by volume 10:30:1 successively
Distilled water, absolute ethyl alcohol, concentrated ammonia liquor (25-28wt%) are added, then 0.3mL tetraethyl orthosilicates are added dropwise and 4h is reacted, magnetic settlement,
Washed successively with distilled water, ethanol, 30 DEG C of heat treatment 4h.Products therefrom is counted as S2。
Step (3)：Product made from weighing 1g steps (2), sequentially adds 20mL absolute ethyl alcohols, 4mL butyl titanates, ultrasound
Scattered 5min, the electric stirring 20min in 50 DEG C of water-baths, add 20mL absolute ethyl alcohols, 1mL distilled water and 0.15mL concentrated hydrochloric acids mixed
Liquid is closed, reaction is finished, be aged, 80 DEG C of heat treatments, 400-550 DEG C of roasting 4h.Products therefrom is counted as S3。
Step (4)：Product made from 1g steps (3) is weighed, while by quantitative lanthanum nitrate (based on La contents 0.05wt%
Calculate) wiring solution-forming, both mix 1h, 100 DEG C of dryings, 400-500 DEG C of roasting 4h in equal volume.Products therefrom is counted as S4。
Step (5)：Product made from 1g steps (4) is weighed, adds in 150mL deionized waters, stirs, is added carbon containing
The folic acid solution of potassium hydrogen phthalate, utilizes potassium bicarbonate solution (4 × 10 after 1d-4mol·L-1) dialysis 1d, dry, produce most
End-product.Products therefrom is counted as S5。S50.1wt% containing folic acid.
With reference to product S1、S2、S3、S4, to product S5Series of tables has been carried out to seek peace analysis：Through polycrystal powder X-ray diffraction and
Transmission electron microscope learns that its inner nuclear layer is Fe3O4、SiO2For undefined structure, TiO2For Detitanium-ore-type, Magnetic Test analysis
Learn S5With magnetic, UV-vis DRS absorption spectroanalysis learns S5Can responding to visible light, FTIR spectrum analysis
Learn S5In containing combine FA.
Embodiment 2：Prepare sandwich construction nano-complex
Step (1)：Prepare 0.24molL-1Iron chloride and 0.12molL-1Frerrous chloride mixed solution, adds several drops
Watery hydrochloric acid, is passed through under nitrogen bubble 40min, stirring condition and adds ammoniacal liquor (6-7wt%) to pH=9, reacts 4h, Magneto separate, according to
It is secondary to be washed with distilled water, ethanol 3 times, 30 DEG C of heat treatment 4h.It is added into citric acid-sodium citrate solution that (citrate is dense
Spend for 0.2molL-1), ultrasonic disperse is uniform, centrifuges and is washed with ethanol 3 times, is dried in vacuo.
Step (2)：Product made from 40mg steps (1) is weighed, is continued under stirring condition, by volume 10:30:1 successively
Distilled water, absolute ethyl alcohol, concentrated ammonia liquor (25-28wt%) are added, then 0.3mL tetraethyl orthosilicates are added dropwise and 4h is reacted, magnetic settlement,
Washed successively with distilled water, ethanol, 30 DEG C of heat treatment 4h.
Step (3)：Product made from weighing 1g steps (2), sequentially adds 20mL absolute ethyl alcohols, 4mL butyl titanates, ultrasound
Scattered 5min, the electric stirring 20min in 50 DEG C of water-baths, add 20mL absolute ethyl alcohols, 1mL distilled water and 0.15mL concentrated hydrochloric acids mixed
Liquid is closed, reaction is finished, be aged, 80 DEG C of heat treatments, 400-550 DEG C of roasting 4h.
Step (4)：Product made from 1g steps (3) is weighed, while by quantitative cerous nitrate (based on Ce contents 0.1wt%
Calculate) wiring solution-forming, both mix 1h, 100 DEG C of dryings, 400-500 DEG C of roasting 4h in equal volume.
Step (5)：Product made from 1g steps (4) is weighed, adds in 150mL deionized waters, stirs, is added carbon containing
The folic acid solution of potassium hydrogen phthalate, utilizes potassium bicarbonate solution (4 × 10 after 1d-4mol·L-1) dialysis 1d, dry, produce most
End-product.Products therefrom is counted as S6。S60.1wt% containing folic acid.
To product S6Series of tables has been carried out to seek peace analysis：Learned through polycrystal powder X-ray diffraction and transmission electron microscope
Its inner nuclear layer is Fe3O4、SiO2For undefined structure, TiO2For Detitanium-ore-type, S is learned in Magnetic Test analysis6It is ultraviolet with magnetic
It can be seen that diffusing reflection absorption spectroanalysis learns S6S is learned in energy responding to visible light, FTIR spectrum analysis6In containing combine
FA。
Embodiment 3：Prepare sandwich construction nano-complex
Step (1)：Prepare 0.24molL-1Iron chloride and 0.12molL-1Frerrous chloride mixed solution, adds several drops
Watery hydrochloric acid, is passed through under nitrogen bubble 40min, stirring condition and adds ammoniacal liquor (6-7wt%) to pH=9, reacts 4h, Magneto separate, according to
It is secondary to be washed with distilled water, ethanol 3 times, 30 DEG C of heat treatment 4h.It is added into citric acid-sodium citrate solution that (citrate is dense
Spend for 0.2molL-1), ultrasonic disperse is uniform, centrifuges and is washed with ethanol 3 times, is dried in vacuo.
Step (2)：Product made from 40mg steps (1) is weighed, is continued under stirring condition, by volume 10:30:1 successively
Distilled water, absolute ethyl alcohol, concentrated ammonia liquor (25-28wt%) are added, then 0.3mL tetraethyl orthosilicates are added dropwise and 4h is reacted, magnetic settlement,
Washed successively with distilled water, ethanol, 30 DEG C of heat treatment 4h.
Step (3)：Product made from weighing 1g steps (2), sequentially adds 20mL absolute ethyl alcohols, 4mL butyl titanates, ultrasound
Scattered 5min, the electric stirring 20min in 50 DEG C of water-baths, add 20mL absolute ethyl alcohols, 1mL distilled water and 0.15mL concentrated hydrochloric acids mixed
Liquid is closed, reaction is finished, be aged, 80 DEG C of heat treatments, 400-550 DEG C of roasting 4h.
Step (4)：Product made from 1g steps (3) is weighed, while by quantitative zinc acetate (based on Zn contents 0.5wt%
Calculate) wiring solution-forming, both mix 1h, 100 DEG C of dryings, 400-500 DEG C of roasting 4h in equal volume.
Step (5)：Product made from 1g steps (4) is weighed, adds in 150mL deionized waters, stirs, is added carbon containing
The folic acid solution of potassium hydrogen phthalate, utilizes potassium bicarbonate solution (4 × 10 after 1d-4mol·L-1) dialysis 1d, dry, produce most
End-product.Products therefrom is counted as S7。S70.1wt% containing folic acid.
To product S7Series of tables has been carried out to seek peace analysis：Learned through polycrystal powder X-ray diffraction and transmission electron microscope
Its inner nuclear layer is Fe3O4、SiO2For undefined structure, TiO2For Detitanium-ore-type, S is learned in Magnetic Test analysis7It is ultraviolet with magnetic
It can be seen that diffusing reflection absorption spectroanalysis learns S7S is learned in energy responding to visible light, FTIR spectrum analysis7In containing combine
FA。
Embodiment 4：
By product S obtained above5Tumour cell, specific implementation are killed applied to photocatalysis：Experiment is in desinfection chamber and nothing
Carried out in bacterium cleaning operating desk.This experiment is collected using SGC-7901gastriccarcinomacellline as subject cell after Secondary Culture
The cancer cell of logarithmic phase, it is 1 × 10 that concentration, which is made,6Cells/mL single cell suspension.Control group and experimental group are divided into, i.e.,
Blank control group, light control group, S5Control group, TiO2+ light control group, S5+ illumination experiment group.Every group of cell set 5 it is parallel
Hole is compareed, and repeats experiment three times.
1mL single cell suspensions are inoculated in the corresponding hole of 96 orifice plates first, CO is placed in224h is incubated in incubator.Treat thin
After born of the same parents' adherent growth, old nutrient solution is discarded.
Blank control group：Cellar culture SGC -7901 cells.
Light control group：1mL fresh mediums are added in each hole of setting, is irradiated with light source, irradiation is finished, continues to incubate
24h is educated, cell survival rate is detected.
S5Control group：1mL fresh mediums are added in each hole of setting, 200 μ g S is added5, continue to be incubated 24h, inspection
Survey cell survival rate.
TiO2+ light control group：1mL fresh mediums are added in each hole of setting, 200 μ g TiO is added2, use light source
Irradiation, irradiation is finished, and is continued to be incubated 24h, is detected cell survival rate.
S5+ illumination experiment group：1mL fresh mediums are added in each hole of setting, 200 μ g S is added5, shone with light source
Penetrate, irradiation is finished, continue to be incubated 24h, detect cell survival rate.
Experiment light source used is 300W xenon lamps, light source direct irradiation, light away from 30cm, irradiation time chooses 0.5 respectively, 1,
1.5h.Survival condition and taken pictures, used using Nikon ECLIPSE Ti inverted microscope observation of cell metamorphosis, analysis
Mtt assay determines cell survival rate on Bio-Rad iMark enzyme-linked immunosorbent assay instruments.Check analysis and time factor analysis result
Show, independent S5On tumor cell survival situation substantially without influence, independent illumination has relatively low lethal effect, S5Illumination experiment group
There is significant photocatalysis killing activity to tumour cell three time points, and be directly proportional to action time.With TiO2
Light group check analysis result shows, S5Photocatalysis inactivating efficacy be better than TiO2。
Embodiment 5：
By product S obtained above5Applied to photo-catalytic degradation of methyl-orange waste water from dyestuff, specific implementation：Reaction is urged in light
Change in reaction bulb and carry out, methyl orange initial concentration is 10mg/L in reaction solution, volume is 100mL, and photochemical catalyst consumption is 1g/L,
PH=5 is adjusted with hydrochloric acid, solution temperature is constant at 20 DEG C, lucifuge 30min, with 300W xenon lamps as light source from top direct irradiation
Solution reaction, light is away from 20cm, separated in time sampling, in maximum absorption wave strong point UV -2102PC UV, visible light light splitting light
Degree meter mensuration absorbance, by η=(A0–At)/A0× 100% calculates A in methyl orange degradation rate, formula0And AtMethyl orange is represented respectively
The initial absorbance of solution and the absorbance of t.Simple TiO2Under equal conditions tested on an equal basis, to compare.It is logical
Cross comparison S5With simple TiO2Both η-t relations discoveries, S5Simple TiO is better than to the degradation rate of methyl orange2, with enhanced
Photocatalytic activity；It is moreover found that after the completion of reaction, S5Catalyst can be separated with high-strength magnet from suspension, 2min
It is basically separated completely, is easy to quickly reclaim catalyst and regeneration cycle is used.
The preferred embodiment of the application is the foregoing is only, the application is not limited to, for the skill of this area
For art personnel, the application can have various modifications and variations.It is all within spirit herein and principle, made any repair
Change, equivalent, improvement etc., should be included within the protection domain of the application.
Claims (10)
1. a kind of sandwich construction nano-complex, it is characterised in that the sandwich construction nano-complex formula is FeaOb–
SiO2–TiO2–<X+FA>, with FeaObFor kernel, SiO is coated with successively in its outer layer2Layer, TiO2Layer and<X+FA>Double modified layers,
Wherein, X is Zn, La or Ce, and FA is folic acid, and a, b are the natural number more than zero.
2. compound as claimed in claim 1, it is characterised in that the FeaObFor magnetic Fe3O4Or magnetic Fe2O3Or both
The mixture of formation.
3. compound as claimed in claim 1, it is characterised in that the FeaObContent be 0.0001-95wt%, SiO2's
Content is 0.0001-95wt%, TiO2Content be 1-95wt%, X content is 0.01-0.5wt%, and surplus is FA.
4. compound as claimed in claim 2, it is characterised in that the Fe2O3Crystal formation be γ types, SiO2Structure be nothing
Sizing, TiO2Crystal formation be Anatase.
5. compound as claimed in claim 2, it is characterised in that FeaObMean particle dia is 0.0001-30nm, SiO2Thickness is
0.0001-50nm, TiO2Thickness is 0.0001-50nm, and the overall dimensions of the compound are no more than 150nm.
6. a kind of preparation method of sandwich construction nano-complex, it is characterised in that including：
By FeaObIt is well mixed with distilled water, absolute ethyl alcohol, concentrated ammonia liquor, then tetraethyl orthosilicate is added dropwise and reacted, reaction is finished,
Magnetic settlement, is washed, and heat treatment obtains FeaOb–SiO2；
By above-mentioned FeaOb–SiO2It is well mixed with absolute ethyl alcohol, metatitanic acid alcohol ester, ultrasonic disperse adds absolute ethyl alcohol, distilled water
With concentrated hydrochloric acid mixed liquor, water-bath is aged, is heat-treated, and roasting produces FeaOb–SiO2–TiO2；
By above-mentioned FeaOb–SiO2–TiO2Add in salting liquid, be well mixed, dry, roasting obtains FeaOb–SiO2–TiO2–X；
By above-mentioned FeaOb–SiO2–TiO2- X water dispersion solution is mixed with the folic acid solution of saliferous, is dialysed, and is dried, is produced.
7. method as claimed in claim 6, it is characterised in that the salt in the salting liquid is zinc acetate, lanthanum nitrate or nitric acid
Cerium.
8. method as claimed in claim 6, it is characterised in that the salt in the folic acid solution of the saliferous is sodium acid carbonate, carbon
Sour sodium, saleratus or potassium carbonate.
9. sandwich construction nano-complex prepared by the method described in claim any one of 6-8.
10. application of the sandwich construction nano-complex described in claim 1-5,9 any one in photocatalysis field.
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