CN107413325A - A kind of rare earth/carbon co-doped flexible TiO2Nano fibrous membrane and preparation method thereof - Google Patents
A kind of rare earth/carbon co-doped flexible TiO2Nano fibrous membrane and preparation method thereof Download PDFInfo
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- CN107413325A CN107413325A CN201710670266.0A CN201710670266A CN107413325A CN 107413325 A CN107413325 A CN 107413325A CN 201710670266 A CN201710670266 A CN 201710670266A CN 107413325 A CN107413325 A CN 107413325A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 81
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 77
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 59
- 239000012528 membrane Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000000835 fiber Substances 0.000 claims abstract description 30
- 239000002243 precursor Substances 0.000 claims abstract description 27
- 239000010936 titanium Substances 0.000 claims abstract description 27
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 26
- -1 rare earth metal salt Chemical class 0.000 claims abstract description 26
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 26
- 239000002904 solvent Substances 0.000 claims abstract description 20
- 238000001354 calcination Methods 0.000 claims abstract description 19
- 238000009987 spinning Methods 0.000 claims abstract description 17
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 16
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 12
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 claims description 6
- 235000011187 glycerol Nutrition 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 150000000703 Cerium Chemical class 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 150000000917 Erbium Chemical class 0.000 claims description 4
- 150000000921 Gadolinium Chemical class 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 150000001206 Neodymium Chemical class 0.000 claims description 4
- 150000001213 Praseodymium Chemical class 0.000 claims description 4
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 4
- 159000000008 strontium salts Chemical class 0.000 claims description 4
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 3
- 229920001577 copolymer Polymers 0.000 claims description 3
- JLRJWBUSTKIQQH-UHFFFAOYSA-K lanthanum(3+);triacetate Chemical compound [La+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JLRJWBUSTKIQQH-UHFFFAOYSA-K 0.000 claims description 3
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical class Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims description 3
- 239000002048 multi walled nanotube Substances 0.000 claims description 3
- 239000002109 single walled nanotube Substances 0.000 claims description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 3
- 229920000428 triblock copolymer Polymers 0.000 claims description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052691 Erbium Inorganic materials 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical group CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims description 2
- XWFVFZQEDMDSET-UHFFFAOYSA-N gadolinium(3+);trinitrate;hexahydrate Chemical group O.O.O.O.O.O.[Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XWFVFZQEDMDSET-UHFFFAOYSA-N 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- 150000002603 lanthanum Chemical class 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical group [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- GJKFIJKSBFYMQK-UHFFFAOYSA-N lanthanum(3+);trinitrate;hexahydrate Chemical group O.O.O.O.O.O.[La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GJKFIJKSBFYMQK-UHFFFAOYSA-N 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002070 nanowire Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229920001451 polypropylene glycol Polymers 0.000 claims description 2
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 2
- YJPVTCSBVRMESK-UHFFFAOYSA-L strontium bromide Chemical class [Br-].[Br-].[Sr+2] YJPVTCSBVRMESK-UHFFFAOYSA-L 0.000 claims description 2
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical group CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 2
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 2
- ROHFMCNIVFLSTQ-UHFFFAOYSA-K trichloroneodymium;hydrate Chemical class O.Cl[Nd](Cl)Cl ROHFMCNIVFLSTQ-UHFFFAOYSA-K 0.000 claims description 2
- 230000036571 hydration Effects 0.000 claims 2
- 238000006703 hydration reaction Methods 0.000 claims 2
- 150000001336 alkenes Chemical class 0.000 claims 1
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
- 229910052712 strontium Inorganic materials 0.000 claims 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 9
- 230000032683 aging Effects 0.000 abstract description 2
- 238000012805 post-processing Methods 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 7
- 235000010215 titanium dioxide Nutrition 0.000 description 7
- 239000002121 nanofiber Substances 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 6
- 239000004408 titanium dioxide Substances 0.000 description 6
- 239000004094 surface-active agent Substances 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000001523 electrospinning Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 229910052684 Cerium Inorganic materials 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000693 micelle Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000012855 volatile organic compound Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- BQODPTQLXVVEJG-UHFFFAOYSA-N [O].C=C Chemical compound [O].C=C BQODPTQLXVVEJG-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005686 electrostatic field Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- RLDBHKUGRPXFBF-UHFFFAOYSA-N lanthanum;hydrate Chemical compound O.[La] RLDBHKUGRPXFBF-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- LMCBEWMQFKWHGU-UHFFFAOYSA-N propan-2-ol;titanium Chemical compound [Ti].CC(C)O LMCBEWMQFKWHGU-UHFFFAOYSA-N 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- AMGRXJSJSONEEG-UHFFFAOYSA-L strontium dichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Sr]Cl AMGRXJSJSONEEG-UHFFFAOYSA-L 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- 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
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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
- B01J35/39—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
- 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
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
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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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
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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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
- B01J37/033—Using Hydrolysis
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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
- B01J37/082—Decomposition and pyrolysis
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The present invention relates to a kind of rare earth/carbon co-doped flexible TiO2Nano fibrous membrane and preparation method thereof, step are as follows：Precursor solution is prepared first, and precursor solution is made up of titanium source, rare earth metal salt, carbon source, nonionic surfactant and solvent；Electrostatic spinning is carried out again and obtains precursor fibre film, and it is 10~0 DEG C to apply 50~100 DEG C of constant temperature thermal field in spinning section during electrostatic spinning and control the temperature of reception device；Finally calcining obtains rare earth/carbon co-doped flexible TiO in air atmosphere2Nano fibrous membrane.The pliability of final obtained product is 10~50mN, and tensile break strength is 3~5MPa, and absorbable light abstraction width is expanded to 550~700nm.Preparation method of the present invention, without adding polymer or aging, without post processing, technique is simple, and cost is cheap, and product has good tensile break strength, flexibility and visible light catalytic performance.
Description
Technical field
The invention belongs to field of new materials, is related to a kind of rare earth/carbon co-doped flexible TiO2Nano fibrous membrane and its preparation
Method.
Background technology
Titanium dioxide (TiO2) monodimension nanometer material is because of spies such as its photocatalysis property is stable, cheap, no biotoxicities
Point, the volatile organic matter (VOCs) in photocatalysis hydrogen production, industry, and caused in terms of the degraded such as indoor, in-car VOCs
Extensive concern.But a kind of wide variety of catalysis material is used as, it has following subject matter：1)TiO2Greater band gap
(Eg=3.0~3.2eV), can only be low by the ultraviolet excitation below 400 nano wave lengths, solar energy utilization ratio.2) light induced electron-
Hole to easily it is compound, cause light quantum utilization rate low, so as to reduce the catalytic activity of material.3) most of one-dimensional titanium dioxides
Titanium nano material generally existing fragility it is big, low intensity the problem of.The problem of above-mentioned, turns into limitation nano titanium dioxide photocatalysis
The wide variety of bottleneck problem of material.Therefore, people utilize element doping, absorption of the titanium dioxide to visible ray is realized, and
Effectively suppress the compound of photo-generate electron-hole pair, so as to improve catalytic activity, and prepared by the flexibility for realizing fiber.
In the research of early stage, mainly with single metal or nonmetal doping, such as C, S, N, Fe, Ni, Zn, La, Ce.
Maruska etc. reports to be responded by the titania-doped visible light catalytic that makes it have of transition metal (Fe, Ni etc.),
Asahi etc. reports N substitutions TiO2In lattice after a small amount of O, it can make catalyst that there is visible light catalytic response, then
Lettmann etc. chances on when doing N doping, also has visible light catalysis activity in the sample of no doping, so as to find carbon
Dopen Nano TiO2Visible light catalysis activity, for this exploitation with visible light catalytic response titania-doped research just
Attract wide attention.
Patent CN 104607171 discloses a kind of preparation side of praseodymium doped dioxide composite nanofiber photocatalyst
Method, (2014) 1191-1201 of Applied Physics A 117 report a kind of preparation of cerium doped titanium dioxide nanofiber
Method, a small amount of rare earth metal are incorporated into TiO2Lattice or interstitial void in, effectively inhibit photo-generate electron-hole to answering
Close, while enhance the interaction between crystal boundary, while improving catalytic activity, also expanded its visible absorption scope, but
Its visible absorption wavelength focuses mostly in below 500nm.
Patent CN 102021676A disclose a kind of preparation method of titanium dioxide/active carbon composite nanofibrous membrane,
Synthetic Metals 193 (2014) 125-131 reports a kind of preparation side of titanium dioxide/carbon nano tube nano fiber
Method, research are found in C and thulium co-doped nano TiO2In material, a small amount of C enters TiO2In lattice, Ti-C is formed
Key, doped energy-band is formed, its energy gap is narrowed, is advantageous to its absorption to visible ray, although C introducing can make catalysis
The light abstraction width of agent becomes big, expands to more than 700nm, but C presence result in the catalytic activity reduction of catalyst.
In recent years, multi-element doping is of increased attention.Especially carbon is more favored with rare earth doped.
Improve fibre strength.However, on rare earth/carbon co-doped flexible titanium dioxide nanofiber preparation and research report still
It is rare.Therefore, a kind of rare earth/carbon co-doped flexible TiO is developed2Nano-fiber material tool is of great significance.
The content of the invention
The purpose of the present invention is to overcome that technique in the prior art is complex, costly and bad properties of product lacks
Falling into, there is provided a kind of simple production process, cost are cheap, product photocatalysis performance and its flexible preferably rare earth/and it is carbon co-doped soft
Property TiO2Nano fibrous membrane and preparation method thereof.
To reach above-mentioned purpose, the present invention adopts the following technical scheme that：
A kind of rare earth/carbon co-doped flexible TiO2The preparation method of nano fibrous membrane, step are as follows：
(1) precursor solution is prepared, the precursor solution is by titanium source, rare earth metal salt, carbon source, non-ionic surface active
Agent and solvent composition；
(2) carry out electrostatic spinning and obtain precursor fibre film, apply constant temperature thermal field in spinning section during the electrostatic spinning
And the temperature of reception device is controlled, the temperature of the constant temperature thermal field is 50~100 DEG C, and the temperature of the reception device is -10~0
℃；
(3) calcining obtains rare earth/carbon co-doped flexible TiO in air atmosphere2Nano fibrous membrane.
As preferable technical scheme：
A kind of rare earth/carbon co-doped flexible TiO as described above2The preparation method of nano fibrous membrane, the preparation forerunner
The concrete operations of liquid solution are：Titanium source and rare earth metal salt dissolving are stirred into 30~150min in a solvent, then sequentially added
Carbon source and nonionic surfactant stir 10~90min and are well mixed.
On the one hand it is first to make titanium source carry out partial hydrolysis to produce hydroxyl by titanium source, the purpose of rare earth metal salt dissolving in a solvent
Base, on the other hand it is to be well mixed rare earth metal salt and titanium source.If simultaneously by titanium source, rare earth metal salt, carbon source and nonionic
Surface-active is added in solvent, is unfavorable for titanium source hydrolysis, is influenceed the growth of micelle, is unfavorable for uniformly dividing for rare earth ion
Cloth.
Rare earth/carbon co-doped flexible TiO as described above2The preparation method of nano fibrous membrane, in the precursor solution
The mol ratio of titanium source, rare earth metal salt and solvent is 1:0.001~0.1:10~100, titanium source, carbon source and non-ionic surface active
The mol ratio of agent is 1:0.001~0.1:0.05~0.25.
Rare earth/carbon co-doped flexible TiO as described above2The preparation method of nano fibrous membrane, the titanium source are isopropanol
Titanium, butyl titanate, titanium tetrachloride, titanium trichloride or titanyl sulfate；
The rare earth metal salt is lanthanum salt, cerium salt, gadolinium salt, erbium salt, praseodymium salt, strontium salt or neodymium salt；
The solvent is ethanol, ethylene glycol, isopropanol, glycerine, acetic acid or N,N-dimethylformamide；
The carbon source is graphene, single-walled carbon nanotube, multi-walled carbon nanotube, carbon quantum dot, activated carbon or carbon black；
The nonionic surfactant is PEO-PPOX-PEO triblock copolymer, gathered
Oxygen ethene polyoxypropylene, glycerine polyoxyethylene polyoxypropylene blocked copolymer, ethylenediamine polyoxyethylene oxypropylene block
Formula polyethers or propane diols polyoxyethylene poly-oxygen propylene aether.
A kind of rare earth/carbon co-doped flexible TiO as described above2The preparation method of nano fibrous membrane, the lanthanum salt are six
Nitric hydrate lanthanum, lanthanum acetate or seven hydrated lanthanum chlorides, the cerium salt are six nitric hydrate ceriums or seven chloride hydrate ceriums, the gadolinium salt
For gadolinium nitrate hexahydrate, six chloride hydrate gadoliniums or eight hydrated sulfuric acid gadoliniums, the erbium salt is five nitric hydrate erbiums or six chloride hydrates
Erbium, the praseodymium salt are six nitric hydrate praseodymiums or eight hydrated sulfuric acid praseodymiums, and the strontium salt is that Strontium dichloride hexahydrate or six are hydrated strontium bromides,
The neodymium salt is six nitric hydrate neodymiums or six Neodymium chloride hydrates.
A kind of rare earth/carbon co-doped flexible TiO as described above2The preparation method of nano fibrous membrane, the electrostatic spinning
Parameter be：Relative humidity 20~70%, 0.1~15mL/h of rate of flooding, 10~60kV of voltage, between reception device and spinning nozzle
20~40cm of distance, the reception device is metal roller or metal plate.
A kind of rare earth/carbon co-doped flexible TiO as described above2The preparation method of nano fibrous membrane, the temperature of the calcining
Degree progressively rises to 400~1000 DEG C from room temperature, and heating rate is 0.1~10 DEG C/min, and is kept under highest calcining heat
10~360min.
The present invention also provides one kind rare earth as made from method produced above/carbon co-doped flexible TiO2Nano fibrous membrane,
Rare earth/carbon co-doped flexible TiO2The pliability of nano fibrous membrane is 10~50mN, rare earth/carbon co-doped flexible TiO2Nanowire
The tensile break strength for tieing up film is 3~5MPa, and absorbable light abstraction width is expanded to 550~700nm.
As preferable technical scheme：
Rare earth/carbon co-doped flexible TiO as described above2Nano fibrous membrane, the rare earth/carbon co-doped flexible TiO2Receive
The average diameter of fiber be 10~400nm in rice tunica fibrosa, and relative standard deviation is 1~5%, internal grain size for 10~
80nm.Fiber diameter range shows fiber thickness, and fibre diameter is smaller, and single fiber pliability is preferable, is advantageous to tunica fibrosa softness
The raising of degree；For relative standard deviation to characterize the uniformity of distribution of fiber diameters, deviation is smaller, and Fiber Uniformity is better；
Crystallite dimension and fiber film dynamic performance are closely related, and the reduction of crystallite dimension is also beneficial to the lifting of photocatalysis performance.
Inventive principle：
Titanium source is added in solvent by the first step of the present invention, and hydrolysis-condensation reaction occurs under stirring, adds rare earth
The purpose of metal salt is during subsequent calcination, reduces fiber surface microdefect, suppresses TiO2Grain growth, crystallite dimension are got over
Small, crystal grain is higher than surface, and surface-active bits number is more, and photocatalytic activity is improved accordingly, is adding carbon source
After surfactant, hydrogen bond can be formed between titanium source, carbon source and surfactant, carbon source is evenly distributed on presoma molten
In liquid, the spinning solution of stable homogeneous is obtained；Apply 50~100 DEG C of constant temperature thermal field in spinning section during electrostatic spinning, promote
The quick volatilization of solvent in spinning jet so that surfactant concentration reaches critical micelle concentration, then passes through self assembly shape
Into micella, and arranged under the quick drawing-off effect of electric field force along fiber axial direction direction gage entire row, micella unit phase each other in fiber
It is mutually parallel, there is one-dimensional order, in addition, thermal field and Electrostatic Field Coupling inducing action can promote TiO in spinning solution2In presoma
Hydroxyl and carbon source between form stronger hydrogen bond or covalent bond effect so that TiO2Presoma and the uniform Assembled distribution of carbon source exist
Micellar surface., can be with wink because reception device has relatively low temperature (- 10~0 DEG C) when fiber is collected into reception device
Between consolidate and retain the orderly self-assembled structures inside precursor fibre.
Beneficial effect：
(1) a kind of rare earth/carbon co-doped flexible TiO of the invention2The preparation method of nano fibrous membrane, it polymerize without adding
Thing or aging, without post processing, by applying constant temperature thermal field in spinning process, and reception substrate temperature is reduced, make carbon source
It is uniformly distributed and consolidates in precursor fibre, and Ti content is high in spinning solution, titanium dioxide nanofiber yield is high, prepares work
Skill is simple, and cost is cheap；
(2) a kind of rare earth/carbon co-doped flexible TiO of the invention2Nano fibrous membrane, have good tension failure strong
Degree, flexible and visible light catalytic performance.
Embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair
Bright rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, art technology
Personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Fixed scope.
Embodiment 1
A kind of rare earth/carbon co-doped flexible TiO2The preparation method of nano fibrous membrane, step are as follows：
(1) titanium source isopropyl titanate and rare earth metal salt lanthanum nitrate hexahydrate are dissolved in etoh solvent and stir 30min, so
After sequentially add carbon source graphite alkene and nonionic surfactant PEO-PPOX-PEO three block
Copolymer stirring 90min is well mixed with obtaining precursor solution, titanium source wherein in solution, rare earth metal salt, solvent, carbon source with it is non-
The mol ratio of ionic surface active agent is 1:0.001:100:0.001:0.25；
(2) precursor fibre film is made by electrospinning process in above-mentioned precursor solution, in spinning during electrostatic spinning
Section apply 50 DEG C constant temperature thermal field and control metal roller reception device temperature be 0 DEG C；The parameter of electrostatic spinning is：Relatively
Humidity 20%, rate of flooding 15mL/h, voltage 10kV, the distance 40cm between reception device and spinning nozzle；
(3) above-mentioned precursor fibre film is placed in calcining in air atmosphere and obtains rare earth/carbon co-doped flexible TiO2Nanometer
Tunica fibrosa, calcining refer to that the temperature of calcining progressively rises to 650 DEG C from room temperature, and heating rate is 10 DEG C/min, and is forged in highest
120min is kept at a temperature of burning.
Final obtained rare earth/carbon co-doped flexible TiO2The average diameter of fiber is 200nm in nano fibrous membrane, and phase
It is 1% to standard deviation, fibrous inside crystallite dimension is 10nm, rare earth/carbon co-doped flexible TiO2The softness of nano fibrous membrane
Spend for 10mN, tensile break strength 5MPa, the absorption region of visible ray is expanded to 700nm.
Comparative example 1
A kind of rare earth/carbon co-doped flexible TiO2The preparation method of nano fibrous membrane, its basic step and parameter and implementation
Example 1 is identical, and difference is to be not provided with constant temperature thermal field during electrostatic spinning, and reception device temperature is set into normal temperature.
Its obtained rare earth/carbon co-doped flexible TiO2The average diameter of fiber is 300nm in nano fibrous membrane, and relatively
Standard deviation is 3%, and fibrous inside crystallite dimension is 45nm, the rare earth/carbon co-doped flexible TiO2The softness of nano fibrous membrane
Spend for 50mN, tensile break strength 0.8MPa, the absorption region of visible ray is expanded to 500nm, passes through pair with embodiment 1
Than it can be found that obtained rare earth/carbon co-doped flexible TiO in embodiment 12Nano fibrous membrane ensure that it is certain flexible
Meanwhile its absorption region to visible ray is substantially increased, photocatalysis performance is far superior to rare earth/carbon co-doped flexible TiO2Receive
Rice tunica fibrosa.
Embodiment 2
A kind of rare earth/carbon co-doped flexible TiO2The preparation method of nano fibrous membrane, step are as follows：
(1) titanium source butyl titanate and rare earth metal salt lanthanum acetate are dissolved in solvent ethylene glycol and stir 150min, so
After sequentially add carbon source single-walled carbon nanotube and non-ionic surfactant polyoxyethylene polyoxypropylene stirring 10min be well mixed
With precursor solution, titanium source wherein in solution, rare earth metal salt, solvent, the mol ratio of carbon source and nonionic surfactant
For 1:0.1:10:0.1:0.05；
(2) precursor fibre film is made by electrospinning process in above-mentioned precursor solution, in spinning during electrostatic spinning
Section apply 100 DEG C constant temperature thermal field and control metal plate reception device temperature be -10 DEG C；The parameter of electrostatic spinning is：
Relative humidity 70%, rate of flooding 0.1mL/h, voltage 60kV, the distance 20cm between reception device and spinning nozzle；
(3) above-mentioned precursor fibre film is placed in calcining in air atmosphere and obtains rare earth/carbon co-doped flexible TiO2Nanometer
Tunica fibrosa, calcining refer to that the temperature of calcining progressively rises to 1000 DEG C from room temperature, and heating rate is 0.1 DEG C/min, and in highest
360min is kept under calcining heat.
Final obtained rare earth/carbon co-doped flexible TiO2The average diameter of fiber is 300nm in nano fibrous membrane, and phase
It is 5% to standard deviation, fibrous inside crystallite dimension is 80nm, rare earth/carbon co-doped flexible TiO2The softness of nano fibrous membrane
Spend for 50mN, tensile break strength 3MPa, the absorption region of visible ray is expanded to 580nm.
Embodiment 3
A kind of rare earth/carbon co-doped flexible TiO2The preparation method of nano fibrous membrane, step are as follows：
(1) titanium source titanium tetrachloride and the hydrated lanthanum chloride of rare earth metal salt seven are stirred into 90min in solvent ethylene glycol, then
Sequentially add carbon source multi-walled carbon nanotube and nonionic surfactant glycerine polyoxyethylene polyoxypropylene blocked copolymer
Stir 50min and be well mixed and match somebody with somebody to obtain precursor solution, titanium source, rare earth metal salt, solvent, carbon source and nonionic table wherein in solution
The mol ratio of face activating agent is 1:0.05:55:0.05:0.15；
(2) precursor fibre film is made by electrospinning process in above-mentioned precursor solution, in spinning during electrostatic spinning
Section apply 75 DEG C constant temperature thermal field and control metal roller reception device temperature be -5 DEG C；The parameter of electrostatic spinning is：Phase
To humidity 45%, rate of flooding 7.5mL/h, voltage 35kV, the distance 30cm between reception device and spinning nozzle；
(3) above-mentioned precursor fibre film is placed in calcining in air atmosphere and obtains rare earth/carbon co-doped flexible TiO2Nanometer
Tunica fibrosa, calcining refer to that the temperature of calcining progressively rises to 700 DEG C from room temperature, and heating rate is 5 DEG C/min, and is calcined in highest
At a temperature of keep 185min.
Final obtained rare earth/carbon co-doped flexible TiO2The average diameter of fiber is 205nm in nano fibrous membrane, and phase
It is 3% to standard deviation, fibrous inside crystallite dimension is 45nm, rare earth/carbon co-doped flexible TiO2The softness of nano fibrous membrane
Spend for 40mN, tensile break strength 3.5MPa, the absorption region of visible ray is expanded to 650nm.
Embodiment 4~27
The preparation process of embodiment 4~27 prepares parameter, electrospinning parameters, calcining with embodiment 1, wherein precursor solution
Parameter and rare earth/carbon co-doped flexible TiO2Nano fibrous membrane performance parameter (note as shown in 1~table of table 6：Mixing time 1 is titanium
Source and rare earth metal salt are dissolved in the mixing time after solvent, after mixing time 2 is adds carbon source and nonionic surfactant
The time of stirring)
Table 1
Table 2
Table 3
Table 4
Table 5
Table 6
Claims (9)
- A kind of 1. rare earth/carbon co-doped flexible TiO2The preparation method of nano fibrous membrane, it is characterized in that, step is as follows：(1) prepare precursor solution, the precursor solution by titanium source, rare earth metal salt, carbon source, nonionic surfactant and Solvent forms；(2) carry out electrostatic spinning and obtain precursor fibre film, apply constant temperature thermal field in spinning section and control during the electrostatic spinning The temperature of reception device processed, the temperature of the constant temperature thermal field is 50~100 DEG C, and the temperature of the reception device is -10~0 DEG C；(3) calcining obtains rare earth/carbon co-doped flexible TiO in air atmosphere2Nano fibrous membrane.
- A kind of 2. rare earth according to claim 1/carbon co-doped flexible TiO2The preparation method of nano fibrous membrane, its feature It is, the concrete operations of the preparation precursor solution are：By titanium source and rare earth metal salt dissolving in a solvent stirring 30~ 150min, then sequentially adds carbon source and nonionic surfactant stirs 10~90min and is well mixed.
- A kind of 3. rare earth according to claim 1/carbon co-doped flexible TiO2The preparation method of nano fibrous membrane, its feature It is, the mol ratio of titanium source, rare earth metal salt and solvent is 1 in the precursor solution:0.001~0.1:10~100, titanium The mol ratio in source, carbon source and nonionic surfactant is 1:0.001~0.1:0.05~0.25.
- A kind of 4. rare earth according to claim 3/carbon co-doped flexible TiO2The preparation method of nano fibrous membrane, its feature It is, the titanium source is isopropyl titanate, butyl titanate, titanium tetrachloride, titanium trichloride or titanyl sulfate；The rare earth metal salt is lanthanum salt, cerium salt, gadolinium salt, erbium salt, praseodymium salt, strontium salt or neodymium salt；The solvent is ethanol, ethylene glycol, isopropanol, glycerine, acetic acid or N,N-dimethylformamide；The carbon source is graphene, single-walled carbon nanotube, multi-walled carbon nanotube, carbon quantum dot, activated carbon or carbon black；The nonionic surfactant is PEO-PPOX-PEO triblock copolymer, polyoxy second Alkene polyoxypropylene, glycerine polyoxyethylene polyoxypropylene blocked copolymer, ethylenediamine polyoxyethylene oxypropylene block formula are gathered Ether or propane diols polyoxyethylene poly-oxygen propylene aether.
- A kind of 5. rare earth according to claim 4/carbon co-doped flexible TiO2The preparation method of nano fibrous membrane, its feature It is, the lanthanum salt is lanthanum nitrate hexahydrate, lanthanum acetate or seven hydrated lanthanum chlorides, and the cerium salt is six nitric hydrate ceriums or seven water Cerium chloride is closed, the gadolinium salt is gadolinium nitrate hexahydrate, six chloride hydrate gadoliniums or eight hydrated sulfuric acid gadoliniums, and the erbium salt is five hydration nitre Sour erbium or six chloride hydrate erbiums, the praseodymium salt are six nitric hydrate praseodymiums or eight hydrated sulfuric acid praseodymiums, and the strontium salt is six chloride hydrates Strontium or six hydration strontium bromides, the neodymium salt is six nitric hydrate neodymiums or six Neodymium chloride hydrates.
- A kind of 6. rare earth according to claim 1/carbon co-doped flexible TiO2The preparation method of nano fibrous membrane, its feature It is, the parameter of the electrostatic spinning is：Relative humidity 20~70%, 0.1~15mL/h of rate of flooding, 10~60kV of voltage, 20~40cm of distance between reception device and spinning nozzle, the reception device are metal roller or metal plate.
- A kind of 7. rare earth according to claim 1/carbon co-doped flexible TiO2The preparation method of nano fibrous membrane, its feature It is, the temperature of the calcining progressively rises to 400~1000 DEG C from room temperature, and heating rate is 0.1~10 DEG C/min, and most 10~360min is kept under high calcining heat.
- 8. using rare earth/carbon co-doped flexible TiO made from the preparation method as described in any one of claim 1~72Nanowire Film is tieed up, it is characterized in that：Rare earth/carbon co-doped flexible TiO2The pliability of nano fibrous membrane is 10~50mN, rare earth/carbon co-doped Flexible TiO2The tensile break strength of nano fibrous membrane is 3~5MPa, and absorbable light abstraction width is expanded to 550~700nm.
- 9. rare earth according to claim 8/carbon co-doped flexible TiO2Nano fibrous membrane, it is characterised in that the rare earth/ Carbon co-doped flexible TiO2The average diameter of fiber is 10~400nm in nano fibrous membrane, and relative standard deviation is 1~5%, Internal grain size is 10~80nm.
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