CN107376975A - Visible light catalysis activity N doping nucleocapsid shape titanium dioxide and preparation method thereof - Google Patents
Visible light catalysis activity N doping nucleocapsid shape titanium dioxide and preparation method thereof Download PDFInfo
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- CN107376975A CN107376975A CN201710706426.2A CN201710706426A CN107376975A CN 107376975 A CN107376975 A CN 107376975A CN 201710706426 A CN201710706426 A CN 201710706426A CN 107376975 A CN107376975 A CN 107376975A
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- titanium dioxide
- shape titanium
- nucleocapsid shape
- doping
- core
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 238000006555 catalytic reaction Methods 0.000 title description 5
- 230000000694 effects Effects 0.000 title description 4
- 238000000034 method Methods 0.000 claims abstract description 32
- 239000011258 core-shell material Substances 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000002105 nanoparticle Substances 0.000 claims abstract description 6
- 239000011800 void material Substances 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 6
- 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 6
- 239000000463 material Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical group NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 2
- 235000010215 titanium dioxide Nutrition 0.000 claims 9
- 239000012535 impurity Substances 0.000 claims 1
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 238000012876 topography Methods 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002060 nanoflake Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- B01J35/39—
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/396—
-
- 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
-
- 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
- B01J37/086—Decomposition of an organometallic compound, a metal complex or a metal salt of a carboxylic acid
Abstract
The invention provides a kind of N to adulterate nucleocapsid shape titanium dioxide, wherein described N doping nucleocapsid shape titanium dioxide has core-shell structure, the core-shell structure is comprising the solid spherical core being made up of nano particle and by the laminar hollow outer shell of ultrathin nanometer, and it is 300 500nm void space between wherein described hollow outer shell inner surface and the internal layer ball outer surface, and N doping mass percents are 1.5 2.0%.Present invention also offers the method for preparing this N doping nucleocapsid shape titanium dioxide.It is characteristic of the invention that：Avoid when tradition prepares complex topography nano material to the demand of template, preparation process is very easy, and does not need subsequent heat treatment.
Description
Technical field
The present invention relates to one kind to prepare N doped titanium dioxide photocatalysts, and particularly a kind of solvent-thermal method is without template
Under the conditions of the disposable method for preparing the titanium dioxide optical catalyst with shell core shape special appearance structure that N is adulterated.
Background technology
Titanium dioxide has been widely used for environmental catalysis, energy storage, killed as a kind of photochemical catalyst of most application prospect
The numerous areas such as bacterium, photocell, senser element.But because its bandwidth is larger, it is ultraviolet less than 400nm that wavelength can only be absorbed
Light, and there is no catalysis efficiency under light irradiation of the wavelength more than 400nm, limit and ability is absorbed to sunshine.Therefore,
How to improve it and ability is absorbed to sunshine, it is played catalytic action in bigger irradiation optical wavelength range should to it
Application with promoting and to this inexhaustible clean energy resource of sunshine has very important significance.
Research shows, by reasonably being modified titanium dioxide, passes through semiconductor coupling, metal and nonmetal doping
Etc. technological means, titanium dioxide can be expanded to the absorbing boundary of exposure light to visible region, so as to improve its photocatalysis effect
Energy.But the usual complex steps of semiconductor coupling technology；And foreign material doping is generally unstable, easily lost in subsequent heat treatment
Deactivation.Therefore the effective doping techniques of development stability are very necessary.
In recent years, increasing research shows that the shape characteristic of nano material can largely influence its physics and chemistry
Property, and then influence its effectiveness.Low-density, high-specific surface area, abundant porosity and three-dimensional multilayer structure are considered to
Enough effectively improve titanium dioxide to absorb exposure light, so as to improve its effectiveness.Core-shell structure material has height
Specific surface area, high mass exchange rate, and its core-shell structure can be by improving to multipath reflection/refraction effect of exposure light
Its absorption rate to exposure light.And core-shell structured nanomaterials are prepared at present and are folded typically by multi-step assembling multiple forms
Add, and then remove removing template to obtain.Program is complicated, and needs consumptive mould material.Therefore, simple and effective preparation is developed
Method is particularly significant.
The content of the invention
It is an object of the invention to provide a kind of method for the core-shell structure titanium dioxide for preparing N doping, this method has
Preparation process is simple, without template, do not need subsequent heat treatment, can be realized simultaneously by disposably preparing N doping and
The structure of core-shell structure, the waste of program and cost is avoided, improve the stability of product.
To reach above-mentioned purpose, the invention provides a kind of N to adulterate nucleocapsid shape titanium dioxide, wherein the N adulterates nucleocapsid
Shape titanium dioxide has core-shell structure, and the core-shell structure is comprising the solid spherical core being made up of nano particle and by ultra-thin
The hollow outer shell of nano flake composition, and between wherein described hollow outer shell inner surface and the internal layer ball outer surface
For 300-500nm void space, and N doping mass percents are 1.5-2.0%.
According to one embodiment of the invention, the overall particle diameter of the core-shell structure is 1.5-2.0 μm, specific surface area
Not less than 250m2/g。
According to one embodiment of the invention, the integral thickness of the shell is about 150-250nm.
According to one embodiment of the invention, the particle diameter of the nano particle is less than 10nm, and the ultra-thin subfraction is thin
The thickness of piece is 0.4-4nm.
According to one embodiment of the invention, N doping nucleocapsid shape titanium dioxide can absorbing wavelength be more than 400nm
Exposure light.
Present invention also offers a kind of method for preparing and nucleocapsid shape titanium dioxide being adulterated according to N of the present invention, wherein
Methods described is disposably prepared with solvent-thermal method, and methods described comprises the following steps：
A) N element donor is added into solvent and stirred, it is subsequent to add water and continue stirring extremely mixing
It is even to form solution a；
B) under agitation, tetralkyl titanate is added dropwise into the solution a, stirs to form mixed solution,
The mixed solution is warming up to more than 180 DEG C of temperature and reacted more than 24 hours at said temperatures, terminates and cools down
To room temperature, product is separated and eluted with alcohol, is dried in vacuo at the temperature below 100 DEG C, generation N doping nucleocapsid shape dioxies
Change titanium.
According to one embodiment of the invention, the N element donor is diethylenetriamines.
According to one embodiment of the invention, the solvent is isopropanol.
According to one embodiment of the invention, the water is deionized water or distilled water.
According to one embodiment of the invention, N element donor:Water:Solvent:The volume ratio of tetralkyl titanate is
0.03-0.04:0.1:45-50:1.3-1.7。
According to one embodiment of the invention, the tetralkyl titanate is tetraisopropyl titanate.
According to one embodiment of the invention, wherein step B) mixed solution is transferred in reactor, and
It is positioned in Muffle furnace and heats up.
According to one embodiment of the invention, the alcohol for elution is absolute ethyl alcohol.
According to one embodiment of the invention, methods described need not add any template or material, and described
Method does not need subsequent heat treatment.
Compared with the prior art, its advantage is the present invention：Reagent preparation is few, program is simple to operation, without using template,
It is not required to be heat-treated by subsequent anneal.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph (a, b) and transmission electron microscope picture (c, d) of product according to an embodiment of the invention.
Embodiment
The method that solvent-thermal method prepares N doping shell core shape titanium dioxide, specific implementation method are as follows：
It is molten that 0.032mL diethylenetriamines (commercially available, Sigma Co., USA) is added to 50mL isopropanols under magnetic stirring
In liquid, 0.1mL deionized waters are added after continuing stirring 5 minutes, and continuing stirring makes it well mixed for 10 minutes.Then in magnetic force
Under stirring, 1.5mL tetraisopropyl titanates (commercially available, Sigma Co., USA) are added dropwise into above-mentioned solution, after stirring 20 minutes
The mixed solution of formation is transferred in polytetrafluoroethyllining lining reactor.Then reactor is positioned in Muffle furnace and with 2
DEG C/min heating rate is warming up to 200 DEG C, and kept for 24 hours at such a temperature.After question response terminates and is cooled to room temperature,
Product is centrifuged and eluted with absolute ethyl alcohol, then the three-dimensional knot of the shell core shape of i.e. generation N doping after 70 DEG C of vacuum drying
Structure titanium dioxide.Through field emission scanning electron microscope (HIT (Hitachi), SU8000) and transmission electron microscopy
Mirror (JEOL (JEOL), JEM2100) sign product is core-shell structure (referring to Fig. 1), and internal layer spheroid core is less than by particle diameter
10nm nano particle composition, outer layer hollow shell are formed by thickness for the ultra-thin subfraction thin slice self assembly less than 4nm.Overall shell
Nuclear structure outward appearance average grain diameter is 1.7 μm, and outer shell integral thickness is 200nm, and specific surface area is through specific surface area and pore analysis
Instrument (Mike Mo Ruitike companies of the U.S. (Micromeritics), ASAP2000) is characterized as 258m2/g.Half in hollow outer shell
It is 300-500nm void space between footpath and the internal layer ball radius, N doping ratios are 1.5-2.0%.
The shell core shape three-dimensional structure titanium dioxide that the N is adulterated is through UV-Vis DRS spectrum (HIT
(Hitachi), U4100) characterize, the shell core shape three-dimensional structure titanium dioxide of N doping can absorbing wavelength it is visible more than 400nm
Light.It is molten that the shell core shape three-dimensional structure titanium dioxide that N prepared by 0.02g is adulterated is distributed to the rhodamine B that 50ml concentration is 5mg/L
In liquid, after being stirred 2 hours under dark conditions, it is placed under argon lamp light source and ultraviolet less than 400nm with filter blocks wavelength
Light, light-catalyzed reaction is carried out under visible ray of the wavelength more than 400nm, solution is through spectrophotometry after reacting 3 hours
Count detection be degradable, it was demonstrated that N doping shell core shape three-dimensional structure titanium dioxide can absorbing wavelength be more than 400nm it is visible
Light and catalytic degradation organic pollution.
On the basis of above-described embodiment, it is diethylenetriamines to change reaction reagent proportioning:Deionized water:Isopropanol (body
Product ratio)=0.03:0.1:50, add titanium precursors tetraisopropyl titanate amount and be changed to 1.0ml, same with above-described embodiment anti-
Answer under step, then can not generate shell core shape titanium dioxide, but generation formed by nano flake self assembly it is three-dimensional laminated flower-shaped
Structure.
Operating process and method described above for this patent, any formal limitation is not done to this patent.It is any ripe
The research and technical staff of this area are known, in the case where not departing from the art of this patent aspects, using the above to this
The non-innovative variation and modification (only changing source chemicals adding proportion and reaction duration etc.) that art solutions are made, belong to
In the scope of claims protection.
Claims (14)
1. a kind of N adulterates nucleocapsid shape titanium dioxide, wherein N doping nucleocapsid shape titanium dioxide has core-shell structure, it is described
Core-shell structure includes the solid spherical core that is made up of nano particle and by the laminar hollow outer shell of ultrathin nanometer, and
It is 300-500nm void space between wherein described hollow outer shell inner surface and the internal layer ball outer surface, and N mixes
Impurity level percentage is 1.5-2.0%.
2. N according to claim 1 adulterates nucleocapsid shape titanium dioxide, wherein the overall particle diameter of the core-shell structure is
1.5-2.0 μm, specific surface area is not less than 250m2/g。
3. N according to claim 1 adulterates nucleocapsid shape titanium dioxide, wherein the integral thickness of the shell is about 150-
250nm。
4. N according to claim 1 adulterates nucleocapsid shape titanium dioxide, wherein the particle diameter of the nano particle is less than 10nm,
The thickness of the ultra-thin subfraction thin slice is 0.4-4nm.
5. N according to claim 1 adulterates nucleocapsid shape titanium dioxide, wherein N doping nucleocapsid shape titanium dioxide can
Absorbing wavelength is more than 400nm exposure light.
A kind of 6. method of the N doping nucleocapsid shape titanium dioxide prepared any one of claim 1 to 5, wherein the side
Method is disposably prepared with solvent-thermal method, and methods described comprises the following steps：
A) N element donor is added into solvent and stirred, then add water and continue stirring to it is well mixed with
Form solution a；
B) under agitation, tetralkyl titanate is added dropwise into the solution a, stirs to form mixed solution, by institute
State mixed solution to be warming up to more than 180 DEG C of temperature and react more than 24 hours at said temperatures, terminate and be cooled to room
Wen Hou, product is separated and eluted with alcohol, is dried in vacuo at the temperature below 100 DEG C, generation N doping nucleocapsid shape titanium dioxides
Titanium.
7. according to the method for claim 6, wherein the N element donor is diethylenetriamines.
8. according to the method for claim 6, wherein the solvent is isopropanol.
9. according to the method for claim 6, wherein the water is deionized water or distilled water.
10. the method according to claim 11, wherein N element donor:Water:Solvent:The volume ratio of tetralkyl titanate is
0.03-0.04:0.1:45-50:1.3-1.7。
11. according to the method for claim 6, wherein the tetralkyl titanate is tetraisopropyl titanate.
12. according to the method for claim 6, wherein step B) mixed solution is transferred in reactor, and put
It is placed in Muffle furnace and heats up.
13. according to the method for claim 6, wherein being absolute ethyl alcohol for the alcohol eluted.
14. according to the method for claim 6, wherein methods described need not add any template or material, and institute
The method of stating does not need subsequent heat treatment.
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|---|---|---|---|
| CN201710706426.2A CN107376975A (en) | 2017-08-17 | 2017-08-17 | Visible light catalysis activity N doping nucleocapsid shape titanium dioxide and preparation method thereof |
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| CN201710706426.2A CN107376975A (en) | 2017-08-17 | 2017-08-17 | Visible light catalysis activity N doping nucleocapsid shape titanium dioxide and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107986380A (en) * | 2017-12-02 | 2018-05-04 | 延海平 | A kind of N doping coateds TiO2The technique of photocatalyst for degrading waste water |
| CN110409197A (en) * | 2019-07-30 | 2019-11-05 | 浙江迈实科技有限公司 | A kind of preparation method of multi-functional stamp cotton-containing fabrics |
| CN110424152A (en) * | 2019-07-30 | 2019-11-08 | 浙江迈实科技有限公司 | A kind of preparation method for the PRINTED FABRIC loading photocatalyst |
| CN110438821A (en) * | 2019-07-30 | 2019-11-12 | 浙江迈实科技有限公司 | A kind of preparation method of multi-functional stamp polyester fabric |
| CN110605134A (en) * | 2019-08-30 | 2019-12-24 | 浙江迈实科技有限公司 | Hollow core-shell structure nitrogen-doped TiO2Method for preparing microspheres |
| CN110624591A (en) * | 2019-09-26 | 2019-12-31 | 浙江迈实科技有限公司 | Nitrogen-doped titanium dioxide nano-microsphere and preparation method thereof |
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|---|---|---|---|---|
| CN107986380A (en) * | 2017-12-02 | 2018-05-04 | 延海平 | A kind of N doping coateds TiO2The technique of photocatalyst for degrading waste water |
| CN110409197A (en) * | 2019-07-30 | 2019-11-05 | 浙江迈实科技有限公司 | A kind of preparation method of multi-functional stamp cotton-containing fabrics |
| CN110424152A (en) * | 2019-07-30 | 2019-11-08 | 浙江迈实科技有限公司 | A kind of preparation method for the PRINTED FABRIC loading photocatalyst |
| CN110438821A (en) * | 2019-07-30 | 2019-11-12 | 浙江迈实科技有限公司 | A kind of preparation method of multi-functional stamp polyester fabric |
| CN110605134A (en) * | 2019-08-30 | 2019-12-24 | 浙江迈实科技有限公司 | Hollow core-shell structure nitrogen-doped TiO2Method for preparing microspheres |
| CN110624591A (en) * | 2019-09-26 | 2019-12-31 | 浙江迈实科技有限公司 | Nitrogen-doped titanium dioxide nano-microsphere and preparation method thereof |
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