CN109046304A - Hydrogenate the preparation method of the flower-shaped titanium dioxide of grey - Google Patents
Hydrogenate the preparation method of the flower-shaped titanium dioxide of grey Download PDFInfo
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- CN109046304A CN109046304A CN201811022168.7A CN201811022168A CN109046304A CN 109046304 A CN109046304 A CN 109046304A CN 201811022168 A CN201811022168 A CN 201811022168A CN 109046304 A CN109046304 A CN 109046304A
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- flower
- titanium dioxide
- shaped titanium
- grey
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 157
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000004094 surface-active agent Substances 0.000 claims abstract description 16
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 13
- 150000003608 titanium Chemical class 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 9
- 239000001257 hydrogen Substances 0.000 claims abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 9
- 238000000137 annealing Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims abstract description 3
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 3
- 238000012986 modification Methods 0.000 claims abstract description 3
- 230000004048 modification Effects 0.000 claims abstract description 3
- 239000012429 reaction media Substances 0.000 claims abstract description 3
- 235000019441 ethanol Nutrition 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 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 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000007547 defect Effects 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000004043 dyeing Methods 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 238000004847 absorption spectroscopy Methods 0.000 abstract description 7
- 230000001699 photocatalysis Effects 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 3
- 239000003990 capacitor Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 abstract description 2
- 238000000862 absorption spectrum Methods 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 2
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229940069328 povidone Drugs 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- B01J35/40—
Abstract
The invention discloses a kind of preparation methods for hydrogenating the flower-shaped titanium dioxide of grey, the preparation of the present invention hydrogenation flower-shaped titanium dioxide of grey, first using titanium salt as presoma, using pure and mild acid as reaction medium, using surfactant as structural modification agent, flower-shaped titanium dioxide is prepared by solvent-thermal method, then after flower-shaped titanium dioxide calcination to be removed to the surfactant of flower-shaped titanium dioxide surface, the flower-shaped titanium dioxide of grey is made in high annealing under an atmosphere of hydrogen.X-ray diffractogram shows that the crystal phase of the flower-shaped titanium dioxide of hydrogenation prepared by the present invention is Rutile Type.Ultraviolet-visible absorption spectroscopy figure shows that hydrogenating flower-shaped titanium dioxide has apparent photoresponse in visible light region, and the flower-shaped titanium dioxide after showing hydrogenation treatment has good visible light-responded.Therefore, it is had a good application prospect in terms of photoelectric conversion, photocatalysis, gas sensor capacitor.
Description
Technical field
The present invention relates to the preparation methods of a kind of flower-shaped titanium dioxide more particularly to a kind of with visible light-responded grey
The preparation method of flower-shaped titanium dioxide, belongs to field of material preparation.
Background technique
Since Fujishima in 1972 et al. discovery titanium dioxide can be split water under the irradiation of sunlight as hydrogen
Gas and oxygen, henceforth the photocatalysis performance of titanium dioxide receives everybody and widely pays close attention to.There are three types of crystal forms for titanium dioxide:
Brockite, anatase and Rutile Type, wherein good with anatase and Rutile Type photocatalysis effect.Although titanium dioxide is ultraviolet
Area has good light absorption, but UV energy only accounts for 5% or so of solar energy, and TiO 2 visible light is inhaled
Receipts are less desirable, and the energy that the visible light in sunlight is contained is far longer than the energy that ultraviolet light is contained.Therefore,
It is to improve an approach of the photocatalytic activity of titanium dioxide that titanium dioxide, which is improved, in the utilization of visible region.
Summary of the invention
The purpose of the present invention is being directed to the visible light-responded poor problem of existing titanium dioxide, a kind of hydrogenation ash is provided
The preparation method of dyeing defect shape titanium dioxide.
The present invention hydrogenates the preparation of the flower-shaped titanium dioxide of grey, first using titanium salt as presoma, using pure and mild acid as reaction
Medium prepares flower-shaped titanium dioxide by solvent-thermal method using surfactant as structural modification agent, then by flower-shaped titanium dioxide
After titanium calcining removes the surfactant of flower-shaped titanium dioxide surface, the flower-shaped dioxy of grey is made in high annealing under an atmosphere of hydrogen
Change titanium.Specifically include following processing step:
(1) preparation of flower-shaped titanium dioxide
First titanium salt is slowly added into concentrated acid, 0.5 ~ 2h is stirred at room temperature；Aqueous surfactant solution is slowly added dropwise and stirs 1 ~ 3h；
Then low-carbon alcohols are added and stir 1 ~ 3h；Mixed solution is transferred in high-pressure hydrothermal reaction kettle, in 120 ~ 180 DEG C react 5 ~ for 24 hours；Instead
Reaction suspension is centrifuged after answering, is filtered, is washed, it is dry, obtain flower-shaped titanium dioxide.
The titanium salt is isopropyl titanate or butyl titanate；The concentrated acid is the concentrated hydrochloric acid that concentration is 10 ~ 12mol/L；It is dense
Acid is 10:1 ~ 15:1 with titanium salt solution volume ratio.
The surfactant is polyvinylpyrrolidone or neopelex；The aqueous solution of surfactant
Concentration is 3 ~ 9mg/ml；The additional amount of surfactant solution is the 20 ~ 30 of titanium salt solution volume.
The low-carbon alcohols are ethyl alcohol, propyl alcohol, ethylene glycol, and low-carbon alcohols and surfactant solution volume ratio are 1:1 ~ 6:1.
The drying is dried at 50 ~ 70 DEG C.
(2) preparation of the flower-shaped titanium dioxide of grey is hydrogenated: flower-shaped titanium dioxide calcined to 1 under the conditions of 450 ~ 600 DEG C ~
3h is cooled to room temperature, is subsequently placed in tube furnace, is warming up to 250 ~ 600 DEG C under an atmosphere of hydrogen with 2 ~ 8 DEG C/min, annealing 0.5
~ 5h, is cooled to room temperature, and obtains hydrogenation grey titania powder.
Below by scanning electron microscope (SEM) photograph, X-ray diffractogram, ultraviolet-visible absorption spectroscopy figure is to hydrogenating flower-shaped two in the present invention
The appearance structure and performance of titanium oxide further explain.
Fig. 1 is the scanning electron microscope (SEM) photograph for the flower-shaped titanium dioxide that the present invention is prepared by solvent-thermal method.It can be with from Fig. 2
See, flower-shaped titanium dioxide is the flower-like structure that the diameter assembled by titanium dioxide nano-rod is about 3um or so, and size is equal
One, regular appearance and soilless sticking phenomenon occur.
Fig. 2 is the X-ray diffractogram of the flower-shaped titanium dioxide of hydrogenation prepared by the present invention.From figure 2 it can be seen that hydrogenation flower
Superior crystallinity is presented in shape titanium dioxide, in X-ray diffractogram the angle of diffraction degree of each diffraction maximum be respectively as follows: 27.4 °,
36.1 °, 39.2 °, 41.2 °, 44 °, 54.3 °, 56.6 °, 62.8 °, 69 °, 69.8 °, come under Rutile Type (PDF#75-1749)
Characteristic diffraction peak, show that the crystal phase of the flower-shaped titanium dioxide of hydrogenation prepared by us is Rutile Type.
Fig. 3 is the flower-shaped titanium dioxide ultraviolet-visible absorption spectroscopy figure after hydrogenation.From figure 3, it can be seen that after hydrogenation
There is apparent photoresponse in visible light region, the flower-shaped titanium dioxide after showing hydrogenation treatment has good visible light-responded.
Therefore, it is had a good application prospect in terms of photoelectric conversion, photocatalysis, gas sensor capacitor.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of flower-shaped titanium dioxide prepared by the present invention.
Fig. 2 is that the X-ray of flower-shaped titanium dioxide prepared by the present invention is spread out figure.
Fig. 3 is the ultraviolet-visible absorption spectra figure that the embodiment of the present invention 1 prepares the flower-shaped titanium dioxide of grey.
Fig. 4 is the ultraviolet-visible absorption spectra figure that the embodiment of the present invention 2 prepares the flower-shaped titanium dioxide of grey.
Fig. 5 is the ultraviolet-visible absorption spectra figure that the embodiment of the present invention 3 prepares the flower-shaped titanium dioxide of grey.
Fig. 6 is the ultraviolet-visible absorption spectra figure that the embodiment of the present invention 4 prepares the flower-shaped titanium dioxide of grey.
Specific embodiment
Below by specific example to preparation, structure, pattern and the performance of the present invention hydrogenation flower-shaped titanium dioxide of grey
Deng further explanation.
Embodiment 1
Take concentrated hydrochloric acid 15mL(12mol/L) in round-bottomed flask, quickly 1mL isopropyl titanate is added slowly in concentrated hydrochloric acid under stirring,
1h is stirred at room temperature；Be slowly dropped into 30ml aqueous povidone solution (concentration 9mg/mL) stirring 2h, then plus ethylene glycol 90ml,
Stir 2h；Then mixed solution is transferred in 200ml high-pressure hydrothermal reaction kettle, in 150 DEG C of reaction 12h；It after reaction will be anti-
It answers suspension to be centrifuged 5min in 6000r/min, filters, successively use ultrapure water, ethyl alcohol, acetone washing 3 times, it is finally dry at 60 DEG C
It is dry, obtain flower-shaped titanium dioxide.SEM pattern shows the flower-like structure (see figure 1) that diameter is about 3um or so；
The preparation of the flower-shaped titanium dioxide of grey: above-mentioned flower-shaped titanium dioxide is calcined into 2h at 550 DEG C, is cooled to room temperature, then
It is placed in tube furnace, 250 DEG C of annealing 5h is warming up to the speed of 5 DEG C/min under an atmosphere of hydrogen, is cooled to room temperature, obtains grey
Titania powder, be denoted as sample 1.Ultraviolet-visible absorption spectroscopy shows there is very weak visible light-responded (see figure 3).
Embodiment 2
Flower-shaped titanium dioxide preparation is the same as embodiment 1；
The preparation of the flower-shaped titanium dioxide of grey: flower-shaped titanium dioxide is calcined into 2h under the conditions of 550 DEG C, is cooled to room temperature, then
It is placed in tube furnace, 350 DEG C of annealing 5h is warming up to 5 DEG C/min under an atmosphere of hydrogen, are cooled to room temperature to obtain the dioxy of grey
Change titanium powder, is denoted as sample 2.Ultraviolet-visible absorption spectroscopy shows there is weaker visible light-responded (see figure 4).
Embodiment 3
Flower-shaped titanium dioxide preparation is the same as embodiment 1；
The preparation of the flower-shaped titanium dioxide of grey: flower-shaped titanium dioxide is calcined into 2h under the conditions of 550 DEG C, is cooled to room temperature, then
It is placed in tube furnace, 450 DEG C of annealing 5h is warming up to 5 DEG C/min under an atmosphere of hydrogen, is cooled to room temperature, obtains grey titanium dioxide
Titanium powder is denoted as sample 3.Ultraviolet-visible absorption spectroscopy shows there is good visible light-responded (see figure 5).
Embodiment 4
Flower-shaped titanium dioxide preparation is the same as embodiment 1；
The preparation of the flower-shaped titanium dioxide of grey: flower-shaped titanium dioxide is calcined into 2h under the conditions of 550 DEG C, is cooled to room temperature, then
It is placed in tube furnace, 600 DEG C of annealing 5h is warming up to 5 DEG C/min under an atmosphere of hydrogen, is cooled to room temperature, obtains grey titanium dioxide
Titanium powder is denoted as sample 4.Ultraviolet-visible absorption spectroscopy shows there is good visible light-responded (see figure 6).
Claims (8)
1. a kind of preparation method for hydrogenating the flower-shaped titanium dioxide of grey, molten with low-carbon alcohols and acid first using titanium salt as presoma
Liquid is as reaction medium, using surfactant as structural modification agent, prepares flower-shaped titanium dioxide by solvent-thermal method, then will
After flower-shaped titanium dioxide calcination removes the surfactant of flower-shaped titanium dioxide surface, ash is made in high annealing under an atmosphere of hydrogen
Dyeing defect shape titanium dioxide.
2. a kind of preparation method for hydrogenating the flower-shaped titanium dioxide of grey as described in claim 1, it is characterised in that: including following step
It is rapid:
(1) preparation of flower-shaped titanium dioxide: titanium salt solution is slowly dropped in concentrated acid, 0.5 ~ 2h is stirred at room temperature；It is slowly added dropwise
Aqueous surfactant solution stirs 1 ~ 3h；It adds low-carbon alcohols and stirs 1 ~ 3h；Then mixed solution is transferred to high pressure hydro-thermal reaction
In kettle, in 120 ~ 180 DEG C react 5 ~ for 24 hours；After reaction, reaction suspension is centrifuged, and is filtered, and is washed, dry, obtains flower-shaped two
Titanium oxide；
(2) it hydrogenates the preparation of the flower-shaped titanium dioxide of grey: flower-shaped titanium dioxide is calcined into 1 ~ 3h under the conditions of 450 ~ 600 DEG C, drop
It warms to room temperature, is subsequently placed in tube furnace, be warming up to 250 ~ 600 DEG C under an atmosphere of hydrogen with 2 ~ 8 DEG C/min, anneal 0.5 ~ 5h,
It is cooled to room temperature, obtains hydrogenation grey titania powder.
3. a kind of preparation method for hydrogenating the flower-shaped titanium dioxide of grey as claimed in claim 2, it is characterised in that: in step (1),
The titanium salt is isopropyl titanate or butyl titanate.
4. a kind of preparation method for hydrogenating the flower-shaped titanium dioxide of grey as claimed in claim 2, it is characterised in that: in step (1),
The concentrated acid is the concentrated hydrochloric acid that concentration is 10 ~ 12mol/L, and concentrated acid and titanium salt volume ratio are 10:1 ~ 15:1.
5. a kind of preparation method for hydrogenating the flower-shaped titanium dioxide of grey as claimed in claim 2, it is characterised in that: in step (1),
The surfactant is polyvinylpyrrolidone or neopelex.
6. a kind of preparation method for hydrogenating the flower-shaped titanium dioxide of grey as claimed in claim 5, it is characterised in that: surfactant
Concentration of aqueous solution be 3 ~ 9mg/ml；Surfactant solution additional amount is 20 ~ 30 times of titanium salt volume.
7. a kind of preparation method for hydrogenating the flower-shaped titanium dioxide of grey as claimed in claim 2, it is characterised in that: in step (1),
The low-carbon alcohols are ethyl alcohol, propyl alcohol, ethylene glycol, and low-carbon alcohols and surfactant solution volume ratio are 1:1 ~ 6:1.
8. a kind of preparation method for hydrogenating the flower-shaped titanium dioxide of grey as claimed in claim 2, it is characterised in that: step (1)
In, the drying is dried at 50 ~ 70 DEG C.
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| CN110124724A (en) * | 2019-06-25 | 2019-08-16 | 西北师范大学 | A kind of preparation method of functionalization graphene quantum dot/composite titania material |
| CN110124725A (en) * | 2019-06-25 | 2019-08-16 | 西北师范大学 | A kind of preparation and application hydrogenating titanium dioxide/graphene quantum dot composite material |
| CN110550655A (en) * | 2019-10-18 | 2019-12-10 | 吉林大学 | Method for preparing titanium dioxide nano particles in gray anatase phase |
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Application publication date: 20181221 |