CN107899562A - A kind of preparation method of flower-shaped hierarchy titanium dioxide gas-phase photocatalysis material - Google Patents
A kind of preparation method of flower-shaped hierarchy titanium dioxide gas-phase photocatalysis material Download PDFInfo
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- CN107899562A CN107899562A CN201711193028.1A CN201711193028A CN107899562A CN 107899562 A CN107899562 A CN 107899562A CN 201711193028 A CN201711193028 A CN 201711193028A CN 107899562 A CN107899562 A CN 107899562A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 239000000463 material Substances 0.000 title claims abstract description 52
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 32
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 24
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000010936 titanium Substances 0.000 claims abstract description 15
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011148 porous material Substances 0.000 claims abstract description 10
- 150000001412 amines Chemical class 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 16
- 238000001354 calcination Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 5
- 241000673705 Viburnum tinus Species 0.000 claims description 4
- 238000005452 bending Methods 0.000 claims description 2
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical group [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000011941 photocatalyst Substances 0.000 claims description 2
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims 1
- 238000005119 centrifugation Methods 0.000 claims 1
- 229960001124 trientine Drugs 0.000 claims 1
- 238000006555 catalytic reaction Methods 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 3
- 239000003960 organic solvent Substances 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 24
- 235000010215 titanium dioxide Nutrition 0.000 description 24
- 229960005196 titanium dioxide Drugs 0.000 description 23
- 239000007789 gas Substances 0.000 description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- -1 Titanium alkoxides Chemical class 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000015572 biosynthetic process 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
- 238000004140 cleaning Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000004817 gas chromatography Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- 238000012549 training Methods 0.000 description 3
- 229910052724 xenon Inorganic materials 0.000 description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 3
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- VOZKAJLKRJDJLL-UHFFFAOYSA-N 2,4-diaminotoluene Chemical compound CC1=CC=C(N)C=C1N VOZKAJLKRJDJLL-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
- 238000001198 high resolution scanning electron microscopy Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000003911 water pollution Methods 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- B01J35/39—
-
- B01J35/51—
-
- B01J35/613—
-
- B01J35/615—
-
- B01J35/647—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/10—Single element gases other than halogens
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention discloses a kind of preparation method of flower-shaped hierarchy titanium dioxide gas-phase photocatalysis material.This method hydrolyzes titanium source under organic solvent effect, porous function titanic oxide material is synthesized by solvent thermal reaction using organic molecule amine surfactants as template.Advantage of the invention is that preparation method is quick and easy, it is repeated high, and titanic oxide material prepared by this method has similar flower-shaped porous hierarchical structure, it is with high-specific surface area and abundant pore passage structure, gas phase catalysis excellent performance, and catalyst repeats utilization, there is important application value in terms of VOC is removed.
Description
Technical field
The present invention relates to catalysis material synthesis technical field, and in particular to a kind of flower-shaped hierarchy titanium dioxide gas phase
The preparation method of catalysis material.
Background technology
Titanium dioxide is a kind of important semi-conducting material, there is its unique physical and chemical properties.Titanium dioxide exists
The fields such as photocatalysis, solar cell, lithium ion battery have a wide range of applications, and cause the concern of people.Research shows,
Titanium dioxide is being used to purification air, degradation of organic substances, administers water pollution etc., has well as photochemical catalyst
Effect.
The specific surface area of increase titanium dioxide can improve its photocatalysis performance, be due to that big specific surface area adds dioxy
Change the contact area of titanium and adsorbent and add the avtive spot quantity of reaction.And by increasing the ratio surface of titanium dioxide
Accumulate to improve its photocatalytic, mainly there are two kinds of approach：First, the small titanium dioxide granule of size is prepared, particle size is got over
Small, its specific surface area is bigger, this approach is mainly with the P25 type commercial titanium dioxides powder of Degussa companies production using the most
Extensively, its specific surface area is 50 (± 15) m2/g；Second, by preparing poriferous titanium dioxide material, due to the presence in duct, two
The specific surface area increase of titanium oxide, its photocatalysis performance are also greatly improved.
But current titanium dioxide gas-phase photocatalysis material preparation method is complicated, is difficult to synthesize on a large scale, cannot
Meet the needs of existing industry.Therefore there is an urgent need for a kind of technique is simple, the flower with high gas phase catalysis activity that can be synthesized on a large scale
The preparation method of shape porous hierarchical structure titanium dioxide gas-phase photocatalysis material.
The content of the invention
Based on above the deficiencies in the prior art, technical problem solved by the invention is to provide technique simple, can advise greatly
The preparation method of the flower-shaped porous hierarchical structure titanium dioxide gas-phase photocatalysis material with high gas phase catalysis activity of mould synthesis.
In order to solve the above technical problem, the present invention provides a kind of flower-shaped hierarchy titanium dioxide gas-phase photocatalysis material
Preparation method, a kind of preparation method of flower-shaped hierarchy titanium dioxide gas-phase photocatalysis material, it is characterised in that comprising such as
Lower step：
Step 1: by solvent and template according to 60mL：10-15min is at the uniform velocity stirred in the ratio mixing of 30-240 μ L；
Step 2: adding titanium source in the solution obtained to step 1, the ratio of the titanium source and template is 2-4mL：30-
240 μ L, uniform stirring 20-30min；
12-24h is reacted Step 3: reaction solution obtained by step 2 is placed under the conditions of 200 DEG C -220 DEG C；
Step 4: step 3 products therefrom is filtered to take filter residue, with washes of absolute alcohol and centrifuge, repeated washing,
Centrifugal process at least three times, is then dried in 40-70 DEG C of condition；
Step 5: step 4 products therefrom is obtained into the flower-shaped hierarchy gas phase two in 300-500 DEG C of calcining
Titania photocatalyst material.
As the preferred of above-mentioned technical proposal, flower-shaped hierarchy titanium dioxide gas-phase photocatalysis material provided by the invention
Preparation method further comprise the part or all of of following technical characteristic：
As the improvement of above-mentioned technical proposal, the template is polyamino organic molecule amine.
As the improvement of above-mentioned technical proposal, the polyamino organic molecule amine is selected from diethyl triamine, triethyl group four
Amine or tetraethylenepentamine.
As the improvement of above-mentioned technical proposal, the titanium source is butyl titanate.
As the improvement of above-mentioned technical proposal, the preparation of the flower-shaped hierarchy titanium dioxide gas-phase photocatalysis material
Method, it is characterised in that：The solvent is isopropanol.
As the improvement of above-mentioned technical proposal, the titanium dioxide gas-phase photocatalysis material is by the thick bending nanometers of 4-8nm
The micron ball of piece composition, has the flower-shaped hierarchy of class laurustinus, according to its different specific surface area of calcining heat up to 77-
210m2/ g, pore size 5.9-8.9nm.
Before reaction starts, Titanium alkoxides and polyamino small molecule amine are dispersed in isopropanol, as temperature raises, isopropyl
Etherification reaction occurs for alcohol, and a small amount of water of generation promotes Titanium alkoxides hydrolysis Ti (OH)4, Ti (OH)4Rapid polycondensation generation surface is rich
TiO containing-OH2Spheric granules.With the progress of reaction, Ti (OH)4On spheric granules surface and the amino of polyamino small molecule amine
(-NH2,-NH-) it is mutually bonded, and then form organic amine-titanium compound of a large amount of laminated structures in particle surface, be built into tool
There is the presoma of class silk ball floral structure, this presoma is converted into sheet TiO through calcining rear surface sheet-like composite2, silk ball is flower-shaped
Structure be maintained, that is, prepare we needs the flower-shaped hierarchy titanium dioxide gas-phase photocatalysis material of class silk ball.
Compared with prior art, technical scheme has the advantages that：Having been synthesized using hydro-thermal method is had
The flower-shaped titanic oxide material of porous hierarchical structure, synthetic method is simple, and cost is low, can largely synthesize, raw suitable for industry
Production.This flower-shaped titanic oxide material of porous hierarchical structure has very high specific surface area and abundant pore passage structure, and has
Preferable gas-phase photocatalysis performance, the speed of gas phase degraded acetone are about 1.3 times of commercial titanium dioxide material P25.
Advantage of the invention is that preparation method is quick and easy, repeatability is high, and titanium dioxide titanium prepared by this method
The microballoon that material is made of curved nanometer sheet, has the flower-shaped porous hierarchical structure of similar silk ball, it is with high-specific surface area
With abundant pore passage structure, third is can be repeated for after the gas that gas phase catalysis excellent performance, and catalyst remove absorption through high temperature
Ketone gas is degraded, and has important application value in terms of VOC is removed.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, and in order to allow the above and other objects, features and advantages of the present invention can
Become apparent, below in conjunction with preferred embodiment, describe in detail as follows.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, will simply it be situated between to the attached drawing of embodiment below
Continue.
Fig. 1 (a) is that the high-resolution SEM of the flower-shaped titanic oxide material embodiment 1 of porous hierarchical structure schemes；
Fig. 1 (b) is that the low resolution SEM of the flower-shaped titanic oxide material embodiment 1 of porous hierarchical structure schemes, attached drawing in the upper right corner
For laurustinus；
Fig. 2 is the XRD diagram of the flower-shaped titanic oxide material of porous hierarchical structure；
Fig. 3 (a) is nitrogen adsorption-desorption curve figure of the flower-shaped titanic oxide material of porous hierarchical structure；
Fig. 3 (b) is the graph of pore diameter distribution of the flower-shaped titanic oxide material of porous hierarchical structure；
Fig. 4 is the flower-shaped titanic oxide material of porous hierarchical structure and the gas phase catalysis degraded acetone performance comparison figure of P25.
Embodiment
The following detailed description of the present invention embodiment, its as part of this specification, by embodiment come
Illustrate the principle of the present invention, other aspects of the present invention, feature and its advantage will become apparent by the detailed description.
Embodiment 1
(1) take the isopropanol of 60mL to pour into ptfe autoclave, add 60 μ L diethyl triamine conducts inside
Template, at the uniform velocity stirs 10min.
(2) after 10min, 3mL butyl titanates, uniform stirring 20min are added into solution obtained in (1).
(3) after the completion of stirring, the magneton in reaction kettle is taken out, packaged reaction kettle, is put into air dry oven, temperature
It is set as 200 DEG C, insulation reaction 24h.
(4) reaction kettle is taken out from air dry oven, outwells the isopropanol in kettle, obtains yellow solid, absolute ethyl alcohol is clear
Product is washed, the speed of 8000r/min centrifuges 10min, repeats this step wash products three times, and product is put into 40 after cleaning
Dried in DEG C baking oven.
(5) dried product is obtained the flower-shaped hierarchy gas phase titanium-dioxide photo and urged in 400 DEG C of calcinings
Agent material.
(6) the above-mentioned products of 10mg are scattered in 2mL ethanol solutions, ultrasonic disperse 15min, resulting solution is placed in glass training
Support in ware, 40 DEG C of dry 12h, gas phase test sample is made.
(7) sample in (6) is placed in sealing reactor, injects 2 μ L acetone solns, the xenon lamp of 300W with syringe
According to using gas-chromatography fid detector, detection VOC gas acetone concentrations change.
Embodiment 2
(1) take 60mL isopropanols to pour into ptfe autoclave, add 240 μ L diethyl triamines inside as mould
Plate agent, at the uniform velocity stirs 10min.
(2) after 10min, 4mL butyl titanates, uniform stirring 20min are added into solution obtained in (1).
(3) after the completion of stirring, the magneton in reaction kettle is taken out, packaged reaction kettle, is put into air dry oven, temperature
It is set as 200 DEG C, insulation reaction 24h.
(4) reaction kettle is taken out from air dry oven, outwells the isopropanol in kettle, obtains yellow solid, absolute ethyl alcohol is clear
Product is washed, the speed of 8000r/min centrifuges 10min, repeats this step wash products three times, and product is put into 50 after cleaning
Dried in DEG C baking oven.
(5) dried product is obtained the flower-shaped hierarchy gas phase titanium-dioxide photo and urged in 300 DEG C of calcinings
Agent material.
(6) the above-mentioned products of 10mg are scattered in 2mL ethanol solutions, ultrasonic disperse 15min, resulting solution is placed in glass training
Support in ware, 40 DEG C of dry 12h, gas phase test sample is made.
(7) sample in (6) is placed in sealing reactor, injects 2 μ L acetone solns, the xenon lamp of 300W with syringe
According to using gas-chromatography fid detector, detection VOC gas acetone concentrations change.
Embodiment 3
(1) take 60mL isopropanols to pour into ptfe autoclave, add 30 μ L diethyl triamines inside as mould
Plate agent, at the uniform velocity stir 10min.
(2) after 10min, 2mL butyl titanates, uniform stirring 20min are added into solution obtained in (1).
(3) after the completion of stirring, the magneton in reaction kettle is taken out, packaged reaction kettle, is put into air dry oven, temperature
It is set as 200 DEG C, insulation reaction 24h.
(4) reaction kettle is taken out from air dry oven, outwells the isopropanol in kettle, obtains yellow solid, absolute ethyl alcohol is clear
Product is washed, the speed of 8000r/min centrifuges 10min, repeats this step wash products three times, and product is put into 60 after cleaning
Dried in DEG C baking oven.
(5) dried product is obtained the flower-shaped hierarchy gas phase titanium-dioxide photo and urged in 500 DEG C of calcinings
Agent material.
(6) the above-mentioned products of 10mg are scattered in 2mL ethanol solutions, ultrasonic disperse 15min, resulting solution is placed in glass training
Support in ware, 40 DEG C of dry 12h, gas phase test sample is made.
(7) sample in (6) is placed in sealing reactor, injects 2 μ L acetone solns, the xenon lamp of 300W with syringe
According to using gas-chromatography fid detector, detection VOC gas acetone concentrations change.
The SEM figures of the flower-shaped titanic oxide material of porous hierarchical structure prepared by Fig. 1 this implementation of position 1, Fig. 2 is XRD diagram,
Fig. 3 is nitrogen adsorption curve map and graph of pore diameter distribution, and Fig. 4 is the flower-shaped titanic oxide material of porous hierarchical structure and the gas phase of P25
Catalytic degradation acetone performance comparison figure.
As can be seen from Figure 1 the flower-shaped titanic oxide material of large area porous hierarchical structure prepared, wherein titanium dioxide
Titanium is spherical, and size is more homogeneous, and particle diameter is about 1 μm, and bead is made of curved nanometer sheet, is had similar to as shown in drawings
Laurustinus flower-shaped hierarchy.Fig. 2 is XRD diagram, it is seen that the titanic oxide material prepared is anatase crystal, and Fig. 3 is
The nitrogen adsorption curve map and graph of pore diameter distribution of the flower-shaped titanic oxide material of porous hierarchical structure, are to adsorb-take off wherein in left figure
Attached curve, right figure are graph of pore diameter distribution.The flower-shaped titanic oxide material of porous hierarchical structure for understanding to prepare by test result
Specific surface area is 126.5m2/ g, pore size 8.9nm, it was demonstrated that a process for preparing have the porous of high-specific surface area
The flower-shaped titanic oxide material of hierarchy.Fig. 4 be embodiment one prepared by the flower-shaped titanic oxide material of porous hierarchical structure with
The gas phase catalysis degraded acetone performance comparison figure of P25, by formula ln (C0/ C)=kt calculating gained kP25=0.0386min-1, k400
=0.0493min-1, the gas phase catalysis degraded acetone reaction rate constant of our institute's prepared materials is about 1.3 times of P25.It is different real
The experimental data for applying example shows that the laminated structure of the increase material surface with the reaction time constantly increases；Increase small point of polyamino
The usage amount of sub- amine, can form flower-like structure in the short period；With the increase of small molecule amine amino quantity used, formation
Flower-like structure surface lamella constantly increases, material specific surface area increase；After 300 degree of calcinings, unbodied material is converted into sharp
Titanium ore phase, as calcining heat increases the ratio increase of Anatase in material, when calcining heat reaches 600 degree, produces golden red
Stone phase titanic oxide, the sample after 400 degree of calcinings have the optimal effect for removing acetone VOC, the sample of same calcination condition
In, the high sample of specific surface area has best catalytic activity.
Each raw material cited by the present invention, and bound, the section value of each raw material of the present invention, and technological parameter
Bound, the section value of (such as temperature, time) can realize the present invention, embodiment numerous to list herein.
The above is the preferred embodiment of the present invention, cannot limit the right model of the present invention with this certainly
Enclose, it is noted that for those skilled in the art, without departing from the principle of the present invention, may be used also
To make some improvement and variation, these are improved and variation is also considered as protection scope of the present invention.
Claims (6)
1. a kind of preparation method of flower-shaped hierarchy titanium dioxide gas-phase photocatalysis material, it is characterised in that include following step
Suddenly：
Step 1: by solvent and template according to 60mL：10-15min is at the uniform velocity stirred in the ratio mixing of 30-240 μ L；
Step 2: adding titanium source in the solution obtained to step 1, the ratio of the titanium source and template is 2-4mL：30-240μ
L, uniform stirring 20-30min；
20-24h is reacted Step 3: reaction solution obtained by step 2 is placed under the conditions of 200 DEG C -220 DEG C；
Step 4: step 3 products therefrom is filtered to take filter residue, with washes of absolute alcohol and centrifuge, repeated washing, centrifugation
Process at least three times, is then dried in 40-70 DEG C of condition；
Step 5: step 4 products therefrom is obtained into the flower-shaped hierarchy gas phase titanium dioxide in 300-500 DEG C of calcining
Titanium photocatalyst material.
2. the preparation method of flower-shaped hierarchy titanium dioxide gas-phase photocatalysis material as claimed in claim 1, its feature exist
In：The template is polyamino organic molecule amine.
3. the preparation method of flower-shaped hierarchy titanium dioxide gas-phase photocatalysis material as claimed in claim 2, its feature exist
In：The polyamino organic molecule amine is selected from diethyl triamine, trientine or tetraethylenepentamine.
4. the preparation method of flower-shaped hierarchy titanium dioxide gas-phase photocatalysis material as claimed in claim 1, its feature exist
In：The titanium source is butyl titanate.
5. the preparation method of flower-shaped hierarchy titanium dioxide gas-phase photocatalysis material as claimed in claim 1, its feature exist
In：The solvent is isopropanol.
6. the preparation method of the flower-shaped hierarchy titanium dioxide gas-phase photocatalysis material as described in claim 1-5, its feature
It is：The titanium dioxide gas-phase photocatalysis material is the micron ball being made of the thick bending nanometer sheets of 4-8nm, has class laurustinus
Flower-shaped hierarchy, specific surface area 77-210m2/ g, pore size 5.9-8.9nm.
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| CN201711193028.1A CN107899562B (en) | 2017-11-24 | 2017-11-24 | Preparation method of flower-shaped hierarchical titanium dioxide gas-phase photocatalytic material |
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| CN201711193028.1A CN107899562B (en) | 2017-11-24 | 2017-11-24 | Preparation method of flower-shaped hierarchical titanium dioxide gas-phase photocatalytic material |
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| CN107899562A true CN107899562A (en) | 2018-04-13 |
| CN107899562B CN107899562B (en) | 2020-08-04 |
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| CN110180542A (en) * | 2019-04-01 | 2019-08-30 | 武汉理工大学 | A kind of titanium dioxide/graphene/metal simple-substance tri compound catalysis material and photo-reduction preparation method |
| CN112604652A (en) * | 2019-12-20 | 2021-04-06 | 厦门市建筑科学研究院有限公司 | Composite material and preparation method thereof |
| CN114632516A (en) * | 2022-01-25 | 2022-06-17 | 北京科技大学 | Nano-sheet catalyst for catalytic oxidation of VOC and preparation and application methods thereof |
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| CN104860348A (en) * | 2015-04-22 | 2015-08-26 | 武汉理工大学 | Nanosheet-constructed titanium dioxide, and preparation method and application thereof |
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| CN110180542B (en) * | 2019-04-01 | 2022-06-03 | 武汉理工大学 | Titanium dioxide/graphene/metal simple substance ternary composite photocatalytic material and photoreduction preparation method |
| CN112604652A (en) * | 2019-12-20 | 2021-04-06 | 厦门市建筑科学研究院有限公司 | Composite material and preparation method thereof |
| CN112604652B (en) * | 2019-12-20 | 2022-08-12 | 厦门市建筑科学研究院有限公司 | Composite material and preparation method thereof |
| CN114632516A (en) * | 2022-01-25 | 2022-06-17 | 北京科技大学 | Nano-sheet catalyst for catalytic oxidation of VOC and preparation and application methods thereof |
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