CN108144596B - A kind of 3DOM-TiO that window is controllable2Photochemical catalyst preparation method - Google Patents
A kind of 3DOM-TiO that window is controllable2Photochemical catalyst preparation method Download PDFInfo
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- CN108144596B CN108144596B CN201711468610.4A CN201711468610A CN108144596B CN 108144596 B CN108144596 B CN 108144596B CN 201711468610 A CN201711468610 A CN 201711468610A CN 108144596 B CN108144596 B CN 108144596B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000004793 Polystyrene Substances 0.000 claims abstract description 30
- 229920002223 polystyrene Polymers 0.000 claims abstract description 24
- 239000013078 crystal Substances 0.000 claims abstract description 10
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 3
- 239000000084 colloidal system Substances 0.000 claims abstract description 3
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 21
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000011324 bead Substances 0.000 claims description 8
- 239000000839 emulsion Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 6
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- 239000003292 glue Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000006227 byproduct Substances 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000005429 filling process Methods 0.000 claims description 3
- 238000003837 high-temperature calcination Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 239000003999 initiator Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 239000008340 white lotion Substances 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 238000007146 photocatalysis Methods 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 7
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000001338 self-assembly Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- APQHKWPGGHMYKJ-UHFFFAOYSA-N Tributyltin oxide Chemical compound CCCC[Sn](CCCC)(CCCC)O[Sn](CCCC)(CCCC)CCCC APQHKWPGGHMYKJ-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- 241001062009 Indigofera Species 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 229920006389 polyphenyl polymer Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000005303 weighing Methods 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
- 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F112/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F112/02—Monomers containing only one unsaturated aliphatic radical
- C08F112/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F112/06—Hydrocarbons
- C08F112/08—Styrene
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of 3DOM-TiO that window is controllable2The preparation of photochemical catalyst, comprising steps of the synthesis of polystyrene, the preparation of polystyrene colloid crystal template (PS) and the 3DOM-TiO for having different size window light2The preparation of photochemical catalyst.The beneficial effects of the present invention are: the preparation method is relatively simple, preparation condition is easy to control, the controllable 3DOM-TiO of prepared window2Photochemical catalyst has many advantages, such as without secondary pollution, and photocatalysis efficiency is high, has certain application value.
Description
Technical field
The present invention relates to the TiO of a kind of pair of three-dimensional order pore structure2The preparation of window size regulation, belongs to photocatalysis technology
Field.This photochemical catalyst can efficiently use the ultraviolet light in sunlight, to improve photocatalysis efficiency.
Background technique
In numerous materials, TiO2As a kind of conventional semiconductors catalysis material, not by chemical property stabilization, illumination
Photoetch occurs, without the unique advantages such as overt toxicity, at low cost, it is considered to be one of most promising catalysis material.However
Photo-generate electron-hole pairs are easy to generate in conjunction in order to solve the problems, such as that semiconductor material is shared, we mainly pass through simply
Efficient means are in TiO2Material internal realizes controllably constructing for three-dimensional order pore structure, while from structure and surface chemical property
On studied, further enhance its light absorption in UV light region, improve photocatalytic activity.
Using polystyrene (PS) ball of self assembly as three-dimensional ordered macroporous TiO2(3DOM-TiO2) hard template, by filling out
Fill TiO2Precursor solution prepares the 3DOM-TiO with different connecting holes aperture2Catalysis material.Pass through SEM, TEM, XRD
Equal characterization methods, it was demonstrated that macropore and connecting hole aperture can be well controlled.
This patent mainly changes PS ball contact area by way of change the self assembly of PS ball, to control 3DOM-
TiO2Connection window diameter.The related photocatalysis rule of this window size can be other three with interconnecting pore structure
It ties up material and reference is provided.
Summary of the invention
The technical problem to be solved by the present invention is based on the above issues, the present invention provides a kind of 3DOM- that window is controllable
TiO2Preparation method.
The present invention solves a technical solution used by its technical problem: the controllable 3DOM-TiO of window2Preparation side
Method carries out as steps described below:
(1) synthesis of polystyrene: using styrene as raw material, PVP K-30 (PVP, molecular weight 40000)
Make catalyst and initiator respectively with ammonium persulfate (APS), under N2 protection, 70 DEG C of oil bath reaction 15h can obtain milky polyphenyl
Vac emulsion；
(2) preparation of polystyrene colloid crystal template (PS): end of reaction, by product (white emulsion) natural cooling
To room temperature, polystyrene emulsion is centrifuged with natural subsidence, high speed and ultrahigh rotating speed respectively, after will centrifugation product ultrasonic disperse in second
Alcohol is placed in 40 DEG C of oil baths and dries, and obtains 1 μm of diameter or so, three kinds of PS bead templates being sequentially increased of contact area；
(3) there is the 3DOM-TiO of different size window light2The preparation of photochemical catalyst: this experiment uses colloidal crystal templates method
Prepare 3DOM-TiO2.The PS bead template of different centrifugal rotational speeds is soaked respectively in butyl titanate precursor liquid, is impregnated, is taken out
Filter, drying, so that PS glue crystal template is fully filled.After the completion of filling process, by high-temperature calcination, PS template is removed, is obtained
The 3DOM-TiO in different connecting holes aperture2, and it is named as 3DOM-TiO2- S, 3DOM-TiO2- M, 3DOM-TiO2-L。
Further, reaction must be in N in the step (1)2Protection is lower to be carried out, and temperature is no more than 75 DEG C or low
In 65 DEG C；
Further, the high speed of the step (2) and ultrahigh speed are respectively 8000rpm and 16000rpm, when centrifugation
Between be 10min；
Further, butyl titanate precursor liquid is with molar ratio 1:10:0.6:7:2 difference in the step (3)
Measure butyl titanate (TBOT), ethyl alcohol, acetic acid, hydrochloric acid and distilled water, the vitreosol being mixed to form.
The controllable 3DOM-TiO of window2Photochemical catalyst application, be used for photocatalytic degradation methylenum careuleum (MB) solution, press
It is carried out according to following step:
It weighs 30mg catalyst to be put into test tube, 50mL 25mg/L MB solution is added, use 1000W mercury lamp as light source,
Carry out photocatalytic degradation reaction.Dark reaction time is 90min, and after illumination, every 5min takes time sample, is centrifuged, and then survey its suction
Luminosity.
The beneficial effects of the present invention are: the preparation method is relatively simple, preparation condition is easy to control, and prepared window is controllable
3DOM-TiO2Photochemical catalyst is environmentally protective high performance catalyst, and pollution-free, high catalytic efficiency applies valence with certain
Value.
Detailed description of the invention
The following further describes the present invention with reference to the drawings.
Fig. 1 is the scanning electron microscope (SEM) photograph for three kinds of PS crystalline substance glue pattern plates that the embodiment of the present invention 1 is prepared；
Fig. 2 is the controllable 3DOM-TiO of window that the embodiment of the present invention 1 is prepared2The scanning electron microscope (SEM) photograph of catalyst；
Fig. 3 is the controllable 3DOM-TiO of window that the embodiment of the present invention 1 is prepared2The X-ray diffractogram of catalyst；
Fig. 4 is the controllable 3DOM-TiO of window that the embodiment of the present invention 1 is prepared2Catalyst light degradation methylenum careuleum it is dense
Degree is with light application time variation diagram.
Specific embodiment
Presently in connection with specific embodiment, the invention will be further described, following embodiment be intended to illustrate invention rather than
Limitation of the invention further.
Embodiment 1
(1) PS bead is synthesized by traditional dispersion copolymerization method.Electronic balance weighs 8g styrene, and it is anhydrous to be dissolved in 100mL
In ethyl alcohol, solution A is obtained.Electronic balance weighs 0.06g PVP K-30 (PVP, molecular weight 40000) and 0.15g mistake
Ammonium sulfate (APS), is dissolved in 12mL deionized water, obtains solution B.Solution A is mixed with solution B, is transferred to 250mL three-necked flask
In, three-necked flask is put into oil bath pan and is preheated to 70 DEG C by drum nitrogen deoxygenation 40min, reaction time 15h.After completion of the reaction, will
Product (white emulsion) cooled to room temperature.
(2) after completion of the reaction, by product (white emulsion) cooled to room temperature, respectively with 0rpm (natural subsidence),
The centrifugation of 8000rpm, 16000rpm revolving speed, centrifugation product, which is placed in 40 DEG C of oil baths, dries, and obtains 1 μm of diameter or so, contact area
Three kinds of PS bead templates being sequentially increased.
(3) this experiment prepares 3DOM-TiO using colloidal crystal templates method2.Precursor solution is prepared, first with molar ratio
1:10:0.6:7:2 measures butyl titanate (TBOT), ethyl alcohol, acetic acid, hydrochloric acid and distilled water respectively, is mixed to form vitreosol.
The PS bead template of different centrifugal rotational speeds is soaked respectively in the vitreosol, impregnate 30min, after be removed by suction filtration under vacuum it is extra molten
Glue, dry 2h at 75 DEG C.It is multiple to repeat aforesaid operations, so that PS glue crystal template is fully filled.After the completion of filling process, pass through
High-temperature calcination removes PS template, when heating, temperature is first slowly increased to 300 DEG C, constant temperature 4h, then be warming up to 500 DEG C, constant temperature
6h finally makes system natural cooling, obtains the 3DOM-TiO in different connecting holes aperture2。
The three kinds of PS bead templates and window prepared using Japanese JSM-6360A type scanning electron microscope observation embodiment 1
The controllable 3DOM-TiO of mouth2The pattern of catalyst, scanning electron microscope (SEM) photograph is as depicted in figs. 1 and 2, it can be seen from the figure that this implementation
Three kinds of PS prepared by mode are small
The contact area of ball increases with self assembly speed and is increased, and 3DOM-TiO2Window be also gradually increased.
The controllable 3DOM-TiO of window prepared by embodiment 12The crystal phase structure of catalyst is by Rigaku D/max
2500PC rotation x-ray diffractometer analysis, wherein X-ray is Cu targetVoltage 40kV, electric current
100mA, step-length are 0.02 °, 5 °~80 ° of scanning range.For X ray diffracting spectrum as shown in figure 3, as seen from the figure, window is controllable
3DOM-TiO2For anatase.
By the controllable 3DOM-TiO of the window prepared in embodiment 12As photocatalyst for degrading methylene blue solution, the Central Asia
First indigo plant solution concentration is 25mg/L, takes 3DOM-TiO2Catalyst 30mg, it is flat that first dark reaction 90min makes solution reach adsorption-desorption
Weighing apparatus, then carries out ultraviolet catalytic reaction, is used as light source using 1000W mercury lamp, every 5min with dropper extraction 3ml reaction solution in from
In heart pipe, be put into supercentrifuge be centrifuged 3min after, after with ultraviolet specrophotometer measure photocatalysis effect.
The controllable 3DOM-TiO of window prepared by embodiment 12Catalyst is as shown in Figure 4 to the degradation property of methylenum careuleum.
From fig. 4, it can be seen that the 3DOM-TiO that window is controllable2It is better than common nano-TiO to the degradation effect of methylenum careuleum2Piece (TiO2), NPs and
And in 35min methylenum careuleum almost by 3DOM-TiO2- L degradation, 3DOM-TiO2Photocatalysis performance with window increase
And enhance.
It is enlightenment with embodiments of the invention described above, through the above description, relevant staff completely can be
In the range of this invention technical idea, various changes and amendments are carried out.The technical scope of this invention is simultaneously
The content being not limited on specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.
Claims (2)
1. a kind of 3DOM-TiO that window is controllable2Photochemical catalyst preparation method, which comprises the following steps:
(1) synthesis of polystyrene: using styrene as raw material, PVP K-30 and over cure that molecular weight is 40000
Sour ammonium, makees catalyst and initiator respectively, in N2Under protection, 70 DEG C of oil bath reaction 15h can obtain milky polystyrene emulsion；
(2) preparation of polystyrene colloid crystal template: end of reaction, by product as white lotion cooled to room temperature, respectively
With natural subsidence, high speed and ultrahigh rotating speed are centrifuged polystyrene emulsion, after centrifugation product ultrasonic disperse in ethyl alcohol is placed in 40
It is dried in DEG C oil bath, obtains 1 μm of diameter or so, three kinds of PS bead templates being sequentially increased of contact area；
(3) there is the 3DOM-TiO of different size window light2The preparation of photochemical catalyst: 3DOM- is prepared using colloidal crystal templates method
TiO2, the PS bead template of different centrifugal rotational speeds is soaked respectively in butyl titanate precursor liquid, is impregnated, is filtered, drying makes
It obtains PS glue crystal template to be fully filled, after the completion of filling process, by high-temperature calcination, removes PS template, obtain different connecting holes
The 3DOM-TiO in aperture2；
Butyl titanate precursor liquid is to measure four fourth of metatitanic acid respectively with 0.6 ﹕ of molar ratio 1 ﹕, 10 ﹕, 7 ﹕ 2 in the step (3)
Ester, ethyl alcohol, acetic acid, hydrochloric acid and distilled water, the vitreosol being mixed to form.
2. according to the method described in claim 1, it is characterized in that: the high speed and ultrahigh speed be respectively 8000rpm and
16000rpm, centrifugation time 10min.
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