CN107803194A - A kind of Fast back-projection algorithm Ti3+/TiO2The method of photochemical catalyst - Google Patents
A kind of Fast back-projection algorithm Ti3+/TiO2The method of photochemical catalyst Download PDFInfo
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- CN107803194A CN107803194A CN201710944926.XA CN201710944926A CN107803194A CN 107803194 A CN107803194 A CN 107803194A CN 201710944926 A CN201710944926 A CN 201710944926A CN 107803194 A CN107803194 A CN 107803194A
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- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000003054 catalyst Substances 0.000 title claims abstract description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000010936 titanium Substances 0.000 claims abstract description 23
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000005516 engineering process Methods 0.000 claims abstract description 7
- 229910000048 titanium hydride Inorganic materials 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 4
- 230000005855 radiation Effects 0.000 claims description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 150000003609 titanium compounds Chemical class 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000004408 titanium dioxide Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 229910010280 TiOH Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012538 light obscuration Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000006862 quantum yield reaction Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000005457 Black-body radiation Effects 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910009973 Ti2O3 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002883 imidazolyl group Chemical group 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000007144 microwave assisted synthesis reaction Methods 0.000 description 1
- 238000000120 microwave digestion Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001443 photoexcitation Effects 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- GQUJEMVIKWQAEH-UHFFFAOYSA-N titanium(III) oxide Chemical compound O=[Ti]O[Ti]=O GQUJEMVIKWQAEH-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
-
- 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
-
- 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
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/346—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Plasma & Fusion (AREA)
- Optics & Photonics (AREA)
- Electromagnetism (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of Fast back-projection algorithm Ti3+/TiO2The method of photochemical catalyst, belong to photocatalysis technology field.Utilize TiO or TiH2It is presoma etc. low price titanium compound, Ti is controlled by microwave-hydrothermal method2+To Ti3+Oxidation, Fast back-projection algorithm Ti3+/TiO2Photochemical catalyst.
Description
Technical field
The present invention relates to the photocatalysis technology of field of environmental improvement, more particularly to a kind of Fast back-projection algorithm Ti3+/TiO2Photocatalysis
The method of agent.
Background technology
By using the solar energy of low energy densities, conductor photocatalysis material can realize that degradation of contaminant etc. is advanced
Oxidizing process and photodissociation aquatic products hydrogen etc. produce clean energy resource process, have huge application potential.In recent decades, both at home and abroad
Researcher to TiO2Based on photochemical catalyst carried out substantial amounts of research, and achieve huge progress.But still
So there is the problem of the following aspects：(1) spectral response range is narrower, TiO2As a kind of broadband semiconductor, its forbidden band
Width is 3.2 eV, and this just determines that it can only be utilized and accounts for ultraviolet light of the solar spectrum less than 5%, to the utilization rate ratio of solar energy
It is relatively low.(2) quantum yield is relatively low, TiO2In photoexcitation process, light induced electron and hole-recombination probability are higher, directly results in
Quantum yield in catalytic process is relatively low.Under this background, there is an urgent need to improve the quantum efficiency of titanium dioxide and extend it
Photoresponse scope.
In the recent period, numerous researchers, which report, utilizes Ti3+Ion is in TiO2The mode of lattice auto-dope, TiO can be made2Obtain
Obtain visible light catalysis activity well.Wherein, Zuo et al. reduces to obtain Ti using one-step method3+/TiO2Material, with metatitanic acid isopropyl
Ester is placed in for the presoma of titanium in the ethanol solution of ethyl imidazol(e) addition, and 500 are heated under the conditions of air atmosphereoC processing 5 is small
When, the final titania powder sample for obtaining blueness.They think that imidazole ring reacts what is formed with oxygen in the reaction
Reducibility gas CO and NO, in Ti3+Key effect is played in auto-dope titanium dioxide building-up process, it is as reducing agent Ti4+
It is reduced to Ti3+。
However, by Ti4+It is changed into Ti3+Reducing process prepare Ti3+/TiO2Have some limitations.On the one hand, from electricity
TiO is seen on electrode potential2(s)→Ti2O3(s) redox potential is relatively low (E=- 0.56 V), so high energy particle must be used
The methods of bombardment, reducing atmosphere processing or vacuum at high temperatures are annealed just can guarantee that Ti4+It is changed into Ti3+.Secondly, this reduction
Method has strict requirements to Preparation equipment and operating process, so as to increase the difficulty of preparation, it is impossible to meets a wide range of production.Separately
On the one hand, because electrode potential is understood, Ti2+→Ti3+Redox potential (E=- 0.37V) be less than Ti4+→Ti3+Oxidation
Reduction potential (+0.10V), aoxidized by Low-valent Titanium and prepare Ti3+The reaction of defect has spontaneous.Therefore, we can be by low
Valency titanium precursor thing prepares Ti3+/TiO2。
The content of the invention
The present invention provides a kind of Fast back-projection algorithm Ti3+/TiO2The method of photochemical catalyst, rung to quickly obtain with visible ray
The TiO answered2Photochemical catalyst.
The preparation method of the photochemical catalyst utilizes TiO, TiH2It is auxiliary in microwave condition etc. low price titanium source as titanium precursors
Help and Ti is quickly obtained under thermal and hydric environment3+/TiO2.Its technical scheme comprises the following steps：
（1）By a certain amount of low price titanium precursors TiO or TiH2In the HCl solution being distributed to, ultrasonic disperse；
（2）Mixed liquor is transferred in polytetrafluoroethylene (PTFE) reaction body, is put into after sealing in micro-wave digestion/synthesis reactor
（MDS-6, Shanghai Xin Yi Co., Ltds）, with 180oC takes out after reacting 1 hour；
（3）After the powder deionized water and absolute ethyl alcohol of collection respectively cleaning, drying in oven is placed in.
Preparing Ti3+/TiO2During, TiO can react with HCl produces Ti3+Ion, and then Ti3+Ion and water
Reaction is converted into TiOH2+Intermediate, and TiOH2+Intermediate and the dissolved oxygen reaction generation TiO in water2Once TiO2Nucleus
Formed, remaining Ti in solution3+Ion can be promptly around the nucleus growth.
TiO made from this method2In light blue, and common TiO2White, DRS spectrum analyses show the catalyst
The cut-off obvious red shift in side is absorbed, and a new absorption band occurs in visible region.Due to the electronics quilt in Lacking oxygen
Adjacent Ti4+Attracted, Ti is formed in the localized modes at Ti centers3+Auto-dope, and substantial amounts of Lacking oxygen or Ti3+Auto-dope
Can be in TiO2Conduction band below or valence band above introduce new energy level, TiO can be significantly changed2Light absorbs situation.
Beneficial effects of the present invention are embodied in following three aspects：1. low price titanium compound is utilized, with the oxidation side of simplicity
Formula prepares Ti3+/TiO2.2. the time required for catalyst synthesis can be greatly lowered using Microwave-assisted synthesis method.3.
In building-up process, Ti3+New energy level can be introduced in the forbidden band of titanium dioxide with Lacking oxygen, lifts TiO2Sample is to visible ray
Absorb and respond.
Brief description of the drawings
Fig. 1 is with TiO（It is left）And TiH2（It is right）For presoma, Ti is synthesized3+/TiO2The photo in kind of sample.
Fig. 2 is with TiH2For presoma, Ti is synthesized3+/TiO2The XRD spectra of sample.
Fig. 3 Degussas P25 and Ti3+/TiO2The UV, visible light extinction spectrum of two kinds of powder samples.
Embodiment
The present invention is elaborated with reference to the accompanying drawings and examples.
Embodiment 1
By 250 mg TiH2It is dispersed in 15mL 3M HCl solution, ultrasonic disperse 5 minutes.Mixed liquor is transferred to 70 mL
Polytetrafluoroethylene (PTFE) reacting tank body in, with 180 in microwave reactor (MDS-6, the new instrument in Shanghai)oC takes out after reacting 1 hour,
After the powder deionized water and absolute ethyl alcohol of collection are respectively cleaned three times, it is placed in 80 in baking ovenoC is dried.
Compared under conventional heating pattern, heat exchange pattern driving chemical reaction of the thermal source dependent on black body radiation will
Energy is conducted to the mode of reactant molecule from heating source, and the particularity of microwave heating is the globality heating in its medium, this
Energy can be directly conducted to reactant molecule by kind mode.It is indicated above that the crystal growth rate under microwave radiation technology heat condition
Far above under conventional heat condition, so Microwave-assisted firing can improve reaction combined coefficient and save the energy.Wherein Fig. 1 right is to be somebody's turn to do
The digital photograph of sample, by the Ti of the oxidized preparation of low price titanium source3+/TiO2Sample presents light blue.To Ti3+/TiO2Carry out XRD
Test（Fig. 2）After show TiO2Sample is with Rutile Type（JCPDS card No. 03-065-0191）It is leading, comprising micro-
The brockite of amount.By commercial catalyst Degussa P25 and Ti3+/TiO2The UV, visible light extinction spectrum of two kinds of powder samples（Fig. 3
It is shown）Understand, compared to P25 samples, Ti3+/TiO2Sample in 400nm to having wider ultraviolet/visible light absorption band between 1000nm,
Expand absorption region of the titanium dioxide in visible region.
Embodiment 2
250 mg TiO is dispersed in 15mL 3M HCl solution, ultrasonic disperse 5 minutes.Mixed liquor is transferred to 70 mL's
In polytetrafluoroethylene (PTFE) reacting tank body, with 200 in microwave reactor (MDS-6, the new instrument in Shanghai)oC takes out after reacting 1 hour, will
After the powder deionized water and absolute ethyl alcohol of collection are respectively cleaned three times, it is placed in 80 in baking ovenoC is dried, and obtains sample Ti3+/
TiO2。
Claims (5)
1. the present invention provides a kind of Fast back-projection algorithm Ti3+/TiO2The method of photochemical catalyst, to quickly obtain with visible light-responded
TiO2Photochemical catalyst.
2. the preparation method of photochemical catalyst utilizes lower valency titanium source according to claim 1（TiO、TiH2）As titanium precursors.
3. the preparation method of photochemical catalyst uses microwave radiation technology hydrothermal synthesis method according to claim 1.
4. according to claim 3 during microwave radiation technology hydrothermal synthesis method, temperature is 150 DEG C~200 DEG C.
5. according to claim 3 during microwave radiation technology hydrothermal synthesis method, polytetrafluoroethylene (PTFE) reaction pressure tank is 1.3 MPa
~2.2 MPa.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710944926.XA CN107803194A (en) | 2017-10-12 | 2017-10-12 | A kind of Fast back-projection algorithm Ti3+/TiO2The method of photochemical catalyst |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710944926.XA CN107803194A (en) | 2017-10-12 | 2017-10-12 | A kind of Fast back-projection algorithm Ti3+/TiO2The method of photochemical catalyst |
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| Publication Number | Publication Date |
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| CN107803194A true CN107803194A (en) | 2018-03-16 |
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| CN201710944926.XA Pending CN107803194A (en) | 2017-10-12 | 2017-10-12 | A kind of Fast back-projection algorithm Ti3+/TiO2The method of photochemical catalyst |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043716A (en) * | 2013-01-06 | 2013-04-17 | 中国检验检疫科学研究院 | Preparation method of titanium dioxide nanosphere |
| CN103641163A (en) * | 2013-11-28 | 2014-03-19 | 武汉大学 | Preparation method of nano TiO2 powder and method for preparing oxygen gas indicator from nano TiO2 powder |
| CN104148041A (en) * | 2014-04-30 | 2014-11-19 | 上海师范大学 | Anatase phase TiO2 cubic photocatalyst as well as preparation method and application thereof |
-
2017
- 2017-10-12 CN CN201710944926.XA patent/CN107803194A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043716A (en) * | 2013-01-06 | 2013-04-17 | 中国检验检疫科学研究院 | Preparation method of titanium dioxide nanosphere |
| CN103641163A (en) * | 2013-11-28 | 2014-03-19 | 武汉大学 | Preparation method of nano TiO2 powder and method for preparing oxygen gas indicator from nano TiO2 powder |
| CN104148041A (en) * | 2014-04-30 | 2014-11-19 | 上海师范大学 | Anatase phase TiO2 cubic photocatalyst as well as preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 裴增夏: "宽禁带光催化剂的缺陷调控、机理及其应用", 《中国优秀硕士学位论文全文数据库 工程科技I缉》 * |
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Application publication date: 20180316 |