CN104741134A - Preparation method of TiO2/ZnS two-layer composite nanotube array - Google Patents
Preparation method of TiO2/ZnS two-layer composite nanotube array Download PDFInfo
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- CN104741134A CN104741134A CN201410521312.7A CN201410521312A CN104741134A CN 104741134 A CN104741134 A CN 104741134A CN 201410521312 A CN201410521312 A CN 201410521312A CN 104741134 A CN104741134 A CN 104741134A
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- 239000002071 nanotube Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000002131 composite material Substances 0.000 title claims abstract description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title abstract 16
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 35
- 150000001875 compounds Chemical class 0.000 claims description 25
- 229910052782 aluminium Inorganic materials 0.000 claims description 15
- 239000004411 aluminium Substances 0.000 claims description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 14
- 238000009415 formwork Methods 0.000 claims description 13
- 230000003647 oxidation Effects 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 3
- 239000002243 precursor Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- 238000010335 hydrothermal treatment Methods 0.000 claims 1
- 239000010865 sewage Substances 0.000 abstract description 14
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 8
- 239000004065 semiconductor Substances 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 238000005286 illumination Methods 0.000 abstract description 2
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract description 2
- 230000002596 correlated effect Effects 0.000 abstract 1
- 231100000956 nontoxicity Toxicity 0.000 abstract 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 4
- 238000005215 recombination Methods 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000012855 volatile organic compound Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
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- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
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- 238000011084 recovery Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
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- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention relates to a preparation method of a TiO2/ZnS two-layer composite nanotube array. TiO2 is a broad-band-gap (3.2eV) semiconductor material and is a photocatalytic material researched intensively in multiple correlated fields due to the advantages such as strong oxidization capability, no photocorrosion after illumination, high catalytic activity, wide source, no toxicity and no harm, however, TiO2 also has the defects that the quantum efficiency is low, powder particles can be agglomerated and inactivated easily and TiO2 cannot be recycled easily in a using process; therefore, TiO2 is modified for solving the problems and improving the photocatalytic efficiency. Porous anodic alumina is used as a template, and ZnS is nested in TiO2 nanotubes by a liquid-phase layer-by-layer assembling method. According to the acquired two-layer composite nanotubes, the contact area of TiO2 and ZnS is increased greatly; the charge separation rate is improved and the photocatalytic efficiency is improved due to the special valence band structure of TiO2 and ZnS; and the nanotubes are distributed in an array mode and can be recovered from sewage easily, secondary pollution can be avoided, and therefore, the nanotube array has very important application significance in the aspect of sewage treatment.
Description
Technical field:
The present invention relates to a kind of preparation method of inorganic composite nano pipe array, particularly relate to a kind of TiO
2the preparation method of/ZnS two-layer compound nano-tube array, in particular, utilize porous anodic alumina films for template adopt liquid phase deposition first prepare AAO/TiO
2nano-tube array, then at AAO/TiO
2array basis adopts hydro-thermal method prepare ZnS and be nested in TiO
2the two-layer compound TiO of nanotube inside
2/ ZnS nano-tube array.This technology belongs to the preparation field of nano material.
Background technology:
In recent years, the volatile organic matter VOCS (Volatile Organic Compounds) that industrial wastewater especially produces from petrochemical industry etc. is increasing on the impact of environment, have a strong impact on the sustainable development of ecological environment, cause the extensive concern of society.Along with country is to the attention of sewage drainage standard, sewage drainage standard is more and more higher, impels enterprise demand low cost, high efficiency, the sewage water treatment method that operating procedure is easy.But existing conventional sewage processing method is not enough to the disposal ability of the volatile organic content of biodegradation difficulty, and many along with greater energy consumption cost, make enterprise hang back, even make a desperate move for interests and abandon sewage disposal operation.Therefore seek a kind of easy economy, efficient sewage water treatment method becomes social foci.
Photocatalysis technology is a kind of novel sewage disposal technology, the hydroxyl radical free radical degradation of contaminant utilizing the Strong oxdiative ability of photohole or indirectly produce, because of it, to have technique simple, energy consumption is low, features such as cost is low and getting most of the attention, especially it has stronger catalytic degradation ability to organic wastewater, high-strength acidic and alkaline waste water etc.TiO
2it is a kind of wide bandgap semiconductor materials, energy gap is about 3.2eV, because it has that oxidability is strong, photoetch does not occur after illumination, catalytic activity is high, chemical stability good, the advantages such as wide cost is low, nontoxic of originating oneself through becoming the comparatively deep a kind of catalysis material of the photocatalysis field researchs such as wastewater treatment, purification of air and sterilization.But TiO
2in use still have following problem: (1) TiO
2forbidden band wider, can only absorbing wavelength at the short-wave band light of below 385nm, energy probably only accounts for 4% of solar energy, how to utilize the visible ray and even infrared energy that account for total luminous energy more than 45%, is to determine that can catalysis material be able to the prerequisite of large-scale practical application.(2) TiO
2photo-generate electron-hole as single semi-conducting material is also higher to recombination rate, and the defects such as its quantum efficiency is low also limit it to a certain extent and use.(3) Conventional nano TiO
2the easy in inactivation of powder particle, be thus unfavorable for long-time utilization, cycle characteristics is poor, and easily reunite and reduce active reaction surface area, adsorption capacity is poor, the tiny critical defects such as recycling that are difficult to of particle, and its application is subject to a definite limitation.
In order to solve the problem, improve photocatalysis efficiency, usually to TiO
2carry out modification, as metal or nonmetallic ion-doped, photoactivate and other semiconductors coupling etc.Semiconductors coupling is wherein a kind of effective means, and it is more in the application of photocell field, still has larger research space in photocatalytic degradation sewage.
The activity of photochemical catalyst and pattern, size and structure have very large contact.For TiO
2/ ZnS composite, most exist with graininess pattern, or with the nanotube-shaped existence form of random dispersion, and majority is attached to TiO with ZnS particle
2pipe outer wall, is difficult to reclaim, easily causes secondary pollution in disposing of sewage.
Summary of the invention:
The object of this invention is to provide a kind of TiO
2the preparation method of/ZnS two-layer compound nano-tube array, to overcome the deficiency in prior art.Utilization porous anodic aluminium oxide is template, adopts the method for layer assembly, semiconductor ZnS is nested into TiO
2in nanotube.This technique belongs to a kind of environmentally friendly preparation method, and this preparation method's technique is simple simultaneously, and equipment requirement is lower, with low cost, has the potentiality of large-scale production and application.
A kind of TiO
2the preparation method of/ZnS two-layer compound nano-tube array, its concrete steps are:
(1) porous anodic alumina films is selected to be template, to analyze pure Zn (CH
3cOO)
2, Na
2s
2o
3and TiF
4as raw material.
(2) TiF of configuration concentration 0.01 ~ 1mol/L
4the aqueous solution, anodic oxidation aluminium formwork is immersed institute and join in solution, keep system temperature 40 ~ 100 DEG C, the time, 3 ~ 15min made TiO
2precursor sol uniform deposition is in the duct of anodic oxidation aluminium formwork.
(3) taking-up of step (2) products obtained therefrom being placed on temperature is dry 0.5 ~ 2h in the baking oven of 50 ~ 100 DEG C, obtains the TiO containing anodic oxidation aluminium formwork
2presoma nano-tube array.
(4) load there is TiO
2the anodic oxidation aluminium formwork of presoma is immersed in the Zn (CH that concentration is 0.01 ~ 2mol/L
3cOO)
2and Na
2s
2o
3in solution, in the water heating kettle taking polytetrafluoroethylene (PTFE) as liner, keep hydrothermal temperature 100 ~ 200 DEG C, hydrothermal conditions 2 ~ 24h.Product deionized water is cleaned, dries, finally obtain ZnS and be nested in TiO
2double-deck TiO in nanotube
2/ ZnS composite nano tube array.
ZnS is as a kind of important metal sulfide semiconductor, and band gap width is about 3.6eV.By TiO
2with ZnS compound, on the one hand due to TiO
2conduction band about 0.75eV lower than ZnS, thus make light induced electron transfer to TiO from ZnS
2on, photohole is then from TiO
2valence band is transferred in the valence band of ZnS, thus improves separation of charge, decrease electron-hole recombinations, improve photocatalysis efficiency.The electronics be separated and hole can freely be reacted with the active material of adsorption.On the other hand, two-layer pipe also makes ZnS and TiO
2contact area has and improves largely, is conducive to the raising of catalytic efficiency.Relative to the catalyst material that dispersity exists, TiO prepared by the present invention
2/ ZnS composite nano tube exists in the form of an array, is easy to from middle recycling of disposing of sewage, and avoids the production cost that secondary pollution also reduces catalyst simultaneously.
The invention has the beneficial effects as follows:
Utilize AAO Template preparation nanotube, caliber can suitably regulate, and course of reaction is easy to control.TiO is modified with ZnS
2nanotube, due to the band structure cross effect of the two, improves separation of charge efficiency, decreases electron-hole recombinations, improve photocatalysis efficiency.Double-layer nanometer tubular construction is conducive to increasing TiO
2with the contact area of ZnS, be beneficial to the separation of photo-generate electron-hole.In addition, catalyst exists with nano-tube array form, is easy to, from middle recovery of disposing of sewage, avoid causing secondary pollution.Excellent photocatalysis performance and the continuity preparation technology of simple possible, make TiO
2/ ZnS two-layer compound nano-tube array has a wide range of applications at sewage treatment area.
Accompanying drawing illustrates:
Fig. 1, TiO
2the upper surface SEM picture of/ZnS two-layer compound nano-tube array
Fig. 2, TiO
2the side SEM picture of/ZnS two-layer compound nano-tube array
Fig. 3, TiO
2the side magnification at high multiple SEM picture of/ZnS two-layer compound nano-tube array
Fig. 4, TiO
2the EDS collection of illustrative plates of/ZnS two-layer compound nano-tube array
Fig. 5, TiO
2the TEM picture of/ZnS two-layer compound nanotube
Detailed description of the invention:
Embodiment 1
The TiF of 0.04M is prepared in beaker
4solution, heating TiF
4solution to 60 DEG C, immerses anodic oxidation aluminium formwork completely and keeps the immersion time to be 9min.Then being taken out by sample and being placed on temperature is dry 1h in the baking oven of 80 DEG C.Subsequently load there is TiO
2the anodic oxidation aluminium formwork of presoma is immersed in the Zn (CH of 0.04M
3cOO)
2with the Na of 0.04M
2s
2o
3in mixed solution, hydro-thermal reaction in the water heating kettle taking polytetrafluoroethylene (PTFE) as liner, hydrothermal temperature 180 DEG C, reaction time 6h.Take out after sample and clean by deionized water, dry and obtain and be nested in TiO by ZnS
2tiO in nanotube
2/ ZnS two-layer compound nano-tube array.Comparatively TiO can be clear that by Fig. 1
2the inside and outside wall of/ZnS two-layer compound nanotube, wall thickness about 60nm, aperture about 200nm.The TiO prepared as seen from Figure 2
2/ ZnS two-layer compound nano-tube array length is about 25 μm.Comparatively TiO can be clear that by Fig. 3
2the nano tube structure of parcel ZnS.Include Ti, the elements such as O, Zn, S, Al, C, Pt, Si in multiple tube array as seen from Figure 4, spray Pt when wherein Pt tests from SEM operates.Al is from anodic oxidation aluminium formwork, and Si comes from silicon chip during SEM test.Ti, O, Zn, S content is obviously higher in addition, tentatively can determine to take anodised aluminium as template, adopts laminated assembling technology successfully to prepare TiO
2/ ZnS two-layer compound nano-tube array structure.Can obviously see that ZnS is nested in TiO by Fig. 5
2double-layer nanometer tubular construction in nanotube.
Claims (8)
1. a TiO
2the preparation method of/ZnS two-layer compound nano-tube array, is characterized in that:
(1) porous anodic alumina films is selected to be template, to analyze pure Zn (CH
3cOO)
2, Na
2s
2o
3and TiF
4as raw material.
(2) certain density TiF is configured
4the aqueous solution, anodic oxidation aluminium formwork is immersed institute and join in solution, keep system temperature certain limit, appropriate time, makes TiO
2precursor sol uniform deposition is in the duct of anodic oxidation aluminium formwork.
(3) step (2) products obtained therefrom is taken out dry a period of time in an oven, obtain the TiO containing anodic oxidation aluminium formwork
2presoma nano-tube array.
(4) load there is TiO
2the anodic oxidation aluminium formwork of presoma is immersed in certain density Zn (CH
3cOO)
2and Na
2s
2o
3in solution, in the water heating kettle taking polytetrafluoroethylene (PTFE) as liner, keep hydrothermal temperature proper range, hydrothermal treatment consists a period of time.Subsequently product is used deionized water wash clean, dry.Finally obtain the TiO containing anodic oxidation aluminium formwork
2the two-layer compound nano-tube array of coated PbS.
2. TiO as claimed in claim 1
2the preparation method of/ZnS two-layer compound nano-tube array, it is characterized in that described template is porous anodic alumina films, film thickness is 20 ~ 60 μm, and channel diameter is 100 ~ 250nm, lower through-hole on fenestra road.
3. TiO as claimed in claim 1
2the preparation method of/ZnS two-layer compound nano-tube array, is characterized in that described TiO
2/ ZnS composite Nano length of tube is 20 ~ 60 μm, and wall thickness is 20 ~ 80nm.
4. TiO as claimed in claim 1
2the preparation method of/ZnS two-layer compound nano-tube array, is characterized in that described TiF
4solution concentration is 0.01 ~ 1mol/L.
5. TiO as claimed in claim 1
2the preparation method of/ZnS two-layer compound nano-tube array, keeps TiF
4solution temperature 40 ~ 100 DEG C, time 3 ~ 15min.
6. TiO as claimed in claim 1
2the preparation method of/ZnS two-layer compound nano-tube array, is characterized in that load is had TiO
2the temperature that the anodic oxidation aluminium formwork of presoma is dry is in an oven 50 ~ 100 DEG C, and drying time is 0.5 ~ 2h.
7. TiO as claimed in claim 1
2the preparation method of/ZnS two-layer compound nano-tube array, is characterized in that described Na
2s
2o
3with Zn (CH
3cOO)
2the concentration of the aqueous solution is 0.01 ~ 2mol/L.
8. TiO as claimed in claim 1
2the preparation method of/ZnS two-layer compound nano-tube array, it is characterized in that adopting hydro-thermal reaction in step (4), hydrothermal temperature is 100 ~ 200 DEG C, hydrothermal conditions 2 ~ 24h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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|---|---|---|---|
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| Publication Number | Publication Date |
|---|---|
| CN104741134A true CN104741134A (en) | 2015-07-01 |
| CN104741134B CN104741134B (en) | 2017-03-29 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108043388A (en) * | 2017-10-09 | 2018-05-18 | 华南理工大学 | Double-layer porous wall titanium alloy nano pipe array visible light catalyst of a kind of aluminium, vanadium codope and preparation method and application |
| CN111844090A (en) * | 2020-07-10 | 2020-10-30 | 重庆工程职业技术学院 | Aluminum alloy mechanical gripper and processing method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101003020A (en) * | 2007-01-11 | 2007-07-25 | 南京大学 | Sensitized titanium oxide and zinc sulfide visible light responsing photocalalyst, and its preparing method |
| CN103007966A (en) * | 2012-12-11 | 2013-04-03 | 湖南大学 | Photocatalyst as well as preparation method and application method thereof |
-
2014
- 2014-10-04 CN CN201410521312.7A patent/CN104741134B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101003020A (en) * | 2007-01-11 | 2007-07-25 | 南京大学 | Sensitized titanium oxide and zinc sulfide visible light responsing photocalalyst, and its preparing method |
| CN103007966A (en) * | 2012-12-11 | 2013-04-03 | 湖南大学 | Photocatalyst as well as preparation method and application method thereof |
Non-Patent Citations (2)
| Title |
|---|
| EN-LONG YANG ET AL.: "Coaxial WO3/TiO2 nanotubes/nanorods with high visible light activity for the photodegradation of 2,3-dichlorophenol", 《CHEMICAL ENGINEERING JOURNAL》 * |
| HONG LI ET AL.: "PREPARATION OF TiO2/ZnS CORE/SHEATH HETEROSTRUCTURE NANOTUBES VIA A WET CHEMICAL METHOD AND THEIR PHOTOCATALYTIC ACTIVITY", 《REACTION KINETICS AND CATALYSIS LETTERS》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108043388A (en) * | 2017-10-09 | 2018-05-18 | 华南理工大学 | Double-layer porous wall titanium alloy nano pipe array visible light catalyst of a kind of aluminium, vanadium codope and preparation method and application |
| CN108043388B (en) * | 2017-10-09 | 2020-09-22 | 华南理工大学 | Aluminum and vanadium co-doped double-layer porous wall titanium alloy nanotube array visible-light-driven photocatalyst and preparation method and application thereof |
| CN111844090A (en) * | 2020-07-10 | 2020-10-30 | 重庆工程职业技术学院 | Aluminum alloy mechanical gripper and processing method thereof |
| CN111844090B (en) * | 2020-07-10 | 2022-02-15 | 重庆工程职业技术学院 | Aluminum alloy mechanical gripper and processing method thereof |
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| CN104741134B (en) | 2017-03-29 |
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