CN101607736A - A kind of surface imprinting functionalization TiO 2Nanotube - Google Patents

A kind of surface imprinting functionalization TiO 2Nanotube Download PDF

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CN101607736A
CN101607736A CNA2009100431834A CN200910043183A CN101607736A CN 101607736 A CN101607736 A CN 101607736A CN A2009100431834 A CNA2009100431834 A CN A2009100431834A CN 200910043183 A CN200910043183 A CN 200910043183A CN 101607736 A CN101607736 A CN 101607736A
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nanotube
tio
compound
doping
surface imprinting
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CN101607736B (en
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刘承斌
罗胜联
唐艳红
杨丽霞
刘荣华
何晔娟
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Hunan University
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Abstract

The present invention relates to a kind of surface imprinting functionalization TiO 2Nanotube, wherein, trace matrix is the composite inorganic semi-conductor, microsphere is an organic pollutant.The present invention is the molecular imprinting synthetic molecularly imprinted polymer physical strength height of trace matrix with the inorganic nano material, and identification point is survivable.As absorption carrier, reduced non-specific adsorption widely, reduce the embedding phenomenon, make it that very optimistic development prospect be arranged at aspects such as photochemical catalysis, analogue enztme, transmitter and bio-identification.

Description

A kind of surface imprinting functionalization TiO 2Nanotube
Technical field
The present invention relates to the imprinting functionalization TiO of a class novel texture 2Nano-tube material.
Background technology
Because the functional not strong and hydrophobicity characteristics of the chemical reaction of most organic pollutant molecules are at possess hydrophilic property TiO 2Surface adsorption is very low, and this also is to utilize TiO 2Eliminate one of bottleneck of hydrophobic organic pollutant, therefore strengthen organic pollutant at TiO 2The absorption research on photocatalyst material surface is extremely important to the efficient reduction of organic pollutant.A kind of analog antibody-antigen-specific identification and bonded artificial bio-membrane mould plate technique-molecular imprinting have caused everybody interest.In this technology, template molecule (microsphere) forms stabilized complex with one or more function monomers by covalent linkage or noncovalent interaction such as hydrogen bond, Van der Waals force, ionization, hydrophobic interaction and π-π effect etc., add linking agent and cause the function monomer polymerization, remove again template molecule obtain molecularly imprinted polymer (Molecularly imprinted polymers, MIP).MIP has the cavity that shape, size and template molecule are complementary, and the functional group of particular arrangement is arranged, and can produce the specific recognition effect with template molecule.Molecular imprinting is showing tempting application prospect aspect the selective enrichment organic pollutant.But, organic polymer trace matrix is being modified TiO 2Have some problems when being used for photochemical catalysis: imprinted polymer covers TiO 2The surface influences TiO 2Photoabsorption and charge transfer; Imprinted polymer can be degraded in photocatalytic process; Organic polymer trace matrix mechanicalness and thermostability are bad, cause the shape memory instability.And inorganic polymer trace film is expected to address the above problem, and it has the big and advantages such as favorable mechanical stability and thermostability of specific surface area, can overcome the rigidity of organic polymer and the shortcoming of inertia difference, becomes the molecular imprinting development trend.
Summary of the invention
The object of the present invention is to provide the imprinting functionalization TiO of a class novel texture 2Nanotube.
The present invention seeks to realize by following manner:
At TiO 2Be combined with on the nanotube walls surface by organic pollutant trace composite inorganic semiconductor film, wherein the trace substrate material is the composite inorganic semi-conductor, and microsphere is an organic pollutant.
Described organic pollutant comprises persistence organic pollutant.
Described composite inorganic semi-conductor trace substrate material is TiO 2, CdS, CdSe, SiC, WO 3, ZnS, ZnO, SnO 2, Nb 2O 5, ZrO 2, V 2O 5, Ta 2O 5And SrTiO 3In the mixture that is composited more than 2 kinds or 2 kinds.
Described composite inorganic semi-conductor is characterized in that the composite inorganic semi-conductor also comprises the doped and compounded inorganic semiconductor.
The doping of described doped and compounded inorganic semiconductor comprises that metal simple-substance mixes, non-metal simple-substance is mixed or magnetic metal oxide mixes.
The metal simple-substance of described doped and compounded inorganic semiconductor mixes and comprises metal-doped more than a kind or a kind among Fe, Pt, Pd, Au and the Ag.
The nonmetal doping of described doped and compounded inorganic semiconductor comprises the nonmetal doping more than a kind or a kind among C, N, S and the B.
The magnetic metal oxide of described doped and compounded inorganic semiconductor is Fe 3O 4
TiO 2Nanotube is pure TiO 2Nanotube, or compound TiO 2Nanotube.
Described compound TiO 2Nanotube comprises that precious metal doping is compound, semi-conductor is compound, ion doping is compound and nonmetal doping compound TiO 2Nanotube, or comprise compound TiO altogether more than 2 kinds or 2 kinds in precious metal doping, semi-conductor, ion doping and the nonmetal doping 2Nanotube.
Compound TiO 2The nanotube precious metal doping is compound to comprise metal-doped compound more than a kind or a kind among Pt, Pd, Au and the Ag.
Compound TiO 2The nanotube nonmetal doping is compound to comprise that the nonmetal doping more than a kind or a kind among C, N, S and the B is compound.
Compound TiO 2Compound CdS, CdSe, SiC, the WO of comprising of the semi-conductor of nanotube 3, ZnS, ZnO, SnO 2, Nb 2O 5, ZrO 2, V 2O 5, Ta 2O 5And SrTiO 3In a kind or a kind compound with semiconductor-on-insulator.
Compound TiO 2The ion doping of nanotube comprises Fe 3+, Co 2+, Cr 3+, Zn 2+, Zr 4+, Nb 5+, Ga 3+, W 6+, Fe (CN) 6 4-, MoS 4 2-, Li +, Na +, K +, Ba 2+, Ca 2+And SO 4 2-In a kind of ion doping compound or more than a kind ion doping compound.
Adopt template, electrochemistry anodic oxidation or Hydrothermal Preparation TiO 2Nanotube; Adopt anode co-oxidation deposition, gas/liquid is permeated mutually or method such as in-situ oxidation reduction prepares compound TiO 2Nanotube; Adopt methods such as sol-gel, galvanic deposit, chemical vapour deposition, physical vapor deposition, self-assembly or spraying thermolysis at TiO 2The nanotube walls surface preparation contains the TiO of organic pollutant 2, CdS, CdSe, SiC, WO 3, ZnS, ZnO, SnO 2, Nb 2O 5, ZrO 2, Ta 2O 5Or SrTiO 3Deng the inorganic semiconductor film; Methods such as employing solvent elution, hydrolysis, thermal treatment or catalyzed degradation are removed the organic pollutant microsphere in the trace thin film layer.
The present invention is the molecular imprinting synthetic molecularly imprinted polymer physical strength height of trace matrix with the inorganic nano material, and identification point is survivable.As absorption carrier, reduced non-specific adsorption widely, reduce the embedding phenomenon, make it that very optimistic development prospect be arranged at aspects such as photochemical catalysis, analogue enztme, transmitter and bio-identification.
Description of drawings
Fig. 1 is for adopting surperficial sol-gel technique imprinting functionalization TiO 2Nanotube principle diagrammatic sketch.
Embodiment
Following examples are intended to illustrate the present invention rather than limitation of the invention further.
Embodiment 1
(1) TiO 2The preparation of nanotube
Under the 35-60V volts DS, be anode with pure titanium or titanium alloy, platinized platinum is a negative electrode, is to prepare TiO in the hydrofluoric acid of 0.5-3% and the dimethyl sulfoxide (DMSO) blended ionogen at hydrofluoric acid quality percentage composition 2Nanotube is calcined nanotube 4-6 hour under 400-500 ℃ of aerobic conditions, makes its crystallization forming.
(2) imprinting functionalization TiO 2The nanotube preparation
Adopt surperficial sol-gel technique preparation: preparation process as shown in Figure 1.Among Fig. 1, M 1=Zn, M 2=Ti, R are sec.-propyl or normal-butyl, ● represent organic pollutant molecule,
Figure G2009100431834D00031
The room that stays in the organic pollutant molecule rear film is removed in representative.
With TiO 2Nanotube is immersed in for some time in the alcoholic solution of the tetra isopropyl oxygen base zinc that contains octabromodiphenyl ether microsphere and tetra-n-butyl oxygen base titanium, and hydrolysis then places air drying again, according to film thickness needs, TiO 2Nanotube can soak-hydrolysis-drying treatment repeatedly, heat drying typing then, and last flush away microsphere after drying can obtain octabromodiphenyl ether trace ZnO-TiO 2The TiO of laminated film modification 2Nanotube.
Embodiment 2
With M among the embodiment 1 1Use Zr instead, all the other conditions can be prepared octabromodiphenyl ether trace ZrO with embodiment 1 2-TiO 2The TiO of laminated film modification 2Nanotube.
Embodiment 3
With M among the embodiment 1 2Use Zr instead, all the other conditions can be prepared octabromodiphenyl ether trace ZnO-ZrO with embodiment 1 2The TiO of laminated film modification 2Nanotube.
Embodiment 4
With M among the embodiment 1 1Use Sn instead, all the other conditions can be prepared octabromodiphenyl ether trace SnO with embodiment 1 2-TiO 2The TiO of laminated film modification 2Nanotube.
Embodiment 5
(1) TiO 2The preparation of nanotube
With embodiment 1.
(2) imprinting functionalization TiO 2The nanotube preparation
With TiO 2Nanotube is immersed in for some time in the CdS-ZnS colloidal sol that contains the chlordecone microsphere, places air drying again, according to film thickness needs, TiO 2Nanotube can soak-drying treatment repeatedly, and the TiO that the microsphere after drying can obtain the modification of chlordecone trace CdS-ZnS laminated film is removed in heat drying typing then at last 2Nanotube.
Embodiment 6
Use CdS among the embodiment 5 instead CdSe, all the other conditions can be prepared the TiO of chlordecone trace CdSe-ZnS laminated film modification with embodiment 5 2Nanotube.
Embodiment 7
(1) TiO 2The preparation of nanotube
With embodiment 1.
(2) C-TiO 2The composite nano tube preparation
TiO with (one) preparation 2Nanotube places the anaerobic vacuum system, is carbon source with the polyoxyethylene glycol, in 500-600 ℃ of calcining 2-12 hour, makes polyoxyethylene glycol dehydration carbonization obtain C-TiO 2Composite nano tube.
(3) imprinting functionalization C-TiO 2The composite nano tube preparation
TiO with (two) step among the embodiment 1 2Nanotube changes C-TiO into 2Composite nano tube, octabromodiphenyl ether changes phenyl-hexachloride into, and all the other prepare phenyl-hexachloride trace ZnO-TiO with (two) step among the embodiment 1 2The C-TiO of laminated film modification 2Composite nano tube.
Embodiment 8
(1) Fe-C-TiO 2The composite nano tube preparation
C-TiO with embodiment 7 preparations 2Nanotube places the FeSO4 electroplate liquid to electroplate, and electroplating current density is 0.002-0.005A/s, obtains Fe-C-TiO 2Composite nano tube.
(2) imprinting functionalization Fe-C-TiO 2The composite nano tube preparation
C-TiO with (three) step among the embodiment 7 2Composite nano tube changes Fe-C-TiO into 2Composite nano tube, all the other prepare phenyl-hexachloride trace ZnO-TiO with (three) step among the embodiment 7 2The Fe-C-TiO of laminated film modification 2Composite nano tube.
Embodiment 9
(1) TiO 2The preparation of nanotube
With embodiment 1.
(2) imprinting functionalization TiO 2The nanotube preparation
With TiO 2Nanotube is immersed in and contains pentachlorobenzene microsphere and Fe 3O 4For some time in the CdS-ZnS colloidal sol of nano particle places air drying again, according to film thickness needs, TiO 2Nanotube can soak-drying treatment repeatedly, and heat drying typing is then removed the microsphere after drying at last and can be obtained pentachlorobenzene trace Fe 3O 4The TiO of-CdS-ZnS laminated film modification 2Nanotube.
Embodiment 10
With TiO among the embodiment 9 2Nanotube is used Fe-C-TiO instead 2Composite nano tube, all the other conditions can be prepared pentachlorobenzene trace Fe with embodiment 9 3O 4The Fe-C-TiO of-CdS-ZnS laminated film modification 2Composite nano tube.

Claims (14)

1, a kind of surface imprinting functionalization TiO 2Nanotube is characterized in that, at TiO 2Be combined with on the nanotube walls surface by organic pollutant trace composite inorganic semiconductor film, wherein the trace substrate material is the composite inorganic semi-conductor, and microsphere is an organic pollutant.
2, a kind of surface imprinting functionalization TiO according to claim 1 2Nanotube is characterized in that, described organic pollutant comprises persistence organic pollutant.
3, a kind of surface imprinting functionalization TiO according to claim 1 2Nanotube is characterized in that, described composite inorganic semi-conductor trace substrate material is TiO 2, CdS, CdSe, SiC, WO 3, ZnS, ZnO, SnO 2, Nb 2O 5, ZrO 2, V 2O 5, Ta 2O 5And SrTiO 3In the mixture that is composited more than 2 kinds or 2 kinds.
4, a kind of surface imprinting functionalization TiO according to claim 3 2Nanotube is characterized in that, described composite inorganic semi-conductor is characterized in that the composite inorganic semi-conductor also comprises the doped and compounded inorganic semiconductor.
5, a kind of surface imprinting functionalization TiO according to claim 4 2Nanotube is characterized in that, the doping of described doped and compounded inorganic semiconductor comprises that metal simple-substance mixes, non-metal simple-substance is mixed or magnetic metal oxide mixes.
6, a kind of surface imprinting functionalization TiO according to claim 5 2Nanotube is characterized in that, the metal simple-substance of described doped and compounded inorganic semiconductor mixes and comprises metal-doped more than a kind or a kind among Fe, Pt, Pd, Au and the Ag.
7, a kind of surface imprinting functionalization TiO according to claim 5 2Nanotube is characterized in that, the nonmetal doping of described doped and compounded inorganic semiconductor comprises the nonmetal doping more than a kind or a kind among C, N, S and the B.
8, a kind of surface imprinting functionalization TiO according to claim 5 2Nanotube is characterized in that, the magnetic metal oxide of described doped and compounded inorganic semiconductor is Fe 3O 4
9, according to each described a kind of surface imprinting functionalization TiO of claim 1-8 2Nanotube is characterized in that, TiO 2Nanotube is pure TiO 2Nanotube, or compound TiO 2Nanotube.
10, a kind of surface imprinting functionalization TiO according to claim 9 2Nanotube is characterized in that, described compound TiO 2Nanotube comprises that precious metal doping is compound, semi-conductor is compound, ion doping is compound and nonmetal doping compound TiO 2Nanotube, or comprise compound TiO altogether more than 2 kinds or 2 kinds in precious metal doping, semi-conductor, ion doping and the nonmetal doping 2Nanotube.
11, a kind of surface imprinting functionalization TiO according to claim 10 2Nanotube is characterized in that, compound TiO 2The nanotube precious metal doping is compound to comprise metal-doped compound more than a kind or a kind among Pt, Pd, Au and the Ag.
12, a kind of surface imprinting functionalization TiO according to claim 10 2Nanotube is characterized in that, compound TiO 2The nanotube nonmetal doping is compound to comprise that the nonmetal doping more than a kind or a kind among C, N, S and the B is compound.
13, a kind of surface imprinting functionalization TiO according to claim 10 2Nanotube is characterized in that, compound TiO 2Compound CdS, CdSe, SiC, the WO of comprising of the semi-conductor of nanotube 3, ZnS, ZnO, SnO 2, Nb 2O 5, ZrO 2, V 2O 5, Ta 2O 5And SrTiO 3In a kind or a kind compound with semiconductor-on-insulator.
14, a kind of surface imprinting functionalization TiO according to claim 10 2Nanotube is characterized in that, compound TiO 2The ion doping of nanotube comprises Fe 3+, Co 2+, Cr 3+, Zn 2+, Zr 4+, Nb 5+, Ga 3+, W 6+, Fe (CN) 6 4-, MoS 4 2-, Li +, Na +, K +, Ba 2+, Ca 2+And SO 4 2-In a kind of ion doping compound or more than a kind ion doping compound.
CN2009100431834A 2009-04-22 2009-04-22 Surface imprinting functionalization TiO2 nano-tube Expired - Fee Related CN101607736B (en)

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Cited By (7)

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CN102125877A (en) * 2011-01-05 2011-07-20 江苏大学 Method for preparing selectively degraded ciprofloxacin photocatalyst
CN102253093A (en) * 2011-03-21 2011-11-23 桂林电子科技大学 Method for preparing sensitive membrane of TiO2 sol-gel molecular engram taste sense sensor
CN102553649A (en) * 2011-12-26 2012-07-11 河海大学 17beta-estradiol molecular imprinted silver-doped TiO2 nanotube and preparation method thereof
CN102553534A (en) * 2011-12-26 2012-07-11 河海大学 17 beta-estradiol molecular imprinting titanium dioxide (TiO2) nano tube and preparation method thereof
WO2013139174A1 (en) * 2012-03-19 2013-09-26 The Hong Kong University Of Science And Technology Incorporating metals, metal oxides and compounds on the inner and outer surfaces of nanotubes and between the walls of the nanotubes and preparation thereof
CN103406117A (en) * 2013-08-27 2013-11-27 南昌航空大学 Preparation of high-selectivity inorganic skeletal biomimic TiO2 photocatalyst by sol-hydrothermal method at low temperature
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CN102125877B (en) * 2011-01-05 2012-12-19 江苏大学 Method for preparing selectively degraded ciprofloxacin photocatalyst
CN102125877A (en) * 2011-01-05 2011-07-20 江苏大学 Method for preparing selectively degraded ciprofloxacin photocatalyst
CN102253093A (en) * 2011-03-21 2011-11-23 桂林电子科技大学 Method for preparing sensitive membrane of TiO2 sol-gel molecular engram taste sense sensor
US9833003B2 (en) 2011-05-04 2017-12-05 WELL Shield LLC Titanium dioxide photocatalytic compositions and uses thereof
CN102553649B (en) * 2011-12-26 2013-09-25 河海大学 17beta-estradiol molecular imprinted silver-doped TiO2 nanotube and preparation method thereof
CN102553534B (en) * 2011-12-26 2013-07-31 河海大学 17 beta-estradiol molecular imprinting titanium dioxide (TiO2) nano tube and preparation method thereof
CN102553534A (en) * 2011-12-26 2012-07-11 河海大学 17 beta-estradiol molecular imprinting titanium dioxide (TiO2) nano tube and preparation method thereof
CN102553649A (en) * 2011-12-26 2012-07-11 河海大学 17beta-estradiol molecular imprinted silver-doped TiO2 nanotube and preparation method thereof
WO2013139174A1 (en) * 2012-03-19 2013-09-26 The Hong Kong University Of Science And Technology Incorporating metals, metal oxides and compounds on the inner and outer surfaces of nanotubes and between the walls of the nanotubes and preparation thereof
CN104350011A (en) * 2012-03-19 2015-02-11 香港科技大学 Incorporating metals, metal oxides and compounds on the inner and outer surfaces of nanotubes and between the walls of the nanotubes and preparation thereof
CN104350011B (en) * 2012-03-19 2016-09-28 香港科技大学 Doping metals, metal-oxide and metal complex and the preparation method of nanotube between the inner surface of nanotube and outer surface and nanotube layer
US10238762B2 (en) 2012-03-19 2019-03-26 The Hong Kong University Of Science And Technology Incorporating metals, metal oxides and compounds on the inner and outer surfaces of nanotubes and between the walls of the nanotubes and preparation thereof
CN103406117A (en) * 2013-08-27 2013-11-27 南昌航空大学 Preparation of high-selectivity inorganic skeletal biomimic TiO2 photocatalyst by sol-hydrothermal method at low temperature
CN103406117B (en) * 2013-08-27 2015-03-11 南昌航空大学 Preparation of high-selectivity inorganic skeletal biomimic TiO2 photocatalyst by sol-hydrothermal method at low temperature

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