CN108772076A - A kind of CdS modifications TiO2The preparation method of nanometer tube composite materials - Google Patents
A kind of CdS modifications TiO2The preparation method of nanometer tube composite materials Download PDFInfo
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- CN108772076A CN108772076A CN201810687367.3A CN201810687367A CN108772076A CN 108772076 A CN108772076 A CN 108772076A CN 201810687367 A CN201810687367 A CN 201810687367A CN 108772076 A CN108772076 A CN 108772076A
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- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000012986 modification Methods 0.000 title description 11
- 230000004048 modification Effects 0.000 title description 8
- 239000002071 nanotube Substances 0.000 claims abstract description 86
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 75
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 75
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 53
- 239000000843 powder Substances 0.000 claims description 39
- 239000000047 product Substances 0.000 claims description 36
- 239000006228 supernatant Substances 0.000 claims description 36
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- 238000005119 centrifugation Methods 0.000 claims description 19
- 238000005406 washing Methods 0.000 claims description 19
- 239000011734 sodium Substances 0.000 claims description 17
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Chemical compound [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 238000000926 separation method Methods 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 47
- 238000005342 ion exchange Methods 0.000 abstract description 23
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 18
- 238000000034 method Methods 0.000 abstract description 11
- 238000001556 precipitation Methods 0.000 abstract description 8
- 238000010521 absorption reaction Methods 0.000 abstract description 7
- 239000003054 catalyst Substances 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 description 17
- 239000000463 material Substances 0.000 description 17
- 239000007787 solid Substances 0.000 description 17
- 238000003756 stirring Methods 0.000 description 16
- 239000002245 particle Substances 0.000 description 12
- 238000004220 aggregation Methods 0.000 description 6
- 230000002776 aggregation Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000000151 deposition Methods 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 239000012612 commercial material Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
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- 239000002994 raw material Substances 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- B01J35/33—
-
- B01J35/39—
-
- 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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
-
- 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
- B01J37/30—Ion-exchange
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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
- 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
- B01J37/343—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 ultrasonic wave energy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention is that a kind of CdS modifies TiO2The preparation method of nanometer tube composite materials.This method is first by NaOH and business TiO2Presoma is prepared in reaction, is converted presoma nanotube by ion exchange and precipitation reaction, while generating CdS and TiO2, make CdS particulate loads in TiO2On nanotube.CdS is supported on TiO by the present invention2On nanotube, TiO can be effectively widened2The visible absorption range of nanotube increases its application field as photochemical catalyst to visible region 535nm or so.The preparation method is simple for process, and equipment requirement is single, and it is small to react required energy expenditure.
Description
Technical field
The invention belongs to catalytic fields, and in particular to a kind of CdS modifications TiO2The preparation method of nanometer tube composite materials and
Its application in photocatalysis field.
Background technology
One-dimensional TiO2Nano material have less crystal boundary, and have big draw ratio, charge can fast transfer, it is larger
The absorption and scattering property of light is remarkably reinforced in specific surface area, these advantages make it in photocatalysis, sensing and photovoltaic
There is prodigious application in field.But due to TiO2Two major defects：First, photo-generate electron-hole is with higher compound
Rate；Second is that the ultraviolet region in sunlight can only be absorbed, 5% sunlight can only be probably absorbed, the utilization rate of sunlight is relatively low.
Therefore CdS is supported on TiO2Composite material is made on nanotube, can realize the broadening in composite material photoresponse region so that
TiO2Photocatalytic activity enhances.
TiO is modified for CdS at present2The preparation of nanometer tube composite materials has many research, such as Peng Lian lances seminar
CdS is set to be supported on TiO by chemical bath organon2On nanotube, this method is simple, but there are problems that, due to precipitation
Reaction is again the place for being easiest to react at nozzle, therefore be easy to block up due to the aggregation of CdS particles at nozzle quickly
Plug.Simultaneously because the effect of surface tension of liquid, reaction solution are not easily accessed in nanotube, and CdS particles are more likely to deposit
In nanometer pipe outer wall, and in the inner wall of nanotube then few depositions.Cho seminar utilizes ultrasonic wave assistant depositing CdS particles,
CdS is filled evenly, distribution of particles density bigger, but ultrasound be easy to cause the fracture of nanotube.Misra is heavy by electrochemistry
Product obtains the TiO of CdS particle modifications2Nanotube, the required electric consumption of this method synthesis is big, and preparation process equipment requirement is high, system
Standby condition is harsh.The present invention prepares presoma using hydrothermal synthesis method, is next prepared using ion exchange and precipitation reaction
The TiO of CdS modifications2Nanometer tube composite materials.Obtained product well-crystallized, required tables of equipment one, technological process is simple, reaction
Condition is easily controllable and low energy consumption, low stain, is appropriate for industrialized production.The CdS of generation modifies TiO2Nanotube composite
Material, the evengranular loads of CdS on the nanotube, avoid the aggregation of CdS particles and caused by blockage.TiO2Nano particle
It is coupled with the narrow gap semiconductor of CdS nano particles, its optic response range can be expanded to visible light from ultraviolet light, improved
Its visible light activity, while TiO2The heterojunction structure that nanotube is generated with the interfaces CdS is conducive to improve photo-generate electron-hole pair
Separative efficiency.
Invention content
It is insufficient present in current techniques it is an object of the invention to be directed to, a kind of CdS modifications TiO is provided2Nanotube is multiple
The preparation method of condensation material.The present invention is first by NaOH and business TiO2Presoma is prepared in reaction, by ion exchange and is sunk
Reaction of forming sediment converts presoma nanotube, while generating CdS and TiO2, make CdS particulate loads in TiO2On nanotube.It should
CdS is supported on TiO by method2On nanotube, TiO can be effectively widened2The visible absorption range of nanotube is to visible region
535nm or so increases its application field as photochemical catalyst.And preparation process is simple, and equipment requirement is single, needed for reaction
Energy expenditure is small.
To achieve the above object, the present invention uses following technical scheme：
A kind of CdS modifications TiO2The preparation method of nanometer tube composite materials, includes the following steps：
(1) preparation of presoma：By TiO2Powder is added in concentrated NaOH solution, ultrasonic disperse 10~30min, Zhi Houzhuan
It moves in hydrothermal reaction kettle, 6~12h is kept the temperature at 100~180 DEG C；Product is washed with deionized water to neutrality, is then centrifuged for point
From presoma nanotube is prepared in drying；
Wherein, 0.5~1gTiO is added in the concentrated NaOH solution per 25mL2Powder；
(2) CdS modifies TiO2The preparation of nanometer tube composite materials：Presoma is placed in Cd (NO3)2·4H2In the solution of O,
And it is stirred 1~3 hour at 30~50 DEG C, solution centrifuges, and removes supernatant, then washed with deionized water centrifugal water；With
Afterwards, obtained solid is added to SC (NH2)2Solution in, and stirred 2~4 hours at 50~80 DEG C, solution centrifuges, and goes
Except supernatant, carry out being dried to obtain yellow powder after residue washing, i.e. CdS modifies TiO2Nanometer tube composite materials.
Wherein, every 30~80mLCd (NO3)2·4H2The solution of O adds 1g presomas, molar ratio Cd (NO3)2·4H2O：SC
(NH2)2=1:0.25~4；Cd(NO3)2·4H2A concentration of 0.1~0.4mol/L of the solution of O, SC (NH2)2A concentration of 0.1
~0.4mol/L.
The concentration of sodium hydroxide solution is 10mol/L.
The frequency of the ultrasonic disperse is 40Hz.
The rotating speed of the centrifugation is 8000~10000r/min.
Above-mentioned composite material：A diameter of 20~30nm of nanotube, and CdS particles have size equal in nanotube surface
The composite material of even, fine dispersion, gained has good photoresponse range, makes TiO2Photocatalytic activity enhancing.
The present invention substantive distinguishing features be：
In current techniques, TiO is modified in CdS2In the preparation method of nanometer tube composite materials, TiO is generally first prepared2Nanometer
Pipe, then carries out CdS precipitating loads, is quickly due to precipitation reaction, at nozzle the place for being easiest to react again, therefore nozzle
Place is easy to block due to the aggregation of CdS particles, influences electronics, photon in TiO2Middle transmission prevents CdS from effectively changing
TiO2Light abstraction width；And what the present invention selected is by NaOH and business TiO2The presoma prepared is reacted, ion exchange is passed through
Presoma nanotube is converted with precipitation reaction, while generating CdS and TiO2, make CdS particulate loads in TiO2Nanotube
On；Presoma is converted using simple ion exchange and precipitation reaction, CdS is formed and modifies TiO2Nanotube composite
Material, CdS is evengranular to be distributed in TiO2On nanotube, avoid particle aggregation and caused by blockage, can effectively improve
Photocatalysis efficiency will be gathered around in the fields such as electrochemistry and catalysis and have broad application prospects.
The present invention has the advantages that：
1, the raw material that the present invention uses belongs to the industrial chemicals of industrialized production, cheap and easy to get；The equipment of use
It is simple to operation, it is applied in industrialized production.
2, the present invention prepares CdS and modifies TiO2The method of nanometer tube composite materials is simpler than general preparation method.Generally
Preparation method using by chemical deposition carry out CdS particles load, need to impregnate in solution for several times, constantly
Cycle, prepares relative complex.The present invention only needs that presoma progress ion exchange and precipitation reaction can be prepared CdS and be repaiied
Adorn TiO2Nanometer tube composite materials, this is a kind of simple and effective synthetic method, is suitable for large batch of production.CdS particle rulers
Very little uniform, fine dispersion, size is 6~10nm.
3, the composite material prepared by the present invention can be avoided effectively compared with composite material prepared by conventional method
The aggregation of CdS particles and caused by blockage.TiO is modified in CdS2It is general to use in the preparation method of nanometer tube composite materials
First generate TiO2Nanotube, then in TiO2The method of precipitate C dS is loaded on nanotube.The synthetic route that the present invention selects is
By NaOH and business TiO2The presoma prepared is reacted, by ion exchange and precipitation reaction, while generating CdS and TiO2, CdS
Particulate load is in TiO2On nanotube, partial particulate is embedded in the inside of nanotube, it is possible to prevente effectively from directly selecting TiO2Nanotube
Blockage caused when CdS loads is carried out, improves electronics or photon in TiO2Transmission speed in nanotube channel, is beneficial to
Its photoelectric properties is promoted.
4, the composite material prepared by the present invention is compared with business TiO2With wider array of photoresponse range.Business TiO2In 380nm
Place shows absorption edge, can only absorb ultraviolet light；And the absorption edge of the composite material prepared by the present invention is in wavelength 535nm
Place, it is with business TiO2Compared to red shift about 155nm so that the composite material prepared by the present invention can not only absorb ultraviolet light, but also
Visible light can be absorbed, the utilization to light is enhanced.
Description of the drawings
The present invention is further described with specific implementation below in conjunction with the accompanying drawings.
Fig. 1 is that CdS prepared by embodiment 1 modifies TiO2The XRD photos of nanometer tube composite materials.
Fig. 2 is the SEM photograph of presoma nanotube prepared by 1 hydro-thermal method of embodiment.
Fig. 3 is that CdS prepared by embodiment 1 modifies TiO2The TEM photos of nanometer tube composite materials.
Fig. 4 is that CdS prepared by embodiment 1 modifies TiO2Nanometer tube composite materials and business TiO2UV-Vis photos.
Specific implementation mode
The present invention realizes in the following way：The TiO of CdS modifications2Presoma is placed in Cd by nanotube complex
(NO3)2·4H2In O solution, ionic reaction is carried out, then, then places it in SC (NH2)2In solution, CdS-loaded TiO is synthesized2
Nanotube complex.
TiO of the present invention2Powder is known commercially available commercial materials, and grain size is 110~280nm；
Embodiment 1：
By 1gTiO2Powder is dissolved in the concentrated NaOH solution of 25mL10M, ultrasonic disperse 30min, is transferred to volume and is
In 50mL reaction kettles, 8h is reacted for 160 DEG C in an oven.Product is washed with deionized to neutrality, is centrifuged, later 60
DEG C baking oven in dry 15h, obtain presoma nanotube.The presoma nanotube of 1g is placed in 0.1MCd (NO3)2·4H2O's
It in solution (50mL), and is stirred continuously at 40 DEG C and carries out ion-exchange reactions 2 hours, by the Na in presoma+It is replaced into
Cd2+, solution centrifuge, remove supernatant, washed three times with deionized water centrifugal water.Then, gained all solids are added to
0.4MSC(NH2)2Solution (50mL) in and stir 3 hours at 70 DEG C, solution centrifuges, and removes supernatant, and spend from
Sub- water centrifugation washing is three times.Product is obtained into yellow powder in dry 6 hours at 60 DEG C, i.e. CdS modifies TiO2Nanotube is compound
Material.
Embodiment 2：
By 1gTiO2Powder is dissolved in the concentrated NaOH solution of 25mL10M, ultrasonic disperse 30min, is transferred to volume and is
In 50mL reaction kettles, 7h is reacted for 160 DEG C in an oven.Product is washed with deionized to neutrality, is centrifuged, later 60
DEG C baking oven in dry 15h, obtain presoma nanotube.The presoma nanotube of 1g is placed in 0.1MCd (NO3)2·4H2O's
It in solution (50mL), and is stirred continuously at 40 DEG C and carries out ion-exchange reactions 2 hours, by the Na in presoma+It is replaced into
Cd2+, solution centrifuge, remove supernatant, washed three times with deionized water centrifugal water.Then, gained all solids are added to
0.4MSC(NH2)2Solution (50mL) in and stir 3 hours at 70 DEG C, solution centrifuges, and removes supernatant, and spend from
Sub- water centrifugation washing is three times.Product is obtained into yellow powder in dry 6 hours at 60 DEG C, i.e. CdS modifies TiO2Nanotube is compound
Material.
Embodiment 3：
By 1gTiO2Powder is dissolved in the concentrated NaOH solution of 25mL10M, ultrasonic disperse 30min, is transferred to volume and is
In 50mL reaction kettles, 9h is reacted for 160 DEG C in an oven.Product is washed with deionized to neutrality, is centrifuged, later 60
DEG C baking oven in dry 15h, obtain presoma nanotube.The presoma nanotube of 1g is placed in 0.1MCd (NO3)2·4H2O's
It in solution (50mL), and is stirred continuously at 40 DEG C and carries out ion-exchange reactions 2 hours, by the Na in presoma+It is replaced into
Cd2+, solution centrifuge, remove supernatant, washed three times with deionized water centrifugal water.Then, gained all solids are added to
0.4MSC(NH2)2Solution (50mL) in and stir 3 hours at 70 DEG C, solution centrifuges, and removes supernatant, and spend from
Sub- water centrifugation washing is three times.Product is obtained into yellow powder in dry 6 hours at 60 DEG C, i.e. CdS modifies TiO2Nanotube is compound
Material.
Embodiment 4：
By 1gTiO2Powder is dissolved in the concentrated NaOH solution of 25mL10M, ultrasonic disperse 30min, is transferred to volume and is
In 50mL reaction kettles, 8h is reacted for 160 DEG C in an oven.Product is washed with deionized to neutrality, is centrifuged, later 60
DEG C baking oven in dry 15h, obtain presoma nanotube.The presoma nanotube of 1g is placed in 0.1MCd (NO3)2·4H2O's
It in solution (50mL), and is stirred continuously at 40 DEG C and carries out ion-exchange reactions 1 hour, by the Na in presoma+It is replaced into
Cd2+, solution centrifuge, remove supernatant, washed three times with deionized water centrifugal water.Then, gained all solids are added to
0.4MSC(NH2)2Solution (50mL) in and stir 3 hours at 70 DEG C, solution centrifuges, and removes supernatant, and spend from
Sub- water centrifugation washing is three times.Product is obtained into yellow powder in dry 6 hours at 60 DEG C, i.e. CdS modifies TiO2Nanotube is compound
Material.
Embodiment 5：
By 1gTiO2Powder is dissolved in the concentrated NaOH solution of 25mL10M, ultrasonic disperse 30min, is transferred to volume and is
In 50mL reaction kettles, 8h is reacted for 160 DEG C in an oven.Product is washed with deionized to neutrality, is centrifuged, later 60
DEG C baking oven in dry 15h, obtain presoma nanotube.The presoma nanotube of 1g is placed in 0.1MCd (NO3)2·4H2O's
It in solution (50mL), and is stirred continuously at 40 DEG C and carries out ion-exchange reactions 3 hours, by the Na in presoma+It is replaced into
Cd2+, solution centrifuge, remove supernatant, washed three times with deionized water centrifugal water.Then, gained all solids are added to
0.4MSC(NH2)2Solution (50mL) in and stir 3 hours at 70 DEG C, solution centrifuges, and removes supernatant, and spend from
Sub- water centrifugation washing is three times.Product is obtained into yellow powder in dry 6 hours at 60 DEG C, i.e. CdS modifies TiO2Nanotube is compound
Material.
Embodiment 6：
By 1gTiO2Powder is dissolved in the concentrated NaOH solution of 25mL10M, ultrasonic disperse 30min, is transferred to volume and is
In 50mL reaction kettles, 8h is reacted for 160 DEG C in an oven.Product is washed with deionized to neutrality, is centrifuged, later 60
DEG C baking oven in dry 15h, obtain presoma nanotube.The presoma nanotube of 1g is placed in 0.1MCd (NO3)2·4H2O's
It in solution (50mL), and is stirred continuously at 40 DEG C and carries out ion-exchange reactions 2 hours, by the Na in presoma+It is replaced into
Cd2+, solution centrifuge, remove supernatant, washed three times with deionized water centrifugal water.Then, gained all solids are added to
0.4MSC(NH2)2Solution (50mL) in and stir 2 hours at 70 DEG C, solution centrifuges, and removes supernatant, and spend from
Sub- water centrifugation washing is three times.Product is obtained into yellow powder in dry 6 hours at 60 DEG C, i.e. CdS modifies TiO2Nanotube is compound
Material.
Embodiment 7：
By 1gTiO2Powder is dissolved in the concentrated NaOH solution of 25mL10M, ultrasonic disperse 30min, is transferred to volume and is
In 50mL reaction kettles, 8h is reacted for 160 DEG C in an oven.Product is washed with deionized to neutrality, is centrifuged, later 60
DEG C baking oven in dry 15h, obtain presoma nanotube.The presoma nanotube of 1g is placed in 0.1MCd (NO3)2·4H2O's
It in solution (50mL), and is stirred continuously at 40 DEG C and carries out ion-exchange reactions 2 hours, by the Na in presoma+It is replaced into
Cd2+, solution centrifuge, remove supernatant, washed three times with deionized water centrifugal water.Then, gained all solids are added to
0.4MSC(NH2)2Solution (50mL) in and stir 4 hours at 70 DEG C, solution centrifuges, and removes supernatant, and spend from
Sub- water centrifugation washing is three times.Product is obtained into yellow powder in dry 6 hours at 60 DEG C, i.e. CdS modifies TiO2Nanotube is compound
Material.
Embodiment 8：
By 1gTiO2Powder is dissolved in the concentrated NaOH solution of 25mL10M, ultrasonic disperse 30min, is transferred to volume and is
In 50mL reaction kettles, 8h is reacted for 160 DEG C in an oven.Product is washed with deionized to neutrality, is centrifuged, later 60
DEG C baking oven in dry 15h, obtain presoma nanotube.The presoma nanotube of 1g is placed in 0.1MCd (NO3)2·4H2O's
It in solution (50mL), and is stirred continuously at 35 DEG C and carries out ion-exchange reactions 2 hours, by the Na in presoma+It is replaced into
Cd2+, solution centrifuge, remove supernatant, washed three times with deionized water centrifugal water.Then, gained all solids are added to
0.4MSC(NH2)2Solution (50mL) in and stir 3 hours at 70 DEG C, solution centrifuges, and removes supernatant, and spend from
Sub- water centrifugation washing is three times.Product is obtained into yellow powder in dry 6 hours at 60 DEG C, i.e. CdS modifies TiO2Nanotube is compound
Material.
Embodiment 9：
By 1gTiO2Powder is dissolved in the concentrated NaOH solution of 25mL10M, ultrasonic disperse 30min, is transferred to volume and is
In 50mL reaction kettles, 8h is reacted for 160 DEG C in an oven.Product is washed with deionized to neutrality, is centrifuged, later 60
DEG C baking oven in dry 15h, obtain presoma nanotube.The presoma nanotube of 1g is placed in 0.1MCd (NO3)2·4H2O's
It in solution (50mL), and is stirred continuously at 45 DEG C and carries out ion-exchange reactions 2 hours, by the Na in presoma+It is replaced into
Cd2+, solution centrifuge, remove supernatant, washed three times with deionized water centrifugal water.Then, gained all solids are added to
0.4MSC(NH2)2Solution (50mL) in and stir 3 hours at 70 DEG C, solution centrifuges, and removes supernatant, and spend from
Sub- water centrifugation washing is three times.Product is obtained into yellow powder in dry 6 hours at 60 DEG C, i.e. CdS modifies TiO2Nanotube is compound
Material.
Embodiment 10：
By 1gTiO2Powder is dissolved in the concentrated NaOH solution of 25mL10M, ultrasonic disperse 30min, is transferred to volume and is
In 50mL reaction kettles, 8h is reacted for 160 DEG C in an oven.Product is washed with deionized to neutrality, is centrifuged, later 60
DEG C baking oven in dry 15h, obtain presoma nanotube.The presoma nanotube of 1g is placed in 0.1MCd (NO3)2·4H2O's
It in solution (50mL), and is stirred continuously at 40 DEG C and carries out ion-exchange reactions 2 hours, by the Na in presoma+It is replaced into
Cd2+, solution centrifuge, remove supernatant, washed three times with deionized water centrifugal water.Then, gained all solids are added to
0.4MSC(NH2)2Solution (50mL) in and stir 3 hours at 60 DEG C, solution centrifuges, and removes supernatant, and spend from
Sub- water centrifugation washing is three times.Product is obtained into yellow powder in dry 6 hours at 60 DEG C, i.e. CdS modifies TiO2Nanotube is compound
Material.
Embodiment 11：
By 1gTiO2Powder is dissolved in the concentrated NaOH solution of 25mL10M, ultrasonic disperse 30min, is transferred to volume and is
In 50mL reaction kettles, 8h is reacted for 160 DEG C in an oven.Product is washed with deionized to neutrality, is centrifuged, later 60
DEG C baking oven in dry 15h, obtain presoma nanotube.The presoma nanotube of 1g is placed in 0.1MCd (NO3)2·4H2O's
It in solution (50mL), and is stirred continuously at 40 DEG C and carries out ion-exchange reactions 2 hours, by the Na in presoma+It is replaced into
Cd2+, solution centrifuge, remove supernatant, washed three times with deionized water centrifugal water.Then, gained all solids are added to
0.4MSC(NH2)2Solution (50mL) in and stir 3 hours at 65 DEG C, solution centrifuges, and removes supernatant, and spend from
Sub- water centrifugation washing is three times.Product is obtained into yellow powder in dry 6 hours at 60 DEG C, i.e. CdS modifies TiO2Nanotube is compound
Material.
Embodiment 12：
By 1gTiO2Powder is dissolved in the concentrated NaOH solution of 25mL10M, ultrasonic disperse 30min, is transferred to volume and is
In 50mL reaction kettles, 8h is reacted for 160 DEG C in an oven.Product is washed with deionized to neutrality, is centrifuged, later 60
DEG C baking oven in dry 15h, obtain presoma nanotube.The presoma nanotube of 1g is placed in 0.1MCd (NO3)2·4H2O's
It in solution (50mL), and is stirred continuously at 40 DEG C and carries out ion-exchange reactions 2 hours, by the Na in presoma+It is replaced into
Cd2+, solution centrifuge, remove supernatant, washed three times with deionized water centrifugal water.Then, gained all solids are added to
0.4MSC(NH2)2Solution (50mL) in and stir 3 hours at 75 DEG C, solution centrifuges, and removes supernatant, and spend from
Sub- water centrifugation washing is three times.Product is obtained into yellow powder in dry 6 hours at 60 DEG C, i.e. CdS modifies TiO2Nanotube is compound
Material.
Embodiment 13：
By 1gTiO2Powder is dissolved in the concentrated NaOH solution of 25mL10M, ultrasonic disperse 30min, is transferred to volume and is
In 50mL reaction kettles, 8h is reacted for 160 DEG C in an oven.Product is washed with deionized to neutrality, is centrifuged, later 60
DEG C baking oven in dry 15h, obtain presoma nanotube.The presoma nanotube of 1g is placed in 0.1MCd (NO3)2·4H2O's
It in solution (50mL), and is stirred continuously at 40 DEG C and carries out ion-exchange reactions 2 hours, by the Na in presoma+It is replaced into
Cd2+, solution centrifuge, remove supernatant, washed three times with deionized water centrifugal water.Then, gained all solids are added to
0.4MSC(NH2)2Solution (50mL) in and stir 3 hours at 80 DEG C, solution centrifuges, and removes supernatant, and spend from
Sub- water centrifugation washing is three times.Product is obtained into yellow powder in dry 6 hours at 60 DEG C, i.e. CdS modifies TiO2Nanotube is compound
Material.
Embodiment 14：
By 1gTiO2Powder is dissolved in the concentrated NaOH solution of 25mL10M, ultrasonic disperse 30min, is transferred to volume and is
In 50mL reaction kettles, 8h is reacted for 150 DEG C in an oven.Product is washed with deionized to neutrality, is centrifuged, later 60
DEG C baking oven in dry 15h, obtain presoma nanotube.The presoma nanotube of 1g is placed in 0.1MCd (NO3)2·4H2O's
It in solution (50mL), and is stirred continuously at 40 DEG C and carries out ion-exchange reactions 2 hours, by the Na in presoma+It is replaced into
Cd2+, solution centrifuge, remove supernatant, washed three times with deionized water centrifugal water.Then, gained all solids are added to
0.4MSC(NH2)2Solution (50mL) in and stir 3 hours at 70 DEG C, solution centrifuges, and removes supernatant, and spend from
Sub- water centrifugation washing is three times.Product is obtained into yellow powder in dry 6 hours at 60 DEG C, i.e. CdS modifies TiO2Nanotube is compound
Material.
Embodiment 15：
By 1gTiO2Powder is dissolved in the concentrated NaOH solution of 25mL10M, ultrasonic disperse 30min, is transferred to volume and is
In 50mL reaction kettles, 8h is reacted for 170 DEG C in an oven.Product is washed with deionized to neutrality, is centrifuged, later 60
DEG C baking oven in dry 15h, obtain presoma nanotube.The presoma nanotube of 1g is placed in 0.1MCd (NO3)2·4H2O's
It in solution (50mL), and is stirred continuously at 40 DEG C and carries out ion-exchange reactions 2 hours, by the Na in presoma+It is replaced into
Cd2+, solution centrifuge, remove supernatant, washed three times with deionized water centrifugal water.Then, gained all solids are added to
0.4MSC(NH2)2Solution (50mL) in and stir 3 hours at 70 DEG C, solution centrifuges, and removes supernatant, and spend from
Sub- water centrifugation washing is three times.Product is obtained into yellow powder in dry 6 hours at 60 DEG C, i.e. CdS modifies TiO2Nanotube is compound
Material.
Embodiment 16：
By 1gTiO2Powder is dissolved in the concentrated NaOH solution of 25mL10M, ultrasonic disperse 30min, is transferred to volume and is
In 50mL reaction kettles, 8h is reacted for 180 DEG C in an oven.Product is washed with deionized to neutrality, is centrifuged, later 60
DEG C baking oven in dry 15h, obtain presoma nanotube.The presoma nanotube of 1g is placed in 0.1MCd (NO3)2·4H2O's
It in solution (50mL), and is stirred continuously at 40 DEG C and carries out ion-exchange reactions 2 hours, by the Na in presoma+It is replaced into
Cd2+, solution centrifuge, remove supernatant, washed three times with deionized water centrifugal water.Then, gained all solids are added to
0.4MSC(NH2)2Solution (50mL) in and stir 3 hours at 70 DEG C, solution centrifuges, and removes supernatant, and spend from
Sub- water centrifugation washing is three times.Product is obtained into yellow powder in dry 6 hours at 60 DEG C, i.e. CdS modifies TiO2Nanotube is compound
Material.
Attached drawing 1 is the CdS modifications TiO prepared2The XRD diagram of nanometer tube composite materials, at 24.61 °, 26.65 °, 28.3 °,
Occurs the peak of CdS (JCPDSNo.01-078-2486) at 48.11 °；There is TiO at 25.33 °2(JCPDSNo.01-080-
0006) peak；SEM photograph in attached drawing 2 can be seen that the presoma nanotube size uniform of preparation, and the nanotube without aggregation
It generates, the length of pipe has big draw ratio up to 2~5 μm, a diameter of 20~30nm；Attached drawing 3 is the CdS modifications prepared
TiO2The TEM photos of nanometer tube composite materials, it can be seen that for CdS particulate loads on the surface of nanotube, size uniform is good to divide
It dissipates, granular size is 6~10nm；Attached drawing 4 is the CdS modifications TiO prepared2Nanometer tube composite materials and business TiO2UV-Vis
Photo, business TiO2Occur absorption edge at 380nm, and the CdS prepared by the present invention modifies TiO2Nanometer tube composite materials exist
There is absorption edge at wavelength 535nm, it is with business TiO2Compared to red shift about 155nm, there is wider array of photoresponse range.
Unaccomplished matter of the present invention is known technology.
Claims (4)
1. a kind of CdS modifies TiO2The preparation method of nanometer tube composite materials, it is characterized in that this approach includes the following steps：
（1）The preparation of presoma：By TiO2Powder is added in concentrated NaOH solution, and 10 ~ 30 min of ultrasonic disperse is transferred to later
In hydrothermal reaction kettle, 6 ~ 12 h are kept the temperature at 100 ~ 180 DEG C；Product is washed with deionized water to neutrality, is then centrifuged for detaching, and dries
It is dry, prepare presoma nanotube；
Wherein, 0.5 ~ 1 gTiO is added in the concentrated NaOH solution of every 25 mL2Powder；
（2）CdS modifies TiO2The preparation of nanometer tube composite materials：Presoma is placed in Cd (NO3)2·4H2In the solution of O, and
It is stirred 1 ~ 3 hour at 30 ~ 50 DEG C, solution centrifuges, and removes supernatant, deionized water centrifugation washing；Then, gained is consolidated
Body is added to SC (NH2)2 Solution in, and stirred 2 ~ 4 hours at 50 ~ 80 DEG C, solution centrifuges, and removes supernatant, remains
It is dry after excess washing, yellow powder is obtained, i.e. CdS modifies TiO2Nanometer tube composite materials；
Wherein, every 30 ~ 80 mLCd (NO3)2·4H2The solution of O adds 1 g presomas, molar ratio to be Cd (NO3)2·4H2O：SC
(NH2)2=1:0.25~4；Cd(NO3)2·4H2A concentration of 0.1 ~ 0.4 mol/L, SC (NH of the solution of O2)2A concentration of 0.1 ~
0.4 mol/L。
2. CdS as described in claim 1 modifies TiO2The preparation method of nanometer tube composite materials, it is characterized in that the hydrogen-oxygen
It is 10 mol/L to change sodium solution concentration.
3. CdS as described in claim 1 modifies TiO2The preparation method of nanometer tube composite materials, it is characterized in that the ultrasound
The frequency of dispersion is 40 Hz.
4. CdS as described in claim 1 modifies TiO2The preparation method of nanometer tube composite materials, it is characterized in that the centrifugation
The rotating speed of separation is 8000 ~ 10000 r/min.
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| EP1518601A1 (en) * | 2002-06-03 | 2005-03-30 | Asahi Kasei Kabushiki Kaisha | Photocatalyst composition |
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| EP1518601A1 (en) * | 2002-06-03 | 2005-03-30 | Asahi Kasei Kabushiki Kaisha | Photocatalyst composition |
| CN1803278A (en) * | 2006-01-19 | 2006-07-19 | 西安交通大学 | Tantalum titanate cadmium sulphide platinum-carried laminated composite catalyst and its preparation method |
| CN103071446A (en) * | 2013-02-02 | 2013-05-01 | 南京理工大学 | Two-step hydrothermal preparation method of magnetic sodium titanate nanotubes and application of magnetic sodium titanate nanotubes to adsorption removal of Pb<2+> in water |
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