CN108479776A - A kind of preparation method of graphene/iron/titanium dioxide composite photocatalyst - Google Patents
A kind of preparation method of graphene/iron/titanium dioxide composite photocatalyst Download PDFInfo
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- CN108479776A CN108479776A CN201810207400.8A CN201810207400A CN108479776A CN 108479776 A CN108479776 A CN 108479776A CN 201810207400 A CN201810207400 A CN 201810207400A CN 108479776 A CN108479776 A CN 108479776A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 189
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 122
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 57
- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 29
- 229960005191 ferric oxide Drugs 0.000 title claims abstract description 23
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 235000013980 iron oxide Nutrition 0.000 title claims abstract description 23
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000002071 nanotube Substances 0.000 claims abstract description 72
- 229910052742 iron Inorganic materials 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000007787 solid Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 11
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 8
- 238000001802 infusion Methods 0.000 claims abstract description 7
- 230000008569 process Effects 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 7
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000005485 electric heating Methods 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 239000007788 liquid Substances 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 239000010865 sewage Substances 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 2
- 229910021645 metal ion Inorganic materials 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 2
- 238000002474 experimental method Methods 0.000 abstract 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 abstract 1
- 239000000463 material Substances 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 5
- 238000007664 blowing Methods 0.000 description 4
- 239000000975 dye Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000007704 transition Effects 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- 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
- B01J37/0201—Impregnation
-
- 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
- B01J37/04—Mixing
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The present invention provides a kind of preparation methods of graphene/iron/titanium dioxide composite photocatalyst,Iron/Titanium dioxide nanotube/ graphene composite material is prepared using wet-chemical mixing method,Wherein iron/titania nanotube can be prepared using iron chloride solid and titania nanotube as source of iron and titania nanotube source by infusion process,Titania nanotube is made by hydro-thermal method by raw material of P25 types nano-titanium dioxide,Pass through scientific matching between each raw material,The stringent control of experiment condition,In conjunction with the good absorption property of graphene and metal ion to the acquisition performance of electronics,Increase the specific surface area of titanium dioxide,Graphene/iron obtained/titania nanotube photocatalysis composite specific surface area is set to increase,Absorption property enhances,It is easy to precipitate after carrying out adsorption treatment to sewage,Convenient for filtering,Advantageously account for separation of solid and liquid problem,It is widened visible light region,Visible light catalytic effect effectively improves.
Description
Technical field
The present invention relates to visible light catalytic nanotube fields, and in particular to a kind of graphene/iron/titanium dioxide complex light is urged
The preparation method of agent.
Background technology
Graphene is a kind of novel carbonaceous thin-film material, with SP between carbon atom2Hydridization is attached, and is formed hexa-atomic by carbon
The honeycomb crystal lattice structure of ring composition, basic structural unit are most stable of benzene hexatomic ring in organic material, theoretic throat
It is two-dimensional material most thin in presently found nature only there are one the thickness of atom for 0.335nm.
TiO2Nanotube makes it in photocatalytic degradation, photodissociation because of its excellent photoelectricity, catalysis, sensing capabilities
The fields such as water hydrogen manufacturing, dye-sensitized solar cells, sensor material are with a wide range of applications.But due to TiO2Itself prohibits
Bandwidth is larger, and electronics can only be excited under the conditions of ultraviolet light occurs transition, strongly limits it in industrial circle
Using.TiO2The visible light catalytic performance of nanotube can, metal nonmetallic by doped portion and noble metal, composite semiconductor
Material is improved.
The unique two-dimension plane structure of graphene itself and excellent electric property are so that it can as a good base
Bottom material and electron acceptor and be applied in semiconductor composite, it can be by fast transfer light induced electron effectively
Inhibit the compound of photo-generate electron-hole.The huge specific surface area of graphene and strong adsorption capacity, contribute to the suction of dye molecule
It is attached, promote the decomposition of dyestuff, to improve photocatalysis efficiency.Therefore, these excellent performances based on graphene, have had at present
Many relevant researchs prepare graphene/titania composite material by a variety of different methods, improving photocatalysis
Efficiency.
Graphene is combined to form hybrid material with titanium dioxide, on the one hand enhances light absorpting ability, has widened its absorption
Range responds visible light；On the other hand electronics transfer is promoted, after TiO2 absorbs photon energy, valence-band electrons are excited
And conduction band is transitted to, excitation electronics flows into graphene sheet layer structure.Exactly because graphene has excellent electric conductivity, swash
Power generation will not be assembled around catalysis material, to reduce the probability of recombination in hole and electronics.Graphene and Ti-O-
C chemical bonds interact, and change TiO2Original energy gap, TiO2Larger photochemical activity is shown in visible region,
To increase TiO2For the utilization rate of visible light, is in addition conducive to the progress of reaction, effectively inhibits photo-generate electron-hole
It is compound；In addition the big specific surface area of graphene itself increases the absorption of dyestuff, may advantageously facilitate the photocatalytic degradation of dyestuff.
However, how more complicated the current method for preparing titanium dioxide/graphene is, the bad control of reaction process, reaction step is opposite
It is cumbersome, and photocatalysis performance needs to be further increased.
Invention content
Limited by energy gap for titanium dioxide, can only absorb a small amount of ultraviolet light of solar radiation, specific surface area it is small and
The problems such as photocatalysis efficiency is low, the present invention provides a kind of preparation method of graphene/iron/titanium dioxide composite photocatalyst,
It can increase material specific surface area, widen visible region, improve visible light catalytic effect.
The present invention uses technical solution below：
A kind of preparation method of graphene/iron/titanium dioxide composite photocatalyst, includes the following steps：
(1) hydro-thermal method prepares titania nanotube：By weight, 1 part of P25 type nano-titanium dioxide is weighed to be scattered in
In the sodium hydroxide solution of 80-100 parts of a concentration of 10mol/L, magnetic agitation 0.4-0.6h is placed in reaction kettle, in electric heating perseverance
150 DEG C of isothermal reaction 48h, are cooled to room temperature in warm air dry oven, low temperature drying, and titanium dioxide is obtained in Muffle kiln roasting
Nanotube；
(2) infusion process prepares iron/titania nanotube：By weight, by 3.5-27 parts of FeCl3·6H2O solids and 80
Titania nanotube mixing obtained by part step (1), and be added in the hydrochloric acid solution of 3200 parts of a concentration of 0.1mol/L, system
At presoma mixed liquor, ultrasonic disperse, at room temperature stirring, low temperature drying, Muffle kiln roasting are then carried out successively, is finally prepared
Obtain iron/titania nanotube；
(3) wet-chemical mixing method prepares iron/Titanium dioxide nanotube/ graphene composite material：By weight, 1 part is weighed
Prepared iron/titania nanotube is placed in beaker in step (2), and 0.01-0.05 parts of graphenes are added, then respectively according to
Secondary 4 parts of absolute ethyl alcohols and the 5 parts of distilled water of pipetting stir mixture in beaker at room temperature, dry in baking oven, in Muffle furnace
Roasting, finally obtains graphene/iron/titania nanotube composite photo-catalyst.
Preferably, by weight, the number of the sodium hydroxide solution of a concentration of 10mol/L described in step (1) is 80 parts.
Preferably, the temperature of low temperature drying described in step (1) is 60 degree, drying time 20-30h；The temperature of roasting
It it is 450 DEG C, the time of roasting is 2h, and heating rate is 5 DEG C per minute.
Preferably, the temperature of low temperature drying described in step (1) is 60 degree, and drying time is for 24 hours.
Preferably, by weight, FeCl described in step (2)3·6H2The number of O solids is 19.5 parts.
Preferably, ultrasonic dispersing time described in step (2) be 5-10min, mixing time 2-3h, low temperature drying
Temperature is 60 DEG C, until drying, calcination temperature is 350 DEG C, roasting time 4h, and heating rate is 1 DEG C per minute.
Preferably, by weight, the number of graphene described in step (3) is 0.03 part.
Preferably, the time stirred at room temperature described in step (3) is 3h, and the temperature dried in baking oven is 80 DEG C, Muffle
The temperature of kiln roasting is 400 DEG C, roasting time 2h.
The invention has the advantages that：
1. the present invention fully combines the acquisition performance of the good absorption property of graphene and metal ion to electronics, increase
The specific surface area of titanium dioxide, has widened visible light region, improves the photocatalytic activity of titania nanotube and its make
With the service life, there is prodigious application potential in terms of sewage disposal；2. titania nanotube is combined with graphene increases absorption
Performance is easy to precipitate after carrying out adsorption treatment to sewage, convenient for filtering, advantageously accounts for separation of solid and liquid problem；3. present invention system
It is simple to make method, material is easy to get, and feasibility is high, can reuse, can devote actual production.
Description of the drawings
Fig. 1 is P25 types nano-titanium dioxide, iron/titania nanotube and graphene/iron/titanium dioxide in embodiment 1
The XRD diagram of nanotube composite photo-catalyst.
Fig. 2 is P25 types nano-titanium dioxide, iron/titania nanotube and graphene/iron/titanium dioxide in embodiment 1
The unrestrained transmitting figure of the UV, visible light of nanotube composite photo-catalyst.
Fig. 3 is that the SEM of P25 type nano-titanium dioxides schemes.
Fig. 4 is the SEM figures of iron/titania nanotube in embodiment 1.
Fig. 5 is the SEM figures of graphene/iron/titania nanotube composite photo-catalyst in embodiment 1.
Wherein, in Fig. 1 and Fig. 21 be P25 type nano-titanium dioxides；2 for iron/titania nanotube (by weight,
FeCl3·6H2The ratio of O solids and titania nanotube is 19.5：80)；3 is compound for graphene/iron/titania nanotube
(by weight, the ratio of graphene and iron/titania nanotube is 0.03 to photochemical catalyst：1).
Specific implementation mode
The present invention is specifically described with reference to the accompanying drawings and examples：
Embodiment 1
(1) preparation of titania nanotube：
By weight, weigh 1 part of P25 types nano-titanium dioxide (its SEM scheme as shown in Figure 3) be scattered in 80 parts it is a concentration of
In the sodium hydroxide solution of 10mol/L, magnetic agitation 0.4-0.6h is placed in reaction kettle, in electric heating constant-temperature blowing drying box
150 DEG C of isothermal reaction 48h, are cooled to room temperature, at 60 DEG C low temperature drying for 24 hours, in Muffle furnace 450 DEG C roasting 2h, wherein heating up
Speed is 5 DEG C per minute, obtains titania nanotube.
(2) infusion process prepares iron/titania nanotube：
By weight, by 19.5 parts of FeCl3·6H2Titania nanotube obtained by O solids and 80 parts of steps (1) is mixed
It closes, and is added in the hydrochloric acid solution of 3200 parts of a concentration of 0.1mol/L, presoma mixed liquor is made, then carry out ultrasound point successively
5-10min is dissipated, stirs 2-3h at room temperature, low temperature drying is until dry, 350 DEG C of roasting 4h in Muffle furnace, wherein heating up at 60 DEG C
Speed is 1 DEG C per minute, and iron/titania nanotube is finally prepared (its SEM schemes as shown in Figure 4).
(3) wet-chemical mixing method prepares iron/Titanium dioxide nanotube/ graphene composite material：
By weight, it weighs iron/titania nanotube prepared in 1 part of step (2) to be placed in beaker, is added 0.03
Part graphene, then pipettes 4 parts of absolute ethyl alcohols and 5 parts of distilled water in beaker, mixture is stirred at room temperature successively respectively
3h, 80 DEG C of dryings in baking oven, 400 DEG C of roasting 2h in Muffle furnace finally obtain graphene/iron/titania nanotube complex light
Catalyst (its SEM schemes as shown in Figure 5).
Wherein, P25 types nano-titanium dioxide, iron/titania nanotube and graphene/iron/titania nanotube are multiple
The XRD diagram of closing light catalyst is as shown in Figure 1, wherein open squares represent TiO2 characteristic peaks；Filled box represents sodium chloride feature
Peak.
P25 types nano-titanium dioxide, iron/titania nanotube and graphene/iron/titania nanotube complex light are urged
The unrestrained transmitting figure of the UV, visible light of agent is as shown in Figure 2.
Embodiment 2
(1) preparation of titania nanotube：
By weight, it is molten to weigh the sodium hydroxide that 1 part of P25 type nano-titanium dioxide is scattered in 100 parts of a concentration of 10mol/L
In liquid, magnetic agitation 0.4-0.6h is placed in reaction kettle, and 150 DEG C of isothermal reaction 48h, cold in electric heating constant-temperature blowing drying box
But to room temperature, low temperature drying 20h at 60 DEG C, 450 DEG C of roasting 2h in Muffle furnace, wherein heating rate is 5 DEG C per minute, is obtained
Titania nanotube.
(2) infusion process prepares iron/titania nanotube：
By weight, by 27 parts of FeCl3·6H2O solids are mixed with the titania nanotube obtained by 80 parts of steps (1),
And be added in the hydrochloric acid solution of 3200 parts of a concentration of 0.1mol/L, presoma mixed liquor is made, then carries out ultrasonic disperse successively
5-10min stirs 2-3h at room temperature, and low temperature drying is until dry, 350 DEG C of roasting 4h in Muffle furnace, wherein heating speed at 60 DEG C
Degree is 1 DEG C per minute, and iron/titania nanotube is finally prepared.
(3) wet-chemical mixing method prepares iron/Titanium dioxide nanotube/ graphene composite material：
By weight, it weighs iron/titania nanotube prepared in 1 part of step (2) to be placed in beaker, is added 0.05
Part graphene, then pipettes 4 parts of absolute ethyl alcohols and 5 parts of distilled water in beaker, mixture is stirred at room temperature successively respectively
3h, 80 DEG C of dryings in baking oven, 400 DEG C of roasting 2h in Muffle furnace finally obtain graphene/iron/titania nanotube complex light
Catalyst.
Embodiment 3
(1) preparation of titania nanotube：
By weight, it is molten to weigh the sodium hydroxide that 1 part of P25 type nano-titanium dioxide is scattered in 90 parts of a concentration of 10mol/L
In liquid, magnetic agitation 0.4-0.6h is placed in reaction kettle, and 150 DEG C of isothermal reaction 48h, cold in electric heating constant-temperature blowing drying box
But to room temperature, low temperature drying obtains titania nanotube in Muffle kiln roasting.
(2) infusion process prepares iron/titania nanotube：
By weight, by 3.5 parts of FeCl3·6H2Titania nanotube obtained by O solids and 80 parts of steps (1) is mixed
It closes, and is added in the hydrochloric acid solution of 3200 parts of a concentration of 0.1mol/L, presoma mixed liquor is made, then carry out ultrasound point successively
It dissipates, stirs at room temperature, low temperature drying is until iron/titania nanotube is finally prepared in drying, Muffle kiln roasting.
(3) wet-chemical mixing method prepares iron/Titanium dioxide nanotube/ graphene composite material：
By weight, it weighs iron/titania nanotube prepared in 1 part of step (2) to be placed in beaker, is added 0.01
Part graphene, then pipettes 4 parts of absolute ethyl alcohols and 5 parts of distilled water in beaker, mixture is stirred at room temperature successively respectively,
Dry in baking oven, Muffle kiln roasting finally obtains graphene/iron/titania nanotube composite photo-catalyst.
Embodiment 4
(1) preparation of titania nanotube：
By weight, it is molten to weigh the sodium hydroxide that 1 part of P25 type nano-titanium dioxide is scattered in 90 parts of a concentration of 10mol/L
In liquid, magnetic agitation 0.4-0.6h is placed in reaction kettle, and 150 DEG C of isothermal reaction 48h, cold in electric heating constant-temperature blowing drying box
But to room temperature, low temperature drying 30h at 60 DEG C, 450 DEG C of roasting 2h in Muffle furnace, wherein heating rate is 5 DEG C per minute, is obtained
Titania nanotube.
(2) infusion process prepares iron/titania nanotube：
By weight, by 3.5 parts of FeCl3·6H2Titania nanotube obtained by O solids and 80 parts of steps (1) is mixed
It closes, and is added in the hydrochloric acid solution of 3200 parts of a concentration of 0.1mol/L, presoma mixed liquor is made, then carry out ultrasound point successively
5-10min is dissipated, stirs 2-3h at room temperature, low temperature drying is until dry, 350 DEG C of roasting 4h in Muffle furnace, wherein heating up at 60 DEG C
Speed is 1 DEG C per minute, and iron/titania nanotube is finally prepared.
(3) wet-chemical mixing method prepares iron/Titanium dioxide nanotube/ graphene composite material：
By weight, it weighs iron/titania nanotube prepared in 1 part of step (2) to be placed in beaker, is added 0.01
Part graphene, then pipettes 4 parts of absolute ethyl alcohols and 5 parts of distilled water in beaker, mixture is stirred at room temperature successively respectively
3h, 80 DEG C of dryings in baking oven, 400 DEG C of roasting 2h in Muffle furnace finally obtain graphene/iron/titania nanotube complex light
Catalyst.
Certainly, above description is not limitation of the present invention, and the present invention is also not limited to the example above, this technology neck
The variations, modifications, additions or substitutions that the technical staff in domain is made in the essential scope of the present invention should also belong to the present invention's
Protection domain.
Claims (8)
1. a kind of preparation method of graphene/iron/titanium dioxide composite photocatalyst, which is characterized in that include the following steps：
(1) hydro-thermal method prepares titania nanotube：By weight, it weighs 1 part of P25 type nano-titanium dioxide and is scattered in 80-100
In the sodium hydroxide solution of a concentration of 10mol/L of part, magnetic agitation 0.4-0.6h is placed in reaction kettle, in electric heating constant temperature air blast
150 DEG C of isothermal reaction 48h, are cooled to room temperature in drying box, low temperature drying, and nano titania is obtained in Muffle kiln roasting
Pipe；
(2) infusion process prepares iron/titania nanotube：By weight, by 3.5-27 parts of FeCl3·6H2O solids and 80 parts of steps
Suddenly the titania nanotube mixing obtained by (1), and be added in the hydrochloric acid solution of 3200 parts of a concentration of 0.1mol/L, before being made
Body mixed liquor is driven, ultrasonic disperse, at room temperature stirring, low temperature drying, Muffle kiln roasting is then carried out successively, is finally prepared
Iron/titania nanotube；
(3) wet-chemical mixing method prepares iron/Titanium dioxide nanotube/ graphene composite material：By weight, 1 part of step is weighed
(2) prepared iron/titania nanotube is placed in beaker in, and 0.01-0.05 parts of graphenes are added, then move successively respectively
It takes 4 parts of absolute ethyl alcohols and 5 parts of distilled water in beaker, mixture is stirred at room temperature, it is dry in baking oven, it is roasted in Muffle furnace
It burns, finally obtains graphene/iron/titania nanotube composite photo-catalyst.
2. a kind of preparation method of graphene/iron/titanium dioxide composite photocatalyst according to claim 1, feature
It is, by weight, the number of the sodium hydroxide solution of a concentration of 10mol/L described in step (1) is 80 parts.
3. a kind of preparation method of graphene/iron/titanium dioxide composite photocatalyst according to claim 1 or 2, special
Sign is that the temperature of low temperature drying described in step (1) is 60 degree, drying time 20-30h；The temperature of roasting is 450 DEG C,
The time of roasting is 2h, and heating rate is 5 DEG C per minute.
4. a kind of preparation method of graphene/iron/titanium dioxide composite photocatalyst according to claim 3, feature
It is, drying time described in step (1) is for 24 hours.
5. a kind of preparation method of graphene/iron/titanium dioxide composite photocatalyst according to claim 1, feature
It is, by weight, FeCl described in step (2)3·6H2The number of O solids is 19.5 parts.
6. a kind of preparation method of graphene/iron/titanium dioxide composite photocatalyst according to claim 1 or 5, special
Sign is that ultrasonic dispersing time described in step (2) is 5-10min, and the temperature of mixing time 2-3h, low temperature drying are 60
DEG C, until drying, calcination temperature is 350 DEG C, roasting time 4h, and heating rate is 1 DEG C per minute.
7. a kind of preparation method of graphene/iron/titanium dioxide composite photocatalyst according to claim 1, feature
It is, by weight, the number of graphene described in step (3) is 0.03 part.
8. a kind of preparation method of graphene/iron/titanium dioxide composite photocatalyst according to claim 1 or claim 7, special
Sign is that the time stirred at room temperature described in step (3) is 3h, and the temperature dried in baking oven is 80 DEG C, Muffle kiln roasting
Temperature be 400 DEG C, roasting time 2h.
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