CN108722386B - Polymer-induced graphene growth multi-morphology TiO2Method for preparing photocatalyst - Google Patents
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 21
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 38
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- 230000001699 photocatalysis Effects 0.000 claims abstract description 23
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- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 22
- 239000001257 hydrogen Substances 0.000 claims abstract description 22
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- 238000004519 manufacturing process Methods 0.000 claims abstract description 20
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- 239000000178 monomer Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 15
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- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 6
- 229930192474 thiophene Natural products 0.000 claims description 5
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 3
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- 125000000168 pyrrolyl group Chemical group 0.000 claims description 2
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- LCRMGUFGEDUSOG-UHFFFAOYSA-N naphthalen-1-ylsulfonyloxymethyl naphthalene-1-sulfonate;sodium Chemical compound [Na].C1=CC=C2C(S(=O)(OCOS(=O)(=O)C=3C4=CC=CC=C4C=CC=3)=O)=CC=CC2=C1 LCRMGUFGEDUSOG-UHFFFAOYSA-N 0.000 description 1
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- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
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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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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- B01J35/23—
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- B01J35/39—
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- B01J35/393—
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- B01J35/40—
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- B01J35/51—
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- 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
- B01J37/009—Preparation by separation, e.g. by filtration, decantation, screening
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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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
- B01J37/035—Precipitation on carriers
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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
- B01J37/04—Mixing
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a polymer-induced graphene growth multi-morphology TiO2A method of photocatalyst comprising the steps of: 1) mixing graphene and distilled water, and carrying out ultrasonic stirring to obtain a graphene dispersion liquid; 2) under the condition of ice-water bath, mixing and stirring a dispersing agent, a polymer monomer and a graphene dispersion liquid to obtain a first mixed solution; 3) under the condition of ice-water bath, dissolving a titanium-containing compound in concentrated acid to obtain a second mixed solution; 4) under the condition of ice-water bath, mixing and stirring the second mixed solution and an initiator to obtain a third mixed solution; mixing and stirring the first mixed solution and the third mixed solution, and then carrying out hydrothermal reaction; after the reaction is finished, carrying out post-treatment to obtain TiO2A graphene composite material. The invention combines the characteristics of promoting electron transfer and exposing high-energy surface by multiple heterojunctions to realize high-efficiency photocatalytic hydrogen production and photodegradation of organic pollutants. The preparation method of the invention has the advantages of simple operation, short reaction time, uniform grain size and less agglomeration.
Description
Technical Field
The invention belongs to the technical field of photocatalysis. More particularly, relates to polymer-induced graphene growth multi-morphology TiO2A method of photocatalyst.
Background
The semiconductor photocatalysis water decomposition hydrogen production and the solar energy conversion into chemical energy have the outstanding advantages of low energy consumption, easy operation, environmental protection and the like, and an effective way is provided for solving the problems of environment and energy.
TiO2Is a traditional photocatalyst and is widely used in the fields of photocatalytic degradation of organic matters and hydrogen production. But TiO 22The method has the defect that the electron-hole is easy to recombine, and needs continuous optimization, such as morphology regulation and design of heterogeneous composite materials. Graphene, which is a novel nano material which is the thinnest, the largest in strength and the strongest in electric conduction and heat conduction performance and is discovered at present, has a large specific surface area, can be used as a carrier material of metal nanoparticles, and the performance of the graphene in the aspect of carrier transmission provides a method for preparing an advanced catalyst. Thus, TiO2The photocatalysis performance can be greatly improved by compounding the graphene.
TiO reported so far2The shape regulation is mainly a hydrothermal method, a surfactant induction method or a seed crystal growth method. The single hydrothermal method, the surfactant induction method and the seed crystal growth method have high requirements on the component proportion and the reaction conditions in the reaction precursor solution, the yield is low, the synthesis steps are complicated, and the repeatability is poor. After the graphene is added, the composition of the solution is changed, and the expected morphological structure is difficult to obtain.
Therefore, the invention provides a method for growing multi-morphology TiO on polymer-induced graphene2The method of the photocatalyst has the advantages of simple operation, uniform grain size, controllable appearance and less agglomeration; most importantly, the conductive polymer can further contribute to enhancing electron transfer and prolonging electron service life, and finally the composite material with high full light and visible light photocatalytic activity is obtained.
Disclosure of Invention
The invention aims to provide polymer-induced graphene growth multi-morphology TiO2A method of photocatalyst. The method comprises the steps of dispersing grapheneMixing an agent, a titanium-containing compound, a polymer and an initiator, and then carrying out hydrothermal reaction under certain conditions to obtain TiO2A graphene composite material.
In order to achieve the purpose, the invention adopts the following technical scheme:
polymer-induced graphene growth multi-morphology TiO2A method of photocatalyst comprising the steps of:
1) mixing graphene and distilled water, and carrying out ultrasonic stirring to obtain a graphene dispersion liquid;
2) under the condition of ice-water bath, mixing and stirring a dispersing agent, a polymer monomer and a graphene dispersion liquid to obtain a first mixed solution;
3) under the condition of ice-water bath, dissolving a titanium-containing compound in concentrated acid to obtain a second mixed solution;
4) under the condition of ice-water bath, mixing and stirring the second mixed solution and an initiator to obtain a third mixed solution; mixing and stirring the first mixed solution and the third mixed solution, and then carrying out hydrothermal reaction; after the reaction is finished, carrying out post-treatment to obtain TiO2Graphene composite material (TiO)2/RGO composite).
Further, the titanium-containing compound is present in the anatase form; preferably, the titanium-containing compound is titanium tetrachloride, metatitanic acid, tetrabutyl titanate or tetraisopropyl titanate;
further, the graphene is prepared by one of a chemical vapor deposition method, a micro-mechanical separation method, an oxidation-reduction method, a solvent stripping method or a solvothermal method. The graphene prepared by the method has the characteristics of high conductivity, high strength and super-large specific surface area.
Further, the dispersing agent is sodium dodecyl sulfate, sodium methylene dinaphthalene sulfonate, sodium acrylate, sodium polyacrylate, alkylphenol polyoxyethylene ether phosphate or methacrylate.
Further, the initiator is potassium persulfate, sodium persulfate or ammonium persulfate; preferably, the initiator is ammonium persulfate; the initiator can improve the rate of hydrothermal reaction and reduce energy consumption.
Further, the polymer monomer is pyrrole, aniline, thiophene, phenylene sulfide, sulfur nitride, acetylene or phthalonitrile. In the step 4), the polymer monomer in the first mixed solution forms a polymer through an initiator, and then titanium dioxide with different morphologies grows on the graphene by induction, so that TiO is realized2And (3) uniformly compounding the sheet layer and the graphene sheet layer.
Further, the concentrated acid is concentrated hydrochloric acid, concentrated nitric acid, concentrated sulfuric acid or concentrated acetic acid; preferably, the concentrated acid is 36.5 wt% concentrated hydrochloric acid, 65 wt% concentrated nitric acid, 98 wt% concentrated sulfuric acid or 99.5 wt% concentrated acetic acid; more preferably, the concentrated acid is 36.5 wt% concentrated hydrochloric acid. The concentrated acid of the invention is used for inhibiting the titanium-containing compound from hydrolyzing to generate TiO2。
Further, the temperature of the hydrothermal reaction is 100-300 ℃, and the time of the hydrothermal reaction is 5-48 h.
Further, the post-treatment is to centrifuge, wash and filter the product after reaction, and then dry and grind into powder.
Further, the washing is carried out by using two organic solvents, wherein the organic solvent is ethanol, acetone, dimethyl sulfoxide or dimethylformamide; preferably, the organic solvent is ethanol or acetone. The organic solvent washing is adopted in the invention to remove the dispersant of the reaction.
Further, the mass ratio of the graphene to the distilled water is as follows: 1: 1000-; the mass ratio of the graphene to the polymer monomer is 1: 0.1-50; the mass ratio of the graphene to the titanium-containing compound is 1: 1-10.
Further, the mass ratio of the dispersing agent to the distilled water is 1: 1000-10000.
Further, the mass ratio of the titanium-containing compound to the concentrated acid is 1: 0.1-10; the mass ratio of the initiator to the concentrated acid is 1: 1-50.
The invention induces the graphene to grow titanium dioxide and TiO with different shapes2TiO in/graphene composite material2The shape of the nano-particles can be two-dimensional sheet, rod, sphere, flower or quantum dot; the selection of different polymer monomers or reaction conditions can be controlledMaking TiO2The morphology factor of (1).
The second purpose of the invention is to provide TiO2Application of/graphene composite material and TiO2The graphene composite material can be used for photocatalytic hydrogen production and photocatalytic degradation of organic matters.
TiO of the invention2The graphene composite material improves the performances of photocatalytic hydrogen production and photocatalytic degradation of organic matters through the following three modes: a. the change of oxidation-reduction potential caused by multi-component recombination generates a large amount of active species such as OH and O which can decompose water to produce hydrogen and oxidize organic substances2 2-(ii) a b. Exposing a plurality of active sites; c. a heterogeneous interface.
The invention utilizes polymer to induce the growth of multi-morphology TiO on graphene2The method mainly comprises the steps of adsorbing a titanium-containing compound after covalent grafting or conjugate compounding of a polymer chain and graphene, then generating bending winding in a hydrothermal reaction, and growing TiO with different morphologies on the graphene according to the difference of polymer types2Formation of TiO2A graphene composite material. Under the irradiation of visible light or all light, photo-generated electrons can pass through TiO2Transfer of graphene composites to TiO2The conduction band of the organic dye can promote the separation of electrons and holes to generate a large amount of active species capable of decomposing water to produce hydrogen or degrading dyes, such as OH and O22- - - -; in addition, the LUMO-HOMO energy level of the conductive polymer can further enhance electron transfer and prolong electron lifetime, thereby improving pure TiO2Photocatalytic activity of the monolith.
The invention has the following beneficial effects:
1. TiO prepared by the invention2The graphene composite material has a wide light absorption range and has high-efficiency photocatalytic hydrogen production and organic matter photodegradation properties; and TiO 22The graphene composite material also has good repeatability and excellent stability.
2. The invention combines the characteristics of promoting electron transfer and exposing high-energy surface by multiple heterojunctions to realize high-efficiency photocatalytic hydrogen production and photodegradation of organic pollutants.
3. The preparation method of the invention has the advantages of simple operation, short reaction time, uniform grain size and less agglomeration.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 shows lamellar TiO in example 1 of the present invention2XRD pattern of/RGO composite material.
FIG. 2 shows lamellar TiO in example 1 of the present invention2Can be seen in the figure.
FIG. 3 shows lamellar TiO in example 1 of the present invention2The UV of the/RGO composite can be seen.
FIG. 4 shows lamellar TiO in example 1 of the present invention2Transmission electron microscopy of the/RGO composite.
FIG. 5 shows a spherical TiO particle in example 4 of the present invention2Transmission electron microscopy of the/RGO composite.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below with reference to preferred embodiments and the accompanying drawings. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
Example 1
Polymer-induced graphene growth lamella TiO2A method of photocatalyst comprising the steps of:
1) preparing graphene by taking graphene oxide as a raw material by adopting an oxidation-reduction method;
2) mixing 10mg of graphene and 20mg of distilled water, and carrying out ultrasonic stirring for 15min to obtain a graphene dispersion liquid;
3) under the condition of ice-water bath, adding 5mg of sodium dodecyl sulfate and 50mg of aniline into the graphene dispersion liquid, and then mixing and stirring to obtain a first mixed solution;
4) under the condition of ice-water bath, dissolving 0.5mL of titanium tetrachloride in 0.6mL of concentrated hydrochloric acid, and then stirring for 15min to obtain a second mixed solution;
5) mixing the second mixed solution with 70mg of water under ice-water bath conditionMixing potassium sulfate and stirring for 30min to obtain a third mixed solution; slowly dripping the third mixed solution into the first mixed solution, uniformly stirring, moving into a hydrothermal reaction kettle, and carrying out hydrothermal reaction for 18h at the temperature of 150 ℃; centrifuging the product after the reaction is finished, washing the product twice by using ethanol and acetone respectively, drying the product for 4 hours at the temperature of 60 ℃, and grinding the product into powder to obtain TiO2A graphene composite material.
When XRD is combined with FIG. 1, TiO can be seen2The anatase phase of the graphene composite material is titanium dioxide, and the anatase content is more than 90%.
As can be seen from the transmission electron micrograph of FIG. 4, TiO2TiO in/graphene composite material2Is a two-dimensional sheet structure.
As can be seen from the UV-visible images in conjunction with FIGS. 2 and 3, pure TiO2And TiO2The/graphene composite material can absorb 90% of visible light.
Example 2
Polymer-induced graphene growth rod-shaped TiO2The photocatalyst method is the same as that of example 1, except that:
step 3) adding 5mg of sodium dodecyl sulfate and 50mg of thiophene into the graphene dispersion liquid under the ice-water bath condition, and then mixing and stirring to obtain a first mixed solution;
the time of hydrothermal reaction in the step 5) is 24 hours.
Example 3
Polymer-induced graphene growth flower-shaped TiO2The photocatalyst method is the same as that of example 1, except that:
step 3) adding 5mg of sodium dodecyl sulfate and 100mg of thiophene into the graphene dispersion liquid under the ice-water bath condition, and then mixing and stirring to obtain a first mixed solution;
the time of hydrothermal reaction in the step 5) is 36 h.
Example 4
Polymer-induced graphene-grown spherical TiO2The photocatalyst method is the same as that of example 1, except that:
step 3) adding 5mg of sodium dodecyl sulfate and 50mg of pyrrole into the graphene dispersion liquid under the ice-water bath condition, and then mixing and stirring to obtain a first mixed solution;
the time of hydrothermal reaction in the step 5) is 24 hours.
Example 5
Polymer-induced graphene-grown quantum dot TiO2The photocatalyst method is the same as that of example 1, except that:
step 3) adding 5mg of sodium dodecyl sulfate and 100mg of pyrrole into the graphene dispersion liquid under the ice-water bath condition, and then mixing and stirring to obtain a first mixed solution;
the time of hydrothermal reaction in the step 5) is 36 h.
Examples 6 to 11
Polymer-induced graphene growth TiO2The photocatalyst method is the same as that of example 1, except that: the mass ratio of the graphene to the distilled water in the step 2) is 1:1000, 1:3000, 1:5000, 1:7000, 1:9000 and 1:10000 respectively.
Examples 12 to 17
Polymer-induced graphene growth TiO2The photocatalyst method is the same as that of example 1, except that: the mass ratio of the sodium dodecyl sulfate to the distilled water in the step 3) is 1:1000, 1:3000, 1:5000, 1:7000, 1:9000 and 1:10000 respectively.
Examples 18 to 23
Polymer-induced graphene growth TiO2The photocatalyst method is the same as that of example 1, except that: in the step 4), the mass ratio of the titanium tetrachloride to the concentrated hydrochloric acid is 1:1, 1:2, 1:4, 1:6, 1:8 and 1:10 respectively.
Examples 24 to 29
Polymer-induced graphene growth TiO2The photocatalyst method is the same as that of example 1, except that: in the step 5), the mass ratio of the potassium persulfate to the concentrated hydrochloric acid is 1:1, 1:10, 1:20, 1:30, 1:40 and 1: 50.
Examples 30 to 35
Polymer-induced growth of TiO on graphene2The photocatalytic method is the same as that of example 1, except that: the mass ratio of the graphene to the titanium tetrachloride in the step 4) is 1:0.5, 1:1, 1:1.5, 1:2, 1:2.5 and 1:3 respectively.
Example 36
Polymer-induced growth of TiO on graphene2The photocatalytic method is the same as that of example 1, except that: in the step 4), the titanium-containing compounds are metatitanic acid respectively.
Example 37
Polymer-induced growth of TiO on graphene2The photocatalytic method is the same as that of example 1, except that: the titanium-containing compounds in the step 4) are tetrabutyl titanate respectively.
Comparative example 1
Polymer-induced growth of TiO on graphene2The photocatalysis method is characterized in that: graphene is not added in step 2).
Comparative example 2
Polymer-induced growth of TiO on graphene2The photocatalytic method is the same as that of example 1, except that: in step 3) without addition of polymer monomers
Comparative example 3
Polymer-induced growth of TiO on graphene2The photocatalyst method is the same as that of example 1, except that: in the step 3), dispersant sodium dodecyl sulfate is not added.
Example 38
TiO2Graphene4The composite material is used as a photocatalyst for photocatalytic hydrogen production: 10mg of TiO2the/RGO composite material is put into an aqueous solution containing triethanolamine sacrificial agent and stirred for 5 hours to be uniformly dispersed, then the temperature of the reaction system is maintained at room temperature by using condensed water, and the test is carried out, and the obtained results are shown in Table 1:
TABLE 1 photocatalytic hydrogen production (all-optical) test results
TABLE 2 photocatalytic hydrogen production (visible light) test results
Experiments prove that the TiO prepared by the invention2The hydrogen production rate of the graphene composite material reaches 2.76-13.81 mmol/g-1·h-1The hydrogen production amount reaches 138-. In addition, the photocatalytic composite material has good stability and can be recycled for multiple times. As can be seen from examples 1 to 5, the addition of different polymer monomers has a great influence on the hydrogen production performance, and pyrrole>Thiophene(s)>Aniline. As can be seen from comparative examples 1-3, the polymer monomer and the titanium-containing compound cannot be well dispersed in the solvent without adding the graphene, and the product is aggregated into large particles and cannot be uniformly compounded, so that the hydrogen production rate and the hydrogen production amount are greatly reduced; no TiO achievement without addition of polymeric monomers2The preparation has controllable appearance, and the absorption of the photocatalytic material in visible light is influenced, so that the hydrogen production rate and the hydrogen production amount are greatly reduced; the polymer monomer can not be well dispersed in the aqueous solution without adding the dispersant of sodium dodecyl benzene sulfonate, and can not be effectively mixed with TiO2The combination forms a heterojunction, and the transmission of photogenerated electron holes is limited, so that the hydrogen production rate and the hydrogen production quantity are greatly reduced.
Example 39
TiO2the/RGO composite material is used as a photocatalyst for photocatalytic degradation of organic pollutants:
10mg of TiO2the/RGO composite material is added into organic pollutant solution (such as methyl orange, methylene blue and rhodamine B) with the concentration of 10mg/L and stirred for 10-120min to be uniformly dispersed, then the reaction system temperature is maintained at room temperature by condensed water, and the test is carried out, and the obtained result is shown in the table 2:
TABLE 2 test results of photocatalytic degradation of organic pollutants
Experiments prove that the TiO of the invention is prepared in 45-90 min2the/RGO composite material can completely degrade methyl orange, methylene blue can completely degrade within 65-100min, and rhodamine B can completely degrade within 80-145 min. Moreover, the photocatalytic composite material has good stability and can be recycled for multiple times. As can be seen from comparative examples 1 to 3, no graphene was added, so that the polymer and TiO were2The precursor can not be well dispersed in the solvent, and the product is aggregated into large particles and can not be uniformly compounded, so that the capability of degrading organic pollutants is greatly reduced; no TiO achievement without addition of polymeric monomers2The appearance can be controlled, and the capability of degrading organic pollutants is influenced; the sodium dodecyl benzene sulfonate is not added as a dispersing agent, so that the polymer monomer cannot be well dispersed in the aqueous solution and cannot be effectively mixed with TiO2Binding, affects the ability to degrade organic contaminants.
And (4) conclusion: a large number of experiments prove that the polymer can induce TiO with multiple morphologies to grow on graphite2The TiO can be controlled by changing the amount of the added component and the conditions of the hydrothermal reaction2In the form of polymers, TiO2And RGO, and the photocatalytic performance of the composite material can be weakened to different degrees by changing any one of the components or additionally adding any one of the components. TiO finally obtained2the/RGO composite material has high photocatalytic activity.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be included within the scope of the present invention.
Claims (6)
1. PolymerCompound-induced graphene growth multi-morphology TiO2A method of photocatalyst, comprising the steps of:
1) mixing graphene and distilled water, and carrying out ultrasonic stirring to obtain a graphene dispersion liquid;
2) under the condition of ice-water bath, mixing and stirring a dispersing agent, a polymer monomer and a graphene dispersion liquid to obtain a first mixed solution;
3) under the condition of ice-water bath, dissolving a titanium-containing compound in concentrated acid to obtain a second mixed solution;
4) under the condition of ice-water bath, mixing and stirring the second mixed solution and an initiator to obtain a third mixed solution; mixing and stirring the first mixed solution and the third mixed solution, and then carrying out hydrothermal reaction; after the reaction is finished, carrying out post-treatment to obtain TiO2A graphene composite material;
the temperature of the hydrothermal reaction is 100-300 ℃, and the time of the hydrothermal reaction is 5-48 h;
the polymer monomer is selected from pyrrole, aniline or thiophene;
the dispersing agent is sodium dodecyl sulfate;
the titanium-containing compound is titanium tetrachloride, metatitanic acid, tetrabutyl titanate or tetraisopropyl titanate.
2. The method of claim 1, wherein the initiator is potassium persulfate, sodium persulfate, or ammonium persulfate.
3. The method of claim 1, wherein the concentrated acid is concentrated hydrochloric acid, concentrated nitric acid, concentrated sulfuric acid, or concentrated acetic acid.
4. The method according to claim 1, wherein the mass ratio of the graphene to the distilled water is: 1: 1000-; the mass ratio of the graphene to the polymer monomer is 1: 0.1-50; the mass ratio of the dispersing agent to the distilled water is 1: 1000-10000.
5. The method of claim 1, wherein the mass ratio of the initiator to the concentrated acid is 1:1 to 50; the mass ratio of the titanium-containing compound to the concentrated acid is 1: 0.1-10.
6. A TiO prepared by the process of any one of claims 1 to 52The application of the graphene composite material in photocatalytic hydrogen production and photocatalytic degradation of organic matters.
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