CN105148894A - Preparation method of hydroxylation titanium oxide/graphene visible light catalysis material - Google Patents

Preparation method of hydroxylation titanium oxide/graphene visible light catalysis material Download PDF

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CN105148894A
CN105148894A CN201510607549.1A CN201510607549A CN105148894A CN 105148894 A CN105148894 A CN 105148894A CN 201510607549 A CN201510607549 A CN 201510607549A CN 105148894 A CN105148894 A CN 105148894A
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graphene
preparation
tio
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visible light
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CN105148894B (en
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陈传盛
曹时义
刘天贵
梁波
于伟伟
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Changsha University of Science and Technology
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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
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

Abstract

The invention relates to a preparation method of a surface hydroxylation titanium oxide/graphene visible light catalysis material. According to the method, butyl titanate, graphene and nitrate serve as raw materials, organic electrolyte serves as surfactant, and the surface hydroxylation graphene/TiO<2> catalysis material is obtained through the steps of sol application, thermostatic water bath, ultraviolet irradiation, microwave irradiation, washing, drying and the like. The preparation method has the greatest advantage that ultraviolet pre-oxidation and microwave irradiation are utilized for achieving surface hydroxylation, the preparation process is simple, the energy consumption is low, rapid synthesis can be achieved, and large-scale production is easy to achieve; meanwhile, more defects such as oxygen vacancy and Ti<3+> are caused to a composite by surface hydroxylation, surface activity is increased, forbidden bandwidth of the composite is decreased, the spectral response range is widened, the obtained graphene/TiO<2> catalysis material is great in absorption performance and high in activity, durability and antibacterial performance, and the preparation method has a wide application prospect in fields such as sewage treatment, photocatalytic water splitting, air purification, solar cells, antibacterial materials and the like.

Description

A kind of preparation method of hydroxylating titanium oxide/Graphene visible light catalytic material
Technical field
The invention belongs to field of photocatalytic material, relate to the preparation method of a kind of hydroxylating titanium oxide/Graphene visible light catalytic material.
Background technology
Photocatalysis technology is a kind of New Environment Protection Technology, and catalysis material can directly utilize sunshine degradation of organic substances, and energy consumption is lower, and non-secondary pollution and degraded thoroughly, are expected to the approach providing a cheapness feasible for solving day by day serious environmental problem.Titanium oxide (TiO 2) abundant raw material cheapness, there is good weatherability, acid-alkali-corrosive-resisting, higher calorifics, chemical stability, the performance that semiconductor light sensitivity etc. are unique, can be good at absorbing or shielding ultraviolet light, and it is strong that the electronics excited after absorbing luminous energy (hole) has reducing power (oxidisability), is with a wide range of applications in fields such as sensor, coating, cosmetics, solar cell and photocatalysis.But, TiO 2greater band gap, lower to the utilization rate of sunshine, and the easy compound of the electronics produced during its optical excitation and hole, photo-quantum efficiency is low.Graphene has high electron mobility and large electronic storage capacities, can catch and transmit light induced electron and hole, and its large specific area can disperse TiO 2nano particle, improves catalytic activity.Therefore, utilize Graphene as carrier, the photocatalysis performance of titanium oxide can be effectively enhanced.
Although Graphene is carrier can improve TiO 2photocatalysis performance, but in compound system, only make use of Graphene specific area and disperse TiO greatly 2and good conductivity promotes the separation of photo-generate electron-hole, itself does not have photocatalytic activity, therefore is widening TiO 2spectral response range and improve catalytic activity aspect be limited.In addition, Graphene/TiO is prepared at present 2method major part severe reaction conditions, technics comparing is complicated, and synthesis cycle is long, and cost is higher, is unfavorable for large-scale production, significantly limit Graphene/TiO 2the practical application of catalysis material.
Summary of the invention
For the deficiencies in the prior art, the object of this invention is to provide a kind of yellow Graphene/TiO under ultraviolet-visible with strong absorption, high activity and durability 2the preparation method of compound catalyze material.The present invention is carrier with Graphene, utilizes ultraviolet light and the oxidation of microwave radiation technology nitrate to realize TiO 2surface hydroxylation, widens TiO 2spectral response range and catalytic activity, obtain the yellow Graphene/TiO with strong absorption, high catalytic activity and durability 2composite photocatalyst material.
Technical conceive of the present invention is: be carrier with Graphene, and the specific area utilizing it large and excellent electric property, stop TiO 2reunite, increasing specific surface area, strengthens its conductive capability and extinction characteristic; By organic matter finishing, improve dispersion and the surface-active of Graphene, strengthen Graphene and TiO 2between combination, make between them, to form effective cooperative effect; Utilize UV-irradiation and microwave to assist reducible graphene oxide, and decompose organic bath, simplify preparation technology; Utilize burst of ultraviolel nitrate to produce great amount of hydroxy group, make TiO 2surface hydroxylation, widens Graphene/TiO 2the spectral response range of composite photocatalyst material and photocatalytic activity, obtain the Graphene/TiO of excellent performance 2catalysis material.
For realizing the present invention, technical scheme of the present invention is:
A preparation method for hydroxylating titanium oxide/Graphene visible light catalytic material, concrete steps are:
(1) be that the graphene solution of 0.8-2.0g/L adds 10-30mL deionized water for ultrasonic dispersion 20-40min by 3-20mL concentration, obtain graphene dispersing solution;
(2) 1-3mL acetic acid, 2-6mL titanium salt, 0.01-0.5g surfactant are dissolved in 10-30mL ethanol successively, then add the deionized water that 20-60mL is dissolved with 1-3mL nitric acid or nitrate (concentration is 1-3mol/L), obtain transparent liquid a;
(3) by above-mentioned graphene dispersing solution instillation clear solution a, ultrasonic agitation 10-30min under 20-40 DEG C of condition, obtains homodisperse brown solution b;
(4) in described homodisperse brown solution b, instill the alkaline solution that 5-30mL concentration is 0.1-3.0mol/L, adjustment pH is 1.6-8.0, stirs ultrasonic disperse 5-20min, obtains homodisperse grey solution c;
(5) constant temperature 20-60min at described homodisperse grey solution c is placed on water-bath 50-80 DEG C, stirs ultrasonic disperse 5-20min, obtains homodisperse mucus d;
(6) described mucus d is carried out intensive treatment, first irradiate 0.5-3h with under the uviol lamp of power 100-500W, emission wavelength 300-395nm, then in the micro-wave oven of power 300-650W, dutycycle 30%-80%, react 0.5-2h, finally obtain product;
(7) above-mentioned reactant filtered and use distilled water and absolute ethanol washing 3-4 time, then washings being toasted 8-16h at 60-80 DEG C, then obtaining product after grinding.
Step (1) described Graphene is graphene oxide or redox graphene.
Titanium salt described in step (2) is butyl titanate, and surfactant is CTAB, polyacrylic acid or Sodium Polyacrylate.
Nitric acid described in step (2) is red fuming nitric acid (RFNA), and nitrate is sodium nitrate or ammonium nitrate.
Alkali lye described in step (4) is ammoniacal liquor or NaOH.
Intensive treatment described in step (6) is UV-irradiation and microwave radiation processing.
Principle of the present invention is: with Graphene and butyl titanate for raw material, organic bath is surfactant, uses UV-irradiation and microwave auxiliary azotate to carry out surface hydroxylation, widens Graphene/TiO 2the spectral response range of composite photocatalyst material and photocatalytic activity.The specific area that Graphene is large and good electric conductivity, stop TiO 2nanoparticle agglomerates, reduces the compound that photo-generate electron-hole is right, improves photocatalysis performance; Organic bath is as surfactant, and the dispersion of Graphene and surface-active, strengthen Graphene and TiO 2between combination, promote the performance of Graphene performance; The energy of UV-irradiation and microwave is high, energy decomposing organic matter; The Strong oxdiative performance of nitrate makes Graphene/TiO 2catalysis material surface produces more Lacking oxygen and blemish, forms abundant hydroxyl, improves material capturing and shifting light induced electron, reduces TiO 2energy gap, widen its optical absorption characteristics, thus obtain strong absorption, high efficiency Graphene/TiO 2catalysis material.
The maximum feature of the present invention utilizes UV-irradiation and microwave auxiliary azotate surface hydroxylation, the Graphene/TiO of fabricated in situ surface hydroxylation 2nano composite material, preparation technology is simple, and Fast back-projection algorithm, energy consumption is low, is easy to large-scale production.Meanwhile, surface hydroxylation can make Graphene/TiO 2composite produces more Lacking oxygen and blemish, improves its surface-active, and the energy gap that narrows, and widens optical absorption characteristics.In addition, the specific area that Graphene is huge and excellent electric property, will improve TiO 2adsorption capacity and promote hydroxylating TiO 2middle light induced electron and right being separated in hole, thus acquisition has strong absorption, highly active catalysis material.Described catalysis material can be applicable to the fields such as sewage disposal, light degradation water, purification of air, solar cell and anti-biotic material.
Compared with prior art, advantage of the present invention is:
1, the present invention uses ultraviolet irradiation and microwave radiation means, do not need through conventional heating methods remove organic bath, its treatment temperature is low, have Fast back-projection algorithm, low energy consumption, low cost, simple to operate, be easy to the features such as large-scale production; In addition, burst of ultraviolel technology can direct-reduction graphene oxide, improves the electric conductivity of Graphene, gives full play to the enhancing effect of Graphene, thus obtains the high nano catalytic material of catalytic activity.
2, the present invention adopts nitric acid or nitrate to carry out surface hydroxylation, on the one hand, makes Graphene/TiO 2composite material surface produces a large amount of hydroxyls, improves the activity of composite material surface, enhances the ability of composite absorbing dye; On the other hand, composite material surface is made to form more defect (as Lacking oxygen and Ti 3+), reduce the band gap of material, expanded spectral response range, thus obtain the hydroxylating Graphene/TiO of strong absorption, high catalytic efficiency 2compound catalyze material.
Accompanying drawing explanation
Fig. 1 is Graphene/TiO that embodiment 1 obtains 2with hydroxylating TiO 2the XRD figure of/Graphene sample;
Fig. 2 is that the sample of embodiment 1 acquisition is to degraded situation under the absorption of rhodamine and ultraviolet light;
Fig. 3 is the scanning electron microscope (SEM) photograph of the sample that embodiment 2 obtains; Wherein, a is TiO 2sEM figure, b is Graphene/TiO 2sEM figure, c is hydroxylating TiO 2sEM figure, d is hydroxylating TiO 2the SEM figure of/Graphene;
Fig. 4 is the UV-vis DRS spectrum of the sample that embodiment 2 obtains; Wherein, a is TiO 2with hydroxyl TiO 2uV-vis DRS spectrum, b is Graphene/TiO 2with hydroxyl TiO 2the UV-vis DRS spectrum of/graphene composite material;
Fig. 5 is that the sample of embodiment 2 acquisition is under visible light to absorption and the degraded situation of rhodamine;
Fig. 6 is the hydroxylating TiO that embodiment 3 obtains 2/ Graphene sample is to the degraded situation under the absorption of the rhodamine b solution of high concentration and uviol lamp;
Fig. 7 is hydroxylating Graphene/TiO that embodiment 3 obtains 2the anti-microbial property of composite; A is physiological saline and penicillin control group, and b is hydroxylating TiO 2, c is the Graphene/TiO of 3mL Graphene synthesis 2composite, d is the Graphene/TiO of 6mL Graphene synthesis 2composite, e is the Graphene/TiO of 8mL Graphene synthesis 2composite.Wherein, L1 be sample to colibacillary fungistatic effect, L2 is the fungistatic effect of sample to staphylococcus aureus, and L3 is the fungistatic effect of sample coatings to the bacterium under natural conditions.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention will be further explained;
embodiment 1
(1) be that the redox graphene solution of 1.2g/L adds ultrasonic disperse 30min in 20mL by 20mL concentration, obtain graphene dispersing solution;
(2) 2mL acetic acid, 4mL titanium salt, 0.05g polyacrylic acid are dissolved in 20mL ethanol successively, then add the deionized water that 20mL is dissolved with 3mL1.0mol/L ammonium nitrate, obtain transparent liquid a;
(3) by above-mentioned graphene dispersing solution instillation clear solution a, ultrasonic agitation 10min under 25 DEG C of conditions, obtains homodisperse brown solution b; Wherein, sample 1 and 2 adds 40mL deionized water and replaces graphene dispersing solution;
(4) instilling 32.8mL concentration at described homodisperse brown solution b is the NaOH of 1.0M, regulates pH to be 3.2, stirs ultrasonic disperse 5min, obtains homodisperse grey solution c;
(5) constant temperature 30min at described homodisperse grey solution c is placed on water-bath 60 DEG C, stirs ultrasonic disperse 10min, obtains homodisperse mucus d; Wherein, sample 1 and 3 adds 40mL deionized water and replaces concentrated nitric acid solution;
(6) irradiate 0.5h by under the uviol lamp of described mucus d power 100W, emission wavelength 365nm, then in the micro-wave oven of power 650W, dutycycle 30%, react 0.5h, obtain reactant;
(7) above-mentioned reactant filtered and use distilled water and absolute ethanol washing 3 times, then washings being toasted 10h at 65 DEG C, then obtaining product after grinding.
Fig. 1 is the X diffraction analysis of titanium oxide/Graphene and hydroxylating titanium oxide/Graphene sample, and the sample of acquisition is mainly by TiO 2composition, and hydroxylating causes TiO 2crystal grain diminishes, and weakens TiO 2degree of crystallinity;
Fig. 2 is that sample is to the absorption of rhodamine and degraded situation.Can draw from figure, Graphene improves TiO significantly 2absorption property, and can in the shorter time by complete for rhodamine b dye degrades;
embodiment 2
(1) be that the graphene oxide solution of 2g/L adds 20mL deionized water for ultrasonic dispersion 30min by 6mL concentration, obtain graphene dispersing solution;
(2) 1mL acetic acid, 2mL titanium salt and 0.05gCTAB are dissolved in 20mL ethanol successively, are dissolved in 10mL ethanol successively, then add the deionized water that 40mL is dissolved with 2mL65% red fuming nitric acid (RFNA), obtain transparent liquid a;
(3) by above-mentioned graphene dispersing solution instillation clear solution a, ultrasonic agitation 10min under 25 DEG C of conditions, obtains homodisperse brown solution b;
(4) in described homodisperse brown solution b, instill the NaOH that 32.8mL concentration is 1.0M, regulate pH to be 3.2, stir ultrasonic disperse 5min, obtain homodisperse grey solution c;
(5) constant temperature 30min at described homodisperse grey solution c is placed on water-bath 60 DEG C, stirs ultrasonic disperse 10min, obtains homodisperse mucus d;
(6) first described mucus d is irradiated 30min with under the uviol lamp of power 100W, emission wavelength 365nm, then in the micro-wave oven of power 650W, dutycycle 30%, react 0.5h, finally obtain product;
(7) above-mentioned reactant filtered and use distilled water and absolute ethanol washing 3 times, then washings being toasted 10h at 65 DEG C, then after grinding, obtaining the Graphene/TiO of surface hydroxylation 2product.
Fig. 3 is the ESEM result figure of sample.Therefrom can find out, TiO 2a () is formed by many particle agglomerations; Graphene/TiO 2b can observe many aggregates in () is dispersed on graphene layer; And hydroxylated TiO2 (c) and Graphene/TiO 2d () then shows as more block shape.This illustrates that hydroxylating is conducive to increasing the overall dimensions of material, can favourable enhancing its reclaim characteristic;
Fig. 4 is that in the diffuse reflection spectrum of sample, (Fig. 3 a and Fig. 3 b) finds out, hydroxylating can strengthen TiO 2and Graphene/TiO 2to the absorption of visible ray, and greatly reduce TiO 2and Graphene/TiO 2band gap width;
Fig. 5 is that sample is to the absorption of rhodamine and Visible Light Induced Photocatalytic situation.Can draw from figure, surface hydroxyl functionalized graphene/TiO 2show more excellent photocatalysis performance, by complete for rhodamine b dye degrades in 2 hours;
embodiment 3
(1) be that the redox graphene solution of 2g/L adds 20mL deionized water for ultrasonic dispersion 30min by 8mL concentration, obtain graphene dispersing solution;
(2) 1mL acetic acid, 2mL titanium salt and 0.05g Sodium Polyacrylate are dissolved in 10mL ethanol successively, then add the deionized water that 20mL is dissolved with 3mL2.0mol/L sodium nitrate, obtain transparent liquid a;
(3) by above-mentioned graphene dispersing solution instillation clear solution a, ultrasonic agitation 10min under 25 DEG C of conditions, obtains homodisperse brown solution b;
(4) in described homodisperse brown solution b, instill the ammoniacal liquor that concentration is 2.0M, regulate pH to be 3, stir ultrasonic disperse 5min, obtain homodisperse grey solution c;
(5) constant temperature 30min at described homodisperse grey solution c is placed on water-bath 60 DEG C, stirs ultrasonic disperse 10min, obtains homodisperse mucus d;
(6) first described mucus d is irradiated 30min with under the uviol lamp of power 100W, emission wavelength 365nm, then in the micro-wave oven of power 650W, dutycycle 30%, react 0.5h, finally obtain product;
(7) above-mentioned reactant filtered and use distilled water and absolute ethanol washing 3 times, then washings being toasted 10h at 65 DEG C, then after grinding, obtaining the Graphene/TiO of surface hydroxylation 2product;
(8) volume changing redox graphene is that 3mL and 6mL repeats above experiment respectively, obtains the hydroxylating Graphene/TiO of different Graphene content 2composite.
Fig. 6 is the hydroxylating TiO obtained 2/ Graphene sample is to the absorption of the rhodamine b solution of high concentration and degraded situation.Therefrom can find out, sample shows very strong absorption and degradation capability.
Fig. 7 is the antibacterial situation of the hydroxylating sample of different Graphene content.Draw from the large I of inhibition zone, along with the increase of Graphene content, hydroxylating Graphene/TiO 2the bacteriostasis property of composite granule strengthens.When Graphene use amount is 6mL, the bacteriostasis property of sample is best.Further increase Graphene consumption, the inhibition zone of sample reduces.In addition, never can obtain with colony count in sample coatings, hydroxylating Graphene/TiO 2composite granule has good bacteriostasis.

Claims (6)

1. a preparation method for hydroxylating titanium oxide/Graphene visible light catalytic material, is characterized in that, concrete steps are:
(1) be that the graphene solution of 0.8-2.0g/L adds 10-30mL deionized water for ultrasonic dispersion 20-40min by 3-20mL concentration, obtain graphene dispersing solution;
(2) 1-3mL acetic acid, 2-6mL titanium salt, 0.01-0.5g surfactant are dissolved in 10-30mL ethanol successively, then add the deionized water that 20-60mL is dissolved with 1-3mL nitric acid or nitrate (concentration is 1-3mol/L), obtain transparent liquid a;
(3) by above-mentioned graphene dispersing solution instillation clear solution a, ultrasonic agitation 10-30min under 20-40 DEG C of condition, obtains homodisperse brown solution b;
(4) in described homodisperse brown solution b, instill the alkaline solution that 5-30mL concentration is 0.1-3.0mol/L, adjustment pH is 1.6-8.0, stirs ultrasonic disperse 5-20min, obtains homodisperse grey solution c;
(5) be positioned at temperature is 50-80 DEG C at described homodisperse grey solution c, constant temperature water bath 20-60min, stirs ultrasonic disperse 5-20min afterwards, obtains homodisperse mucus d;
(6) described mucus d is carried out intensive treatment, first irradiate 0.5-3h with under the uviol lamp of power 100-500W, emission wavelength 300-395nm, then in the micro-wave oven of power 300-650W, dutycycle 30%-80%, react 0.5-2h, finally obtain product;
(7) above-mentioned reactant filtered and use distilled water and absolute ethanol washing 3-4 time, then washings being toasted 8-16h at 60-80 DEG C, after grinding, obtain product.
2. the preparation method of hydroxylating titanium oxide/Graphene visible light catalytic material according to claim 1, it is characterized in that, step (1) described Graphene is graphene oxide and redox graphene.
3. the preparation method of hydroxylating titanium oxide/Graphene visible light catalytic material according to claim 1 or 2, it is characterized in that, titanium salt described in step (2) is butyl titanate, and surfactant is softex kw (CTAB), polyacrylic acid or Sodium Polyacrylate.
4. the preparation method of hydroxylating titanium oxide/Graphene visible light catalytic material according to claim 1 or 2, it is characterized in that, the nitric acid described in step (2) is red fuming nitric acid (RFNA), and nitrate is sodium nitrate or ammonium nitrate.
5. the preparation method of hydroxylating titanium oxide/Graphene visible light catalytic material according to claim 1 or 2, it is characterized in that, the alkali lye described in step (4) is ammoniacal liquor or NaOH.
6. the preparation method of hydroxylating titanium oxide/Graphene visible light catalytic material according to claim 1 or 2, it is characterized in that, the intensive treatment described in step (6) is ultraviolet irradiation and microwave radiation processing.
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