CN105148894B - A kind of preparation method of hydroxylating titanium oxide/graphene visible light catalytic material - Google Patents
A kind of preparation method of hydroxylating titanium oxide/graphene visible light catalytic material Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of surface hydroxylation titanium oxide/graphene catalysis material.This method is using butyl titanate, graphene, sodium nitrate or ammonium nitrate as raw material, cetyl trimethylammonium bromide (or polyacrylic acid or Sodium Polyacrylate) obtains graphene/TiO of surface hydroxylation as surfactant by colloidal sol, water bath with thermostatic control, ultraviolet light, microwave radiation, washing, drying and other steps2Catalysis material.The characteristics of of the invention maximum is to realize TiO using ultraviolet pre-oxidation and microwave radiation2Surface hydroxylation, preparation process is simple, and low energy consumption, and energy Fast back-projection algorithm is easy to large-scale production；Meanwhile surface hydroxylation makes composite material form the defects of more (such as Lacking oxygen and Ti3+), increase surface-active, reduce the energy gap of composite material, widen spectral response range, obtain graphene/TiO of strong absorption, high activity, durability and bacteriostasis property2Catalysis material is with a wide range of applications in fields such as sewage disposal, photocatalytic water, air purification, air purification, solar cell and anti-biotic materials.
Description
Technical field
The invention belongs to field of photocatalytic material, are related to a kind of hydroxylating titanium oxide/graphene visible light catalytic material
Preparation method.
Background technology
Photocatalysis technology is a kind of New Environment Protection Technology, and catalysis material can directly utilize sunlight degradation of organic substances, energy
Consume it is relatively low, non-secondary pollution and degrade it is thorough, be expected to for solve the environmental problem of getting worse provide one it is cheap feasible
Approach.Titanium oxide (TiO2) abundant raw material is cheap, has good weatherability, acid-alkali-corrosive-resisting, higher calorifics, chemistry are steady
Qualitative, the unique performance such as semiconductor photosensitive can be good at absorbing or shielding ultraviolet light, and absorb what is excited after luminous energy
Electronics (hole) has reducing power (oxidisability) by force, in necks such as sensor, coating, cosmetics, solar cell and photocatalysis
Domain is with a wide range of applications.However, TiO2Greater band gap, it is relatively low to the utilization rate of sunlight, and its light excitation when institute
The electronics of generation is easily compound with hole, and photo-quantum efficiency is low.Graphene has high electron mobility and big Electronic saving energy
Power can capture and transmit light induced electron and hole, and its big specific surface area can disperse TiO2Nano particle improves catalysis and lives
Property.Therefore, by the use of graphene as carrier, the photocatalysis performance of titanium oxide can be effectively enhanced.
Although graphene can improve TiO for carrier2Photocatalysis performance, but in compound system, merely with graphite
Alkene large specific surface area disperses TiO2And good conductivity promotes the separation of photo-generate electron-hole, itself does not have photocatalysis and lives
Property, therefore widening TiO2Spectral response range and improve catalytic activity in terms of be limited.In addition, prepare at present graphene/
TiO2Method major part severe reaction conditions, technics comparing is complicated, and synthesis cycle is long, and cost is higher, is unfavorable for extensive life
Production, significantly limits graphene/TiO2The practical application of catalysis material.
Invention content
In view of the deficiencies of the prior art, there is strong absorption, height the object of the present invention is to provide one kind under ultraviolet-visible
Yellow graphene/TiO of activity and durability2The preparation method of composite catalyzing material.The present invention is utilized using graphene as carrier
Ultraviolet light and microwave radiation technology sodium nitrate or ammonium nitrate oxidation realize TiO2Surface hydroxylation widens TiO2Spectral response range and
Catalytic activity obtains yellow graphene/TiO with strong absorption, high catalytic activity and durability2Composite photocatalyst material.
The present invention technical concept be：Using graphene as carrier, using its big specific surface area and excellent electric property,
Prevent TiO2Reunite, increasing specific surface area enhances its conductive capability and extinction characteristic；By organic matter surface modification, stone is improved
The dispersion of black alkene and surface-active enhance graphene and TiO2Between combination, make to form effective synergistic effect between them；Profit
With ultraviolet light and microwave radiation auxiliary can redox graphene and decompose organic bath, simplify preparation process；Profit
Great amount of hydroxy group is generated with burst of ultraviolel sodium nitrate or ammonium nitrate, makes TiO2Surface hydroxylation widens graphene/TiO2Complex light is urged
Change the spectral response range and photocatalytic activity of material, obtain the graphene/TiO haveing excellent performance2Catalysis material.
To realize the present invention, the technical scheme is that：
A kind of preparation method of hydroxylating titanium oxide/graphene visible light catalytic material, the specific steps are：
(1) graphene solution of a concentration of 0.8-2.0g/L of 3-20mL is added in into ultrasonic disperse in 10-30mL deionized waters
20-40min obtains graphene dispersing solution；
(2) by 1-3mL acetic acid, 2-6mL butyl titanates, 0.01-0.5g cetyl trimethylammonium bromides (CTAB) or poly-
Acrylic acid or Sodium Polyacrylate are dissolved in successively in 10-30mL ethyl alcohol, then add in 20-60mL dissolved with 1-3mL sodium nitrate or nitric acid
The deionized water of ammonium salt solution, the sodium nitrate or concentration of ammonium nitrate solution are 1-3mol/L, obtain transparent liquid a；
(3) graphene dispersing solution for obtaining above-mentioned steps (1) is instilled in the clear solution a that step (2) obtains, in 20-
10-30min is stirred by ultrasonic under the conditions of 40 DEG C, obtains homodisperse brown solution b；
(4) a concentration of 0.1- of 5-30mL are instilled in the homodisperse brown solution b obtained in above-mentioned steps (3)
The ammonium hydroxide or NaOH solution of 3.0mol/L, adjusting pH are 1.6-8.0, stir ultrasonic disperse 5-20min, obtain homodisperse grey
Solution c；
(5) it is at 50-80 DEG C that the homodisperse grey solution c obtained in above-mentioned steps (4), which is positioned over temperature, and water-bath is permanent
Warm 20-60min stirs ultrasonic disperse 5-20min, obtains homodisperse mucus d later；
(6) the mucus d for obtaining above-mentioned steps (5) carries out intensive treatment, first in power 100-500W, emission wavelength
0.5-3h is irradiated under the ultraviolet lamp of 300-395nm, then power 300-650W, duty ratio 30%-80% micro-wave oven in it is anti-
0.5-2h is answered, finally obtains reaction product；
(7) reaction product that above-mentioned steps (6) obtain is filtered and is washed 3-4 times with distilled water and absolute ethyl alcohol, then
Washings at 60-80 DEG C is toasted into 8-16h, product is obtained after grinding.Step (1) described graphene is for graphene oxide or also
Former graphene oxide.
The principle of the present invention is：Using graphene and butyl titanate as raw material, organic bath is surfactant, uses purple
Outer light irradiation and microwave radiation auxiliary sodium nitrate or ammonium nitrate carry out surface hydroxylation, widen graphene/TiO2Composite photocatalyst
The spectral response range and photocatalytic activity of material.The big specific surface area of graphene and good electric conductivity prevent TiO2It receives
Rice grain is reunited, and reduces the compound of photo-generate electron-hole pair, improves photocatalysis performance；Organic bath as surfactant,
Dispersion and the surface-active of graphene are improved, enhances graphene and TiO2Between combination, promote graphene performance performance；It is purple
The energy of outer light irradiation and microwave radiation is high, can decomposing organic matter；The strong oxidation performance of sodium nitrate or ammonium nitrate make graphene/
TiO2Catalysis material surface generates more Lacking oxygen and surface defect, forms abundant hydroxyl, improves material to photoproduction electricity
The capture and transfer of son reduce TiO2Energy gap, its optical absorption characteristics is widened, so as to obtain strong absorption, efficient
Graphene/TiO2Catalysis material.
The characteristics of of the invention maximum is to utilize ultraviolet light and microwave radiation auxiliary sodium nitrate or ammonium nitrate surface hydroxyl
Change, graphene/TiO of fabricated in situ surface hydroxylation2Nanocomposite, preparation process is simple, and Fast back-projection algorithm, low energy consumption,
It is easy to large-scale production.Meanwhile surface hydroxylation can make graphene/TiO2Composite material generates more Lacking oxygen and surface lacks
It falls into, improves its surface-active and the energy gap that narrows, widen optical absorption characteristics.In addition, the huge specific surface area of graphene and excellent
Different electric property will improve TiO2Adsorption capacity and promote hydroxylating TiO2Middle light induced electron and the separation in hole pair, from
And obtain the catalysis material with strong absorption, high activity.The catalysis material can be applied to sewage disposal, light degradation water, air
The fields such as purification, solar cell and anti-biotic material.
Compared with prior art, advantage of the invention is that：
1st, the present invention needs not move through conventional heating methods removal organic electrolysis using ultraviolet irradiation and microwave radiation means
Matter, treatment temperature is low, have the characteristics that Fast back-projection algorithm, low energy consumption, low cost, it is easy to operate, be easy to large-scale production；Separately
Outside, burst of ultraviolel technology can be reduced directly graphene oxide, improve the electric conductivity of graphene, give full play to the enhancing of graphene
Effect, so as to obtain the high nano catalytic material of catalytic activity.
2nd, the present invention carries out surface hydroxylation using sodium nitrate or ammonium nitrate, on the one hand, makes graphene/TiO2Composite material
Surface generates a large amount of hydroxyl, improves the activity of composite material surface, enhances the ability of composite material absorption dyestuff；It is another
Aspect makes composite material surface form the defects of more (such as Lacking oxygen and Ti3+), the band gap of material is reduced, has expanded spectrum
Response range, so as to obtain hydroxylating graphene/TiO of strong absorption, high catalytic efficiency2Composite catalyzing material.
Description of the drawings
Fig. 1 is graphene/TiO that embodiment 1 obtains2With hydroxylating TiO2The XRD diagram of/graphene sample；
Fig. 2 is the sample of the acquisition of embodiment 1 to situation of degrading under the absorption of rhodamine and ultraviolet light；
Fig. 3 is the scanning electron microscope (SEM) photograph for the sample that embodiment 2 obtains：Wherein a is TiO2SEM figure, b is graphene/TiO2's
SEM schemes, and c is hydroxylating TiO2SEM figure, d is hydroxylating TiO2The SEM figures of/graphene；
Fig. 4 is the UV-vis DRS spectrum for the sample that embodiment 2 obtains；Wherein, a is TiO2With hydroxyl TiO2Purple
Outer visible diffusing reflection spectrum, b are graphene/TiO2With hydroxyl TiO2The UV-vis DRS spectrum of/graphene composite material；
Fig. 5 is the sample of the acquisition of embodiment 2 under visible light to the absorption of rhodamine and degradation situation；
Fig. 6 is the hydroxylating TiO that embodiment 3 obtains2/ graphene sample to the absorption of the rhodamine b solution of high concentration and
Degradation situation under ultraviolet lamp.
Fig. 7 is hydroxylating graphene/TiO that embodiment 3 obtains2The anti-microbial property of composite material；A is physiological saline and blueness
Mycin control group, b are hydroxylating TiO2, c is graphene/TiO of 3mL graphenes synthesis2Composite material, d are that 6mL graphenes close
Into graphene/TiO2Composite material, e are graphene/TiO of 8mL graphenes synthesis2Composite material.Wherein, L1 is sample pair
The fungistatic effect of Escherichia coli, L2 are fungistatic effect of the sample to staphylococcus aureus, and L3 is sample coatings to natural conditions
Under bacterium fungistatic effect.
Specific embodiment
With reference to embodiment and attached drawing, the present invention will be further explained；
Embodiment 1
(1) the redox graphene solution of a concentration of 1.2g/L of 20mL is added in into ultrasonic disperse in 20mL deionized waters
30min obtains graphene dispersing solution；
(2) 2mL acetic acid, 4mL titanium salts, 0.05g polyacrylic acid are dissolved in successively in 20mL ethyl alcohol, then add in 20mL dissolved with
The deionized water of 3mL 1.0mol/L ammonium nitrate solutions, obtains transparent liquid a；
(3) graphene dispersing solution for obtaining above-mentioned steps (1) is instilled in clear solution a, and ultrasound is stirred under the conditions of 25 DEG C
10min is mixed, obtains homodisperse brown solution b；Wherein, sample 1 and 2 adds in 40mL deionized waters and replaces graphene dispersing solution；
(4) the homodisperse brown solution b obtained in above-mentioned steps (3) instills a concentration of 1.0mol/L's of 32.8mL
NaOH, it is 3.2 to adjust pH, stirs ultrasonic disperse 5min, obtains homodisperse grey solution c；
(5) the homodisperse grey solution c obtained in above-mentioned steps (4) is placed on constant temperature 30min at 60 DEG C of water-bath, stirs
Ultrasonic disperse 10min is mixed, obtains homodisperse mucus d；Wherein, sample 1 and 3 add in 40mL deionized waters instead of ammonium nitrate go from
Sub- aqueous solution；
(6) the homodisperse mucus d for obtaining above-mentioned steps (5) is in power 100W, the ultraviolet lamp of emission wavelength 365nm
Lower irradiation 0.5h, then power 650W, duty ratio 30% micro-wave oven in react 0.5h, obtain reactant；
(7) reactant that above-mentioned steps (6) obtain is filtered and is washed 3 times with distilled water and absolute ethyl alcohol, then will washed
It washs object and 10h is toasted at 65 DEG C, product is obtained after then grinding.
Fig. 1 is the X diffraction analysis of titanium oxide/graphene and hydroxylating titanium oxide/graphene sample, and the sample of acquisition is main
It is by TiO2Composition, and hydroxylating leads to TiO2Crystal grain becomes smaller, and weakens TiO2Crystallinity；
Fig. 2 is sample to the absorption of rhodamine and degradation situation.It can be obtained from figure, graphene significantly increases TiO2It inhales
Attached performance, and rhodamine b dyestuffs can be degraded completely in the shorter time；
Embodiment 2
(1) graphene oxide solution of a concentration of 2g/L of 6mL is added in into ultrasonic disperse 30min in 20mL deionized waters, obtained
Graphene dispersing solution；
(2) 1mL acetic acid, 2mL butyl titanates and 0.05g CTAB are dissolved in successively in 20mL ethyl alcohol, it is molten then adds in 40mL
There is the deionized water of 65% concentrated nitric acids of 2mL, obtain transparent liquid a；
(3) graphene dispersing solution for obtaining above-mentioned steps (1) is instilled in clear solution a, and ultrasound is stirred under the conditions of 25 DEG C
10min is mixed, obtains homodisperse brown solution b；
(4) instill a concentration of 1.0mol/L's of 32.8mL in the homodisperse brown solution b obtained in above-mentioned steps (3)
NaOH, it is 3.2 to adjust pH, stirs ultrasonic disperse 5min, obtains homodisperse grey solution c；
(5) the homodisperse grey solution c obtained in above-mentioned steps (4) is placed on constant temperature 30min at 60 DEG C of water-bath, stirs
Ultrasonic disperse 10min is mixed, obtains homodisperse mucus d；
(6) the homodisperse mucus d for obtaining above-mentioned steps (5) is first in power 100W, the purple of emission wavelength 365nm
30min is irradiated under outer lamp, then power 650W, duty ratio 30% micro-wave oven in react 0.5h, finally obtain reaction product；
(7) reactant that above-mentioned steps (6) obtain is filtered and is washed 3 times with distilled water and absolute ethyl alcohol, then will washed
It washs object and 10h is toasted at 65 DEG C, graphene/TiO of surface hydroxylation is obtained after then grinding2Product.
Fig. 3 is the scanning electron microscope result figure of sample.Where it can be seen that TiO2(Fig. 3 a) is formed by many particle agglomerations；Stone
Black alkene/TiO2Many aggregates are can observe in (Fig. 3 b) to be dispersed on graphene layer；And hydroxylated TiO2(Fig. 3 c) and graphite
Alkene/TiO2(Fig. 3 d) then shows as more block shape.This illustrates that hydroxylating is conducive to increase the overall dimensions of material, can be advantageous
Enhance it and recycle characteristic；
Fig. 4 finds out that hydroxylating can enhance TiO for (Fig. 4 a and Fig. 4 b) in the diffusing reflection spectrum of sample2And graphene/TiO2
Absorption to visible ray, and greatly reduce TiO2And graphene/TiO2Band gap width；
Fig. 5 is sample to the absorption of rhodamine and Visible Light Induced Photocatalytic situation.It can be obtained from figure, surface hydroxyl graphite
Alkene/TiO2More excellent photocatalysis performance is shown, rhodamine b dyestuffs are degraded completely in 2 hours；
Embodiment 3
(1) the redox graphene solution of a concentration of 2g/L of 8mL is added in into ultrasonic disperse in 20mL deionized waters
30min obtains graphene dispersing solution；
(2) 1mL acetic acid, 2mL butyl titanates and 0.05g Sodium Polyacrylates are dissolved in successively in 10mL ethyl alcohol, then added in
20mL obtains transparent liquid a dissolved with the deionized water of 3mL 2.0mol/L sodium nitrate solutions；
(3) graphene dispersing solution for obtaining above-mentioned steps (1) is instilled in clear solution a, and ultrasound is stirred under the conditions of 25 DEG C
10min is mixed, obtains homodisperse brown solution b；
(4) ammonium hydroxide of a concentration of 2.0mol/L is instilled in the homodisperse brown solution b obtained in above-mentioned steps (3),
It is 3 to adjust pH, stirs ultrasonic disperse 5min, obtains homodisperse grey solution c；
(5) the homodisperse grey solution c obtained in above-mentioned steps (4) is placed on constant temperature 30min at 60 DEG C of water-bath, stirs
Ultrasonic disperse 10min is mixed, obtains homodisperse mucus d；
(6) the homodisperse mucus d for obtaining above-mentioned steps (5) is first in power 100W, the purple of emission wavelength 365nm
30min is irradiated under outer lamp, then power 650W, duty ratio 30% micro-wave oven in react 0.5h, finally obtain reaction product；
(7) reactant that above-mentioned steps (6) obtain is filtered and is washed 3 times with distilled water and absolute ethyl alcohol, then will washed
It washs object and 10h is toasted at 65 DEG C, graphene/TiO of surface hydroxylation is obtained after then grinding2Product；
(8) volume for changing redox graphene is the experiment more than 3mL and 6mL is repeated respectively, obtains different graphite
Hydroxylating graphene/TiO of alkene content2Composite material.
Fig. 6 is the hydroxylating TiO obtained2/ graphene sample is to the absorption of the rhodamine B solution of high concentration and degradation feelings
Condition.Where it can be seen that sample shows very strong absorption and degradation capability.
Fig. 7 is the antibacterial situation of the hydroxylating sample of different graphene contents.It can be obtained from inhibition zone size, with graphite
The increase of alkene content, hydroxylating graphene/TiO2The bacteriostasis property enhancing of composite granule.When graphene usage amount is 6mL, sample
The bacteriostasis property of product is best.Graphene dosage is further increased, the inhibition zone of sample reduces.In addition, never in sample coatings
Colony count can obtain, hydroxylating graphene/TiO2Composite granule has good bacteriostasis.
Claims (2)
1. a kind of preparation method of hydroxylating titanium oxide/graphene visible light catalytic material, it is characterized in that, the specific steps are：
(1) graphene solution of a concentration of 0.8-2.0g/L of 3-20mL is added in into ultrasonic disperse 20- in 10-30mL deionized waters
40min obtains graphene dispersing solution；
(2) by 1-3mL acetic acid, 2-6mL butyl titanates, 0.01-0.5g cetyl trimethylammonium bromides (CTAB) or polypropylene
Acid or Sodium Polyacrylate are dissolved in successively in 10-30mL ethyl alcohol, and it is molten dissolved with 1-3mL sodium nitrate or ammonium nitrate then to add in 20-60mL
The deionized water of liquid, the sodium nitrate or concentration of ammonium nitrate solution are 1-3mol/L, obtain transparent liquid a；
(3) graphene dispersing solution for obtaining above-mentioned steps (1) is instilled in the clear solution a that step (2) obtains, at 20-40 DEG C
Under the conditions of 10-30min is stirred by ultrasonic, obtain homodisperse brown solution b；
(4) instill a concentration of 0.1-3.0mol/L's of 5-30mL in the homodisperse brown solution b obtained in above-mentioned steps (3)
Ammonium hydroxide or NaOH solution, adjusting pH are 1.6-8.0, stir ultrasonic disperse 5-20min, obtain homodisperse grey solution c；
(5) it is constant temperature water bath at 50-80 DEG C that the homodisperse grey solution c obtained in above-mentioned steps (4), which is positioned over temperature,
20-60min stirs ultrasonic disperse 5-20min, obtains homodisperse mucus d later；
(6) the mucus d for obtaining above-mentioned steps (5) carries out intensive treatment, first in power 100-500W, emission wavelength 300-
0.5-3h is irradiated under the ultraviolet lamp of 395nm, then power 300-650W, duty ratio 30%-80% micro-wave oven in react
0.5-2h finally obtains reaction product；
(7) reaction product that above-mentioned steps (6) obtain is filtered and is washed 3-4 times with distilled water and absolute ethyl alcohol, then will washed
It washs object and 8-16h is toasted at 60-80 DEG C, product is obtained after grinding.
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.
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| CN109304224A (en) * | 2017-07-28 | 2019-02-05 | 孙梓译 | Long-acting water purification material and preparation method thereof |
| CN109304060A (en) * | 2017-07-28 | 2019-02-05 | 孙梓译 | Material for air purification and preparation method thereof with self-catalysis effect |
| CN110614091B (en) * | 2019-09-30 | 2023-05-30 | 华东理工大学 | Spindle-shaped mesogenic TiO 2 Composite photocatalyst, preparation method and application thereof |
| CN110773142A (en) * | 2019-11-14 | 2020-02-11 | 嘉兴烯成新材料有限公司 | Preparation and application of reduced hydroxylated graphene composite semiconductor catalyst |
| CN113354104A (en) * | 2021-07-01 | 2021-09-07 | 云南华谱量子材料有限公司 | Ecological system suitable for deepwater environment restoration and construction method thereof |
| CN117160437A (en) * | 2023-10-23 | 2023-12-05 | 重庆工商大学 | Defective calcium hydroxystannate photocatalyst and preparation method and application thereof |
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