CN103143338B - Porous titanium dioxide/graphene composite material and preparation method thereof - Google Patents
Porous titanium dioxide/graphene composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a porous titanium dioxide/graphene composite material and a preparation method thereof. The preparation method comprises the steps of: adding aniline and graphene into a surfactant-containing protonic acid solution according to a certain ratio; preparing a nanometer polyaniline/graphene composite material through an in-situ polymerization method; preparing titanium dioxide sol by using a sol-gel method; adding 0.05-0.20g of nanometer polyaniline/graphene composite material into 50mL of sol, uniformly mixing; standing and aging the sol for 3-5 days; drying in a drying oven at the temperature of 60-120 DEG C; milling; calcining the obtained composite for 30 minutes -2 hours at the temperature of 200-550 DEG C; and removing the polyaniline, thereby obtaining the porous titanium dioxide/graphene composite material. According to the invention, the porous titanium dioxide/graphene is prepared by utilizing the nanometer polyaniline and the titanium dioxide is deposited on the graphene, so that the contact area of the titanium dioxide and pollutants is increased, the separating efficiency of photo-generated electrons and holes is improved and the photocatalytic efficiency is improved.
Description
Technical field
The present invention relates to a kind of preparation method and application thereof of titanic oxide material, particularly a kind of poriferous titanium dioxide/graphene composite material and application thereof.
Background technology
Titanium dioxide is a kind of efficient, nontoxic, photochemical catalyst that stable chemical nature, anti-photooxidation are strong, cheap.Optically catalytic TiO 2/photo-electrocatalytic technology causes extensive attention in organic wastewater exhaust-gas treatment application aspect that is poisonous, bio-refractory.Nano titanium dioxide degradable efficiency is high, but can only carry out light-catalyzed reaction under UV-irradiation, and the separation rate in its light induced electron and hole still has much room for improvement.For promoting the performance of titanium dioxide, preparing the composite of titanium dioxide and changing its application form and become one of emphasis direction of titanium dioxide research.The materials such as metal, metal oxide, graphite, organic matter are all for the preparation of composite titania material.
Utilize template can prepare specific modality titanium dioxide or to titanium dioxide pore-creating.The titanium dioxide with pore passage structure has larger specific area and stronger effect of mass transmitting, thus has stronger photocatalysis performance.The non-surface-active agents such as surfactant and glucose such as polyethers, polyethylene glycol and softex kw are the template comparatively commonly used.Polyaniline is typical conducting polymer composite, due to its structure diversification, good, the easy processing of environmental stability, cheap and become the study hotspot of conducting polymer.In several customary preparation methods of polyaniline, the polyaniline that situ aggregation method obtains mostly is threadiness.Be that the report of Template preparation specific form titanium dioxide have not been reported with polyaniline.
Graphene is the Two-dimensional Carbon atomic crystal be found in recent years, has the electrical properties more excellent than other material with carbon elements, good electric conductivity and chemical stability.In the composite, Graphene can play the effect of electron transmission passage, thus improves the chemical property of composite further.Meanwhile, Graphene also can strengthen the adhesive ability of compound in matrix.
Summary of the invention
The object of the invention is to provide a kind of poriferous titanium dioxide/graphene composite material and preparation method thereof for the deficiencies in the prior art.
Thinking of the present invention is: at microemulsion system situ synthesizing nano polyaniline/graphene composite material.In TiO 2 sol, add nano polyaniline/Graphene, utilize calcining to remove polyaniline to compound pore-creating, make titanium dioxide deposition obtained composite on Graphene.
A preparation method for poriferous titanium dioxide/graphene composite material, comprises the steps:
Under A, nitrogen environment, be the protonic acid solution of 0.02M ~ 1M and concentration by concentration be that the DBSA of 0.02M ~ 1M is with volume ratio 1:1 ~ 8:1 mixing, add Graphene simultaneously, add aniline after magnetic agitation 1h ~ 3h, Graphene and aniline mass ratio are 1:2 ~ 1:40; After Keep agitation 1h ~ 3h, dropwise drip ammonium persulfate, aniline and ammonium persulfate mol ratio are 1:0.5 ~ 1:1.5; 12h ~ 24h is reacted at 0 DEG C ~ 30 DEG C; Acetone, deionized water washing for several times final vacuum is dry, nano polyaniline/graphene composite material of milling to obtain;
B, prepare TiO 2 sol by sol-gel process, in colloidal sol, add the nano polyaniline/graphene composite material accounting for colloidal sol 0.08wt% ~ 8.0wt%, mix;
C, by 60 DEG C ~ 120 DEG C oven dry of rearmounted for still aging for colloidal sol 3 ~ 5d baking oven;
D, mill after calcine 30min ~ 2h by gained compound 200 ~ 550 DEG C, remove polyaniline, obtain poriferous titanium dioxide/graphene composite material.
The application of poriferous titanium dioxide/graphene composite material prepared by described preparation method, is applied to photocatalysis degradation organic contaminant in waste gas, waste water treatment reactor.
Poriferous titanium dioxide/graphene composite material prepared by described preparation method, wherein poriferous titanium dioxide and Graphene form composite construction by adulterating, and most titanium dioxide deposition is on graphene sheet layer; Described composite construction is micron or nanoscale.
Described poriferous titanium dioxide/graphene composite material, loose structure is obtained compound pore-creating by nano polyaniline.
Described poriferous titanium dioxide/graphene composite material, described loose structure is distributed in inside and the surface of composite construction.
Described poriferous titanium dioxide/graphene composite material, described Graphene is present in composite construction with multiple single-layer graphene form.
Poriferous titanium dioxide/graphene composite material prepared by the present invention adds due to the good Graphene of electric conductivity, and light induced electron will be passed to bringing of Graphene, thus reduces the recombination rate of hole and electronics.The introducing of Graphene also makes the forbidden band of titanium dioxide narrow, and extend photoresponse scope, the maximum absorption wavelength of composite moves to visible-range.Meanwhile, titanium dioxide has been endowed more meso-hole structures, and specific area increases, and improves effect of mass transmitting.Some all improves the catalytic performance of titanium dioxide to the modification of material above.
Poriferous titanium dioxide/graphene composite material prepared by the inventive method can be applied to photocatalysis degradation organic contaminant in waste gas, waste water treatment reactor.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1: the preparation method of poriferous titanium dioxide/graphene composite material, comprises the steps:
(1) under nitrogen environment, in 100mL hydrochloric acid solution (1M), add 40mL DBSA (0.02M), Graphene 0.10g, after magnetic agitation 1h, add aniline 0.2mL, after Keep agitation 1h, dropwise drip ammonium persulfate 0.6g, at 25 DEG C, react 24h.
(2) solution in step (1) is washed for several times successively with suction filtration form acetone, ethanol and deionized water.The dry 24h of vacuum drying chamber.To mill to obtain nano polyaniline/graphene composite material.
(3) prepare TiO 2 sol by sol-gel process, in 50mL colloidal sol, add nano polyaniline/graphene composite material 0.02g, ultrasonic 10min, mixes.
(4) by rearmounted for still aging for colloidal sol 3d 60 DEG C, baking oven oven dry.
(5) calcine 40min by gained compound 450 DEG C after milling, remove polyaniline, obtain poriferous titanium dioxide/graphene composite material.
In 20mL methyl orange solution (20mg/L), add the above-mentioned compound of 50mg, 300W Hg lamp irradiation, aeration stirs 30min, and methyl orange degradation rate can reach 89%.The illumination of 500W xenon lamp simulating nature is penetrated, and aeration stirs 1h, and methyl orange degradation rate can reach 49%.
Embodiment 2: the preparation method of poriferous titanium dioxide/graphene composite material, comprises the steps:
(1) under nitrogen environment, in 50mL salpeter solution (1M), add 20mL DBSA (0.02M), Graphene 0.08g, after magnetic agitation 1h, add aniline 0.3mL, after Keep agitation 1h, dropwise drip ammonium persulfate 0.8g, at 0 DEG C, react 24h.
(2) solution in step (1) is washed for several times successively with suction filtration form acetone, ethanol and deionized water.The dry 24h of vacuum drying chamber.To mill to obtain nano polyaniline/graphene composite material.
(3) prepare TiO 2 sol by sol-gel process, in 50mL colloidal sol, add nano polyaniline/graphene composite material 0.06g, ultrasonic 10min, mixes.
(4) by rearmounted for still aging for colloidal sol 3d 80 DEG C, baking oven oven dry.
(5) calcine 60min by gained compound 450 DEG C after milling, remove polyaniline, obtain poriferous titanium dioxide/graphene composite material.
In 20mL methyl orange solution (20mg/L), add the above-mentioned compound of 50mg, 300W Hg lamp irradiation, aeration stirs 30min, and methyl orange degradation rate can reach 95%.The illumination of 500W xenon lamp simulating nature is penetrated, and aeration stirs 1h, and methyl orange degradation rate can reach 56%.
Embodiment 3: the preparation method of poriferous titanium dioxide/graphene composite material, comprises the steps:
(1) under nitrogen environment, in 60mL sulfuric acid solution (1M), add 20mL DBSA (0.05M), Graphene 0.10g, after magnetic agitation 1h, add aniline 0.2mL, after Keep agitation 1h, dropwise drip ammonium persulfate 0.6g, at 25 DEG C, react 24h.
(2) solution in step (1) is washed for several times successively with suction filtration form acetone, ethanol and deionized water.The dry 24h of vacuum drying chamber.To mill to obtain nano polyaniline/graphene composite material.
(3) prepare TiO 2 sol by sol-gel process, in 50mL colloidal sol, add nano polyaniline/graphene composite material 0.05g, ultrasonic 10min, mixes.
(4) by rearmounted for still aging for colloidal sol 2d 80 DEG C, baking oven oven dry.
(5) calcine 30min by gained compound 500 DEG C after milling, remove polyaniline, obtain poriferous titanium dioxide/graphene composite material.
In 20mL methylene blue solution (20mg/L), add the above-mentioned compound of 50mg, 300W Hg lamp irradiation, aeration stirs 30min, and methylene blue degradation rate can reach 94%.The illumination of 500W xenon lamp simulating nature is penetrated, and aeration stirs 1h, and methylene blue degradation rate can reach 52%.
As a comparison, with pure titinium dioxide, simulating pollution thing methyl orange, methylene blue are degraded under the same terms.
Result of the test shows: pure titinium dioxide is respectively 84% and 86% to the degradation rate of methyl orange and methylene blue under Hg lamp irradiation, under xenon lamp, be respectively 28% and 30% to the degradation rate of methyl blue and methylene blue, all lower than the degradation rate of composite to dyestuff.Illustrate that composite has good photocatalysis.
Should be understood that, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection domain that all should belong to claims of the present invention.
Claims (1)
1. a preparation method for poriferous titanium dioxide/graphene composite material, is characterized in that, comprises the steps:
Under A, nitrogen environment, be the protonic acid solution of 0.02M ~ 1M and concentration by concentration be that the DBSA of 0.02M ~ 1M is with volume ratio 1:1 ~ 8:1 mixing, add Graphene simultaneously, add aniline after magnetic agitation 1h ~ 3h, Graphene and aniline mass ratio are 1:2 ~ 1:40; After Keep agitation 1h ~ 3h, dropwise drip ammonium persulfate, aniline and ammonium persulfate mol ratio are 1:0.5 ~ 1:1.5; 12h ~ 24h is reacted at 0 DEG C ~ 30 DEG C; Acetone, deionized water washing for several times final vacuum is dry, nano polyaniline/graphene composite material of milling to obtain;
B, prepare TiO 2 sol by sol-gel process, in colloidal sol, add the nano polyaniline/graphene composite material accounting for colloidal sol 0.08wt% ~ 8.0wt%, mix;
C, by 60 DEG C ~ 120 DEG C oven dry of rearmounted for still aging for colloidal sol 3 ~ 5d baking oven;
D, mill after calcine 30min ~ 2h by gained compound 200 ~ 550 DEG C, remove polyaniline, obtain poriferous titanium dioxide/graphene composite material.
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| CN107626296B (en) * | 2017-09-22 | 2020-04-17 | 长沙理工大学 | Preparation method of oxide quantum dot modified graphene/titanium oxide photocatalytic material |
| CN109433178A (en) * | 2018-10-22 | 2019-03-08 | 南京稞之朗环保科技有限公司 | A kind of carrier photochemical catalyst of titanium dioxide-graphene oxide and preparation method thereof |
| CN109370226A (en) * | 2018-10-24 | 2019-02-22 | 嘉兴市海德姆智能电气有限公司 | A kind of preparation method of electromagnetic shielding material |
| CN111905807A (en) * | 2020-07-06 | 2020-11-10 | 安徽理工大学 | High instantaneous photocurrent nanometer TiO2Polyaniline/graphene composite material and preparation method thereof |
| CN113948691B (en) * | 2021-10-15 | 2023-03-10 | 佛山科学技术学院 | Titanium dioxide composite material and application thereof as energy storage material |
| CN115172065B (en) * | 2022-06-16 | 2023-04-25 | 宁德师范学院 | Three-dimensional capacitance electrode material with polyaniline/titanium dioxide grafted on graphene surface |
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| CN103123869B (en) * | 2012-11-28 | 2017-10-03 | 华中科技大学 | It is a kind of to possess nano titanium oxide graphene composite material preparation method of three-dimensional porous structure and products thereof |
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