CN104399457A - Au/TiO2/CFP (carbon fiber paper) ternary composite nano photocatalyst as well as preparation method and application thereof - Google Patents
Au/TiO2/CFP (carbon fiber paper) ternary composite nano photocatalyst as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the field of preparation and application of composite photocatalytic materials and particularly relates to an Au/TiO2/CFP (carbon fiber paper) ternary composite nano photocatalyst as well as a preparation method and application thereof. According to the preparation method, the Au/TiO2/CFP ternary composite nano photocatalyst is further prepared by an ultraviolet-radiation method on the basis of preparing a TiO2/CFP binary composite photocatalyst by a soaking-hydrothermal reaction method. The Au/TiO2/CFP ternary composite nano photocatalyst not only has relatively strong adsorption performance on volatile organic compounds, but also has relatively strong visible light catalytic activity, so that the integration of adsorption of volatile organic compounds and photocatalytic mineralization is realized, and the reaction rate and the reaction efficiency of degrading organic pollutants in a photocatalytic manner are greatly enhanced. Moreover, the Au/TiO2/CFP ternary composite nano photocatalyst can be applied to the environment protection field as an adsorbent or a photocatalyst.
Description
Technical field
The invention belongs to composite photocatalyst material preparations and applicatio field, be specifically related to a kind of Au/TiO
2/ CFP tri compound nano-photocatalyst and preparation method thereof and application.
Background technology
Volatile organic matter is one of major pollutants in industrial area and urban air, can cause serious harm to surrounding environment and health.For this reason, people have developed the physics of multiple removal volatile organic matter, chemistry and biological method.Wherein, titanium dioxide (TiO
2) photocatalysis oxidation technique as the emerging depollution of environment technology of one, receive extensive concern.TiO
2having the high and lower-price characteristic of Stability Analysis of Structures, photocatalysis efficiency, is the high efficiency photocatalyst that can be used in the depollution of environment.Under UV-irradiation, TiO
2can at room temperature produce the hole with Strong oxdiative ability, volatile organic matter is thoroughly resolved into CO
2and H
2o.But, TiO
2photocatalyst applications also has some shortcomings part.First, TiO
2light-catalyzed reaction need use ultraviolet light, low to the utilization rate of visible ray.Secondly, the recombination process in excitation electron and hole on material, can reduce the activity of photochemical catalyst.Finally, TiO
2the specific area of material is less, to organic limited sorption capacity.These all limit TiO above
2application in the depollution of environment.
Carbon fiber paper (CFP) a kind ofly to be interlocked the carbonaceous material assembled by carbon fiber, may be TiO
2one of excellent carrier of photochemical catalyst.CFP has three-dimensional porous structure, can provide higher specific area, and increase light-catalysed avtive spot for organic absorption.CFP also has higher electric conductivity and electron storage capacitance, can accept TiO
2the light induced electron produced, stops the compound in electronics and hole.Therefore, CFP and TiO
2between interaction be TiO
2the improvement of properties of catalyst provides new opportunity.Meanwhile, noble metal Au and TiO
2compound tense, can absorb visible ray by Au particle surface plasma resonance in quantized mode, be conducive to photochemical catalyst to the absorption of visible ray and utilization.But, at present about CFP, Au and TiO
2the preparation of Three-element composite photocatalyst and the application in photocatalytic degradation volatile organic matter have not been reported.
Summary of the invention
In order to overcome the deficiencies in the prior art and shortcoming, primary and foremost purpose of the present invention is to provide a kind of Au/TiO
2the preparation method of/CFP tri compound nano-photocatalyst.
Another object of the present invention is to the Au/TiO providing said method to prepare
2/ CFP tri compound nano-photocatalyst.
Another object of the present invention is to provide above-mentioned Au/TiO
2the application of/CFP tri compound nano-photocatalyst.
Object of the present invention is realized by following proposal:
A kind of Au/TiO
2the preparation method of/CFP tri compound nano-photocatalyst, comprises following steps:
(1) carbon fiber paper (CFP) is immersed in dense HNO
3with dense H
2sO
4in the nitration mixture of composition, reflux 30 ~ 180min at 85 ~ 95 DEG C, and then washing is to neutral, by the drying precipitate after washing, obtains the carbon fiber paper after purifying;
(2) butyl titanate is joined in ethanol, after stirring, obtain the settled solution that concentration is the butyl titanate of 2 ~ 50g/L;
(3) carbon fiber paper after the purifying of step (1) gained is joined in the settled solution of the butyl titanate of step (2) gained wetting, take out, dry; Repeat wetting and dry run 2 ~ 5 times, obtain butyl titanate solution-wet and dried carbon fiber paper;
(4) prepare the mixing suspension of NaOH and titanium dioxide, wherein the final concentration of NaOH is 50 ~ 200g/L, and the final concentration of titanium dioxide is 4 ~ 20g/L;
(5) by the butyl titanate solution-wet of step (3) gained and dried carbon fiber paper to add in the mixing suspension of gained in step (4) hydro-thermal reaction 6 ~ 48h at 90 ~ 150 DEG C; Products therefrom cyclic washing, to neutral, by the drying precipitate after washing, obtains TiO
2/ CFP binary composite photo-catalyst;
(6) by the TiO of step (5) gained
2/ CFP binary composite photo-catalyst joins the HAuCl that concentration is 5 ~ 15g/L
4in the aqueous solution, lucifuge leaves standstill 0.5 ~ 5h, then irradiates 1 ~ 5h under being placed on ultraviolet; Take out product, cyclic washing, to neutral, by the drying precipitate after washing, obtains Au/TiO
2/ CFP tri compound nano-photocatalyst;
The Functionality, quality and appealing design of the carbon fiber paper described in step (1) elects 0.5 ~ 10g as; The volume of described nitration mixture is preferably 4 ~ 200mL; Described dense HNO
3mass fraction be 69%; Described dense H
2sO
4mass fraction be 98%; Dense HNO in described nitration mixture
3with dense H
2sO
4volume ratio be preferably 1:(1 ~ 5); Described baking temperature is preferably 50 ~ 180 DEG C; Drying time is preferably 3 ~ 12h; The solvent of described washing is preferably water; Described mode of washing is preferably filtration washing;
The Functionality, quality and appealing design of the tetraethyl titanate described in step (2) elects 0.05 ~ 5g as; Ethanol contend described in step (2) is preferably 10 ~ 200mL;
Carbon fiber paper after purifying described in step (3) is preferably 0.01 ~ 1g; Baking temperature described in step (3) is preferably 50 ~ 180 DEG C, and drying time is preferably 10 ~ 30min;
The mixing suspension of the NaOH described in step (4) and titanium dioxide obtains preferably by ultrasonic disperse;
Butyl titanate solution-wet described in step (5) the Functionality, quality and appealing design of dried carbon fiber paper elects 0.01 ~ 1g as; The volume of described mixing suspension is preferably 5 ~ 100mL; The solvent of described washing is preferably water; Described mode of washing is preferably centrifuge washing; Described baking temperature is preferably 50 ~ 180 DEG C, and drying time is preferably 3 ~ 24h;
TiO described in step (6)
2the Functionality, quality and appealing design of/CFP binary composite photo-catalyst elects 0.01 ~ 1.0g as; Described HAuCl
4the volume of the aqueous solution is preferably 5 ~ 50mL; Described baking temperature is preferably 50 ~ 180 DEG C, and drying time is preferably 3 ~ 24h; Cleaning solvent described in step (6) is preferably water;
A kind of Au/TiO
2/ CFP tri compound nano-photocatalyst, prepares according to above-mentioned preparation method; Described Au/TiO
2in/CFP tri compound nano-photocatalyst, diameter is that the carbon fiber surface of 5 ~ 10 microns is wrapped up completely by the titanium dioxide nano thread that diameter is 20 ~ 60 nanometers, reach several microns, and has particle size to be the surface that the gold nano grain of 2 ~ 10 nanometers is dispersed in carbon fiber and titanium dioxide nano thread; Its X-ray diffraction spectrum, laser Raman spectroscopy and x-ray photoelectron power spectrum show that C, Ti and Au tri-kinds of elements coexist in catalyst.UV-Vis diffuse reflection spectroscopy then shows that this tri compound nano-photocatalyst has superior Uv and visible light absorbent properties.
The present invention in infiltration-hydro-thermal reaction legal system for TiO
2on the basis of/CFP binary composite, obtain Au/TiO further by uv irradiation method
2/ CFP tri compound nano-photocatalyst.This photochemical catalyst not only has stronger absorption property to volatile organic matter, and there is stronger visible light catalysis activity, thus achieve the absorption of volatile organic matter and the integrated of photocatalysis mineralising, greatly strengthen reaction rate and the efficiency of photocatalysis degradation organic contaminant, can be used as adsorbent or photochemical catalyst is applied at field of Environment Protection.
Mechanism of the present invention is: carry out nitration mixture acidification by step (1) to carbon fiber paper, removes the impurity that carbon fiber paper adsorbs, obtains the carbon fiber paper after purifying; Adhere to one deck titanium oxide by step (2) and step (3) at carbon fiber paper surface, and it can be used as the original position that next step titanium dioxide nano thread grows; Start to generate titanium dioxide nano thread in the titanium oxide layer of carbon fiber paper surface by step (4) and step (5), these nano wires are long at carbon fiber paper surface, interlaced, cover whole carbon fiber paper surface completely gradually, form TiO
2/ CFP binary complex; Because titanium dioxide surface has the titanium ion of a large amount of positively charged and electronegative oxonium ion, therefore effectively HAuCl can be adsorbed
4auCl in the aqueous solution
4 -and Au
3+ion, and Au simple substance will be become containing Au species photo catalytic reduction by step (6), these simple substance Au will be deposited on titanium dioxide surface, forms Au/TiO
2/ CFP ternary complex.
Compared to the prior art, tool has the following advantages and beneficial effect in the present invention:
(1) carbon fiber paper absorbs and TiO the adsorption and enrichment effect of volatile organic matter, the quantization mode of Au to visible ray by the present invention
2the photocatalysis mineralization of nano wire combines, and prepares a kind of new and effective tri compound nano-photocatalyst.
(2) Au/TiO for preparing of the present invention
2/ CFP tri compound nano-photocatalyst shows good absorption and visible light catalysis activity to volatile organic matter gaseous benzene ethene: 180min is interior is that the cinnamic degradation rate of gas phase of 25 ± 1.5ppmv is up to 90.7% to initial concentration, thus achieve the absorption of volatile organic matter and the integrated of visible light catalytic oxidation, make catalyst can effectively mineralizing and degrading sorbing material adsorb, the volatile organic matter of enrichment, greatly strengthen reaction rate and the efficiency of visible light photocatalytic degradation of organic pollutants.
(3) Au/TiO of the present invention
2/ CFP tri compound nano-photocatalyst at the photochemical catalyst of field of Environment Protection as degraded volatile organic matter, can have wide range of application.
Accompanying drawing explanation
Fig. 1 is Au/TiO
2x-ray powder diffraction (XRD) spectrogram of/CFP tri compound nano-photocatalyst.
Fig. 2 is SEM (SEM) figure of carbon fiber paper (CFP).
Fig. 3 is TiO
2sEM (SEM) figure of/CFP binary composite photo-catalyst.
Fig. 4 is Au/TiO
2the SEM SEM figure of/CFP tri compound nano-photocatalyst.
Fig. 5 is Au/TiO
2transmission electron microscope (TEM) figure of/CFP tri compound nano-photocatalyst.
Fig. 6 is Au/TiO
2/ CFP tri compound nano-photocatalyst is to the cinnamic adsorption breakthrough curve of gas phase and kinetics of photocatalytic degradation curve map.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
The dense HNO related in embodiment
3mass fraction be 69%, dense H
2sO
4mass fraction be 98%;
Embodiment 1
(1) 1g carbon fiber paper is joined the dense HNO of 40mL
3with dense H
2sO
4in the nitration mixture that (volume ratio is 1:3) forms, 90 DEG C of backflow 90min, are washed to neutrality, dry 12h, obtain the carbon fiber paper after purifying for 80 DEG C, for subsequent use;
(2) 0.7g butyl titanate adds in 20mL ethanol, stirs the settled solution that 1min obtains butyl titanate;
(3) carbon fiber paper after the 0.5g purifying of step (1) gained is joined in the settled solution of the butyl titanate of step (2) gained wetting, take out, dry 20min for 80 DEG C; So wetting-drying course repeatedly carries out 5 times, obtains butyl titanate solution-wet and dried carbon fiber paper;
(4) 4.0g NaOH, 0.4g D25 titania powder add in 20mL deionized water, and ultrasonic disperse 20min obtains the mixing suspension of NaOH and titanium dioxide;
(5) by the butyl titanate solution-wet of 0.5g step (3) gained and dried carbon fiber paper adds the mixing suspension of step (4) gained, and load in polytetrafluoroethyltank tank, 110 DEG C of hydro-thermal reaction 48h, after solution cooling in polytetrafluoroethyltank tank, take out the carbon fiber paper with white depositions and be washed to neutrality, dry 8h, obtain TiO for 80 DEG C
2/ CFP binary composite photo-catalyst;
(6) by the TiO of 0.5g step (5) gained
2/ CFP binary composite photo-catalyst joins the HAuCl of 10mL, 10g/L
4in the aqueous solution, lucifuge leaves standstill 1h, then is placed on the high voltage mercury lamp radiation 2h of optical wavelength 365nm; After reaction terminates, take out product and be washed to neutrality, drying 24h, obtain Au/TiO for 80 DEG C
2/ CFP tri compound nano-photocatalyst.
Catalyst activity is tested: take the Au/TiO obtained by 0.5g
2/ CFP tri compound nano-photocatalyst is placed in photo catalysis reactor (ACS Appl.Mater.Interfaces 2012,4,5988-5996), and before reaction, lucifuge leaves standstill 900min, to reach adsorption/desorption balance; The light source used is 300W xenon lamp, and uses optical filter UV filter, after illumination starts, gets 0.2mL gaseous sample every 5min, utilizes to be equipped with in the gas chromatograph of flame ionization detector to analyze concentration of substrate change, adopts C/C
0evaluate degradation rate, wherein C is the concentration of styrene of sample after illumination certain hour, C
0for the initial concentration of styrene of sample.After light application time 180min, the cinnamic degradation rate of gaseous state can reach 90.7%.
Embodiment 2
(1) 10g carbon fiber paper is joined the dense HNO of 200mL
3with dense H
2sO
4in the nitration mixture that (volume ratio is 1:1) forms, 85 DEG C of backflow 180min, are washed to neutrality, dry 3h, obtain the carbon fiber paper after purifying for 180 DEG C, for subsequent use;
(2) 5g butyl titanate adds in 200mL ethanol, stirs the settled solution that 2min obtains butyl titanate;
(3) carbon fiber paper after the 1g purifying of step (1) gained is joined in the settled solution of the butyl titanate of step (2) gained wetting, take out, dry 10min for 180 DEG C; So wetting-drying course repeatedly carries out 4 times, obtains butyl titanate solution-wet and dried carbon fiber paper;
(4) 5.0g NaOH, 0.4g D25 titania powder add in 100mL deionized water, and ultrasonic disperse 60min obtains the mixing suspension of NaOH and titanium dioxide;
(5) by the butyl titanate solution-wet of 1g step (3) gained and dried carbon fiber paper adds the mixing suspension of step (4) gained, and load in polytetrafluoroethyltank tank, 130 DEG C of hydro-thermal reaction 36h, after solution cooling in polytetrafluoroethyltank tank, take out the carbon fiber paper with white depositions and be washed to neutrality, dry 24h, obtain TiO for 120 DEG C
2/ CFP binary composite photo-catalyst;
(6) by the TiO of 1g step (5) gained
2/ CFP binary composite photo-catalyst joins the HAuCl of 50mL, 15g/L
4in the aqueous solution, lucifuge leaves standstill 5h, then is placed on the high voltage mercury lamp radiation 5h of optical wavelength 365nm; After reaction terminates, take out product and be washed to neutrality, drying 12h, obtain Au/TiO for 120 DEG C
2/ CFP tri compound nano-photocatalyst.
Catalyst activity test (with embodiment 1): wherein, Au/TiO
2/ CFP tri compound nano-photocatalyst consumption is 1g, and lucifuge leaves standstill 720min; After illumination 180min, the cinnamic degradation rate of gaseous state can reach 91.0%.
Embodiment 3
(1) 0.5g carbon fiber paper is joined the dense HNO of 4mL
3with dense H
2sO
4in the nitration mixture that (volume ratio is 1:5) forms, 95 DEG C of backflow 30min, are washed to neutrality, dry 10h, obtain the carbon fiber paper after purifying for 50 DEG C, for subsequent use;
(2) 0.05g butyl titanate adds in 10mL ethanol, stirs the settled solution that 10min obtains butyl titanate;
(3) carbon fiber paper after the purifying of 0.01g step (1) gained is joined in the settled solution of the butyl titanate of step (2) gained wetting, take out, dry 30min for 50 DEG C; So wetting-drying course repeatedly carries out 5 times, obtains butyl titanate solution-wet and dried carbon fiber paper;
(4) 0.5g NaOH, 0.04g D25 titania powder add in 10mL deionized water, and ultrasonic disperse 1min obtains the mixing suspension of NaOH and titanium dioxide;
(5) by the butyl titanate solution-wet of 0.01g step (3) gained and dried carbon fiber paper adds the mixing suspension of step (4) gained, and load in polytetrafluoroethyltank tank, 150 DEG C of hydro-thermal reaction 6h, after solution cooling in polytetrafluoroethyltank tank, take out the carbon fiber paper with white depositions and be washed to neutrality, dry 12h, obtain TiO for 50 DEG C
2/ CFP binary composite photo-catalyst;
(6) by the TiO of 0.01g step (5) gained
2/ CFP binary composite photo-catalyst joins the HAuCl of 5mL, 5g/L
4in the aqueous solution, lucifuge leaves standstill 0.5h, then is placed on the high voltage mercury lamp radiation 4h of optical wavelength 365nm; After reaction terminates, take out product and be washed to neutrality, drying 3h, obtain Au/TiO for 180 DEG C
2/ CFP tri compound nano-photocatalyst.
Catalyst activity test (with embodiment 1): wherein, Au/TiO
2/ CFP tri compound nano-photocatalyst consumption is 0.01g, and lucifuge leaves standstill 120min; After illumination 160min, the cinnamic degradation rate of gaseous state can reach 87.3%.
Embodiment 4
(1) 2g carbon fiber paper is joined the dense HNO of 80mL
3with dense H
2sO
4in the nitration mixture that (volume ratio is 1:2) forms, 92 DEG C of backflow 60min, are washed to neutrality, dry 8h, obtain the carbon fiber paper after purifying for 80 DEG C, for subsequent use;
(2) 1.4g butyl titanate adds in 40mL ethanol, stirs the settled solution that 3min obtains butyl titanate;
(3) carbon fiber paper after the 0.6g purifying of step (1) gained is joined in the settled solution of the butyl titanate of step (2) gained wetting, take out, dry 25min for 100 DEG C; So wetting-drying course repeatedly carries out 2 times, obtains butyl titanate solution-wet and dried carbon fiber paper;
(4) 2.0g NaOH, 0.2g D25 titania powder add in 12mL deionized water, and ultrasonic disperse 10min obtains the mixing suspension of NaOH and titanium dioxide;
(5) by the butyl titanate solution-wet of 0.6g step (3) gained and dried carbon fiber paper adds the mixing suspension of step (4) gained, and load in polytetrafluoroethyltank tank, 120 DEG C of hydro-thermal reaction 35h, after solution cooling in polytetrafluoroethyltank tank, take out the carbon fiber paper with white depositions and be washed to neutrality, dry 3h, obtain TiO for 180 DEG C
2/ CFP binary composite photo-catalyst;
(6) by the TiO of 0.1g step (5) gained
2/ CFP binary composite photo-catalyst joins the HAuCl of 15mL, 6g/L
4in the aqueous solution, lucifuge leaves standstill 2h, then is placed on the high voltage mercury lamp radiation 1h of optical wavelength 365nm; After reaction terminates, take out product and be washed to neutrality, drying 20h, obtain Au/TiO for 50 DEG C
2/ CFP tri compound nano-photocatalyst.
Catalyst activity test (with embodiment 1): wherein, Au/TiO
2/ CFP tri compound nano-photocatalyst consumption is 0.02g, and lucifuge leaves standstill 800min; After illumination 120min, the cinnamic degradation rate of gaseous state can reach 81.6%.
Embodiment 5
(1) 3g carbon fiber paper is joined 120mL, dense HNO
3with dense H
2sO
4in the nitration mixture that (volume ratio is 1:2.5) forms, 85 DEG C of backflow 100min, are washed to neutrality, dry 9h, obtain the carbon fiber paper after purifying for 90 DEG C, for subsequent use;
(2) 2.1g butyl titanate adds in 60mL ethanol, stirs the settled solution that 8min obtains butyl titanate;
(3) carbon fiber paper after the 0.35g purifying of step (1) gained is joined in the settled solution of the butyl titanate of step (2) gained wetting, take out, dry 15min for 120 DEG C; So wetting-drying course repeatedly carries out 4 times, obtains butyl titanate solution-wet and dried carbon fiber paper;
(4) 3.5g NaOH, 0.35g D25 titania powder add in 40mL deionized water, and ultrasonic disperse 3min obtains the mixing suspension of NaOH and titanium dioxide;
(5) by the butyl titanate solution-wet of 0.35g step (3) gained and dried carbon fiber paper adds the mixing suspension of step (4) gained, and load in polytetrafluoroethyltank tank, 100 DEG C of hydro-thermal reaction 40h, after solution cooling in polytetrafluoroethyltank tank, take out the carbon fiber paper with white depositions and be washed to neutrality, dry 14h, obtain TiO for 130 DEG C
2/ CFP binary composite photo-catalyst;
(6) by the TiO of 0.35g step (5) gained
2/ CFP binary composite photo-catalyst joins the HAuCl of 20mL, 8g/L
4in the aqueous solution, lucifuge leaves standstill 1.5h, then is placed on the high voltage mercury lamp radiation 2.5h of optical wavelength 365nm; After reaction terminates, take out product and be washed to neutrality, drying 5h, obtain Au/TiO for 150 DEG C
2/ CFP tri compound nano-photocatalyst.
Catalyst activity test (with embodiment 1): wherein, Au/TiO
2/ CFP tri compound nano-photocatalyst consumption is 0.35g, and lucifuge leaves standstill 510min; After illumination 180min, the cinnamic degradation rate of gaseous state can reach 90.1%.
Embodiment 6
(1) 6g carbon fiber paper is joined 150mL, dense HNO
3with dense H
2sO
4in the nitration mixture that (volume ratio is 1:1.5) forms, 75 DEG C of backflow 170min, are washed to neutrality, dry 4h, obtain the carbon fiber paper after purifying for 140 DEG C, for subsequent use;
(2) 4.0g butyl titanate adds in 80mL ethanol, stirs the settled solution that 5min obtains butyl titanate;
(3) carbon fiber paper after the 0.45g purifying of step (1) gained is joined in the settled solution of the butyl titanate of step (2) gained wetting, take out, dry 18min for 150 DEG C; So wetting-drying course repeatedly carries out 3 times, obtains butyl titanate solution-wet and dried carbon fiber paper;
(4) 3.0g NaOH, 0.3g D25 titania powder add in 30mL deionized water, and ultrasonic disperse 30min obtains the mixing suspension of NaOH and titanium dioxide;
(5) by the butyl titanate solution-wet of 0.45g step (3) gained and dried carbon fiber paper adds the mixing suspension of step (4) gained, and load in polytetrafluoroethyltank tank, 140 DEG C of hydro-thermal reaction 30h, after solution cooling in polytetrafluoroethyltank tank, take out the carbon fiber paper with white depositions and be washed to neutrality, dry 5h, obtain TiO for 110 DEG C
2/ CFP binary composite photo-catalyst;
(6) by the TiO of 0.45g step (5) gained
2/ CFP binary composite photo-catalyst joins the HAuCl of 16mL, 9g/L
4in the aqueous solution, lucifuge leaves standstill 3h, then is placed on the high voltage mercury lamp radiation 3h of optical wavelength 365nm.After reaction terminates, take out product and be washed to neutrality, drying 10h, obtain Au/TiO for 100 DEG C
2/ CFP tri compound nano-photocatalyst.
Catalyst activity test (with embodiment 1): wherein, Au/TiO
2/ CFP tri compound nano-photocatalyst consumption is 0.45g, and lucifuge leaves standstill as 600min; After illumination 180min, the cinnamic degradation rate of gaseous state can reach 91.3%.
Embodiment 7
(1) 0.8g carbon fiber paper is joined 30mL, dense HNO
3with dense H
2sO
4in the nitration mixture that (volume ratio is 1:4) forms, 86 DEG C of backflow 50min, are washed to neutrality, dry 11h, obtain the carbon fiber paper after purifying for 70 DEG C, for subsequent use;
(2) 0.06g butyl titanate adds in 30mL ethanol, stirs the settled solution that 6min obtains butyl titanate;
(3) carbon fiber paper after the 0.06g purifying of step (1) gained is joined in the settled solution of the butyl titanate of step (2) gained wetting, take out, dry 28min for 90 DEG C; So wetting-drying course repeatedly carries out 5 times, obtains butyl titanate solution-wet and dried carbon fiber paper;
(4) 0.8g NaOH, 0.08g D25 titania powder add in 15mL deionized water, and ultrasonic disperse 2min obtains the mixing suspension of NaOH and titanium dioxide;
(5) by the butyl titanate solution-wet of 0.06g step (3) gained and dried carbon fiber paper adds the mixing suspension of step (4) gained, and load in polytetrafluoroethyltank tank, 90 DEG C of hydro-thermal reaction 42h, after solution cooling in polytetrafluoroethyltank tank, take out the carbon fiber paper with white depositions and be washed to neutrality, dry 20h, obtain TiO for 70 DEG C
2/ CFP binary composite photo-catalyst;
(6) by the TiO of 0.06g step (5) gained
2/ CFP binary composite photo-catalyst joins the HAuCl of 8mL, 8g/L
4in the aqueous solution, lucifuge leaves standstill 1.2h, then is placed on the high voltage mercury lamp radiation 2.2h of optical wavelength 365nm; After reaction terminates, take out product and be washed to neutrality, drying 18h, obtain Au/TiO for 70 DEG C
2/ CFP tri compound nano-photocatalyst.
Catalyst activity test (with embodiment 1): wherein, Au/TiO
2/ CFP tri compound nano-photocatalyst consumption is 0.06g, and lucifuge leaves standstill 210min; After illumination 180min, the cinnamic degradation rate of gaseous state can reach 89.3%.
Embodiment 8
(1) 8g carbon fiber paper is joined 180mL, dense HNO
3with dense H
2sO
4in the nitration mixture that (volume ratio is 1:3.5) forms, 87 DEG C of backflow 160min, are washed to neutrality, dry 7h, obtain the carbon fiber paper after purifying for 95 DEG C, for subsequent use;
(2) 4.8g butyl titanate adds in 180mL ethanol, stirs the settled solution that 7min obtains butyl titanate;
(3) carbon fiber paper after the 0.48g purifying of step (1) gained is joined in the settled solution of the butyl titanate of step (2) gained wetting, take out, dry 16min for 110 DEG C; So wetting-drying course repeatedly carries out 5 times, obtains butyl titanate solution-wet and dried carbon fiber paper;
(4) 4.8g NaOH, 0.4g D25 titania powder add in 90mL deionized water, and ultrasonic disperse 25min obtains the mixing suspension of NaOH and titanium dioxide;
(5) then by the butyl titanate solution-wet of 0.48g step (3) gained and dried carbon fiber paper adds the mixing suspension of step (4) gained, and load in polytetrafluoroethyltank tank, 125 DEG C of hydro-thermal reaction 25h, after solution cooling in polytetrafluoroethyltank tank, take out the carbon fiber paper with white depositions and be washed to neutrality, dry 18h, obtain TiO for 90 DEG C
2/ CFP binary composite photo-catalyst;
(6) by the TiO of 0.48g step (5) gained
2/ CFP binary composite photo-catalyst joins the HAuCl of 30mL, 12g/L
4in the aqueous solution, lucifuge leaves standstill 2.5h, then is placed on the high voltage mercury lamp radiation 1.5h of optical wavelength 365nm; After reaction terminates, take out product and be washed to neutrality, drying 15h, obtain Au/TiO for 90 DEG C
2/ CFP tri compound nano-photocatalyst.
Catalyst activity test (with embodiment 1): wherein, Au/TiO
2/ CFP tri compound nano-photocatalyst consumption is 0.48g, and lucifuge leaves standstill 300min; After illumination 180min, the cinnamic degradation rate of gaseous state can reach 88.3%.
Embodiment 9
(1) 5g carbon fiber paper is joined 100mL, dense HNO
3with dense H
2sO
4in the nitration mixture that (volume ratio is 1:1.2) forms, 93 DEG C of backflow 110min, are washed to neutrality, dry 5h, obtain the carbon fiber paper after purifying for 100 DEG C, for subsequent use;
(2) 0.25g butyl titanate adds in 50mL ethanol, stirs the settled solution that 4min obtains butyl titanate;
(3) carbon fiber paper after the 0.25g purifying of step (1) gained is joined in the settled solution of the butyl titanate of step (2) gained wetting, take out, dry 11min for 160 DEG C; So wetting-drying course carries out 5 times repeatedly;
(4) 2.5g NaOH, 0.25g D25 titania powder add in 50mL deionized water, and ultrasonic disperse 4min obtains the mixing suspension of NaOH and titanium dioxide;
(5) then by the butyl titanate solution-wet of 0.25g step (3) gained and dried carbon fiber paper adds the mixed solution of step (4) gained, and load in polytetrafluoroethyltank tank, 115 DEG C of hydro-thermal reaction 20h, after solution cooling in polytetrafluoroethyltank tank, take out the carbon fiber paper with white depositions and be washed to neutrality, dry 15h, obtain TiO for 100 DEG C
2/ CFP binary composite photo-catalyst;
(6) by the TiO of 0.25g step (5) gained
2/ CFP binary composite photo-catalyst joins the HAuCl of 25mL, 7g/L
4in the aqueous solution, lucifuge leaves standstill 3.5h, then is placed on the high voltage mercury lamp radiation 3.5h of optical wavelength 365nm.After reaction terminates, take out product and be washed to neutrality, drying 22h, obtain Au/TiO for 105 DEG C
2/ CFP tri compound nano-photocatalyst.
Catalyst activity test (with embodiment 1): wherein, Au/TiO
2/ CFP tri compound nano-photocatalyst consumption is 0.25g, and lucifuge time of repose is 420min; After illumination 180min, the cinnamic degradation rate of gaseous state can reach 90.5%.
Effect example
(1) XRD detects: the Au/TiO prepared embodiment 1
2/ CFP tri compound nano-photocatalyst has carried out XRD analysis, and profiling results as shown in Figure 1.As seen from Figure 1, prepared Au/TiO
2there is typical TiO in the XRD collection of illustrative plates of/CFP tri compound nano-photocatalyst simultaneously
2the characteristic peak of anatase, elemental gold and graphitic carbon.This can predict that prepared photochemical catalyst has certain visible light catalysis activity.
(2) SEM and TEM detects: Fig. 2 is the SEM figure of carbon fiber paper, can find out that carbon fiber paper is interlocked by micron order carbon fiber and assemble.Fig. 3 and Fig. 4 is the TiO that embodiment 1 prepares
2/ CFP binary composite photo-catalyst and Au/TiO
2the SEM figure of/CFP tri compound nano-photocatalyst, TiO as seen from the figure
2nano wire evenly also fully covers the surface of carbon fiber, indicates TiO
2compound between nano wire with carbon fiber not simply mixes.By tem analysis (Fig. 5), Au/TiO can be observed
2nano level Au particle in/CFP tri compound nano-photocatalyst.
(3) Au/TiO
2/ CFP tri compound nano-photocatalyst is to the cinnamic visible light photocatalytic degradation research of gas phase: Fig. 6 is the Au/TiO that embodiment 1 prepares
2/ CFP tri compound nano-photocatalyst is to cinnamic adsorption curve and kinetics of photocatalytic degradation curve.As seen from the figure, this photochemical catalyst shows good absorption and photocatalytic activity, and degradation results shows can reach 90.7% at 180min to cinnamic degradation rate.
The Au/TiO that the embodiment of the present invention 1 ~ 9 is obtained
2in/CFP tri compound nano-photocatalyst, diameter is that the carbon fiber surface of 5 ~ 10 microns is wrapped up completely by the titanium dioxide nano thread that diameter is 20 ~ 60 nanometers, reach several microns, and has particle size to be the surface that the gold nano grain of 2 ~ 10 nanometers is dispersed in carbon fiber and titanium dioxide nano thread; Its X-ray diffraction spectrum, laser Raman spectroscopy and x-ray photoelectron power spectrum show that C, Ti and Au tri-kinds of elements coexist in catalyst.UV-Vis diffuse reflection spectroscopy then shows that this tri compound nano-photocatalyst has superior Uv and visible light absorbent properties.Au/TiO prepared by the present invention can be found out by above result
2/ CFP tri compound nano-photocatalyst is the new material of a kind of high absorption and visible light catalysis activity.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. an Au/TiO
2the preparation method of/CFP tri compound nano-photocatalyst, is characterized in that comprising following steps:
(1) carbon fiber paper is immersed in dense HNO
3with dense H
2sO
4in the nitration mixture of composition, reflux 30 ~ 180min at 85 ~ 95 DEG C, and then washing is to neutral, by the drying precipitate after washing, obtains the carbon fiber paper after purifying;
(2) butyl titanate is joined in ethanol, after stirring, obtain the settled solution that concentration is the butyl titanate of 2 ~ 50g/L;
(3) carbon fiber paper after the purifying of step (1) gained is joined in the settled solution of the butyl titanate of step (2) gained wetting, take out, dry; Repeat wetting and dry run 2 ~ 5 times, obtain butyl titanate solution-wet and dried carbon fiber paper;
(4) prepare the mixing suspension of NaOH and titanium dioxide, wherein the final concentration of NaOH is 50 ~ 200g/L, and the final concentration of titanium dioxide is 4 ~ 20g/L;
(5) by the butyl titanate solution-wet of step (3) gained and dried carbon fiber paper to add in the mixing suspension of gained in step (4) hydro-thermal reaction 6 ~ 48h at 90 ~ 150 DEG C; Products therefrom cyclic washing, to neutral, by the drying precipitate after washing, obtains TiO
2/ CFP binary composite photo-catalyst;
(6) by the TiO of step (5) gained
2/ CFP binary composite photo-catalyst joins the HAuCl that concentration is 5 ~ 15g/L
4in the aqueous solution, lucifuge leaves standstill 0.5 ~ 5h, then irradiates 1 ~ 5h under being placed on ultraviolet; Take out product, cyclic washing, to neutral, by the drying precipitate after washing, obtains Au/TiO
2/ CFP tri compound nano-photocatalyst.
2. Au/TiO according to claim 1
2the preparation method of/CFP tri compound nano-photocatalyst, is characterized in that:
Dense HNO described in step (1)
3mass fraction be 69%.
3. Au/TiO according to claim 1
2the preparation method of/CFP tri compound nano-photocatalyst, is characterized in that:
Dense H described in step (1)
2sO
4mass fraction be 98%.
4. Au/TiO according to claim 1
2the preparation method of/CFP tri compound nano-photocatalyst, is characterized in that:
Dense HNO in nitration mixture described in step (1)
3with dense H
2sO
4volume ratio be 1:(1 ~ 5).
5. Au/TiO according to claim 1
2the preparation method of/CFP tri compound nano-photocatalyst, is characterized in that:
Baking temperature described in step (1) is 50 ~ 180 DEG C; Drying time is 3 ~ 12h.
6. Au/TiO according to claim 1
2the preparation method of/CFP tri compound nano-photocatalyst, is characterized in that:
Baking temperature described in step (3) is 50 ~ 180 DEG C, and drying time is 10 ~ 30min.
7. Au/TiO according to claim 1
2the preparation method of/CFP tri compound nano-photocatalyst, is characterized in that:
Baking temperature described in step (5) is 50 ~ 180 DEG C, and drying time is 3 ~ 24h.
8. Au/TiO according to claim 1
2the preparation method of/CFP tri compound nano-photocatalyst, is characterized in that:
Baking temperature described in step (6) is 50 ~ 180 DEG C, and drying time is 3 ~ 24h.
9. an Au/TiO
2/ CFP tri compound nano-photocatalyst, is characterized in that: the preparation method according to any one of claim 1 ~ 8 prepares.
10. Au/TiO according to claim 9
2the application of/CFP tri compound nano-photocatalyst in field of Environment Protection.
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