CN104826628A - Preparation method of graphene-iron doped TiO2 nanowire with high catalytic degradation activity under visible light - Google Patents
Preparation method of graphene-iron doped TiO2 nanowire with high catalytic degradation activity under visible light Download PDFInfo
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Abstract
The invention relates to a preparation method of a graphene-iron doped TiO2 nanowire with high catalytic degradation activity under visible light, and belongs to the technical field of photocatalysts. The method comprises the following steps: synthesizing an iron doped TiO2 nanowire from TiO2P25 through an alkaline hydrothermal technology, uniformly dispersing the iron doped TiO2 nanowire and graphene oxide according to a certain ratio, and carrying out a hydrothermal synthesis technology to synthesize the graphene-iron doped TiO2 nanowire. The graphene-iron doped TiO2 nanowire synthesized in the invention has strong adsorption ability to organic pollutants, has high catalytic degradation activity on the organic pollutants under visible light, has 2 times higher catalytic degradation ability than TiO2P25, has 1 time higher catalytic degradation ability than the iron doped TiO2 nanowire, and has high practical application values.
Description
Technical field
The present invention relates to a kind of Fen Yin Ji – doped Ti O under visible light with high catalytic degradation activity
2method for making, belong to the technical field preparing photochemical catalyst.
Background technology
In photocatalysis technology, TiO
2as cheap, stable, efficient photocatalyst material, at home and abroad admitted all widely.But TiO
2be wide bandgap semiconductor, only have response at ultraviolet region, and wavelength only accounts for 5% of sunshine gross energy at the ultraviolet light of below 400nm.In addition, the photo-generate electron-hole that titanium dioxide self produces is high to recombination rate, and therefore, only change TiO
2the character such as physics, chemistry, crystal of itself, just can make it be improved to the utilization ratio of visible ray.
Two large thinkings are had: one is to TiO for reaching this purpose
2modification make its response wave length generation red shift, mainly contain the means such as metal/non-metal doping, low-gap semiconductor compound, dye sensitization, pattern modification; Another kind is to TiO
2compound has the ordered nano tubulose structure that efficent electronic transmits, and the transmission of light induced electron is significantly strengthened, thus realizes the improvement of photochemical catalyst.Graphene is the outstanding material of known at present electric conductivity, and the transmission speed of its electronics can reach 1/300 of the light velocity, is conducive in addition improving the adsorption rate of target contaminant at catalyst surface.The preparation method of Graphene the most frequently used is now chemistry redox method.To be first Bian obtain graphite oxide with comparatively extensive chemical oxidant by graphite oxidation to this method, these oxy radicals can interact with cation, for nano particle provides the active sites of coring and increment, thus impel Graphene and inorganic semiconductor material compound, then graphene oxide is partially reduced to Graphene.Therefore by the TiO after modification
2shi Mo Xi – TiO is prepared with Graphene compound
2photochemical catalyst strengthens improvement TiO
2the effective way of photocatalysis performance.
Shi Mo Xi – TiO
2the preparation method of compound and kind are a lot, but Shi Mo Xi – ion doping TiO
2the preparation of nanowire composite is but not yet reported, due to TiO
2nano wire is uniformly dispersed on Graphene, both can by light degradation regional expansion to visible region, simultaneously advantageously in the transmission of light induced electron, reduce the compound that photo-generate electron-hole is right, be conducive in addition improving the adsorption rate of target contaminant at catalyst surface, and ion doping also effectively can reduce TiO
2energy gap, reduce the right compound of photo-generate electron-hole, Shi Mo Xi – ion doping TiO can be predicted
2the photocatalysis performance of compound will improve further.Therefore, Shi Mo Xi – ion doping TiO is prepared
2compound has important Research Significance and application prospect.Based under this background, the present invention has synthesized a kind of Shi Mo Xi – Fe2O3 doping TiO under visible light with high catalytic degradation activity
2nanowire composite photocatalyst.
Summary of the invention
Object of the present invention: doping, pattern modification and compound are had the improvement opportunity such as the material with carbon element that efficent electronic transmits and be combined TiO
2photocatalysis performance carry out deep improvement, improve on the one hand its photocatalytic activity in visible region, improve catalyst on the other hand to the absorption of pollutant and degradation capability, prepare the photochemical catalyst under visible light organic pollution to high catalytic degradation activity.
Technical scheme of the present invention: a kind of Shi Mo Xi – Fe2O3 doping TiO under visible light with high catalytic degradation activity
2the method for making of nano wire, carry out according to following steps:
(1) Fe2O3 doping TiO
2the synthesis of nano wire: 2.0g TiO
2(Degussa P25) and be the FeCl of 1% with titanium source mol ratio
36H
2o coccoid joins in the aqueous solution of 60mL, and stir 10min, now add KOH wherein, the ultrasonic agitation that hockets again 30 ~ 60min, every 15min alternately once, until obtain uniform suspension, this suspension is poured into 100mL containing teflon lined autoclave in, at autoclave being remained on 200 DEG C, room temperature is naturally cooled to after reaction terminates, the product obtained is successively with rare HCl aqueous solution, deionized water and methanol wash are several times, until pH value equals 7, after vacuum filtration, wet recovery product at 70 DEG C dry 6 hours, roasting at last 300 DEG C, finally obtain Fe2O3 doping TiO
2nano wire,
(2) Shi Mo alkene – Fe2O3 doping TiO
2the synthesis of nano wire: graphene oxide is dissolved in ethanol and distilled water solution, ultrasonic process 1h, then adds 2.0g Fe2O3 doping TiO
2nano wire is in obtained solution, hocketed ultrasonic agitation 80min, every 20min alternately once, to obtain uniform suspension, then suspension is placed on containing in teflon-lined autoclave of a 100mL, react a period of time at 120 DEG C after, prepares Graphene-Fe2O3 doping TiO
2nanowire composite, finally, by with ethanol rinse several times, filter the compound that obtains, and at room temperature dry after preserve;
(3) Shi Mo alkene – Fe2O3 doping TiO
2nano wire light degradation organic pollution: 100mg Shi Mo Xi – Fe2O3 doping TiO
2it is in the methylene blue solution of 10mg/L that nano wire photochemical catalyst joins 500mL concentration, stirs 60min in dark, then under 400W Metal halogen lamp, carries out degradation experiment, solution is 15cm apart from light source distance, every 20min clock pipettes 5mL solution, centrifugal, carries out degradation effect detection to supernatant.
The time that above-mentioned steps (1) mesohigh still remains on 200 DEG C is 18 ~ 30h; In step (1), roasting time is 2 ~ 6h; In step (2), graphene oxide quality is 20 ~ 40mg; In step (2), the volume ratio of ethanol and distilled water is 1:3 ~ 1:1.Shi Mo Xi – Fe2O3 doping TiO in step (3)
2the ability of nano wire catalytic degradation methylene blue is under visible light relative to TiO
2(Degussa P25) improves 147 ~ 206%, relative to Fe2O3 doping TiO
2nano wire improves 70 ~ 89%.
The present invention adopts the Fe2O3 doping TiO of water heat transfer
2, more under hydrothermal conditions with Graphene compound, there is under preparing visible ray the Graphene of high catalytic activity-mix iron TiO
2nano wire photochemical catalyst.
Technological merit of the present invention: use Fe2O3 doping TiO
2nano wire improves the recombination rate utilization rate of visible ray being reduced simultaneously to photo-generate electron-hole, by Fe2O3 doping TiO
2the recombination rate of catalyst photo-generate electron-hole is more effectively reduced further and the utilization rate that improve visible ray after nano wire and Graphene compound, the compound of Graphene improves the adsorption capacity of catalyst to organic pollution simultaneously, thus greatly improves photochemical catalyst in visible region degradable organic pollutant ability.
Accompanying drawing explanation
Fig. 1: photocatalyst for degrading methylene blueprint: (a) TiO
2(Degussa P25), (b) Fe2O3 doping TiO
2nano wire, (c) Graphene-mix iron TiO
2nano wire.
Detailed description of the invention
Embodiment can make those skilled in the art comprehensively understand the present invention below, but does not limit the present invention in any way.
Embodiment 1:
(1) Fe2O3 doping TiO
2the synthesis of nano wire: 2.0g TiO
2(Degussa P25) and be the FeCl of 1% with titanium source mol ratio
36H
2o coccoid joins in the aqueous solution of 60mL, and stir 10min, now add the KOH of 30g wherein, hocket ultrasonic agitation 30min again, every 15min hockets once, until obtain uniform suspension, this suspension is poured into 100mL containing teflon lined autoclave in, 18h at autoclave being remained on 200 DEG C, then room temperature is naturally cooled to, the product obtained is successively with rare HCl aqueous solution, deionized water and methanol wash are several times, until pH value equals 7, after vacuum filtration, wet recovery product at 70 DEG C dry 6 hours, roasting 2h at last 300 DEG C, finally obtain Fe2O3 doping TiO
2nano wire,
(2) Shi Mo alkene – Fe2O3 doping TiO
2the synthesis of nano wire: 20mg graphene oxide is dissolved in 20mL ethanol and 60mL distilled water solution, ultrasonic process 1h, then adds 2.0g Fe2O3 doping TiO
2nano wire is in obtained solution, by its ultrasonic agitation 80min, every 20min replaces once, to obtain uniform suspension, then suspension is placed on containing in teflon-lined autoclave of a 100mL, react a period of time at 120 DEG C after, prepares Graphene-Fe2O3 doping TiO
2nanowire composite, finally, by with ethanol rinse several times, filter the compound that obtains, and at room temperature dry after preserve;
(3) Shi Mo alkene – Fe2O3 doping TiO
2nano wire light degradation organic pollution: 100mg Graphene-mix iron TiO
2it is in the methylene blue solution of 10mg/L that nano wire photochemical catalyst joins 500mL concentration, stirs 60min in dark, then under 400W Metal halogen lamp, carries out degradation experiment, solution is 15cm apart from light source distance, every 20min clock pipettes 5mL solution, centrifugal, carries out degradation effect detection to supernatant.Result shows: Shi Mo alkene – Fe2O3 doping TiO
2the ability of nano wire catalytic degradation methylene blue is under visible light relative to TiO
2(Degussa P25) improves 164%, relative to Fe2O3 doping TiO
2nano wire improves 76%.
Embodiment 2:
(1) Fe2O3 doping TiO
2the synthesis of nano wire: 2.0g TiO
2(Degussa P25) and be the FeCl of 1% with titanium source mol ratio
36H
2o coccoid joins in the aqueous solution of 60mL, and stir 10min, now add the KOH of 40g wherein, ultrasonic agitation 30min again, every 15min hockets once, until obtain uniform suspension, this suspension is poured into 100mL containing teflon lined autoclave in, 24h at autoclave being remained on 200 DEG C, then room temperature is naturally cooled to, the product obtained is successively with rare HCl aqueous solution, deionized water and methanol wash are several times, until pH value equals 7, after vacuum filtration, wet recovery product at 70 DEG C dry 6 hours, roasting 2h at last 300 DEG C, finally obtain Fe2O3 doping TiO
2nano wire,
(2) Shi Mo alkene – Fe2O3 doping TiO
2the synthesis of nano wire: 20mg graphene oxide is dissolved in 25mL ethanol and 60mL distilled water solution, ultrasonic process 1h, then adds 2.0g Fe2O3 doping TiO
2nano wire is in obtained solution, by its ultrasonic agitation 80min, every 20min replaces once, to obtain uniform suspension, then suspension is placed on containing in teflon-lined autoclave of a 100mL, react a period of time at 120 DEG C after, prepares Graphene-Fe2O3 doping TiO
2nanowire composite, finally, by with ethanol rinse several times, filter the compound that obtains, and at room temperature dry after preserve;
(3) Shi Mo alkene – Fe2O3 doping TiO
2nano wire light degradation organic pollution: 100mg Graphene-mix iron TiO
2it is in the methylene blue solution of 10mg/L that nano wire photochemical catalyst joins 500mL concentration, stirs 60min in dark, then under 400W Metal halogen lamp, carries out degradation experiment, solution is 15cm apart from light source distance, every 20min clock pipettes 5mL solution, centrifugal, carries out degradation effect detection to supernatant.Result shows: Shi Mo alkene – Fe2O3 doping TiO
2the ability of nano wire catalytic degradation methylene blue is under visible light relative to TiO
2(Degussa P25) improves 206%, relative to Fe2O3 doping TiO
2nano wire improves 89%.
Embodiment 3:
(1) Fe2O3 doping TiO
2the synthesis of nano wire: 2.0g TiO
2(Degussa P25) and be the FeCl of 1% with titanium source mol ratio
36H
2o coccoid joins in the aqueous solution of 60mL, and stir 10min, now add the KOH of 50g wherein, ultrasonic agitation 30min again, every 15min hockets once, until obtain uniform suspension, this suspension is poured into 100mL containing teflon lined autoclave in, 24h at autoclave being remained on 200 DEG C, then room temperature is naturally cooled to, the product obtained is successively with rare HCl aqueous solution, deionized water and methanol wash are several times, until pH value equals 7, after vacuum filtration, wet recovery product at 70 DEG C dry 6 hours, roasting 4h at last 300 DEG C, finally obtain Fe2O3 doping TiO
2nano wire,
(2) Shi Mo alkene – Fe2O3 doping TiO
2the synthesis of nano wire: 20mg graphene oxide is dissolved in 25mL ethanol and 60mL distilled water solution, ultrasonic process 1h, then adds 2.0g Fe2O3 doping TiO
2nano wire is in obtained solution, by its ultrasonic agitation 80min, every 20min replaces once, to obtain uniform suspension, then suspension is placed on containing in teflon-lined autoclave of a 100mL, react a period of time at 120 DEG C after, prepares Graphene-Fe2O3 doping TiO
2nanowire composite, finally, by with ethanol rinse several times, filter the compound that obtains, and at room temperature dry after preserve;
(3) Shi Mo alkene – Fe2O3 doping TiO
2nano wire light degradation organic pollution: 100mg Graphene-mix iron TiO
2it is in the methylene blue solution of 10mg/L that nano wire photochemical catalyst joins 500mL concentration, stirs 60min in dark, then under 400W Metal halogen lamp, carries out degradation experiment, solution is 15cm apart from light source distance, every 20min clock pipettes 5mL solution, centrifugal, carries out degradation effect detection to supernatant.Result shows: Shi Mo alkene – Fe2O3 doping TiO
2the ability of nano wire catalytic degradation methylene blue is under visible light relative to TiO
2(Degussa P25) improves 172%, relative to Fe2O3 doping TiO
2nano wire improves 80%.
Embodiment 4:
(1) Fe2O3 doping TiO
2the synthesis of nano wire: 2.0g TiO
2(Degussa P25) and be the FeCl of 1% with titanium source mol ratio
36H
2o coccoid joins in the aqueous solution of 60mL, and stir 10min, now add the KOH of 40g wherein, ultrasonic agitation 60min again, every 15min hockets once, until obtain uniform suspension, this suspension is poured into 100mL containing teflon lined autoclave in, 30h at autoclave being remained on 200 DEG C, then room temperature is naturally cooled to, the product obtained is successively with rare HCl aqueous solution, deionized water and methanol wash are several times, until pH value equals 7, after vacuum filtration, wet recovery product at 70 DEG C dry 6 hours, roasting 2h at last 300 DEG C, finally obtain Fe2O3 doping TiO
2nano wire,
(2) Shi Mo alkene – Fe2O3 doping TiO
2the synthesis of nano wire: 20mg graphene oxide is dissolved in 25mL ethanol and 60mL distilled water solution, ultrasonic process 1h, then adds 2.0g Fe2O3 doping TiO
2nano wire is in obtained solution, by its ultrasonic agitation 80min, every 20min replaces once, to obtain uniform suspension, then suspension is placed on containing in teflon-lined autoclave of a 100mL, react a period of time at 120 DEG C after, prepares Graphene-Fe2O3 doping TiO
2nanowire composite, finally, by with ethanol rinse several times, filter the compound that obtains, and at room temperature dry after preserve;
(3) Shi Mo alkene – Fe2O3 doping TiO
2nano wire light degradation organic pollution: 100mg Graphene-mix iron TiO
2it is in the methylene blue solution of 10mg/L that nano wire photochemical catalyst joins 500mL concentration, stirs 60min in dark, then under 400W Metal halogen lamp, carries out degradation experiment, solution is 15cm apart from light source distance, every 20min clock pipettes 5mL solution, centrifugal, carries out degradation effect detection to supernatant.Result shows: Shi Mo alkene – Fe2O3 doping TiO
2the ability of nano wire catalytic degradation methylene blue is under visible light relative to TiO
2(Degussa P25) improves 198%, relative to Fe2O3 doping TiO
2nano wire improves 87%.
Embodiment 5:
(1) Fe2O3 doping TiO
2the synthesis of nano wire: 2.0g TiO
2(Degussa P25) and be the FeCl of 1% with titanium source mol ratio
36H
2o coccoid joins in the aqueous solution of 60mL, and stir 10min, now add the KOH of 50g wherein, ultrasonic agitation 30min again, every 15min hockets once, until obtain uniform suspension, this suspension is poured into 100mL containing teflon lined autoclave in, 30h at autoclave being remained on 200 DEG C, then room temperature is naturally cooled to, the product obtained is successively with rare HCl aqueous solution, deionized water and methanol wash are several times, until pH value equals 7, after vacuum filtration, wet recovery product at 70 DEG C dry 6 hours, roasting 6h at last 300 DEG C, finally obtain Fe2O3 doping TiO
2nano wire,
(2) Shi Mo alkene – Fe2O3 doping TiO
2the synthesis of nano wire: 20mg graphene oxide is dissolved in 25mL ethanol and 60mL distilled water solution, ultrasonic process 1h, then adds 2.0g Fe2O3 doping TiO
2nano wire is in obtained solution, by its ultrasonic agitation 80min, every 20min replaces once, to obtain uniform suspension, then suspension is placed on containing in teflon-lined autoclave of a 100mL, react a period of time at 120 DEG C after, prepares Graphene-Fe2O3 doping TiO
2nanowire composite, finally, by with ethanol rinse several times, filter the compound that obtains, and at room temperature dry after preserve;
(3) Shi Mo alkene – Fe2O3 doping TiO
2nano wire light degradation organic pollution: 100mg Graphene-mix iron TiO
2it is in the methylene blue solution of 10mg/L that nano wire photochemical catalyst joins 500mL concentration, stirs 60min in dark, then under 400W Metal halogen lamp, carries out degradation experiment, solution is 15cm apart from light source distance, every 20min clock pipettes 5mL solution, centrifugal, carries out degradation effect detection to supernatant.Result shows: Shi Mo alkene – Fe2O3 doping TiO
2the ability of nano wire catalytic degradation methylene blue is under visible light relative to TiO
2(Degussa P25) improves 147%, relative to Fe2O3 doping TiO
2nano wire improves 70%.
Embodiment 6:
(1) Fe2O3 doping TiO
2the synthesis of nano wire: 2.0g TiO
2(Degussa P25) and be the FeCl of 1% with titanium source mol ratio
36H
2o coccoid joins in the aqueous solution of 60mL, and stir 10min, now add the KOH of 50g wherein, ultrasonic agitation 30min again, every 15min hockets once, until obtain uniform suspension, this suspension is poured into 100mL containing teflon lined autoclave in, 24h at autoclave being remained on 200 DEG C, then room temperature is naturally cooled to, the product obtained is successively with rare HCl aqueous solution, deionized water and methanol wash are several times, until pH value equals 7, after vacuum filtration, wet recovery product at 70 DEG C dry 6 hours, roasting 2h at last 300 DEG C, finally obtain Fe2O3 doping TiO
2nano wire,
(2) Shi Mo alkene – Fe2O3 doping TiO
2the synthesis of nano wire: 20mg graphene oxide is dissolved in 20mL ethanol and 60mL distilled water solution, ultrasonic process 1h, then adds 2.0g Fe2O3 doping TiO
2nano wire is in obtained solution, by its ultrasonic agitation 80min, every 20min replaces once, to obtain uniform suspension, then suspension is placed on containing in teflon-lined autoclave of a 100mL, react a period of time at 120 DEG C after, prepares Graphene-Fe2O3 doping TiO
2nanowire composite, finally, by with ethanol rinse several times, filter the compound that obtains, and at room temperature dry after preserve;
(3) Shi Mo alkene – Fe2O3 doping TiO
2nano wire light degradation organic pollution: 100mg Graphene-mix iron TiO
2it is in the methylene blue solution of 10mg/L that nano wire photochemical catalyst joins 500mL concentration, stirs 60min in dark, then under 400W Metal halogen lamp, carries out degradation experiment, solution is 15cm apart from light source distance, every 20min clock pipettes 5mL solution, centrifugal, carries out degradation effect detection to supernatant.Result shows: Shi Mo alkene – Fe2O3 doping TiO
2the ability of nano wire catalytic degradation methylene blue is under visible light relative to TiO
2(Degussa P25) improves 188%, relative to Fe2O3 doping TiO
2nano wire improves 80%.
Embodiment 7:
(1) Fe2O3 doping TiO
2the synthesis of nano wire: 2.0g TiO
2(Degussa P25) and be the FeCl of 1% with titanium source mol ratio
36H
2o coccoid joins in the aqueous solution of 60mL, and stir 10min, now add the KOH of 40g wherein, ultrasonic agitation 30min again, every 15min hockets once, until obtain uniform suspension, this suspension is poured into 100mL containing teflon lined autoclave in, 24h at autoclave being remained on 200 DEG C, then room temperature is naturally cooled to, the product obtained is successively with rare HCl aqueous solution, deionized water and methanol wash are several times, until pH value equals 7, after vacuum filtration, wet recovery product at 70 DEG C dry 6 hours, roasting 2h at last 300 DEG C, finally obtain Fe2O3 doping TiO
2nano wire,
(2) Shi Mo alkene – Fe2O3 doping TiO
2the synthesis of nano wire: 40mg graphene oxide is dissolved in 40mL ethanol and 40mL distilled water solution, ultrasonic process 1h, then adds 2.0g Fe2O3 doping TiO
2nano wire is in obtained solution, by its ultrasonic agitation 80min, every 20min replaces once, to obtain uniform suspension, then suspension is placed on containing in teflon-lined autoclave of a 100mL, react a period of time at 120 DEG C after, prepares Graphene-Fe2O3 doping TiO
2nanowire composite, finally, by with ethanol rinse several times, filter the compound that obtains, and at room temperature dry after preserve;
(3) Shi Mo alkene – Fe2O3 doping TiO
2nano wire light degradation organic pollution: 100mg Graphene-mix iron TiO
2it is in the methylene blue solution of 10mg/L that nano wire photochemical catalyst joins 500mL concentration, stirs 60min in dark, then under 400W Metal halogen lamp, carries out degradation experiment, solution is 15cm apart from light source distance, every 20min clock pipettes 5mL solution, centrifugal, carries out degradation effect detection to supernatant.Result shows: Shi Mo alkene – Fe2O3 doping TiO
2the ability of nano wire catalytic degradation methylene blue is under visible light relative to TiO
2(Degussa P25) improves 189%, relative to Fe2O3 doping TiO
2nano wire improves 75%.
Embodiment 8:
(1) Fe2O3 doping TiO
2the synthesis of nano wire: 2.0g TiO
2(Degussa P25) and be the FeCl of 1% with titanium source mol ratio
36H
2o coccoid joins in the aqueous solution of 60mL, and stir 10min, now add the KOH of 50g wherein, ultrasonic agitation 60min again, every 15min hockets once, until obtain uniform suspension, this suspension is poured into 100mL containing teflon lined autoclave in, 18h at autoclave being remained on 200 DEG C, then room temperature is naturally cooled to, the product obtained is successively with rare HCl aqueous solution, deionized water and methanol wash are several times, until pH value equals 7, after vacuum filtration, wet recovery product at 70 DEG C dry 6 hours, roasting 2h at last 300 DEG C, finally obtain Fe2O3 doping TiO
2nano wire,
(2) Shi Mo alkene – Fe2O3 doping TiO
2the synthesis of nano wire: 30mg graphene oxide is dissolved in 30mL ethanol and 60mL distilled water solution, ultrasonic process 1h, then adds 2.0g Fe2O3 doping TiO
2nano wire is in obtained solution, by its ultrasonic agitation 80min, every 20min replaces once, to obtain uniform suspension, then suspension is placed on containing in teflon-lined autoclave of a 100mL, react a period of time at 120 DEG C after, prepares Graphene-Fe2O3 doping TiO
2nanowire composite, finally, by with ethanol rinse several times, filter the compound that obtains, and at room temperature dry after preserve;
(3) Shi Mo alkene – Fe2O3 doping TiO
2nano wire light degradation organic pollution: 100mg Graphene-mix iron TiO
2it is in the methylene blue solution of 10mg/L that nano wire photochemical catalyst joins 500mL concentration, stirs 60min in dark, then under 400W Metal halogen lamp, carries out degradation experiment, solution is 15cm apart from light source distance, every 20min clock pipettes 5mL solution, centrifugal, carries out degradation effect detection to supernatant.Result shows: Shi Mo alkene – Fe2O3 doping TiO
2the ability of nano wire catalytic degradation methylene blue is under visible light relative to TiO
2(Degussa P25) improves 166%, relative to Fe2O3 doping TiO
2nano wire improves 72%.
Claims (2)
1. one kind has the stone ink alkene – Fe2O3 doping TiO of high catalytic degradation activity under visible light
2the method for making of nano wire, is characterized in that carrying out according to following steps:
(1) Fe2O3 doping TiO
2the synthesis of nano wire: 2.0g TiO
2(Degussa P25) and be the FeCl of 1% with titanium source mol ratio
36H
2o coccoid joins in the aqueous solution of 60mL, and stir 10min, now add KOH wherein, the ultrasonic agitation that hockets again 30 ~ 60min, every 15min alternately once, until obtain uniform suspension, this suspension is poured into 100mL containing teflon lined autoclave in, 18 ~ 30h at autoclave being remained on 200 DEG C, room temperature is naturally cooled to after reaction terminates, the product obtained is successively with rare HCl aqueous solution, deionized water and methanol wash are several times, until pH value equals 7, after vacuum filtration, wet recovery product at 70 DEG C dry 6 hours, roasting 2 ~ 6h at last 300 DEG C, finally obtain Fe2O3 doping TiO
2nano wire,
(2) Shi Mo alkene – Fe2O3 doping TiO
2the synthesis of nano wire: 20 ~ 40mg graphene oxide is dissolved in the ethanol and distilled water solution that volume ratio is 1:3 ~ 1:1, and ultrasonic process 1h, then adds 2.0g Fe2O3 doping TiO
2nano wire is in obtained solution, hocketed ultrasonic agitation 80min, every 20min alternately once, to obtain uniform suspension, then suspension is placed on containing in teflon-lined autoclave of a 100mL, react a period of time at 120 DEG C after, prepares Graphene-Fe2O3 doping TiO
2nanowire composite, finally, with ethanol rinse several times, filter the compound that obtains, and at room temperature dry after preserve;
(3) Shi Mo alkene – Fe2O3 doping TiO
2nano wire light degradation organic pollution: 100mg Graphene-mix iron TiO
2it is in the methylene blue solution of 10mg/L that nano wire photochemical catalyst joins 500mL concentration, stirs 60min in dark, then under 400W Metal halogen lamp, carries out degradation experiment, solution is 15cm apart from light source distance, every 20min clock pipettes 5mL solution, centrifugal, carries out degradation effect detection to supernatant.
2. method according to claim 1, is characterized in that described catalyst Shi Mo Xi – Fe2O3 doping TiO
2nano wire has good degradation capability to methylene blue under visible light.
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| CN106512975A (en) * | 2016-10-19 | 2017-03-22 | 常州大学 | Preparation method and application of sulfur-doped titanium dioxide-graphene aerogel composite material |
| CN107930617A (en) * | 2017-11-29 | 2018-04-20 | 江南大学 | A kind of witch culture TiO with high catalytic degradation activity2The preparation method of/graphene complex |
| CN107930616A (en) * | 2017-11-29 | 2018-04-20 | 江南大学 | A kind of preparation method of the molybdenum trioxide with high catalytic degradation activity/titanium dioxide/graphene compound |
| CN109759065A (en) * | 2019-01-14 | 2019-05-17 | 中国人民解放***箭军工程大学 | The laminated film of titanium dichloride load nickel ferrite based magnetic loaded and graphene oxide, preparation method and its application in the treatment of waste water |
| CN112058276A (en) * | 2020-08-25 | 2020-12-11 | 常州烯奇新材料有限公司 | Iron ion modified photocatalyst composite material and preparation method thereof |
| CN113694927A (en) * | 2021-09-09 | 2021-11-26 | 江苏盛世基业环保科技有限公司 | Self-dispersion graphene and iron co-doped nano titanium dioxide and preparation method thereof |
| CN113694927B (en) * | 2021-09-09 | 2024-04-12 | 江苏盛世基业环保科技有限公司 | Self-dispersing graphene and iron co-doped nano titanium dioxide and preparation method thereof |
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