CN103551150B - A kind of preparation method of the magnetic composite photocatalyst based on carbonaceous material - Google Patents
A kind of preparation method of the magnetic composite photocatalyst based on carbonaceous material Download PDFInfo
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- CN103551150B CN103551150B CN201310293513.1A CN201310293513A CN103551150B CN 103551150 B CN103551150 B CN 103551150B CN 201310293513 A CN201310293513 A CN 201310293513A CN 103551150 B CN103551150 B CN 103551150B
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Abstract
The present invention is a kind of preparation method of the magnetic composite photocatalyst based on carbonaceous material, belongs to technical field of environmental material preparation.Multi-walled carbon nano-tubes pretreatment is obtained the multi-walled carbon nano-tubes of acidifying; The MWCNTs of activation and ethylene glycol are carried out ultrasonic, then it is ultrasonic to add nine water ferric nitrates, finally adds sodium acetate, polyethylene glycol (1500) and polyvinylpyrrolidone ultrasonic, obtain Fe
3o
4/ MWCNTs.Absolute ethyl alcohol and tetra-n-butyl titanate sealing are stirred, ethanol, distilled water and concentrated hydrochloric acid mixed solution dropwise add, and continue sealing and stir; Open wide and be stirred to colloidal sol shape, add Fe
3o
4/ MWCNTs is at the uniform velocity stirred to gel, obtains TiO after ageing calcining
2/ Fe
3o
4/ MWCNTs composite photo-catalyst.Advantage: the process capable of circulation of photochemical catalyst system effectively can improve light induced electron and hole to separative efficiency; Magnetic photocatalyst contributes to the rate of recovery improving catalyst, can good disposal of mercaptans class waste water.
Description
Technical field
The present invention relates to a kind of method utilizing the method for Hydrothermal Synthesis and combination of sol-gel to prepare magnetic titanium dioxide/tri-iron tetroxide/multi-walled carbon nano-tubes composite photo-catalyst, belong to technical field of environmental material preparation.
Background technology
2-sulfydryl-1-methylimidazole, as a kind of mercaptan, is used for the treatment of hyperthyroidism and non-cyanide is silver-plated.But its resistance to the action of a drug and side effect thereof also have a strong impact on the life of people simultaneously.Therefore, it is very important for rationally processing 2-sulfydryl-1-methylimidazole in sanitary wastewater.At present, adopt multiple technologies, as absorption, biodegradation, hydrodesulfurization and electrochemical degradation disposal of mercaptans.Wherein, photocatalysis technology is because of nontoxic, and stable, instant effect, the feature that energy consumption is low, has played important function at the energy and environmental area.Because semiconductor light-catalyst titanium dioxide has good photocatalytic activity, stability is high, and cost is low and toxicity is low, is widely used in wastewater treatment.The pollutant such as waste water, waste gas come in process life by carrying out modification to titanium dioxide has obtained good effect.
CNT has unique structure, and mechanical strength is high, good electric conductivity and heat endurance, can improve conductor photocatalysis activity in environmental treatment.On the other hand, by magnetic material as ferriferrous oxide nano-particle loads on CNT, be introduced in clean environment field.Because tri-iron tetroxide has magnetic, the magnetic composite photocatalyst of preparation can be separated simply by external magnetic field, and reuses.The more important thing is, the introducing of tri-iron tetroxide and CNT, effectively can improve the photocatalytic activity of titanium dioxide, the photocatalytic degradation capability of Promotion system.
Summary of the invention
The present invention for preparation means, prepares a kind of magnetic TiO based on carbonaceous material with Hydrothermal Synthesis and sol-gel
2/ Fe
3o
4/MWCNTs composite photo-catalyst.Its advantage is to build a cyclic process in system, realizes light induced electron and right being effectively separated in hole; Light source can be effectively utilized to reach the object of mercaptan waste water in environment of effectively degrading.
The technical solution used in the present invention is:
(1) Fe
3o
4the preparation of/MWCNTs: be that the red fuming nitric acid (RFNA) of 1:3 and concentrated sulfuric acid mixed solution stir 6h at 60 DEG C by effective for multi-wall carbon nano-tube volume ratio, washing 50 ~ 70 DEG C of vacuum drying one nights, namely acidification like this obtains the MWCNTs activated; The MWCNTs of activation and the ethylene glycol of certain volume are added ultrasonic 20min in reactor, wherein nine water ferric nitrates and MWCNTs mass ratio are 40:1 to add nine water ferric nitrate ultrasonic dissolution 20min(again), finally add sodium acetate (wherein sodium acetate and nine water ferric nitrate mass ratioes are 6:5), a certain amount of polyethylene glycol (1500) and the ultrasonic 20min of polyvinylpyrrolidone.200 DEG C of Hydrothermal Synthesis 12h, respectively with water and ethanol washing, at 50 ~ 70 DEG C of vacuum drying one nights, namely obtain Fe
3o
4/ MWCNTs.
(2) TiO
2/ Fe
3o
4the preparation of/MWCNTs composite photo-catalyst: by absolute ethyl alcohol and tetra-n-butyl titanate by volume 18:5 join in there-necked flask, 15min are stirred in 40 DEG C of sealings; Be the mixed solution of the ethanol of 180:15:1, distilled water and concentrated hydrochloric acid by volume ratio, dropwise join in above-mentioned solution, the volume ratio of mixed solution and above-mentioned tetra-n-butyl titanate is 196:5, continues sealing and stirs 10min; Non-tight is stirred to colloidal sol shape, by a certain amount of Fe obtained in above-mentioned steps (1)
3o
4/ MWCNTs immerses above-mentioned TiO
2in colloidal sol, Fe
3o
4/ MWCNTs and TiO
2colloidal sol mass ratio is about 1:70, is at the uniform velocity stirred to gel, at room temperature ageing 2
~4h; In nitrogen atmosphere, 500 DEG C of calcining xerogel 4h, naturally cool to room temperature, namely obtain TiO
2/ Fe
3o
4/ MWCNTs composite photo-catalyst.
Wherein the MWCNTs of activation in step (1) is with ethylene glycol than being 30:25mg/mL, and the mass ratio of polyethylene glycol (1500) and polyvinylpyrrolidone is 40:1.
The present invention adopts Hydrothermal Synthesis technology to prepare Fe
3o
4/ MWCNTs, carries out finishing with sol-gel technique to it and prepares the magnetic TiO with higher catalytic activity
2/ Fe
3o
4/ MWCNTs composite photo-catalyst.
Photocatalytic activity evaluation: carry out in GHX-2 type photochemical reaction instrument (purchased from Educational Instrument Factory of Yangzhou University), ultraviolet lamp irradiates, 50mL2-sulfydryl-1-methylimidazole simulated wastewater to be added in reactor and to measure its initial value, then composite photo-catalyst is added, magnetic agitation and open aerator pass into air make catalyst be in suspension or afloat, 10min sample analysis in interval in During Illumination, gets liquid at ultraviolet specrophotometer λ after Magneto separate
max=251nm place measures absorbance, and passes through formula: Dr=[(C
0-C
i)/C
0] × 100% calculates degradation rate, wherein C
0for the initial concentration of 2-sulfydryl-1-methyl imidazole solution during beginning light degradation, C
ifor the concentration of the 2-sulfydryl-1-methyl imidazole solution that timing sampling measures.
Technological merit of the present invention: the process capable of circulation of photochemical catalyst system effectively can improve the right separative efficiency of light induced electron and hole; Magnetic photocatalyst contributes to the rate of recovery improving catalyst; Can disposal of mercaptans class waste water preferably.
Accompanying drawing explanation
The 10mgL of Figure 10 .1g photochemical catalyst ultraviolet degradation 50mL
-12-sulfydryl-1-methylimidazole.TiO
2/ Fe
3o
4the ultraviolet degradation rate of/MWCNTs composite catalyst to the 2-sulfydryl-1-methylimidazole of the 10mg/L of 50mL reaches 82.7%, shows that the photochemical catalyst obtained has good photocatalytic activity.
Fig. 2 XRD collection of illustrative plates.MWCNTs, Fe
3o
4/ MWCNTs and TiO
2/ Fe
3o
4the X-ray diffractogram of/MWCNTs composite photo-catalyst.As can be seen from the figure TiO in composite photo-catalyst
2diffractive features peak be Detitanium-ore-type.
Fig. 3 SEM and EDS:(a) purifying MWCNTs (b) TiO
2/ Fe
3o
4/ MWCNTs.
TEM:(a) purifying MWCNTs (b) TiO
2/ Fe
3o
4/ MWCNTs.
MWCNTs and TiO of purifying
2/ Fe
3o
4the SEM of/MWCNTs composite catalyst, EDS and TEM scheme, and as can be seen from the figure MWCNTs surface changes.
Fig. 4 UV-visDRS spectrogram.TiO
2/ Fe
3o
4the UV-vis DRS figure of/MWCNTs composite catalyst.As can be seen from the figure, composite photo-catalyst has very high absorption intensity in UV, visible light region.
Fig. 5 FT-IR spectrum.Original MWCNTs and TiO
2/ Fe
3o
4the FT – IR spectrogram of/MWCNTs.The modification had composite photo-catalyst is described.
Fig. 6 magnetization curve.TiO
2/ Fe
3o
4the hysteresis curve figure of/MWCNTs composite catalyst.Show that sample has ferromagnetism.
Detailed description of the invention
Below in conjunction with concrete embodiment, the present invention will be further described.
Embodiment: effective for 0.5g multi-wall carbon nano-tube 15mL red fuming nitric acid (RFNA) and the 45mL concentrated sulfuric acid (volume ratio is 1:3) are stirred 6h at 60 DEG C by (1), washing is to neutral and 50 DEG C of vacuum drying one nights, namely acidification like this obtains the MWCNTs activated; MWCNTs and the 25mL ethylene glycol of the 30mg of activation is added ultrasonic 20min in reactor, add 1.239g nine water ferric nitrate (wherein nine water ferric nitrates and MWCNTs mass ratio are 40:1) ultrasonic 20min again, finally add 1.5g sodium acetate (wherein sodium acetate and nine water ferric nitrate mass ratioes are 6:5), 0.4g polyethylene glycol (1500) and the ultrasonic 20min of 10mg polyvinylpyrrolidone.200 DEG C of Hydrothermal Synthesis 12h, respectively with water and ethanol washing several times, at 50 DEG C of vacuum drying one nights, namely obtain Fe
3o
4/ MWCNTs.
(2) TiO
2/ Fe
3o
4the preparation of/MWCNTs composite photo-catalyst: 36mL absolute ethyl alcohol and 10mL tetra-n-butyl titanate (volume ratio 18:5) are joined in there-necked flask, 15min is stirred in 40 DEG C of sealings; 36mL ethanol, 3mL distilled water and 0.2mL concentrated hydrochloric acid mixed solution (volume ratio of mixed solution and above-mentioned tetra-n-butyl titanate is 196:5) are dropwise joined in above-mentioned solution, continues sealing and stir 10min; Open wide again and be stirred to colloidal sol shape, by 1.0gFe obtained in above-mentioned steps (1)
3o
4/ MWCNTs immerses above-mentioned TiO
2colloidal sol (Fe
3o
4/ MWCNTs and TiO
2colloidal sol mass ratio is about 1:70) in, be at the uniform velocity stirred to gel, at room temperature ageing 2h; In nitrogen atmosphere, 500 DEG C of calcining xerogel 4h, naturally cool to room temperature, namely obtain TiO
2/ Fe
3o
4/ MWCNTs composite photo-catalyst.
(3) get 0.1g(2) in sample in ultraviolet light photochemical reaction instrument, carry out photocatalytic degradation test, record the degradation rate of this photochemical catalyst to 2-sulfydryl-1-methylimidazole and in 1h, reach 82.7%(as Fig. 1), this composite photo-catalyst has stronger photocatalytic activity.
(4) as Fig. 2, from MWCNTs, Fe
3o
4/ MWCNTs and TiO
2/ Fe
3o
4tiO in composite photo-catalyst can be found out in the X-ray diffractogram of/MWCNTs composite photo-catalyst
2diffractive features peak be Detitanium-ore-type, this and standard Detitanium-ore-type TiO
2characteristic diffraction peak 2 θ=25.3 ° of crystal, 38 °, 48.1 °, 55.2 ° and 75.1 ° corresponding, this makes TiO in catalyst sample
2keep higher photocatalytic activity; 30.2 °, 35.4 °, 43.1 °, 57.2 ° and 62.8 ° is Fe
3o
4characteristic diffraction peak; 2 θ=25.3 ° are then MWCNTs diffraction maximum.
(5) as Fig. 3, from MWCNTs and TiO of purifying
2/ Fe
3o
4can find out in the SEM of/MWCNTs composite catalyst, EDS and TEM figure that the main component of catalyst sample base material is that Ti, O, Fe and C.MWCNT diameter is about 50nm, top layer load Fe
3o
4, that then cover is TiO
2.
(6) as Fig. 4, from TiO
2/ Fe
3o
4can find out in the UV-vis DRS figure of/MWCNTs composite catalyst, composite photo-catalyst has very high absorption intensity in UV, visible light region, shows that it has good Uv and visible light absorbability.
(7) as Fig. 5, original MWCNTs and TiO
2/ Fe
3o
4in the FT – IR spectrogram of/MWCNTs, 3400 – 3500cm
1shu Yu – OH, 1750cm
1illustrate that – C=O group is formed, 582cm
1belong to Fe – O, other difference of two figure has benefited from Ti – O. and the modification had composite photo-catalyst is described.
(8) as Fig. 6, TiO
2/ Fe
3o
4the hysteresis curve figure of/MWCNTs composite catalyst, saturation magnetization is that 7.25emu/g. coercivity and remanent magnetism are respectively 207.68Oe and 1.59emu/g, shows that sample has ferromagnetism.By TiO
2/ Fe
3o
4/ MWCNTs is scattered in water, the external magnet of beaker, and after a few minutes, solution becomes clarification, also shows that sample has magnetic.
Claims (2)
1., based on a preparation method for the magnetic composite photocatalyst of carbonaceous material, carry out according to following step:
(1) Fe
3o
4the preparation of/MWCNTs: be that the red fuming nitric acid (RFNA) of 1:3 and concentrated sulfuric acid mixed solution stir 6h at 60 DEG C by effective for multi-wall carbon nano-tube volume ratio, washing 50-70 DEG C of vacuum drying one night, namely acidification like this obtains the MWCNTs activated; The MWCNTs of activation and the ethylene glycol of certain volume are added ultrasonic 20min in reactor, add nine water ferric nitrate ultrasonic dissolution 20min again, finally add sodium acetate, a certain amount of polyethylene glycol and the ultrasonic 20min of polyvinylpyrrolidone, 200 DEG C of Hydrothermal Synthesis 12h, respectively with water and ethanol washing, at 50-70 DEG C of vacuum drying one night, namely obtain Fe
3o
4/ MWCNTs;
(2) TiO
2/ Fe
3o
4the preparation of/MWCNTs composite photo-catalyst: by absolute ethyl alcohol and tetra-n-butyl titanate by volume 18:5 join in there-necked flask, 15min are stirred in 40 DEG C of sealings; Be the mixed solution of the ethanol of 180:15:1, distilled water and concentrated hydrochloric acid by volume ratio, dropwise join in above-mentioned solution, the volume ratio of mixed solution and above-mentioned tetra-n-butyl titanate is 196:5, continues sealing and stirs 10min; Non-tight is stirred to colloidal sol shape, by a certain amount of Fe obtained in above-mentioned steps (1)
3o
4/ MWCNTs immerses above-mentioned TiO
2in colloidal sol, Fe
3o
4/ MWCNTs and TiO
2colloidal sol mass ratio is 1:70, is at the uniform velocity stirred to gel, at room temperature ageing 2-4h; In nitrogen atmosphere, 500 DEG C of calcining xerogel 4h, naturally cool to room temperature, namely obtain TiO
2/ Fe
3o
4/ MWCNTs composite photo-catalyst;
The amount of the nine water ferric nitrates added described in step (1) is: nine water ferric nitrates and MWCNTs mass ratio are 40:1; The amount of the sodium acetate added is: sodium acetate and nine water ferric nitrate mass ratioes are 6:5.
2., according to the preparation method of the magnetic composite photocatalyst described in claim 1, it is characterized in that the MWCNTs of the activation described in step (1) and ethylene glycol are than being 30:25mg/mL, the mass ratio of polyethylene glycol and polyvinylpyrrolidone is 40:1.
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