CN105032423A - Multiphase magnetic Fenton-photocatalyst and preparation method thereof and application - Google Patents

Multiphase magnetic Fenton-photocatalyst and preparation method thereof and application Download PDF

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CN105032423A
CN105032423A CN201510469566.3A CN201510469566A CN105032423A CN 105032423 A CN105032423 A CN 105032423A CN 201510469566 A CN201510469566 A CN 201510469566A CN 105032423 A CN105032423 A CN 105032423A
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张少旸
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Abstract

The invention relates to a multiphase magnetic Fenton-photocatalyst which is core-shell type microsphere Fe3O4@TiO2 which is of a three-layer structure. A core Fe3O4 microsphere is formed by stacking nanometer small granules of 15-30 nm, the thickness of a transitional SiO2 layer is 50-150 nm, and the thickness of an outermost TiO2 is 100-300 nm. The prepared photocatalyst has good superparamagnetism, can be separated thoroughly in 30 s under the effect of an outside magnetic field, is easy to recycle, can be recycled, and is environmentally friendly. The multiphase magnetic Fenton-photocatalyst can catalyze hydrogen peroxide under visible light to degrade organic pollutants, a multi-channel reaction pathway is formed, and accordingly high catalytic activity is achieved. A composite microsphere is good in monodispersity and can maintain high activity of a catalyst in wastewater treatment and improve utilization rate.

Description

A kind of heterogeneous magnetic Fenton-like-photochemical catalyst and its preparation method and application
Technical field
The present invention relates to nanometer material science and environmental science, particularly a kind of for the treatment of the Fe needed for poisonous in waste water from dyestuff, hardly degraded organic substance 3o 4siO 2tiO 2fenton-like-photochemical catalyst of heterogeneous magnetic and preparation method thereof.
Background technology
Along with the fast development of dyestuff textile industry, dyestuff textile waste discharge capacity sharply increases.Waste water from dyestuff due to its high colourity, biodegradability poor and containing " three cause " thing etc., serious threat is caused to human environment.Therefore, waste water from dyestuff is administered of far-reaching significance.
High-level oxidation technology produces oxyradical for main body, makes its attack larger molecular organics and react with it, thus destroy organic molecular structure until be decomposed into carbon dioxide and water, reaches the object of efficient degradation toxic organic pollutants.By Fe 2+and H 2o 2the Fenton system formed, owing to having rapidly and efficiently, operating process is simple, without the need to complex device, to follow-up process nonhazardous effect and the advantage such as environmentally friendly, be applied to the waste water treatment engineerings such as paper pulp papermaking, dyestuff, agricultural chemicals gradually.But this reaction needed regulates pH about 3, and H 2o 2dosage is large, and catalyst cannot reuse, and supervenes iron mud etc., limits the extensive use of Fenton reaction.
Heterogeneous Fenton system, utilizes solid catalyst and H 2o 2reaction produces hydroxyl radical free radical, realizes organic oxidation removal.Wherein, with nano level Fe 3o 4magnetic nanoparticle, as main body, is directly applied, or and some Material cladding, then with H 2o 2composition, be then a kind of multiphase-fenton Fenton catalysts of function admirable, water treatment effect is remarkable.
But nano level magnetic nanoparticle, its surface energy is high, very easily reunites, and cannot keep its high activity, must carry out surface treatment.Chinese invention patent (publication number: CN104190472A) discloses a kind of new and effective heterogeneous Fenton catalyst Fe 3o 4the preparations and applicatio of@EDTA, by the finishing of EDTA, improves the performance of magnetic catalyst.Chinese invention patent (publication number: CN104437494A) discloses a kind of class Catalysts and its preparation method and application of graphene coated tri-iron tetroxide microballoon.Similar, utilize the coated of Graphene, under the magnetic ensureing heterogeneous catalyst, promote catalytic efficiency and stability.Chinese invention patent (grant number: CN103331181B) then utilizes layer upon layer electrostatic self-assembling technique, by cationic polyelectrolyte and Nano-meter SiO_2 2granuloplastic alternating sorbent sequence layer is assembled in Fe 3o 4outward, magnetic core shell-type type Fenton catalyst is generated.Clad is loose structure, reduces the surface energy of nanometer, reduces and reunites, also protect the Fe as core simultaneously 3o 4, prevent it poisoning by contaminated wastewater.But the step of LBL self-assembly is long, operation is comparatively loaded down with trivial details.
In recent years, there is researcher in multiphase-fenton Fenton catalyst system, introduce TiO 2light helps reaction.Chinese invention patent (grant number: CN102513138B) a kind of Multi-phase light helps Fenton catalyst, with TiO 2as the carrier of Fe (III), using hydroxyapatite as TiO 2and the isolation transition zone between Fe (III), can catalyze and degrade organic pollutants under visible light, define a kind of reaction path by all kinds of means, obtain high catalytic activity.The people such as Xie Huanling prepare Fe 3o 4siO 2-TiO 2magnetic mesoporous composite material (Inner Mongol University of Technology's journal, 2014,33 (1): 25-31), first prepares Fe by hydro-thermal method 3o 4magnetic nano-particle, then by silicon source, titanium source, pore-foaming agent and Fe 3o 4magnetic nano-particle mixes, then carries out hydro-thermal reaction, obtains the Fe of core-shell type 3o 4siO 2-TiO 2.The core-shell microsphere prepared, core is Fe 3o 4magnetic nano-particle, shell is mesoporous SiO 2-TiO 2compound.Use it for the process of waste water from dyestuff, decolorizing effect is obvious.But SiO in shell 2and TiO 2boundary is unintelligible, part TiO 2may by SiO 2parcel, thus have lost photocatalytic activity.
Thus, there is researcher to point out, build multiphase-fenton Fenton-TiO 2during light body aid system, following problem can not be ignored: (1) is if by direct for free Fe (III) load at TiO 2surface, then Fe (III) may with ionic compartmentation doping form enter TiO 2lattice, destroy TiO 2stability.And also may reciprocation be there is and reduce activity in both.(2) using the material with carbon elements such as Graphene as isolation transition zone, can TiO be made 2surface transfer hydrophobicity to by hydrophily, be unfavorable for the catalytic reaction of waste water.
Summary of the invention
In view of above problem, the object of this invention is to provide a kind of heterogeneous magnetic Fenton-like-photochemical catalyst and its preparation method and application, the pH value of this heterogeneous magnetic Fenton-like-photochemical catalyst, in neutral, realizes Fe under the condition of radiation of visible light 3+with Fe 2+rapid translating, increase Fe 2+catalysis H 2o 2generate the speed of HO, and still have higher catalytic activity after repeatedly recycling.
Concrete technical scheme is as follows:
A kind of heterogeneous magnetic Fenton-like-photochemical catalyst, for having the core-shell microsphere Fe of three-decker 3o 4siO 2tiO 2; Wherein, with Fe 3o 4microballoon is kernel, and outermost layer is by TiO 2the TiO of nano particle composition 2layer, described kernel and described TiO 2siO is passed through between layer 2layer is as isolation transition zone;
Described Fe 3o 4microballoon is by the Fe of 15 ~ 30nm 3o 4nanometer granule is piled up and is formed, and microspherulite diameter is 300 ~ 400nm;
Described SiO 2the thickness of layer is 50 ~ 150nm.
Described TiO 2the particle diameter of nano particle is about 3 ~ 25nm, described TiO 2the thickness of layer is 100 ~ 300nm.
The preparation method of described heterogeneous magnetic Fenton-like-photochemical catalyst, comprises the steps:
(1) hydro-thermal method prepares Fe 3o 4microballoon
By FeCl 3: trisodium citrate: sodium acetate is that 1:0.1 ~ 0.4:1 ~ 3 join in ethylene glycol successively with mass ratio, and after stirring, transfer in water heating kettle, hydro-thermal reaction 8 ~ 12h, is cooled to room temperature at 200 ~ 250 DEG C, centrifugation, product Fe 3o 4after microballoon absolute ethyl alcohol and ultra-pure water wash 3 times respectively, drying for standby;
(2) Fe 3o 4siO 2the preparation of microballoon
By the 0.3 ~ 0.7gFe obtained in step 1 3o 4microballoon ultrasonic disperse in the absolute ethyl alcohol of 100 ~ 300mL, then adds the ammoniacal liquor NH of 1.5 ~ 25mL successively 3h 2the ethyl orthosilicate TEOS of O, 1.0 ~ 10mL, stirring reaction 0.5 ~ 6h at 20 ~ 80 DEG C, centrifugation, the product Fe obtained 3o 4siO 2microballoon, after washing 3 times respectively with ethanol and ultra-pure water, drying for standby;
(3) Fe 3o 4siO 2tiO 2the preparation of nano particle
Get the Fe of preparation in 20 ~ 60mg step 2 3o 4siO 2microballoon, ultrasonic disperse at the isopropanol water solution of 25 ~ 50mL, isopropyl alcohol: the volume ratio of water is 40 ~ 80:1; To add after the TBOT of 30 ~ 200 μ L ultrasonic 30 ~ 50min under room temperature again, question response system mixes; Then, mixed solution is proceeded in water heating kettle, at 180 ~ 200 DEG C, react 8 ~ 10h, be cooled to room temperature, centrifugation, obtain described core-shell microsphere Fe 3o 4siO 2tiO 2, after washing 3 times respectively with ethanol and ultra-pure water, drying for standby.
Preferably, described FeCl 3: trisodium citrate: the mass ratio of sodium acetate is 1:0.2:2.
The application of the Fenton-like-photochemical catalyst of above-mentioned heterogeneous magnetic, using aqueous solution of methylene blue as simulated wastewater, the concentration of methylene blue is 10mg/mL; In 100mL simulated wastewater, add heterogeneous magnetic Fenton-like-photochemical catalyst described in 0.05 ~ 2g, then add hydrogen peroxide;
The concentration ratio of hydrogen peroxide and methylene blue is 2 ~ 100:1, the visible light source of degraded light source used to be wavelength be 400 ~ 800nm;
After wastewater treatment completes, utilize Fe 3o 4siO 2tiO 2the superparamagnetism of microballoon, carries out separation and recovery with magnet by catalyst, reuses.
Tool of the present invention has the following advantages: the core of (1) catalyst is by Fe 3o 4the Fe of the submicron order that nanometer granule is piled up 3o 4microballoon forms, and has good superparamagnetism, magnetic response function admirable, under the effect of external magnetic field, can reach thorough separation in 30s.Therefore, catalyst is easy to reclaim, and can reuse, environmental friendliness;
(2) with SiO 2layer is as kernel Fe 3o 4with outermost layer TiO 2isolation transition zone between nanometer granule, not only due to SiO 2the good hydrophily had, overcomes the hydrophobic shortcoming that material with carbon element etc. brings as transition zone, and SiO 2technology of preparing relative maturity, can realize isolating the thickness of transition zone controlled;
(3) Fe 3o 4siO 2tiO 2in complex microsphere, regulate the SiO of isolation transition zone 2thickness, not only can realize the rapid transition of electronics, kernel Fe can also be substantially avoid 3o 4reunion, promote TiO simultaneously 2photocatalysis performance;
(4) prepare and obtain Fe 3o 4siO 2tiO 2complex microsphere, SiO 2tiO 2clad enhances the absorption property of system, simultaneously due to TiO 2photocatalysis, can catalyzing hydrogen peroxide degradable organic pollutant under visible light, form reaction path by all kinds of means, thus obtain high catalytic activity;
(5) SiO 2tiO 2coated, greatly reduce Fe 3o 4microsphere surface energy, Fe 3o 4siO 2tiO 2complex microsphere monodispersity is good, can keep the high activity of catalyst in wastewater treatment, increase operation rate.
Accompanying drawing explanation
Fig. 1 is the Fe that embodiment 1 prepares 3o 4siO 2the SEM photo of microballoon;
Fig. 2 is the Fe that embodiment 1 prepares 3o 4siO 2tiO 2the photo of the SEM of microballoon;
Fig. 3 is with the Fe prepared in embodiment 2 3o 4siO 2tiO 2the cycle down solution curve figure that complex microsphere obtains as catalyst degradation MB.
Detailed description of the invention
Below in conjunction with accompanying drawing, specific embodiments of the present invention are further described in detail, but should not limit the scope of the invention with this.
Embodiment 1
(1) Fe 3o 4the preparation of microballoon: by 1.3gFeCl 3, 0.5g trisodium citrate, 2.0g sodium acetate joins in the ethylene glycol of 40mL successively, after stirring, is transferred to by mixed solution in the water heating kettle of 100mL, at 200 DEG C after hydro-thermal reaction 10h, is cooled to room temperature, centrifugal, the Fe obtained 3o 4microballoon absolute ethyl alcohol and ultra-pure water wash 3 times respectively, drying for standby;
(2) Fe 3o 4siO 2the preparation of microballoon: get the above-mentioned Fe prepared of 0.4g 3o 4microballoon, ultrasonic disperse, in the absolute ethyl alcohol of 150mL, adds the ammoniacal liquor of 1mL successively in mixed solution, after the ethyl orthosilicate (TEOS) of 5mL, reacts 2h, be cooled to room temperature under room temperature, centrifugal, by the Fe prepared 3o 4siO 2microballoon ethanol and ultra-pure water wash 3 times respectively, drying for standby.The SEM photo of product as shown in Figure 1.
(3) Fe 3o 4siO 2tiO 2the preparation of complex microsphere: prepare Fe by above-mentioned for 30mg 3o 4siO 2microballoon, join in 25mL isopropyl alcohol, after adding 100uL butyl titanate (TBOT) again, ultrasonic 30min under room temperature, then dropwise adds 1mL ultra-pure water in mixed solution, stir 30min, mixed solution is proceeded in 50mL water heating kettle, at 180 DEG C, react 8h, be cooled to room temperature, centrifugal, the Fe obtained 3o 4siO 2tiO 2complex microsphere ethanol and ultra-pure water wash 3 times respectively, drying for standby.The Fe obtained 3o 4siO 2complex microsphere particle diameter is about 580nm, and monodispersity is good.Due to the Fe of kernel 3o 4, its particle diameter is about 460nm, therefore, and the SiO of isolation transition zone 2thickness is about 80nm.The Fe obtained 3o 4siO 2tiO 2the particle diameter of complex microsphere is about 780nm, therefore, and outermost TiO 2the thickness of layer is about 200nm.The SEM photo of product as shown in Figure 2.
(4) light is adopted to help-the dye wastewater of multiphase-fenton Fenton method process MB: with the round-bottomed flask of 50mL for reactor, adopt Xe lamp as light source, with optical filter, the light below 400nm wavelength is filtered, the initial concentration of MB dye wastewater is 10mg/L, adds the Fe of 1.5g/L in waste water 3o 4siO 2tiO 2complex microsphere, as catalyst, after stirring 0.5h, adds the H of 0.176mol/L in system 2o 2, carry out in process in reaction, take out a certain amount of reactant liquor in different preset times in section, centrifugal or with magnet, catalyst is separated completely, supernatant liquor is carried out UV detect to determine the change in concentration of MB.
Result shows, with Fe 3o 4siO 2tiO 2complex microsphere is fine as the effect of the heterogeneous Fenton-photocatalytic method process MB dye wastewater of catalyst, and after reaction 2h, the clearance of MB reaches more than 93%.
(5) by the catalyst Fe in step 4 3o 4siO 2tiO 2complex microsphere attraction is separated completely, with second alcohol and water by Fe 3o 4siO 2tiO 2complex microsphere catalyst detergent is for several times, dry, then repeats the experimental implementation in step 4.
Result shows, the Fe that secondary uses 3o 4siO 2tiO 2complex microsphere catalyst microspheres still keeps good catalytic effect, and after reaction 2h, the clearance of MB reaches more than 93%.
(6) experimental implementation in repetition step 58 times.With Fe 3o 4siO 2tiO 2complex microsphere is as catalyst, and after reusing 8 times, process MB dye wastewater 2h, the clearance of MB still remains on about 90%.
Embodiment 2
" ethyl orthosilicate (TEOS) of 5mL " in embodiment 1 step (2) is adjusted to " ethyl orthosilicate (TEOS) of 3mL " in embodiment 1 in step (2), and other conditions are all identical.Reduce the amount in silicon source, make Fe 3o 4siO 2tiO 2as the SiO of isolation transition zone in complex microsphere 2layer thickness reduces, and is about 60nm.Process MB dye wastewater 2h, the clearance of MB is about 90%, and result as shown in Figure 3.Visible, the SiO of isolation transition zone 2the thickness of layer should not be too low.Otherwise Fe 3o 4with TiO 2interlayer disturbs mutually, can reduce Fe on the contrary 3o 4siO 2tiO 2the catalytic activity of complex microsphere.
Embodiment 3
" adding 100uL butyl titanate (TBOT) more afterwards " in embodiment 1 step (3) is adjusted to " the adding 50uL butyl titanate (TBOT) more afterwards " in embodiment 1 in step (3), and other conditions are all identical.Reduce the amount in titanium source, make Fe 3o 4siO 2tiO 2tiO in complex microsphere 2layer thickness reduces, and is about 60nm.Process MB dye wastewater 2h, the clearance of MB is about 68%.Visible, due to TiO 2have high photocatalytic activity, it is at Fe 3o 4siO 2tiO 2content in complex microsphere should not too low (TiO 2layer thickness is greater than 120nm).
Comparative example
Repeat embodiment 1 step (4), by " the Fe in embodiment 1 step (4) 3o 4rGOTiO 2catalyst microspheres " be adjusted to " Fe in step 1 in embodiment 1 3o 4microballoon ", other conditions are all identical.
After reaction 2h, the clearance of MB only has 47.2%.
The foregoing is only preferred embodiment of the present invention, be not used for limiting practical range of the present invention.Have in any art and usually know the knowledgeable, without departing from the spirit and scope of the present invention, when doing various changes and retouching, therefore protection scope of the present invention is when being as the criterion depending on claims institute confining spectrum.

Claims (4)

1. heterogeneous magnetic Fenton-like-photochemical catalyst, is characterized in that, described heterogeneous magnetic Fenton-like-photochemical catalyst is the core-shell microsphere Fe with three-decker 3o 4siO 2tiO 2; Wherein, with Fe 3o 4microballoon is kernel, and outermost layer is by TiO 2the TiO of nano particle composition 2layer, described kernel and described TiO 2siO is passed through between layer 2layer is as isolation transition zone;
Described Fe 3o 4microballoon is by the Fe of 15 ~ 30nm 3o 4nanometer granule is piled up and is formed, and microspherulite diameter is 300 ~ 400nm;
Described SiO 2the thickness of layer is 50 ~ 150nm.
Described TiO 2the particle diameter of nano particle is about 3 ~ 25nm, described TiO 2the thickness of layer is 100 ~ 300.
2. the preparation method of heterogeneous magnetic Fenton-like-photochemical catalyst described in claim 1, it is characterized in that, described preparation method comprises the steps:
(1) hydro-thermal method prepares Fe 3o 4microballoon
By FeCl 3: trisodium citrate: sodium acetate is that 1:0.1 ~ 0.4:1 ~ 3 join in ethylene glycol successively with mass ratio, and after stirring, transfer in water heating kettle, hydro-thermal reaction 8 ~ 12h, is cooled to room temperature at 200 ~ 250 DEG C, centrifugation, product Fe 3o 4after microballoon absolute ethyl alcohol and ultra-pure water wash 3 times respectively, drying for standby;
(2) Fe 3o 4siO 2the preparation of microballoon
By the 0.3 ~ 0.7gFe obtained in step 1 3o 4microballoon ultrasonic disperse in the absolute ethyl alcohol of 100 ~ 300mL, then adds the ammoniacal liquor of 1.5 ~ 25mL, the ethyl orthosilicate of 1.0 ~ 10mL successively, stirring reaction 0.5 ~ 6h at 20 ~ 80 DEG C, centrifugation, the product Fe obtained 3o 4siO 2microballoon, after washing 3 times respectively with ethanol and ultra-pure water, drying for standby;
(3) Fe 3o 4siO 2tiO 2the preparation of nano particle
Get the Fe of preparation in 20 ~ 60mg step 2 3o 4siO 2microballoon, ultrasonic disperse at the isopropanol water solution of 25 ~ 50mL, isopropyl alcohol: the volume ratio of water is 40 ~ 80:1; To add after the TBOT of 30 ~ 200 μ L ultrasonic 30 ~ 50min under room temperature again, question response system mixes; Then, mixed solution is proceeded in water heating kettle, at 180 ~ 200 DEG C, react 8 ~ 10h, be cooled to room temperature, centrifugation, obtain described core-shell microsphere Fe 3o 4siO 2tiO 2, after washing 3 times respectively with ethanol and ultra-pure water, drying for standby.
3. preparation method according to claim 2, is characterized in that, described FeCl 3: trisodium citrate: the mass ratio of sodium acetate is 1:0.2:2.
4. the application of the Fenton-like-photochemical catalyst of the heterogeneous magnetic of claim 1, is characterized in that, using aqueous solution of methylene blue as simulated wastewater, the concentration of methylene blue is 10mg/mL; In 100mL simulated wastewater, add heterogeneous magnetic Fenton-like-photochemical catalyst described in 0.05 ~ 2g, then add hydrogen peroxide;
The concentration ratio of hydrogen peroxide and methylene blue is 2 ~ 100:1, the visible light source of degraded light source used to be wavelength be 400 ~ 800nm;
After wastewater treatment completes, utilize Fe 3o 4siO 2tiO 2the superparamagnetism of microballoon, carries out separation and recovery with magnet by catalyst, reuses.
CN201510469566.3A 2015-08-04 2015-08-04 Multiphase magnetic Fenton-photocatalyst and preparation method thereof and application Pending CN105032423A (en)

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