CN100406117C - Magnetic photocatalyst and its preparing method - Google Patents

Magnetic photocatalyst and its preparing method Download PDF

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CN100406117C
CN100406117C CNB2006101247399A CN200610124739A CN100406117C CN 100406117 C CN100406117 C CN 100406117C CN B2006101247399 A CNB2006101247399 A CN B2006101247399A CN 200610124739 A CN200610124739 A CN 200610124739A CN 100406117 C CN100406117 C CN 100406117C
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CN1935358A (en
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刘红
刘潘
张惠灵
任大军
孙旋
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Wuhan University of Science and Engineering WUSE
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Abstract

The present invention relates to a composite photocatalyst which can utilize sunlight and has good magnetic separating property and its preparation method. Said preparation method includes the following several steps: firstly, utilizing hydrothermal method to synthesize NiFeO4 nano granules, then utilizing homogeneous precipitation method to directly cover NiFeO4 magnetic nuclear surface by using TiO2 so as to form TiO2 external shell. Said composite photocatalyst can be used for making water supply treatment and waste water treatment.

Description

A kind of magnetic photocatalyst and preparation method thereof
Technical field
The invention belongs to the preparing technical field of nano-photocatalyst.Relate in particular to and a kind ofly can utilize daylight and composite photo-catalyst capable of magnetic separating and preparation method thereof.
Background technology
Photocatalysis technology has huge application potential at aspects such as degraded water body or airborne organic pollutions, has tangible advantage than technology such as electro-catalysis, catalytic wet oxidations aspect the mineralising decomposition of difficult degradation toxic organic compound.But photocatalysis technology is being given not yet industrialization in water treatment and the wastewater treatment, and Main Problems is to utilize sunshine and suspension system photocatalyst powder can not separate well recovery on engineering is used.Photochemical catalyst is fixed on the separation that can solve photochemical catalyst on the materials such as glass, pottery and reclaims problem, but greatly reduced the specific area of catalyst like this, cause photocatalysis efficiency to be starkly lower than suspension system.
Nano spinel NiFe 2O 4A kind of super paramagnetic material, TiO 2Be coated on NiFe 2O 4The outside can solve TiO well 2The problem that catalysis material reclaims is namely with the stronger permanent magnet adsorbing TiO of magnetic 2/ NiFe 2O 4Catalysis material is realized separation and the recovery of photochemical catalyst.Simultaneously, the Fe of trace in the preparation process 3+, Ni 2+Infiltrate TiO by warm-up movement 2Shell can effectively reduce TiO 2Energy gap.From chemical standpoint, transition metal ions Fe 3+, Ni 2+Doping can in semiconductor lattice, introduce defective locations or change its degree of crystallinity, become light induced electron or the catching trap of photohole and prolong its life-span, strengthen semi-conductive photocatalysis, can also make semi-conductive absorbing wavelength range expansion to the visible region, help improving photo-quantum efficiency, improve the photocatalysis efficiency of material.TiO 2Coat NiFe 2O 4The magnetic nano photochemical catalyst composite will have good application prospect because its separability good in water treatment procedure, photocatalytic activity and the absorbing wavelength scope thereof higher than load system can extend to the visible region.
A kind of preparation method of composite photo-catalyst capable of magnetic separating (CN200510027324.5) technology, the method synthesizing magnetic carrier nickel ferrite based magnetic loaded nano particle by low-temperature catalyzed inversion of phases at first, then with the method coating nickel ferrite based magnetic loaded nano particle of the silica with photochemistry inertia and electrochemistry inertia, at last titanium dioxide nano-particle is loaded on the nickel ferrite based magnetic loaded nano particle of coated silica by liquid deposition; A kind of megnetic nano composite photocatalyst and preparation method thereof (CN200610011122.6), this magnetic photocatalyst comprises the magnetic spinel carrier, has the nano-oxide coating of photochemistry and electrochemistry inertia and has high photoactive semiconductor particle titanium dioxide, used magnetic core is the magnetic spinel ferrite with different magnetic performances with the preparation of lamellar precursor method, and used titanium dioxide precursor energy direct hydrolysis in 90～100 ℃ of aqueous solution generates the titanium dioxide of anatase.But they do not see at visible region that response is arranged by the magnetic composite of preparation, and preparation process complexity, cycle are longer.
Summary of the invention
The object of the present invention is to provide that a kind of preparation technology is simple, the cycle is short, have good magnetic separation property in water treatment procedure, than the higher photocatalytic activity of load system and absorbing wavelength scope thereof can extend to the visible region, bigger serface, be difficult to industrialized magnetic photocatalyst and preparation method thereof to solve photocatalysis technology giving in water treatment and the wastewater treatment.
For realizing above-mentioned task, the technical solution adopted in the present invention is: earlier with divalent nickel salt, trivalent iron salt and highly basic n (Ni in molar ratio 2+): n (Fe 3+): n (OH -)=1: 2～3: 8～9 are dissolved in the distilled water, solution are heated to 95～105 ℃ again, and insulation 1～1.5h leaves standstill, cools off the back filtering and washing 2～3 times, promptly gets the hydro-thermal reaction presoma.
Wherein: divalent nickel salt is one or more in nickel nitrate, nickelous sulfate, the nickel chloride; Trivalent iron salt is one or more in ferric nitrate, ferric sulfate, the iron chloride; Highly basic is one or more in potassium hydroxide, NaOH, the lithium hydroxide.
The hydro-thermal reaction presoma is added in the distilled water, making wherein, nickel concentration is 0.45～2.5mol/L, adding additive, to make its concentration be 0.3～2.0mol/L again, regulates pH value to 8.0～13.0 with alkali lye, in the rear immigration autoclave that stirs, compactedness is 60～90%, at 100～250 ℃ of Water Under thermal response 0.5～8h, suction filtration after the cooling is with distilled water washing 2～3 times, the gained filter residue is vacuum drying 2～5h under 70～100 ℃ of conditions, grinds namely to get NiFe 2O 4Nano particle.
Described additive is one or more in glacial acetic acid, sodium acetate, the potassium acetate.
With prepared NiFe 2O 4Nano particle adds in the dispersant solution, makes NiFe 2O 4Concentration be 0.005～0.05mol/L, ultrasonic dispersion 10～30min, add urea, the concentration of urea is 0.01～1.5mol/L, stirring rear is 1.0～6.0 with dilute sulfuric acid regulator solution pH value, add again titanium sulfate, make n (Ti)/n (Ni)=1～80, this mixed liquor is moved into container, under 50～100 ℃ condition, quick oscillation reaction 1～10h, synthetic product washs with distilled water, ethanol respectively after separating, dry 3～5h with heat treatment 0.5～2h of 150～500 ℃, namely gets TiO then under 90～110 ℃ of conditions 2/ NiFe 2O 4Magnetic photocatalyst.
Described dispersant solution is a kind of in lauryl sodium sulfate, dodecyl sodium sulfate, polyethylene glycol, the phosphate solution, and its concentration range is 0.01～2.5mol/L.
With prepared NiFe 2O 4Add in the dispersant solution, make NiFe 2O 4Concentration be 0.005～0.05mol/L, ultrasonic dispersion 10～30min, this mixed liquor is moved in the container, slowly drips ethyl orthosilicate and concentrated ammonia liquor, make n (Si)/n (Ni)=1～10, n (N)/n (Si)=4～10, be warming up to again 50～80 ℃, quick oscillation reaction 3～5h, synthetic product washs with distilled water, ethanol respectively after separating, dry 3～5h under 90～110 ℃ of conditions, with heat treatment 0.5～2h of 150～500 ℃, namely get SiO then 2/ NiFe 2O 4
With prepared SiO 2/ NiFe 2O 4Add in the dispersant solution, make SiO 2/ NiFe 2O 4Concentration be 0.005～0.05mol/L, ultrasonic dispersion 10～30min, add then urea, the concentration of urea is 0.01～1.5mol/L, transferring pH with dilute sulfuric acid after stirring is 1.0～6.0, add again titanium sulfate, make n (Ti)/n (Ni)=1～80, this mixed liquor is moved in the container, quick oscillation reaction 1～10h under 50～100 ℃ condition, synthetic product washs with distilled water, ethanol respectively after separating, dry 3～5h under 90～110 ℃ of conditions, then with heat treatment 0.5～2h of 150～500 ℃, get final product TiO 2/ SiO 2/ NiFe 2O 4Photochemical catalyst.
The present invention is earlier with the synthetic NiFe of hydro-thermal method 2O 4Nano particle utilizes sluggish precipitation at NiFe then 2O 4Magnetic nuclear surface directly coats or interpolation amorphous state SiO 2Coat amorphous TiO behind the intermediate layer 2Shell, heat treatment makes amorphous TiO through uniform temperature again 2Shell is transformed into the anatase phase with high light catalytic activity, simultaneously the Fe of trace 3+, Ni 2+Infiltrate TiO by warm-up movement 2Shell can effectively reduce TiO 2Energy gap, make the absorbing wavelength range expansion to the visible region.Because hydro-thermal method is a kind of new preparation method of nano material, can prepare purity height, good, the single dispersion of crystal formation, shape and the controlled nanoparticle of size, have bigger advantage than additive method, so adopt hydro-thermal method to prepare NiFe 2O 4Magnetic nuclear.The present invention adopts sluggish precipitation to prepare TiO 2Coat NiFe 2O 4Nano composite material is because OH -Homogeneous precipitation agent CO (NH 2) 2Slowly generate by chemical reaction, therefore can avoid density unevenness spare phenomenon, thereby the speed of growth of control clad obtains even, the fine and close composite of coating.Two kinds of Combination of Methods have the advantages that preparation technology is simple, the cycle is short.
The present invention adopts the nano-Ni/Fe of hydro-thermal method preparation 2O 4, complete crystallization, particle are cube shape basically, and the size scope is 1～50nm.Prepared TiO 2/ NiFe 2O 4Photochemical catalyst and TiO 2/ SiO 2/ NiFe 2O 4Photochemical catalyst is the compound particle of nanoscale, presents nucleocapsid structure, wherein NiFe 2O 4Majority is positioned at the center of composite particles, TiO 2Uniform Dispersion is coated on NiFe 2O 4The surface mainly exists with Anatase, and the particle size range of this composite photo-catalyst is 15～100nm, and specific area is 10～100m 2/ g.
Description of drawings
Fig. 1 is the prepared TiO of the present invention 2/ NiFe 2O 4Photochemical catalyst (b, c), TiO 2/ SiO 2/ NiFe 2O 4Photochemical catalyst (a) anatase TiO 2(d) UV-vis diffuse reflection spectrum;
Fig. 2 is the curve (a-TiO take the aqueous solution of methyl orange as the photocatalysis performance of the prepared photochemical catalyst of simulating pollution aqueous systems evaluation the present invention 2/ NiFe 2O 4, b-TiO 2/ SiO 2/ NiFe 2O 4).
The specific embodiment
Embodiment 1
(1) NiFe 2O 4The Hydrothermal Synthesis of nano particle
With NiSO 46H 2O, Fe 2(SO 4) 3XH 2O and KOH press n (Ni 2+): n (Fe 3+): n (OH -)=1: 2～2.5: 8～8.5 are dissolved in the distilled water, and solution is placed on constantly boiling 1～1.5h on the electric furnace.Leave standstill, cool off rear suction filtration, with distilled water washing 2～3 times, namely get the hydro-thermal reaction presoma.
The hydro-thermal reaction presoma is added in the distilled water, making wherein, nickel concentration is 1.0～2.5mol/L, adding acetic acid, to make its concentration be 1.0～2.0mol/L again, regulates pH value to 10.0～13.0 with alkali lye, in the rear immigration autoclave that stirs, compactedness is 60～90%, at 100～250 ℃ of Water Under thermal response 3～8h, suction filtration after the cooling is with distilled water washing 2～3 times, the gained filter residue is vacuum drying 3～5h under 70～100 ℃ of conditions, grinds namely to get NiFe 2O 4Nano particle.
Adopt transmission electron microscope to this NiFe 2O 4Magnetic nuclear characterizes, and finds NiFe 2O 4Particle is cube shape basically, and particle size range is for being 12～25nm.
(2) sluggish precipitation prepares TiO 2/ NiFe 2O 4Photochemical catalyst
With prepared NiFe 2O 4Nano particle adds in the sodium dodecyl sulfate solution of 0.1～1.0mol/L, makes NiFe 2O 4Concentration be 0.01～0.05mol/L, ultrasonic dispersion 10～30min, add urea, the concentration of urea is 1.0～1.5mol/L, stirring rear is 4.0～6.0 with dilute sulfuric acid regulator solution pH value, add again titanium sulfate, make n (Ti)/n (Ni)=5～40, again this mixed liquor is moved into container, under 85～100 ℃ condition, quick oscillation reaction 3～5h, synthetic product washs with distilled water, ethanol respectively after separating, dry 3～5h with heat treatment 1.5～2h of 150～300 ℃, namely gets TiO then under 90～110 ℃ of conditions 2/ NiFe 2O 4Magnetic photocatalyst.
Adopt X-ray diffractometer, transmission electron microscope, BET surface area tester and UV-Vis DRS spectrometer to this TiO 2/ NiFe 2O 4Photochemical catalyst characterizes, and finds TiO 2Uniform Dispersion is coated on NiFe 2O 4The surface mainly exists with Anatase, and the particle size range of this photochemical catalyst is 30～40nm, and specific area is 10.52m 2/ g all has obvious absorption in the 400-700nm visible-range.Fig. 1 is the prepared TiO of the present invention 2/ NiFe 2O 4Photochemical catalyst (b, c) anatase TiO 2(d) UV-vis diffuse reflection spectrum can be found out, anatase TiO 2Be 320～400nm to the Optical Absorption scope, mainly concentrate on ultraviolet region, the visible light that surpasses 400nm is not almost absorbed, but TiO 2/ NiFe 2O 4The absorption spectrum ranges of photochemical catalyst is compared anatase TiO 2Enlarged a lot, obvious absorption is all arranged in 400～700nm visible-range, this is very favourable to exploitation daylight catalyst.
(3) Preparation by Uniform Precipitation TiO 2/ SiO 2/ NiFe 2O 4Photochemical catalyst
With prepared NiFe 2O 4Add in the sodium dodecyl sulfate solution of 0.1～1.0mol/L, make NiFe 2O 4Concentration be 0.01～0.05mol/L, ultrasonic dispersion 10～30min, this mixed liquor is moved in the container, slowly drips ethyl orthosilicate and concentrated ammonia liquor, make n (Si)/n (Ni)=5～10, n (N)/n (Si)=8～10, be warming up to again 60～80 ℃, quick oscillation reaction 3～5h, synthetic product washs with distilled water, ethanol respectively after separating, dry 3～5h under 90～110 ℃ of conditions, with heat treatment 1.5～2h of 250～500 ℃, namely get SiO then 2/ NiFe 2O 4
With prepared SiO 2/ NiFe 2O 4Nano particle adds in the sodium dodecyl sulfate solution of 0.1～1.0mol/L, makes NiFe 2O 4Concentration be 0.02～0.05mol/L, ultrasonic dispersion 10～30min, add urea, the concentration of urea is 1.0～1.5mol/L, stirring rear is 3.0～6.0 with dilute sulfuric acid regulator solution pH value, add again titanium sulfate, make n (Ti)/n (Ni)=5～60, this mixed liquor is moved into container, under 50～100 ℃ condition, quick oscillation reaction 3～5h, synthetic product washs with distilled water, ethanol respectively after separating, dry 3～5h with heat treatment 0.5～2h of 150～300 ℃, namely gets TiO then under 90～110 ℃ of conditions 2/ SiO 2/ NiFe 2O 4Magnetic photocatalyst.
Adopt X-ray diffractometer, transmission electron microscope, BET surface area tester and UV-Vis DRS spectrometer to this TiO 2/ SiO 2/ NiFe 2O 4Photochemical catalyst characterizes, and finds TiO 2Uniform Dispersion is coated on SiO 2/ NiFe 2O 4The surface mainly exists with Anatase, intermediate layer SiO 2Be amorphous state, this photochemical catalyst is the double-coating structure, and particle size range is 50～70nm, and specific area is 12.14m 2/ g all has obvious absorption in the 400-700nm visible-range.Fig. 1 is the prepared TiO of the present invention 2/ SiO 2/ NiFe 2O 4Photochemical catalyst (a) anatase TiO 2(d) UV-vis diffuse reflection spectrum can be found out, anatase TiO 2Be 320～400nm to the Optical Absorption scope, mainly concentrate on ultraviolet region, the visible light that surpasses 400nm is not almost absorbed, but TiO 2/ SiO 2/ NiFe 2O 4The absorption spectrum ranges of photochemical catalyst is compared anatase TiO 2Enlarged a lot, obvious absorption is all arranged in 400～700nm visible-range, this is very favourable to exploitation daylight catalyst.
Embodiment 2
(1) NiFe 2O 4The Hydrothermal Synthesis of nano particle
With NiCl 2, FeCl 3Press n (Ni with NaOH 2+): n (Fe 3+): n (OH -)=1: 2.5～3: 8.5～9 are dissolved in the distilled water, and solution is placed on constantly boiling 1～1.5h on the electric furnace.Leave standstill, cool off rear suction filtration, with distilled water washing 2～3 times, namely get the hydro-thermal reaction presoma.
The hydro-thermal reaction presoma is added in the distilled water, making wherein, nickel concentration is 0.45～1.5mol/L, adding sodium acetate, to make its concentration be 0.3～1.0mol/L again, regulates pH value to 8.0～10.5 with alkali lye, in the rear immigration autoclave that stirs, compactedness is 75～90%, at 150～250 ℃ of Water Under thermal response 0.5～3.5h, suction filtration after the cooling is with distilled water washing 2～3 times, the gained filter residue is vacuum drying 3～5h under 70～100 ℃ of conditions, grinds namely to get NiFe 2O 4Nano particle.
Adopt transmission electron microscope to this NiFe 2O 4Magnetic nuclear characterizes, and finds NiFe 2O 4Particle is cube shape basically, and particle size range is for being 10～20nm.
(2) sluggish precipitation prepares TiO 2/ NiFe 2O 4Photochemical catalyst
With prepared NiFe 2O 4Nano particle adds in 0.5～1.0mol/L polyethylene glycol (molecular weight 4000) solution, makes NiFe 2O 4Concentration be 0.01～0.05mol/L, ultrasonic dispersion 10～30min, add urea, the concentration of urea is 0.02～0.5mol/L, stirring rear is 1.0～5.0 with dilute sulfuric acid regulator solution pH value, add again titanium sulfate, make n (Ti)/n (Ni)=10～80, again this mixed liquor is moved into container, under 55～85 ℃ condition, quick oscillation reaction 1～3h, synthetic product washs with distilled water, ethanol respectively after separating, dry 3～5h with heat treatment 1.5～2h of 200～500 ℃, namely gets TiO then under 90～110 ℃ of conditions 2/ NiFe 2O 4Magnetic photocatalyst.
Adopt X-ray diffractometer, transmission electron microscope, BET surface area tester and UV-Vis DRS spectrometer to this TiO 2/ NiFe 2O 4Photochemical catalyst characterizes, and finds TiO 2Uniform Dispersion is coated on NiFe 2O 4The surface mainly exists with Anatase, and the particle size range of this photochemical catalyst is 25～35nm, and specific area is 20.32m 2/ g all has obvious absorption in the 400-700nm visible-range.
(3) Preparation by Uniform Precipitation TiO 2/ SiO 2/ NiFe 2O 4Photochemical catalyst
With prepared NiFe 2O 4Add in the sodium dodecyl sulfate solution of 0.5～2.0mol/L, make NiFe 2O 4Concentration be 0.01～0.05mol/L, ultrasonic dispersion 10～30min, this mixed liquor is moved in the container, slowly drips ethyl orthosilicate and concentrated ammonia liquor, make n (Si)/n (Ni)=1～6, n (N)/n (Si)=4～7, be warming up to then 50～75 ℃, quick oscillation reaction 3～5h, synthetic product washs with distilled water, ethanol respectively after separating, dry 3～5h under 90～110 ℃ of conditions, with heat treatment 0.5～1.5h of 150～300 ℃, namely get SiO then 2/ NiFe 2O 4
With prepared SiO 2/ NiFe 2O 4Nano particle adds in the sodium dodecyl sulfate solution of 0.5～1.0mol/L, makes NiFe 2O 4Concentration be 0.005～0.03mol/L, ultrasonic dispersion 10～30min, add urea, the concentration of urea is 0.3～1.0mol/L, stirring rear is 1.0～5.0 with dilute sulfuric acid regulator solution pH value, add again titanium sulfate, make n (Ti)/n (Ni)=10～70, again this mixed liquor is moved into container, under 60～100 ℃ condition, quick oscillation reaction 3～5h, synthetic product washs with distilled water, ethanol respectively after separating, dry 3～5h with heat treatment 0.5～2h of 150～300 ℃, namely gets TiO then under 90～110 ℃ of conditions 2/ SiO 2/ NiFe 2O 4Magnetic photocatalyst.
Adopt X-ray diffractometer, transmission electron microscope, BET surface area tester and UV-Vis DRS spectrometer to this TiO 2/ SiO 2/ NiFe 2O 4Photochemical catalyst characterizes, and finds TiO 2Uniform Dispersion is coated on SiO 2/ NiFe 2O 4The surface mainly exists with Anatase, intermediate layer SiO 2Be amorphous state, this photochemical catalyst is the double-coating structure, and particle size range is 40～55nm, and specific area is 25.21m 2/ g all has obvious absorption in the 400-700nm visible-range.

Claims (8)

1. TiO 2/ NiFe 2O 4The preparation method of magnetic photocatalyst is characterized in that earlier divalent nickel salt, trivalent iron salt and highly basic n (Ni in molar ratio 2+): n (Fe 3+): n (OH -)=1: 2～3: 8～9 are dissolved in the distilled water, solution are heated to 95～105 ℃ again, and insulation 1～1.5h leaves standstill, cools off back suction filtration, washing 2～3 times, promptly gets the hydro-thermal reaction presoma;
The hydro-thermal reaction presoma is added in the distilled water, making wherein, nickel concentration is 0.45～2.5mol/L, adding additive, to make its concentration be 0.3～2.0mol/L again, regulates pH value to 8.0～13.0 with alkali lye, in the rear immigration autoclave that stirs, compactedness is 60～90%, at 100～250 ℃ of Water Under thermal response 0.5～8h, suction filtration after the cooling is with distilled water washing 2～3 times, the gained filter residue is vacuum drying 2～5h under 70～100 ℃ of conditions, grinds namely to get NiFe 2O 4Nano particle;
With prepared NiFe 2O 4Nano particle adds in the dispersant solution, makes NiFe 2O 4Concentration be 0.005～0.05mol/L, ultrasonic dispersion 10～30min, add urea, the concentration of urea is 0.01～1.5mol/L, stirring rear is 1.0～6.0 with dilute sulfuric acid regulator solution pH value, add again titanium sulfate, make n (Ti)/n (Ni)=1～80, this mixed liquor is moved into container, under 50～100 ℃ condition, quick oscillation reaction 1～10h, synthetic product washs with distilled water, ethanol respectively after separating, dry 3～5h with heat treatment 0.5～2h of 150～500 ℃, namely gets TiO then under 90～110 ℃ of conditions 2/ NiFe 2O 4Magnetic photocatalyst.
2. TiO 2/ SiO 2/ NiFe 2The preparation method of O magnetic photocatalyst is characterized in that earlier divalent nickel salt, trivalent iron salt and highly basic n (Ni in molar ratio 2+): n (Fe 3+): n (OH -)=1: 2～3: 8～9 are dissolved in the distilled water, solution are heated to 95～105 ℃ again, and insulation 1～1.5h leaves standstill, cools off back suction filtration, washing 2～3 times, promptly gets the hydro-thermal reaction presoma;
The hydro-thermal reaction presoma is added in the distilled water, making wherein, nickel concentration is 0.45～2.5mol/L, adding additive, to make its concentration be 0.3～2.0mol/L again, regulates pH value to 8.0～13.0 with alkali lye, in the rear immigration autoclave that stirs, compactedness is 60～90%, at 100～250 ℃ of Water Under thermal response 0.5～8h, suction filtration after the cooling is with distilled water washing 2～3 times, the gained filter residue is vacuum drying 2～5h under 70～100 ℃ of conditions, grinds namely to get NiFe 2O 4Nano particle;
With prepared NiFe 2O 4Add in the dispersant solution, make NiFe 2O 4Concentration be 0.005～0.05mol/L, ultrasonic dispersion 10～30min, this mixed liquor is moved in the container, slowly drips ethyl orthosilicate and concentrated ammonia liquor, make n (Si)/n (Ni)=1～10, n (N)/n (Si)=4～10, be warming up to again 50～80 ℃, quick oscillation reaction 3～5h, synthetic product washs with distilled water, ethanol respectively after separating, dry 3～5h under 90～110 ℃ of conditions, with heat treatment 0.5～2h of 150～500 ℃, namely get SiO then 2/ NiFe 2O 4
With prepared SiO 2/ NiFe 2O 4Add in the dispersant solution, make SiO 2/ NiFe 2O 4Concentration be 0.005～0.05mol/L, ultrasonic dispersion 10～30min, add urea, the concentration of urea is 0.01～1.5mol/L, stirring rear is 1.0～6.0 with dilute sulfuric acid regulator solution pH value, add again titanium sulfate, make n (Ti)/n (Ni)=1～80, this mixed liquor is moved in the container, quick oscillation reaction 1～10h under 50～100 ℃ condition, synthetic product washs with distilled water, ethanol respectively after separating, dry 3～5h under 90～110 ℃ of conditions, then with heat treatment 0.5～2h of 150～500 ℃, get final product TiO 2/ SiO 2/ NiFe 2O 4Magnetic photocatalyst.
3. according to the preparation method of each described magnetic photocatalyst in the claim 1,2, it is characterized in that described divalent nickel salt is one or more in nickel nitrate, nickelous sulfate, the nickel chloride.
4. according to the preparation method of each described magnetic photocatalyst in the claim 1,2, it is characterized in that described trivalent iron salt is one or more in ferric nitrate, ferric sulfate, the iron chloride.
5. according to the preparation method of each described magnetic photocatalyst in the claim 1,2, it is characterized in that described highly basic is one or more in potassium hydroxide, NaOH, the lithium hydroxide.
6. according to the preparation method of each described magnetic photocatalyst in the claim 1,2, it is characterized in that described additive is one or more in glacial acetic acid, sodium acetate, the potassium acetate.
7. according to the preparation method of each described magnetic photocatalyst in the claim 1,2, it is characterized in that described dispersant solution is a kind of solution in lauryl sodium sulfate, dodecyl sodium sulfate, polyethylene glycol, the phosphate, its concentration range is 0.01～2.5mol/L.
8. according to the prepared magnetic photocatalyst of preparation method of each described magnetic photocatalyst in the claim 1～7.
CNB2006101247399A 2006-10-12 2006-10-12 Magnetic photocatalyst and its preparing method Expired - Fee Related CN100406117C (en)

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