CN106492816A - A kind of magnetic photocatalytic nano composite material and preparation method thereof - Google Patents
A kind of magnetic photocatalytic nano composite material and preparation method thereof Download PDFInfo
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- CN106492816A CN106492816A CN201611037393.9A CN201611037393A CN106492816A CN 106492816 A CN106492816 A CN 106492816A CN 201611037393 A CN201611037393 A CN 201611037393A CN 106492816 A CN106492816 A CN 106492816A
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- nickel ferrite
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- 239000000463 material Substances 0.000 title claims abstract description 42
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 41
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 60
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229940056319 ferrosoferric oxide Drugs 0.000 claims abstract description 30
- 229910000416 bismuth oxide Inorganic materials 0.000 claims abstract description 27
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052709 silver Inorganic materials 0.000 claims abstract description 19
- 239000004332 silver Substances 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 17
- 230000003647 oxidation Effects 0.000 claims abstract description 4
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- 239000008367 deionised water Substances 0.000 claims description 32
- 229910021641 deionized water Inorganic materials 0.000 claims description 32
- 239000000243 solution Substances 0.000 claims description 30
- 238000001035 drying Methods 0.000 claims description 25
- 239000002105 nanoparticle Substances 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 15
- 235000019441 ethanol Nutrition 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 12
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 10
- 239000012670 alkaline solution Substances 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 10
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000010936 titanium Substances 0.000 claims description 10
- 229910052719 titanium Inorganic materials 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 239000003638 chemical reducing agent Substances 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 8
- 239000003381 stabilizer Substances 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 5
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 5
- 235000011152 sodium sulphate Nutrition 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 239000004094 surface-active agent Substances 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 4
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 3
- 239000001632 sodium acetate Substances 0.000 claims description 3
- 235000017281 sodium acetate Nutrition 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical group O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 239000002131 composite material Substances 0.000 abstract description 4
- 229910052797 bismuth Inorganic materials 0.000 abstract description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 abstract description 2
- 230000008878 coupling Effects 0.000 abstract description 2
- 238000010168 coupling process Methods 0.000 abstract description 2
- 238000005859 coupling reaction Methods 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 23
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 16
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 239000004408 titanium dioxide Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/843—Arsenic, antimony or bismuth
- B01J23/8437—Bismuth
-
- B01J35/33—
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Abstract
The invention discloses a kind of magnetic photocatalytic nano composite material and preparation method thereof, magnetic photocatalytic nano composite material, which is mainly made up of bismuth oxide, nickel ferrite based magnetic loaded and ferroso-ferric oxide, the bismuth oxide is nanometer powder shape, nickel ferrite based magnetic loaded is nanometer powder shape, and ferroso-ferric oxide is nanometer powder shape, and the magnetic photocatalytic nano composite material for preparing of the invention can be reclaimed under externally-applied magnetic field, recycling for catalyst is achieved, cost is reduced；Due to the presence of silver, optic catalytic composite material achieves the catalytic degradation under excited by visible light to organic pollution, the range of application of optic catalytic composite material is expanded, simultaneous oxidation bismuth and nickel ferrite based magnetic loaded combine to form hetero-junctions, by light-use Extending to visible region, the band structure of coupling is conducive to the separation in light induced electron and hole, and then improves the efficiency of photocatalytic degradation.
Description
Technical field
The present invention relates to magnetic photocatalytic nano composite material, specifically a kind of magnetic photocatalytic nano composite material and its
Preparation method.
Background technology
Semiconductor-based photochemical catalyst is widely used in environmental area because having many excellent property.Due to
Titanium dioxide have nontoxic, chemically stable and cheap the characteristics of, it is considered to be a kind of preferable photocatalytic semiconductor material, be subject to
Researcher's extensive concern.But, titanium dioxide energy gap larger (~ 3.2eV) only shows photocatalytic activity in ultraviolet band, this
Seriously limit which to apply.Realize optically catalytic TiO 2 under excited by visible light thus become a study hotspot.Including with expensive
Metallic（Such as silver, gold, platinum）The method such as compound is proposed in succession.Wherein, silver is a kind of preferable noble metal.Due to silver nanoparticle
The strong surface plasma body resonant vibration effect that particle has, makes titanium dioxide show photocatalysis work under excited by visible light
Property.
Content of the invention
It is an object of the invention to provide a kind of magnetic photocatalytic nano composite material and preparation method thereof.
For achieving the above object, the present invention provides following technical scheme：
A kind of magnetic photocatalytic nano composite material, which is mainly made up of bismuth oxide, nickel ferrite based magnetic loaded and ferroso-ferric oxide, the oxygen
Change bismuth is nanometer powder shape, and nickel ferrite based magnetic loaded is nanometer powder shape, and ferroso-ferric oxide is nanometer powder shape, and the amount ratio of three's material is 1:
0.2～2：0.1～1.
A kind of preparation method of magnetic photocatalytic nano composite material, which specifically includes following steps:
1) prepared by ferroso-ferric oxide, by molysite with stabilizer and reducing agent according to mass ratio 1:0.2～0.9:1～3 is added to alcohol
In class solvent, the solution that iron concentration is 0.04～0.2M after being completely dissolved, is obtained；Resulting solution is transferred to reaction under high pressure
In kettle, after reacting 8～10 hours at a temperature of 180～220 °C, black product is obtained, the black product is spent respectively
Ionized water and absolute ethyl alcohol are fully washed, and after drying, finally give ferriferrous oxide nano-particle；
2) nickel ferrite based magnetic loaded is prepared, in proportion nickel nitrate and ferric nitrate are substantially dissolved in deionized water, pH is adjusted with alkaline solution a
To 13～14, mixed solution A is obtained；Mixed liquor A is transferred in the stainless steel cauldron of polytetrafluoroethylliner liner, hydro-thermal is carried out
Reaction, after reaction terminates, is cooled to room temperature, deionized water and ethanol washing, obtains nickel ferrite based magnetic loaded powder after drying；
3) bismuth nitrate, sodium sulphate and nickel ferrite based magnetic loaded are dissolved in deionized water by ferroso-ferric oxide, the mixing of nickel ferrite based magnetic loaded bismuth oxide in proportion
In, solution B is obtained, alkaline solution b is mixed to get solution C with solution B；Solution C is transferred to microwave reactor to be reacted,
After reaction terminates, room temperature, deionized water and ethanol washing is cooled to, after drying, visible magnetic photocatalytic material is obtained；
4) by the magnetic photocatalytic material obtained in step 3 and silver nitrate and surfactant according to mass ratio 1:0.1～
0.5:10～15 are added in ethylene glycol, obtain the dispersion that magnetic photocatalytic material nano-particle mass fraction is 0.2～1.5%
Dispersion liquid is warming up to 100～120 °C by liquid, stirring reaction 8～12 hours, collects and obtain product after the completion of question response is abundant, will
Products therefrom is fully washed with absolute ethyl alcohol and deionized water respectively, after drying, you can obtain nickel ferrite based magnetic loaded/bismuth oxide/tetra- oxygen
Change three-iron/silver nanoparticle compound particle；
5) nickel ferrite based magnetic loaded/bismuth oxide/ferroso-ferric oxide/silver nanoparticle compound particle described in step 4 is pressed with absolute ethyl alcohol and ammoniacal liquor
Mass ratio 1：800～1000：4～5 are sufficiently mixed, and are subsequently adding titanium source, titanium source and nickel ferrite based magnetic loaded/bismuth oxide/ferroso-ferric oxide/silver
The mass ratio of nano-complex particle is 1～2:1, stir 12～24 hours at a temperature of 40～50 °C, question response is fully completed
Collect afterwards and obtain product, products therefrom is fully cleaned with absolute ethyl alcohol and deionized water respectively, after drying, 400～
Calcine 2～3 hours in air atmosphere at a temperature of 600 °C, that is, obtain magnetic photocatalytic nano composite material.
As further scheme of the invention：The stabilizer is sodium citrate, and reducing agent is sodium acetate.
Compared with prior art, the invention has the beneficial effects as follows：Magnetic photocatalytic nano composite material prepared by the present invention
Can be reclaimed under externally-applied magnetic field, it is achieved that recycling for catalyst, be reduced cost；Due to the presence of silver, light is urged
Change composite achieves the catalytic degradation under excited by visible light to organic pollution, has expanded the application of optic catalytic composite material
Scope, simultaneous oxidation bismuth and nickel ferrite based magnetic loaded combine to form hetero-junctions, by light-use Extending to visible region, the energy band of coupling
Structure is conducive to the separation in light induced electron and hole, and then improves the efficiency of photocatalytic degradation.
Specific embodiment
Below the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described enforcement
Example is only a part of embodiment of the invention, rather than whole embodiment.Embodiment in based on the present invention, this area are common
The every other embodiment obtained under the premise of creative work is not made by technical staff, belongs to the model of present invention protection
Enclose.
A kind of magnetic photocatalytic nano composite material, which is mainly made up of bismuth oxide, nickel ferrite based magnetic loaded and ferroso-ferric oxide, institute
Bismuth oxide is stated for nanometer powder shape, nickel ferrite based magnetic loaded is nanometer powder shape, ferroso-ferric oxide is nanometer powder shape, the amount ratio of three's material
It is 1:0.2～2：0.1～1.
During the present invention implements 1, a kind of preparation method of magnetic photocatalytic nano composite material, which specifically includes following step
Suddenly：
1）Prepared by ferroso-ferric oxide, by molysite with stabilizer and reducing agent according to mass ratio 1:0.2:1 is added in alcohols solvent,
Solution of the iron concentration for 0.04M is obtained after being completely dissolved；Resulting solution is transferred in autoclave, at 180 °C
At a temperature of reaction 8 hours after, obtain black product, by the black product, deionized water and absolute ethyl alcohol are fully washed respectively
Wash, after drying, finally give ferriferrous oxide nano-particle；
2）Nickel ferrite based magnetic loaded is prepared, in proportion nickel nitrate and ferric nitrate are substantially dissolved in deionized water, pH is adjusted with alkaline solution a
To 13, mixed solution A is obtained；Mixed liquor A is transferred in the stainless steel cauldron of polytetrafluoroethylliner liner, hydro-thermal is carried out anti-
Should, after reaction terminates, room temperature, deionized water and ethanol washing is cooled to, after drying, nickel ferrite based magnetic loaded powder is obtained；
3）Bismuth nitrate, sodium sulphate and nickel ferrite based magnetic loaded are dissolved in deionized water by ferroso-ferric oxide, the mixing of nickel ferrite based magnetic loaded bismuth oxide in proportion
In, solution B is obtained, alkaline solution b is mixed to get solution C with solution B；Solution C is transferred to microwave reactor to be reacted,
After reaction terminates, room temperature, deionized water and ethanol washing is cooled to, after drying, visible magnetic photocatalytic material is obtained；
4）By the magnetic photocatalytic material obtained in step 3 and silver nitrate and surfactant according to mass ratio 1:0.1:10 add
Enter in ethylene glycol, obtain the dispersion liquid that magnetic photocatalytic material nano-particle mass fraction is 0.2%, dispersion liquid is warming up to
100 °C, stirring reaction 8 hours is collected after the completion of question response is abundant and obtains product, products therefrom with absolute ethyl alcohol and is gone respectively
Ionized water is fully washed, after drying, you can obtain nickel ferrite based magnetic loaded/bismuth oxide/ferroso-ferric oxide/silver nanoparticle compound particle；
5）Nickel ferrite based magnetic loaded/bismuth oxide/ferroso-ferric oxide/silver nanoparticle compound particle described in step 4 is pressed with absolute ethyl alcohol and ammoniacal liquor
Mass ratio 1：800：4 are sufficiently mixed, and are subsequently adding titanium source, and titanium source is combined with nickel ferrite based magnetic loaded/bismuth oxide/ferroso-ferric oxide/silver nanoparticle
The mass ratio of particle is 1:1, stir 12 hours at a temperature of 40 °C, collect after the completion of question response is abundant and obtain product, by institute
Obtain product fully to be cleaned with absolute ethyl alcohol and deionized water respectively, after drying, calcine in air atmosphere at a temperature of 400 °C
2 hours, that is, obtain magnetic photocatalytic nano composite material.
During the present invention implements 2, a kind of preparation method of magnetic photocatalytic nano composite material, which specifically includes following step
Suddenly：
1）Prepared by ferroso-ferric oxide, by molysite with stabilizer and reducing agent according to mass ratio 1:0.55:2 are added to alcohols solvent
In, solution of the iron concentration for 0.12M is obtained after being completely dissolved；Resulting solution is transferred in autoclave, at 200 °C
At a temperature of reaction 9 hours after, obtain black product, by the black product, deionized water and absolute ethyl alcohol are fully washed respectively
Wash, after drying, finally give ferriferrous oxide nano-particle；
2）Nickel ferrite based magnetic loaded is prepared, in proportion nickel nitrate and ferric nitrate are substantially dissolved in deionized water, pH is adjusted with alkaline solution a
To 13.5, mixed solution A is obtained；Mixed liquor A is transferred in the stainless steel cauldron of polytetrafluoroethylliner liner, hydro-thermal is carried out anti-
Should, after reaction terminates, room temperature, deionized water and ethanol washing is cooled to, after drying, nickel ferrite based magnetic loaded powder is obtained；
3）Bismuth nitrate, sodium sulphate and nickel ferrite based magnetic loaded are dissolved in deionized water by ferroso-ferric oxide, the mixing of nickel ferrite based magnetic loaded bismuth oxide in proportion
In, solution B is obtained, alkaline solution b is mixed to get solution C with solution B；Solution C is transferred to microwave reactor to be reacted,
After reaction terminates, room temperature, deionized water and ethanol washing is cooled to, after drying, visible magnetic photocatalytic material is obtained；
4）By the magnetic photocatalytic material obtained in step 3 and silver nitrate and surfactant according to mass ratio 1:0.3:12.5
It is added in ethylene glycol, obtains the dispersion liquid that magnetic photocatalytic material nano-particle mass fraction is 0.85%, dispersion liquid is heated up
To 110 °C, stirring reaction 10 hours is collected after the completion of question response is abundant and obtains product, products therefrom is used absolute ethyl alcohol respectively
Fully wash with deionized water, after drying, you can obtain nickel ferrite based magnetic loaded/bismuth oxide/ferroso-ferric oxide/silver nanoparticle compound particle；
5）Nickel ferrite based magnetic loaded/bismuth oxide/ferroso-ferric oxide/silver nanoparticle compound particle described in step 4 is pressed with absolute ethyl alcohol and ammoniacal liquor
Mass ratio 1：900：4.5 are sufficiently mixed, and are subsequently adding titanium source, and titanium source is multiple with nickel ferrite based magnetic loaded/bismuth oxide/ferroso-ferric oxide/silver nanoparticle
The mass ratio for closing particle is 1.5:1, stir 18 hours at a temperature of 45 °C, collect after the completion of question response is abundant and obtain product,
Products therefrom is fully cleaned with absolute ethyl alcohol and deionized water respectively, after drying, in air atmosphere at a temperature of 500 °C
Calcining 2.5 hours, that is, obtain magnetic photocatalytic nano composite material.
During the present invention implements 3, a kind of preparation method of magnetic photocatalytic nano composite material, which specifically includes following step
Suddenly：
1）Prepared by ferroso-ferric oxide, by molysite with stabilizer and reducing agent according to mass ratio 1:0.9:3 are added in alcohols solvent,
Solution of the iron concentration for 0.2M is obtained after being completely dissolved；Resulting solution is transferred in autoclave, in 220 °C of temperature
After the lower reaction of degree 10 hours, black product is obtained, the black product is distinguished deionized water and absolute ethyl alcohol is fully washed,
After drying, ferriferrous oxide nano-particle is finally given；
2）Nickel ferrite based magnetic loaded is prepared, in proportion nickel nitrate and ferric nitrate are substantially dissolved in deionized water, pH is adjusted with alkaline solution a
To 14, mixed solution A is obtained；Mixed liquor A is transferred in the stainless steel cauldron of polytetrafluoroethylliner liner, hydro-thermal is carried out anti-
Should, after reaction terminates, room temperature, deionized water and ethanol washing is cooled to, after drying, nickel ferrite based magnetic loaded powder is obtained；
3）Bismuth nitrate, sodium sulphate and nickel ferrite based magnetic loaded are dissolved in deionized water by ferroso-ferric oxide, the mixing of nickel ferrite based magnetic loaded bismuth oxide in proportion
In, solution B is obtained, alkaline solution b is mixed to get solution C with solution B；Solution C is transferred to microwave reactor to be reacted,
After reaction terminates, room temperature, deionized water and ethanol washing is cooled to, after drying, visible magnetic photocatalytic material is obtained；
4）By the magnetic photocatalytic material obtained in step 3 and silver nitrate and surfactant according to mass ratio 1:0.5:115
It is added in ethylene glycol, obtains the dispersion liquid that magnetic photocatalytic material nano-particle mass fraction is 1.5%, dispersion liquid is heated up
To 20 °C, stirring reaction 12 hours is collected after the completion of question response is abundant and obtains product, by products therefrom respectively with absolute ethyl alcohol and
Deionized water is fully washed, after drying, you can obtain nickel ferrite based magnetic loaded/bismuth oxide/ferroso-ferric oxide/silver nanoparticle compound particle；
5）Nickel ferrite based magnetic loaded/bismuth oxide/ferroso-ferric oxide/silver nanoparticle compound particle described in step 4 is pressed with absolute ethyl alcohol and ammoniacal liquor
Mass ratio 1：1000：5 are sufficiently mixed, and are subsequently adding titanium source, and titanium source is combined with nickel ferrite based magnetic loaded/bismuth oxide/ferroso-ferric oxide/silver nanoparticle
The mass ratio of particle is 2:1, stir 24 hours at a temperature of 50 °C, collect after the completion of question response is abundant and obtain product, by institute
Obtain product fully to be cleaned with absolute ethyl alcohol and deionized water respectively, after drying, calcine in air atmosphere at a temperature of 600 °C
3 hours, that is, obtain magnetic photocatalytic nano composite material.
The stabilizer is sodium citrate, and reducing agent is sodium acetate.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of spirit or essential attributes without departing substantially from the present invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit is required rather than described above is limited, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment is only wrapped
Contain an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical scheme in each embodiment can also form those skilled in the art through appropriately combined
Understandable other embodiment.
Claims (3)
1. a kind of magnetic photocatalytic nano composite material, it is characterised in which is mainly by bismuth oxide, nickel ferrite based magnetic loaded and four oxidations three
Iron constitute, the bismuth oxide be nanometer powder shape, nickel ferrite based magnetic loaded be nanometer powder shape, ferroso-ferric oxide be nanometer powder shape, three
The amount ratio of material is 1:0.2～2：0.1～1.
2. a kind of its preparation method of magnetic photocatalytic nano composite material, it is characterised in which specifically includes following steps:
Prepared by ferroso-ferric oxide, by molysite with stabilizer and reducing agent according to mass ratio 1:0.2～0.9:1～3 is added to alcohols
In solvent, the solution that iron concentration is 0.04～0.2M after being completely dissolved, is obtained；Resulting solution is transferred to autoclave
Interior, at a temperature of 180～220 °C after reaction 8～10 hours, obtain black product, by the black product spend respectively from
Sub- water and absolute ethyl alcohol are fully washed, and after drying, finally give ferriferrous oxide nano-particle；
Prepare nickel ferrite based magnetic loaded, in proportion nickel nitrate and ferric nitrate are substantially dissolved in deionized water, with alkaline solution a adjust pH to
13～14, obtain mixed solution A；Mixed liquor A is transferred in the stainless steel cauldron of polytetrafluoroethylliner liner, hydro-thermal is carried out anti-
Should, after reaction terminates, room temperature, deionized water and ethanol washing is cooled to, after drying, nickel ferrite based magnetic loaded powder is obtained；
Bismuth nitrate, sodium sulphate and nickel ferrite based magnetic loaded are dissolved in deionized water by ferroso-ferric oxide, the mixing of nickel ferrite based magnetic loaded bismuth oxide in proportion
In, solution B is obtained, alkaline solution b is mixed to get solution C with solution B；Solution C is transferred to microwave reactor to be reacted,
After reaction terminates, room temperature, deionized water and ethanol washing is cooled to, after drying, visible magnetic photocatalytic material is obtained；
By the magnetic photocatalytic material obtained in step 3 and silver nitrate and surfactant according to mass ratio 1:0.1～0.5:
10～15 are added in ethylene glycol, obtain the dispersion liquid that magnetic photocatalytic material nano-particle mass fraction is 0.2～1.5%, will
Dispersion liquid is warming up to 100～120 °C, stirring reaction 8～12 hours, collects and obtains product, by gained after the completion of question response is abundant
Product is fully washed with absolute ethyl alcohol and deionized water respectively, after drying, you can obtain nickel ferrite based magnetic loaded/bismuth oxide/tetra- oxidation three
Iron/silver nanoparticle compound particle；
Nickel ferrite based magnetic loaded/bismuth oxide/ferroso-ferric oxide/silver nanoparticle compound particle described in step 4 is pressed matter with absolute ethyl alcohol and ammoniacal liquor
Amount compares 1：800～1000：4～5 are sufficiently mixed, and are subsequently adding titanium source, titanium source and nickel ferrite based magnetic loaded/bismuth oxide/ferroso-ferric oxide/Yin Na
The mass ratio of rice compound particle is 1～2:1, stir 12～24 hours at a temperature of 40～50 °C, after the completion of question response is abundant
Collection obtains product, and products therefrom is fully cleaned with absolute ethyl alcohol and deionized water respectively, after drying, at 400～600 °C
At a temperature of calcine 2～3 hours in air atmosphere, that is, obtain magnetic photocatalytic nano composite material.
3. the preparation method of magnetic photocatalytic nano composite material according to claim 2, it is characterised in that stabilizer is
Sodium citrate, reducing agent are sodium acetate.
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