CN107744821A - A kind of magnetic photocatalyst with SPR responses and preparation method thereof - Google Patents
A kind of magnetic photocatalyst with SPR responses and preparation method thereof Download PDFInfo
- Publication number
- CN107744821A CN107744821A CN201710908271.0A CN201710908271A CN107744821A CN 107744821 A CN107744821 A CN 107744821A CN 201710908271 A CN201710908271 A CN 201710908271A CN 107744821 A CN107744821 A CN 107744821A
- Authority
- CN
- China
- Prior art keywords
- catalyst
- deionized water
- composite
- ethyl alcohol
- several times
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 130
- 239000003054 catalyst Substances 0.000 claims abstract description 81
- 239000002131 composite material Substances 0.000 claims abstract description 59
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- 238000001556 precipitation Methods 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 18
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 89
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 84
- 239000008367 deionised water Substances 0.000 claims description 56
- 229910021641 deionized water Inorganic materials 0.000 claims description 56
- 229910000161 silver phosphate Inorganic materials 0.000 claims description 54
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 39
- 238000001291 vacuum drying Methods 0.000 claims description 37
- 229910001868 water Inorganic materials 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 27
- 238000000926 separation method Methods 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 27
- 239000006185 dispersion Substances 0.000 claims description 26
- 238000002604 ultrasonography Methods 0.000 claims description 17
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 13
- 239000002244 precipitate Substances 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims 2
- 230000015556 catabolic process Effects 0.000 abstract description 15
- 238000006731 degradation reaction Methods 0.000 abstract description 15
- 239000002245 particle Substances 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 7
- 230000009467 reduction Effects 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 5
- 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
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 239000004332 silver Substances 0.000 abstract description 2
- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 description 18
- 229940107698 malachite green Drugs 0.000 description 18
- 150000001875 compounds Chemical class 0.000 description 13
- 238000007144 microwave assisted synthesis reaction Methods 0.000 description 11
- 230000001699 photocatalysis Effects 0.000 description 11
- 238000005406 washing Methods 0.000 description 9
- 239000002105 nanoparticle Substances 0.000 description 8
- 230000003197 catalytic effect Effects 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000002242 deionisation method Methods 0.000 description 3
- -1 hydroxyl radical free radical Chemical class 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000004054 benzoquinones Chemical class 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000002122 magnetic nanoparticle Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000907663 Siproeta stelenes Species 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 238000002703 mutagenesis Methods 0.000 description 1
- 231100000350 mutagenesis Toxicity 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 150000003384 small molecules Chemical group 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
- B01J27/1853—Phosphorus; Compounds thereof with iron group metals or platinum group metals with iron, cobalt or nickel
-
- B01J35/33—
-
- B01J35/39—
-
- B01J35/40—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/346—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The invention belongs to photocatalyst technology field, discloses a kind of magnetic photocatalyst with SPR responses and preparation method thereof, first with microwave irradiation is quick, simple preparation magnetic is good, uniform particle diameter nanometer Fe3O4Particle, magnetic coupling catalyst Ag is prepared using ultrasonic wave added in situ Precipitation afterwards3PO4/Fe3O4, finally prepare Ag/Ag using microwave reduction part silver3PO4/Fe3O4Composite.The present invention quickly prepares photochemical catalyst using Microwave reduction method, and method is simple, highly shortened preparation time；Prepared catalyst has higher activity, further increases light conversion ratio, to MG degradation rate up to more than 99%；And catalyst has a superparamagnetism, reuse is more simple and efficient.
Description
Technical field
The invention belongs to photocatalyst technology field, is to be related to a kind of magnetic nanometer photocatalyst specifically.
Background technology
Malachite green (MG) is a kind of triphenylmethane dye, is widely used in printing and dyeing, leather, textile industry etc..By
In with efficient bactericidal action and cheap, it is also widely used for culture fishery.Malachite green have high toxicity,
High residue and there are carcinogenic, teratogenesis, mutagenesis to organism, therefore, from efficient stable and the cheap processing side of cost
The malachite green that method is removed in water body is significant.
1972, Japanese Scientists Honda and Fujishima existed《Nature》Relevant n-type semiconductor is delivered on magazine
TiO2The paper of the full hydrogen production by water decomposition gas of photocatalysis and oxygen on Single Crystalline Electrodes, the discovery start photocatalysis research in scientific circles
Upsurge.1976, John.H.Carey then reported TiO2Photochemical catalytic oxidation to Polychlorinated biphenyls, this is first by photocatalysis
Technology works applied to pollutant process, there is provided a new approaches of oxidation operation.Compared to traditional Physical, chemistry
The water pollution control means such as method and bioanalysis, photocatalytic method have technique simple, and energy consumption is low, and operating condition is easily controlled, pollution
A kind of the features such as thing degradation efficiency is high, it is considered to be environment protection novel with good development prospect.
At present, there is TiO in the more photochemical catalyst of photocatalysis field research2、ZnO、CdS、BiVO4Deng, but these catalyst
Photoresponse narrow range and the low problem of photocatalysis quantum rate are still suffered from, seriously limits the practical application of photochemical catalyst.In recent years,
Researcher is doped and is modified to unitary semi-conducting material so that its photocatalytic activity increases, but catalytic performance is still
It is relatively low, do not reach the standard of practical application.In addition, light-catalyzed reaction is carried out in suspension system mostly, cause photochemical catalyst outstanding
It is that the recycling of nano-photocatalyst is relatively difficult, and traditional separation method such as centrifuges, filters process tedious and cost
Higher, this also makes troubles to the practical application of common photochemical catalyst and industrialization.Therefore, exploitation rings with higher visible ray
The photochemical catalyst that should and be easily recycled is current study hotspot.In addition, the synthetic method such as hydro-thermal that photochemical catalyst is traditional
Method, solvent-thermal method, time-consuming longer and high to equipment requirement, technical difficulty is big, therefore seeks a kind of fast and effectively synthetic method
Extensive use to photochemical catalyst is significant.
The content of the invention
For photochemical catalyst preparation time present in above-mentioned prior art is long, degradation efficiency is low and reclaims the skills such as difficulty
Art problem, the present invention propose a kind of magnetic photocatalyst Ag/Ag with surface plasma body resonant vibration (SPR) effect3PO4/
Fe3O4Its preparation method, first with microwave irradiation is quick, simple preparation magnetic is good, uniform particle diameter nanometer Fe3O4
Grain, prepares magnetic coupling catalyst Ag using ultrasonic wave added in situ Precipitation afterwards3PO4/Fe3O4, finally utilize microwave reduction portion
Silver is divided to prepare Ag/Ag3PO4/Fe3O4Composite；Even heat transmission is beneficial to nanoparticle nucleated in micro-wave oven, shortens knot
The brilliant time, prepared nano particle diameter is small, narrowly distributing, pattern rule, has higher catalytic activity；Fe simultaneously3O4Deposit
Causing catalyst that there is superparamagnetism, quick recycle can be achieved merely with external magnetic field after the completion of degraded.
In order to solve the above-mentioned technical problem, the present invention is achieved by following technical scheme：
A kind of magnetic photocatalyst with SPR responses, is obtained by following preparation method：
(1) FeCl is weighed3·6H2O is dissolved in deionized water, and it is 25~28% that mass concentration is added under stirring
NH3·H2O to pH is 9~9.5, and is transferred to 5~8min of heating in micro-wave oven, obtains black precipitate；With strong magnet precipitation and separation
Afterwards, washed for several times with deionized water and absolute ethyl alcohol, be placed in 60~80 DEG C of dry 4~6h in vacuum drying chamber, you can received
Rice Fe3O4；
(2) nanometer Fe for obtaining step (1)3O4Quick ultrasonic disperse is in deionized water, by AgNO3With Na2HPO4Press
Mol ratio is 3:1 ratio is successively added in above-mentioned dispersion liquid, and continuation 30~50min of ultrasound to reaction terminates；Wherein Ag3PO4With
Fe3O4Mol ratio be 1:2~2:1；After the precipitation in reaction solution is separated with strong magnet, washed with deionized water and absolute ethyl alcohol
For several times, 60~80 DEG C of dry 4~6h in vacuum drying chamber are placed in, gained solid powder is Ag3PO4/Fe3O4Composite catalyst；
(3) Ag that step (2) obtains is weighed3PO4/Fe3O4Composite catalyst is in AgNO3In solution, Ag3PO4/Fe3O4It is compound
Ag in catalyst3PO4Mole and AgNO3Ag in solution+The ratio between mole be 1:1；Ultrasound simultaneously stirs 30~50min,
Make catalyst dispersed；Above-mentioned dispersion liquid is placed in micro-wave oven, temperature be 90~100 DEG C, power be 300~500W bars
5~15min is heated under part, reaction terminates；After strong magnet precipitation and separation, washed for several times, put with deionized water and absolute ethyl alcohol
60~80 DEG C of dry 4~6h, produce Ag/Ag in vacuum drying chamber3PO4/Fe3O4Composite photo-catalyst.
Preferably, Ag in step (2)3PO4With Fe3O4Mol ratio be 1:1.
Preferably, in step (3) during microwave stove heat, temperature is 95 DEG C, power 300W, heat time 10min.
A kind of preparation method of the magnetic photocatalyst with SPR responses, this method follow the steps below：
(1) FeCl is weighed3·6H2O is dissolved in deionized water, and it is 25~28% that mass concentration is added under stirring
NH3·H2O to pH is 9~9.5, and is transferred to 5~8min of heating in micro-wave oven, obtains black precipitate；With strong magnet precipitation and separation
Afterwards, washed for several times with deionized water and absolute ethyl alcohol, be placed in 60~80 DEG C of dry 4~6h in vacuum drying chamber, you can received
Rice Fe3O4；
(2) nanometer Fe for obtaining step (1)3O4Quick ultrasonic disperse is in deionized water, by AgNO3With Na2HPO4Press
Mol ratio is 3:1 ratio is successively added in above-mentioned dispersion liquid, and continuation 30~50min of ultrasound to reaction terminates；Wherein Ag3PO4With
Fe3O4Mol ratio be 1:2~2:1；After the precipitation in reaction solution is separated with strong magnet, washed with deionized water and absolute ethyl alcohol
For several times, 60~80 DEG C of dry 4~6h in vacuum drying chamber are placed in, gained solid powder is Ag3PO4/Fe3O4Composite catalyst；
(3) Ag that step (2) obtains is weighed3PO4/Fe3O4Composite catalyst is in AgNO3In solution, Ag3PO4/Fe3O4It is compound
Ag in catalyst3PO4Mole and AgNO3Ag in solution+The ratio between mole be 1:1；Ultrasound simultaneously stirs 30~50min,
Make catalyst dispersed；Above-mentioned dispersion liquid is placed in micro-wave oven, temperature be 90~100 DEG C, power be 300~500W bars
5~15min is heated under part, reaction terminates；After strong magnet precipitation and separation, washed for several times, put with deionized water and absolute ethyl alcohol
60~80 DEG C of dry 4~6h, produce Ag/Ag in vacuum drying chamber3PO4/Fe3O4Composite photo-catalyst.
Preferably, Ag in step (2)3PO4With Fe3O4Mol ratio be 1:1.
Preferably, in step (3) during microwave stove heat, temperature is 95 DEG C, power 300W, heat time 10min.
The beneficial effects of the invention are as follows：
The present invention quickly prepares photochemical catalyst using Microwave reduction method, and prepared catalyst has higher activity, and
It is convenient to recycle：
(1) the magnetic Ag/Ag of tool prepared by the present invention3PO4/Fe3O4Composite nanometer particle, show malachite of degrading
The superior function of green (MG), Ag3PO4As a kind of n-type semiconductor, its energy gap is 2.36eV, can be with absorbing wavelength<525nm
Visible ray and ultraviolet light, the organic pollution in the water body that can degrade；Fe3O4So that the specific surface area of composite nanometer particle increases
Add, and increase the avtive spot with MG effects；Ag causes composite catalyst to have surface plasma body resonant vibration (SPR) effect,
Greatly improve the degradation efficiency of catalyst；Ag/Ag prepared by the present invention3PO4/Fe3O4Nano particle is added to 20mg/L MG
In waste water, it is seen that the clearance under light in 30min is up to more than 99%.
(2) present invention prepares the Fe of uniform particle sizes with Microwave reduction method3O4And its is compound in the catalyst, both effectively
Ground prevents the compound of electron-hole pair, also composite nanometer particle is had superparamagnetism, is achieved that merely with external magnetic field
The quick recycling of photochemical catalyst.
(3) present invention prepares Ag/Ag using the method for Microwave-assisted synthesis3PO4/Fe3O4Photochemical catalyst, can simply,
Rapidly synthesizing nano-particle, in micro-wave oven even heat transmission be advantageous to nanoparticle nucleated, shorten crystallization time, thus institute
The nano particle diameter of preparation is small, narrowly distributing, pattern rule, has higher catalytic activity.
In summary, magnetic photocatalyst of the invention and preparation method thereof uses Microwave-assisted Reduction method, and method is simple,
It highly shortened preparation time；Prepared catalyst further increases light conversion ratio, to MG degradation rate up to 99% with
On；Because catalyst has a superparamagnetism, reuse is more simple and efficient.
Brief description of the drawings
Fig. 1 is the photocatalytic activity figure of the prepared catalyst of embodiment 1~9；
Fig. 2 is the recycling rate of waterused figure that embodiment 1 prepares catalyst；
Fig. 3 is the cover test degradation rate figure of the prepared catalyst of embodiment 1；
Fig. 4 is the Ag/Ag3PO4/Fe3O4 composite nanometer particles degraded MG mechanism figures prepared by the present invention.
Embodiment
Below by specific embodiment, the present invention is described in further detail, and following examples can make this specialty
The present invention, but do not limit the invention in any way is more completely understood in technical staff.
Following examples the use of the model of micro-wave oven is XH-800C, Beijing XiangHu Science and Technology Development Co., Ltd..
FeCl used in following examples3·6H2O、NH3·H2O、AgNO3、Na2HPO4It is AR, Tianjin
Yuan Li Chemical Co., Ltd.s of city.
Embodiment 1
The present embodiment prepares Ag/Ag using Microwave-assisted synthesis3PO4/Fe3O4Composite, comprise the following steps：
(1) FeCl is weighed3·6H2O is dissolved in deionized water, and the NH of mass concentration 28% is added under stirring3·
H2O to pH is 9, and is transferred in micro-wave oven and heats 8min, obtains black precipitate；After strong magnet precipitation and separation, deionization is used
Water and absolute ethyl alcohol washing for several times, are placed in 60 DEG C of dry 6h in vacuum drying chamber, you can obtain nanometer Fe3O4；
(2) nanometer Fe for obtaining step (1)3O4Quick ultrasonic disperse is in deionized water, by AgNO3With Na2HPO4Press
Mol ratio is 3:1 ratio is successively added in above-mentioned dispersion liquid, is continued ultrasonic 50min and is terminated to reaction；Wherein Ag3PO4With
Fe3O4Mol ratio be 1:1；After the precipitation in reaction solution is separated with strong magnet, washed for several times with deionized water and absolute ethyl alcohol,
60 DEG C of dry 6h in vacuum drying chamber are placed in, gained solid powder is Ag3PO4/Fe3O4Composite catalyst；
(3) Ag that step (2) obtains is weighed3PO4/Fe3O4Composite catalyst is in AgNO3In solution, Ag3PO4/Fe3O4It is compound
Ag in catalyst3PO4Mole and AgNO3Ag in solution+The ratio between mole be 1:1；Ultrasound simultaneously stirs 50min, makes to urge
Agent is dispersed；Above-mentioned dispersion liquid is placed in micro-wave oven, 10min is heated under the conditions of temperature is 95 DEG C, power is 300W,
Reaction terminates；After strong magnet precipitation and separation, washed for several times with deionized water and absolute ethyl alcohol, be placed in vacuum drying chamber 60 DEG C
6h is dried, produces Ag/Ag3PO4/Fe3O4Composite photo-catalyst.
Embodiment 2
The present embodiment prepares Ag/Ag using Microwave-assisted synthesis3PO4/Fe3O4Composite, comprise the following steps：
(1) FeCl is weighed3·6H2O is dissolved in deionized water, and the NH of mass concentration 28% is added under stirring3·
H2O to pH is 9, and is transferred in micro-wave oven and heats 8min, obtains black precipitate；After strong magnet precipitation and separation, deionization is used
Water and absolute ethyl alcohol washing for several times, are placed in 60 DEG C of dry 6h in vacuum drying chamber, you can obtain nanometer Fe3O4；
(2) nanometer Fe for obtaining step (1)3O4Quick ultrasonic disperse is in deionized water, by AgNO3With Na2HPO4Press
Mol ratio is 3:1 ratio is successively added in above-mentioned dispersion liquid, is continued ultrasonic 50min and is terminated to reaction；Wherein Ag3PO4With
Fe3O4Mol ratio be 2：1；After the precipitation in reaction solution is separated with strong magnet, washed for several times with deionized water and absolute ethyl alcohol,
60 DEG C of dry 6h in vacuum drying chamber are placed in, gained solid powder is Ag3PO4/Fe3O4Composite catalyst；
(3) Ag that step (2) obtains is weighed3PO4/Fe3O4Composite catalyst is in AgNO3 solution, Ag3PO4/Fe3O4It is compound
Ag in catalyst3PO4Mole and AgNO3Ag in solution+The ratio between mole be 1:1；Ultrasound simultaneously stirs 50min, makes to urge
Agent is dispersed；Above-mentioned dispersion liquid is placed in micro-wave oven, 10min is heated under the conditions of temperature is 95 DEG C, power is 300W,
Reaction terminates；After strong magnet precipitation and separation, washed for several times with deionized water and absolute ethyl alcohol, be placed in vacuum drying chamber 60 DEG C
6h is dried, produces Ag/Ag3PO4/Fe3O4Composite photo-catalyst.
Embodiment 3
The present embodiment prepares Ag/Ag using Microwave-assisted synthesis3PO4/Fe3O4Composite, comprise the following steps：
(1) FeCl is weighed3·6H2O is dissolved in deionized water, and the NH of mass concentration 28% is added under stirring3·
H2O to pH is 9, and is transferred in micro-wave oven and heats 8min, obtains black precipitate；After strong magnet precipitation and separation, deionization is used
Water and absolute ethyl alcohol washing for several times, are placed in 70 DEG C of dry 5h in vacuum drying chamber, you can obtain nanometer Fe3O4；
(2) nanometer Fe for obtaining step (1)3O4Quick ultrasonic disperse is in deionized water, by AgNO3With Na2HPO4Press
Mol ratio is 3:1 ratio is successively added in above-mentioned dispersion liquid, is continued ultrasonic 40min and is terminated to reaction；Wherein Ag3PO4With
Fe3O4Mol ratio be 1：2；After the precipitation in reaction solution is separated with strong magnet, washed for several times with deionized water and absolute ethyl alcohol,
70 DEG C of dry 5h in vacuum drying chamber are placed in, gained solid powder is Ag3PO4/Fe3O4Composite catalyst；
(3) Ag that step (2) obtains is weighed3PO4/Fe3O4Composite catalyst is in AgNO3 solution, Ag3PO4/Fe3O4It is compound
Ag in catalyst3PO4Mole and AgNO3Ag in solution+The ratio between mole be 1:1；Ultrasound simultaneously stirs 40min, makes to urge
Agent is dispersed；Above-mentioned dispersion liquid is placed in micro-wave oven, 10min is heated under the conditions of temperature is 95 DEG C, power is 300W,
Reaction terminates；After strong magnet precipitation and separation, washed for several times with deionized water and absolute ethyl alcohol, be placed in vacuum drying chamber 70 DEG C
5h is dried, produces Ag/Ag3PO4/Fe3O4Composite photo-catalyst.
Embodiment 4
The present embodiment prepares Ag/Ag using Microwave-assisted synthesis3PO4/Fe3O4Composite, comprise the following steps：
(1) FeCl is weighed3·6H2O is dissolved in deionized water, and the NH of mass concentration 26% is added under stirring3·
H2O to pH is 8.5, and is transferred in micro-wave oven and heats 6min, obtains black precipitate；After strong magnet precipitation and separation, spend from
Sub- water and absolute ethyl alcohol washing for several times, is placed in 60 DEG C of dry 6h in vacuum drying chamber, you can obtain nanometer Fe3O4；
(2) nanometer Fe for obtaining step (1)3O4Quick ultrasonic disperse is in deionized water, by AgNO3With Na2HPO4Press
Mol ratio is 3:1 ratio is successively added in above-mentioned dispersion liquid, is continued ultrasonic 40min and is terminated to reaction；Wherein Ag3PO4With
Fe3O4Mol ratio be 1:1；After the precipitation in reaction solution is separated with strong magnet, washed for several times with deionized water and absolute ethyl alcohol,
60 DEG C of dry 6h in vacuum drying chamber are placed in, gained solid powder is Ag3PO4/Fe3O4Composite catalyst；
(3) Ag that step (2) obtains is weighed3PO4/Fe3O4Composite catalyst is in AgNO3 solution, Ag3PO4/Fe3O4It is compound
Ag in catalyst3PO4Mole and AgNO3Ag in solution+The ratio between mole be 1:1；Ultrasound simultaneously stirs 40min, makes to urge
Agent is dispersed；Above-mentioned dispersion liquid is placed in micro-wave oven, 10min is heated under the conditions of temperature is 90 DEG C, power is 300W,
Reaction terminates；After strong magnet precipitation and separation, washed for several times with deionized water and absolute ethyl alcohol, be placed in vacuum drying chamber 60 DEG C
6h is dried, produces Ag/Ag3PO4/Fe3O4Composite photo-catalyst.
Embodiment 5
The present embodiment prepares Ag/Ag using Microwave-assisted synthesis3PO4/Fe3O4Composite, comprise the following steps：
(1) FeCl is weighed3·6H2O is dissolved in deionized water, and the NH of mass concentration 26% is added under stirring3·
H2O to pH is 8.5, and is transferred in micro-wave oven and heats 6min, obtains black precipitate；After strong magnet precipitation and separation, spend from
Sub- water and absolute ethyl alcohol washing for several times, is placed in 70 DEG C of dry 5h in vacuum drying chamber, you can obtain nanometer Fe3O4；
(2) nanometer Fe for obtaining step (1)3O4Quick ultrasonic disperse is in deionized water, by AgNO3With Na2HPO4Press
Mol ratio is 3:1 ratio is successively added in above-mentioned dispersion liquid, is continued ultrasonic 30min and is terminated to reaction；Wherein Ag3PO4With
Fe3O4Mol ratio be 1:1；After the precipitation in reaction solution is separated with strong magnet, washed for several times with deionized water and absolute ethyl alcohol,
70 DEG C of dry 5h in vacuum drying chamber are placed in, gained solid powder is Ag3PO4/Fe3O4Composite catalyst；
(3) Ag that step (2) obtains is weighed3PO4/Fe3O4Composite catalyst is in AgNO3 solution, Ag3PO4/Fe3O4It is compound
Ag in catalyst3PO4Mole and AgNO3Ag in solution+The ratio between mole be 1:1；Ultrasound simultaneously stirs 30min, makes to urge
Agent is dispersed；Above-mentioned dispersion liquid is placed in micro-wave oven, heated under the conditions of temperature is 100 DEG C, power is 300W
10min, reaction terminate；After strong magnet precipitation and separation, washed for several times with deionized water and absolute ethyl alcohol, be placed in vacuum drying chamber
In 70 DEG C of dry 5h, produce Ag/Ag3PO4/Fe3O4Composite photo-catalyst.
Embodiment 6
The present embodiment prepares Ag/Ag using Microwave-assisted synthesis3PO4/Fe3O4Composite, comprise the following steps：
(1) FeCl is weighed3·6H2O is dissolved in deionized water, and the NH of mass concentration 26% is added under stirring3·
H2O to pH is 8.5, and is transferred in micro-wave oven and heats 6min, obtains black precipitate；After strong magnet precipitation and separation, spend from
Sub- water and absolute ethyl alcohol washing for several times, is placed in 60 DEG C of dry 6h in vacuum drying chamber, you can obtain nanometer Fe3O4；
(2) nanometer Fe for obtaining step (1)3O4Quick ultrasonic disperse is in deionized water, by AgNO3With Na2HPO4Press
Mol ratio is 3:1 ratio is successively added in above-mentioned dispersion liquid, is continued ultrasonic 40min and is terminated to reaction；Wherein Ag3PO4With
Fe3O4Mol ratio be 1:1；After the precipitation in reaction solution is separated with strong magnet, washed for several times with deionized water and absolute ethyl alcohol,
60 DEG C of dry 6h in vacuum drying chamber are placed in, gained solid powder is Ag3PO4/Fe3O4Composite catalyst；
(3) Ag that step (2) obtains is weighed3PO4/Fe3O4Composite catalyst is in AgNO3 solution, Ag3PO4/Fe3O4It is compound
Ag in catalyst3PO4Mole and AgNO3Ag in solution+The ratio between mole be 1:1；Ultrasound simultaneously stirs 40min, makes to urge
Agent is dispersed；Above-mentioned dispersion liquid is placed in micro-wave oven, 10min is heated under the conditions of temperature is 95 DEG C, power is 400W,
Reaction terminates；After strong magnet precipitation and separation, washed for several times with deionized water and absolute ethyl alcohol, be placed in vacuum drying chamber 60 DEG C
6h is dried, produces Ag/Ag3PO4/Fe3O4Composite photo-catalyst.
Embodiment 7
The present embodiment prepares Ag/Ag using Microwave-assisted synthesis3PO4/Fe3O4Composite, comprise the following steps：
(1) FeCl is weighed3·6H2O is dissolved in deionized water, and the NH of mass concentration 25% is added under stirring3·
H2O to pH is 9.5, and is transferred in micro-wave oven and heats 5min, obtains black precipitate；After strong magnet precipitation and separation, spend from
Sub- water and absolute ethyl alcohol washing for several times, is placed in 80 DEG C of dry 4h in vacuum drying chamber, you can obtain nanometer Fe3O4；
(2) nanometer Fe for obtaining step (1)3O4Quick ultrasonic disperse is in deionized water, by AgNO3With Na2HPO4Press
Mol ratio is 3:1 ratio is successively added in above-mentioned dispersion liquid, is continued ultrasonic 40min and is terminated to reaction；Wherein Ag3PO4With
Fe3O4Mol ratio be 1:1；After the precipitation in reaction solution is separated with strong magnet, washed for several times with deionized water and absolute ethyl alcohol,
80 DEG C of dry 4h in vacuum drying chamber are placed in, gained solid powder is Ag3PO4/Fe3O4Composite catalyst；
(3) Ag that step (2) obtains is weighed3PO4/Fe3O4Composite catalyst is in AgNO3 solution, Ag3PO4/Fe3O4It is compound
Ag in catalyst3PO4Mole and AgNO3Ag in solution+The ratio between mole be 1:1；Ultrasound simultaneously stirs 40min, makes to urge
Agent is dispersed；Above-mentioned dispersion liquid is placed in micro-wave oven, 10min is heated under the conditions of temperature is 95 DEG C, power is 500W,
Reaction terminates；After strong magnet precipitation and separation, washed for several times with deionized water and absolute ethyl alcohol, be placed in vacuum drying chamber 80 DEG C
4h is dried, produces Ag/Ag3PO4/Fe3O4Composite photo-catalyst.
Embodiment 8
The present embodiment prepares Ag/Ag using Microwave-assisted synthesis3PO4/Fe3O4Composite, comprise the following steps：
(1) FeCl is weighed3·6H2O is dissolved in deionized water, and the NH of mass concentration 25% is added under stirring3·
H2O to pH is 9.5, and is transferred in micro-wave oven and heats 5min, obtains black precipitate；After strong magnet precipitation and separation, spend from
Sub- water and absolute ethyl alcohol washing for several times, is placed in 60 DEG C of dry 6h in vacuum drying chamber, you can obtain nanometer Fe3O4；
(2) nanometer Fe for obtaining step (1)3O4Quick ultrasonic disperse is in deionized water, by AgNO3With Na2HPO4Press
Mol ratio is 3:1 ratio is successively added in above-mentioned dispersion liquid, is continued ultrasonic 50min and is terminated to reaction；Wherein Ag3PO4With
Fe3O4Mol ratio be 1:1；After the precipitation in reaction solution is separated with strong magnet, washed for several times with deionized water and absolute ethyl alcohol,
60 DEG C of dry 6h in vacuum drying chamber are placed in, gained solid powder is Ag3PO4/Fe3O4Composite catalyst；
(3) Ag that step (2) obtains is weighed3PO4/Fe3O4Composite catalyst is in AgNO3 solution, Ag3PO4/Fe3O4It is compound
Ag in catalyst3PO4Mole and AgNO3Ag in solution+The ratio between mole be 1:1；Ultrasound simultaneously stirs 50min, makes to urge
Agent is dispersed；Above-mentioned dispersion liquid is placed in micro-wave oven, 5min is heated under the conditions of temperature is 95 DEG C, power is 300W,
Reaction terminates；After strong magnet precipitation and separation, washed for several times with deionized water and absolute ethyl alcohol, be placed in vacuum drying chamber 60 DEG C
6h is dried, produces Ag/Ag3PO4/Fe3O4Composite photo-catalyst.
Embodiment 9
The present embodiment prepares Ag/Ag using Microwave-assisted synthesis3PO4/Fe3O4Composite, comprise the following steps：
(1) FeCl is weighed3·6H2O is dissolved in deionized water, and the NH of mass concentration 25% is added under stirring3·
H2O to pH is 9.5, and is transferred in micro-wave oven and heats 5min, obtains black precipitate；After strong magnet precipitation and separation, spend from
Sub- water and absolute ethyl alcohol washing for several times, is placed in 60 DEG C of dry 6h in vacuum drying chamber, you can obtain nanometer Fe3O4；
(2) nanometer Fe for obtaining step (1)3O4Quick ultrasonic disperse is in deionized water, by AgNO3With Na2HPO4Press
Mol ratio is 3:1 ratio is successively added in above-mentioned dispersion liquid, is continued ultrasonic 40min and is terminated to reaction；Wherein Ag3PO4With
Fe3O4Mol ratio be 1:1；After the precipitation in reaction solution is separated with strong magnet, washed for several times with deionized water and absolute ethyl alcohol,
60 DEG C of dry 6h in vacuum drying chamber are placed in, gained solid powder is Ag3PO4/Fe3O4Composite catalyst；
(3) Ag that step (2) obtains is weighed3PO4/Fe3O4Composite catalyst is in AgNO3 solution, Ag3PO4/Fe3O4It is compound
Ag in catalyst3PO4Mole and AgNO3Ag in solution+The ratio between mole be 1:1；Ultrasound simultaneously stirs 40min, makes to urge
Agent is dispersed；Above-mentioned dispersion liquid is placed in micro-wave oven, 15min is heated under the conditions of temperature is 95 DEG C, power is 300W,
Reaction terminates；After strong magnet precipitation and separation, washed for several times with deionized water and absolute ethyl alcohol,
60 DEG C of dry 6h in vacuum drying chamber are placed in, produce Ag/Ag3PO4/Fe3O4Composite photo-catalyst.
The major parameter table of 1 embodiment of table 1~9
The advantage of preparation method of the present invention is carried out below with reference to the performance test results of the photochemical catalyst of embodiment 1~9
Further illustrate.
(1) photocatalysis performance is tested
Ag/Ag prepared by embodiment 1~93PO4/Fe3O4Magnetic nanoparticle is used for MG photocatalytic degradation, specific step
It is rapid as follows：
(1) configuration concentration is 5mg/L MG solution.
(2) using 150ml beaker as photo catalysis reactor.15mg Ag/Ag are added in beaker3PO4/Fe3O4
Nano particle and 50mL concentration are 5mg/L MG solution, dark place stirring 60min, make to reach absorption-solution between catalyst and MG
Inhale balance.3mL is sampled, with the isolated supernatant liquid of strong magnet, labeled as M0
(3) light source uses xenon source of the power for 100W, and light source is placed in 9cm above the page.3ml is sampled every 5min,
M1, M2, M3, M4, M5, M6 are respectively labeled as after being separated with strong magnet, sample is detected in ripple using ultraviolet-visible spectrophotometer
Absorbance at long 617nm.
(4) degradation rate-time graph is made, as shown in Figure 1.
As Fig. 1 and table 2 it can be found that the catalyst prepared by embodiment 1~9 is respectively provided with preferable photocatalytic degradation to MG
Effect, the degradation rate in 30min is between 80%~99%.
In catalyst prepared by embodiment 1~9, the Ag/Ag prepared by embodiment 13PO4/Fe3O4Photochemical catalyst is to MG
Degradation property it is best.This is due to Ag/Ag prepared by embodiment 13PO4/Fe3O4Ratio between middle each component can reach most
Good synergy.Appropriate Ag can make catalyst have SPR effects, nano-particle is shown in visible region very strong
Visible absorption effect, and then considerably improve the performance of catalyst.If Ag too high levels, electron-hole can be turned into
Complex centre, reduce catalytic performance.
The photocatalytic activity of composite catalyst in the embodiment 1~9 of table 2
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 |
| Degradation rate % | 99.5 | 96.6 | 92.9 | 91.2 | 90.5 | 84.4 | 82.9 | 89.6 | 80.3 |
(2) measure of the rate of recovery
As shown in Fig. 2 the catalyst prepared by embodiment 1 is carried out 8 times after recycling, it is still reachable to MG degradation rate
To more than 85%, the composite catalyst for illustrating to prepare has preferable reusing.This is due to that catalyst possesses magnetic, profit
Efficient recovery can be realized with external magnetic field, thus inference, the catalyst prepared in embodiment 2~9 also has preferably weight
Multiple usability.Catalyst merely with external magnetic field can high efficiente callback, reduce cost, there is good application prospect.
(3) Ag/Ag of Microwave-assisted synthesis3PO4/Fe3O4Light of the magnetic nanoparticle to organic dye molecule in water body
Catalytic degradation mechanism
With the Ag/Ag prepared by embodiment 13PO4/Fe3O4Exemplified by catalyst, masking experiment is carried out to probe into light degradation machine
Reason：With Na2- EDTA is hole trapping agents, and isopropanol is hydroxyl radical free radical capturing agent, and benzoquinones is distinguished for superoxide radical capturing agent
Tested.As seen from Figure 3, when adding isopropanol, the catalytic activity of system is significantly suppressed, degradation efficiency drop
To 15% or so；After adding benzoquinones, the price reduction rate to MG is 55%；Add Na2After-EDTA, the change very little of catalysis degradation modulus,
It reduced by only 10%.This shows in Photocatalytic Degradation Process, aoxidized with hydroxyl radical free radical based on, superoxide radical takes second place, empty
Cave oxidation is played a part of little.
By above-mentioned experiment, possible light-catalyzed reaction mechanism can be deduced, as shown in Figure 4：Ag3PO4Band gap width be
2.4eV, under the irradiation of visible ray, its valence-band electrons can be excited, and quickly reach Ag, because localised plasmon resonance shows
As and Fe3O4With good electric conductivity, by Ag3PO4It flow to the electrons that Ag electronics and Ag are inspired and moves to Fe3O4's
Surface, and the water molecule reaction with being adsorbed onto catalyst surface generates hydroxyl radical free radical, and super oxygen is generated with the oxygen molecule of absorption
Free radical.It is small-molecule substance that hydroxyl, superoxide radical, hole aoxidize MG respectively.
Although the preferred embodiments of the present invention are described above in conjunction with accompanying drawing, the invention is not limited in upper
The embodiment stated, above-mentioned embodiment is only schematical, be not it is restricted, this area it is common
Technical staff in the case of present inventive concept and scope of the claimed protection is not departed from, may be used also under the enlightenment of the present invention
By make it is many in the form of specific conversion, these are belonged within protection scope of the present invention.
Claims (6)
1. a kind of magnetic photocatalyst with SPR responses, it is characterised in that obtained by following preparation method：
(1) FeCl is weighed3·6H2O is dissolved in deionized water, and the NH that mass concentration is 25~28% is added under stirring3·
H2O to pH is 8.5~9.5, and is transferred to 5~8min of heating in micro-wave oven, obtains black precipitate；With strong magnet precipitation and separation
Afterwards, washed for several times with deionized water and absolute ethyl alcohol, be placed in 60~80 DEG C of dry 4~6h in vacuum drying chamber, you can received
Rice Fe3O4；
(2) nanometer Fe for obtaining step (1)3O4Quick ultrasonic disperse is in deionized water, by AgNO3With Na2HPO4By mole
Than for 3:1 ratio is successively added in above-mentioned dispersion liquid, and continuation 30~50min of ultrasound to reaction terminates；Wherein Ag3PO4With
Fe3O4Mol ratio be 1:2~2:1；After the precipitation in reaction solution is separated with strong magnet, washed with deionized water and absolute ethyl alcohol
For several times, 60~80 DEG C of dry 4~6h in vacuum drying chamber are placed in, gained solid powder is Ag3PO4/Fe3O4Composite catalyst；
(3) Ag that step (2) obtains is weighed3PO4/Fe3O4Composite catalyst is in AgNO3In solution, Ag3PO4/Fe3O4Composite catalyzing
Ag in agent3PO4Mole and AgNO3Ag in solution+The ratio between mole be 1:1；Ultrasound simultaneously stirs 30~50min, makes to urge
Agent is dispersed；Above-mentioned dispersion liquid is placed in micro-wave oven, under the conditions of temperature is 90~100 DEG C, power is 300~500W
5~15min is heated, reaction terminates；After strong magnet precipitation and separation, washed for several times, be placed in true with deionized water and absolute ethyl alcohol
60~80 DEG C of dry 4~6h, produce Ag/Ag in empty drying box3PO4/Fe3O4Composite photo-catalyst.
2. a kind of magnetic photocatalyst with SPR responses according to claim 1, it is characterised in that in step (2)
Ag3PO4With Fe3O4Mol ratio be 1:1.
3. a kind of magnetic photocatalyst with SPR responses according to claim 1, it is characterised in that micro- in step (3)
During ripple stove heat, temperature is 95 DEG C, power 300W, heat time 10min.
4. a kind of preparation method of the magnetic photocatalyst as claimed in claim 1 with SPR responses, it is characterised in that should
Method follows the steps below：
(1) FeCl is weighed3·6H2O is dissolved in deionized water, and the NH that mass concentration is 25~28% is added under stirring3·
H2O to pH is 9~9.5, and is transferred to 5~8min of heating in micro-wave oven, obtains black precipitate；After strong magnet precipitation and separation,
Washed for several times with deionized water and absolute ethyl alcohol, be placed in 60~80 DEG C of dry 4~6h in vacuum drying chamber, you can obtain nanometer
Fe3O4；
(2) nanometer Fe for obtaining step (1)3O4Quick ultrasonic disperse is in deionized water, by AgNO3With Na2HPO4By mole
Than for 3:1 ratio is successively added in above-mentioned dispersion liquid, and continuation 30~50min of ultrasound to reaction terminates；Wherein Ag3PO4With
Fe3O4Mol ratio be 1:2~2:1；After the precipitation in reaction solution is separated with strong magnet, washed with deionized water and absolute ethyl alcohol
For several times, 60~80 DEG C of dry 4~6h in vacuum drying chamber are placed in, gained solid powder is Ag3PO4/Fe3O4Composite catalyst；
(3) Ag that step (2) obtains is weighed3PO4/Fe3O4Composite catalyst is in AgNO3In solution, Ag3PO4/Fe3O4Composite catalyzing
Ag in agent3PO4Mole and AgNO3Ag in solution+The ratio between mole be 1:1；Ultrasound simultaneously stirs 30~50min, makes to urge
Agent is dispersed；Above-mentioned dispersion liquid is placed in micro-wave oven, under the conditions of temperature is 90~100 DEG C, power is 300~500W
5~15min is heated, reaction terminates；After strong magnet precipitation and separation, washed for several times, be placed in true with deionized water and absolute ethyl alcohol
60~80 DEG C of dry 4~6h, produce Ag/Ag in empty drying box3PO4/Fe3O4Composite photo-catalyst.
A kind of 5. preparation method of magnetic photocatalyst with SPR responses according to claim 4, it is characterised in that
Ag in step (2)3PO4With Fe3O4Mol ratio be 1:1.
A kind of 6. preparation method of magnetic photocatalyst with SPR responses according to claim 4, it is characterised in that
In step (3) during microwave stove heat, temperature is 95 DEG C, power 300W, heat time 10min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710908271.0A CN107744821A (en) | 2017-09-29 | 2017-09-29 | A kind of magnetic photocatalyst with SPR responses and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710908271.0A CN107744821A (en) | 2017-09-29 | 2017-09-29 | A kind of magnetic photocatalyst with SPR responses and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107744821A true CN107744821A (en) | 2018-03-02 |
Family
ID=61254692
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710908271.0A Pending CN107744821A (en) | 2017-09-29 | 2017-09-29 | A kind of magnetic photocatalyst with SPR responses and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107744821A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108704653A (en) * | 2018-06-14 | 2018-10-26 | 浙江理工大学 | It is a kind of to have magnetic silver phosphate composite photocatalyst and its preparation method and application |
| CN110836919A (en) * | 2019-11-29 | 2020-02-25 | 金陵科技学院 | Chiral recognition material and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103007973A (en) * | 2012-12-14 | 2013-04-03 | 陕西科技大学 | Silver/silver phosphate composite material and preparation method thereof |
| CN103623803A (en) * | 2012-08-30 | 2014-03-12 | 上海纳晶科技有限公司 | Visible light photocatalyst and preparation method therefor |
| CN105879890A (en) * | 2016-04-18 | 2016-08-24 | 长沙学院 | Magnetic composite photocatalyst as well as preparation method and application thereof |
| CN106925308A (en) * | 2017-04-06 | 2017-07-07 | 太原理工大学 | A kind of surface plasma nano catalysis material and its preparation method and application |
| CN107051556A (en) * | 2017-04-20 | 2017-08-18 | 合肥学院 | A kind of liquid phase in-situ reducing prepares Ag/Ag3PO4The method of composite photocatalyst powder |
-
2017
- 2017-09-29 CN CN201710908271.0A patent/CN107744821A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103623803A (en) * | 2012-08-30 | 2014-03-12 | 上海纳晶科技有限公司 | Visible light photocatalyst and preparation method therefor |
| CN103007973A (en) * | 2012-12-14 | 2013-04-03 | 陕西科技大学 | Silver/silver phosphate composite material and preparation method thereof |
| CN105879890A (en) * | 2016-04-18 | 2016-08-24 | 长沙学院 | Magnetic composite photocatalyst as well as preparation method and application thereof |
| CN106925308A (en) * | 2017-04-06 | 2017-07-07 | 太原理工大学 | A kind of surface plasma nano catalysis material and its preparation method and application |
| CN107051556A (en) * | 2017-04-20 | 2017-08-18 | 合肥学院 | A kind of liquid phase in-situ reducing prepares Ag/Ag3PO4The method of composite photocatalyst powder |
Non-Patent Citations (2)
| Title |
|---|
| 余锐等，: ""四足状Ag/Ag3PO4异质结构作为高效、稳定的可见光等离子体光催化剂"", 《池州学院学报》 * |
| 夏阁遥等，: ""磁性Fe3O4/Ag3PO4复合光催化剂催化降解染料废水中的孔雀石绿"", 《环境工程学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108704653A (en) * | 2018-06-14 | 2018-10-26 | 浙江理工大学 | It is a kind of to have magnetic silver phosphate composite photocatalyst and its preparation method and application |
| CN110836919A (en) * | 2019-11-29 | 2020-02-25 | 金陵科技学院 | Chiral recognition material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Qu et al. | Visible-light-responsive K-doped g-C3N4/BiOBr hybrid photocatalyst with highly efficient degradation of Rhodamine B and tetracycline | |
| CN102580742B (en) | Activated carbon-loaded cuprous oxide photocatalyst and preparation method thereof | |
| CN101816943B (en) | High-efficiency nano silver/silver bromide sunshine photocatalytic material and preparation method thereof | |
| Li et al. | New insight into the mechanism of enhanced photo-Fenton reaction efficiency for Fe-doped semiconductors: a case study of Fe/g-C3N4 | |
| CN107456991A (en) | A kind of g C3N4Quantum dot loads the preparation method of Bismuth tungstate nano-sheet photochemical catalyst | |
| Wei et al. | Preparation, characterization and visible-light-driven photocatalytic activity of a novel Fe (III) porphyrin-sensitized TiO2 nanotube photocatalyst | |
| Zhu et al. | Synthesis of novel ternary photocatalyst Ag3PO4/Bi2WO6/multi-walled carbon nanotubes and its enhanced visible-light photoactivity for photodegradation of norfloxacin | |
| CN109675607A (en) | Fe3O4The preparation method of@ZnO@N-C composite photocatalyst material | |
| CN107020142A (en) | The preparation method of foamed nickel supported carbon nitrogen/reduced graphene photochemical catalyst | |
| CN106984312B (en) | A kind of composite photocatalyst and preparation method thereof | |
| Huang et al. | Construction of a novel Z-scheme V2O5/NH2-MIL-101 (Fe) composite photocatalyst with enhanced photocatalytic degradation of tetracycline | |
| CN106563477A (en) | Ternary composite visible light photocatalyst, preparation method and application thereof | |
| CN110560092A (en) | MoS2/BiVO4Preparation method and application of heterojunction composite photocatalyst | |
| CN107935103A (en) | A kind for the treatment of process of silver-based composite photocatalyst for degrading dyeing waste water | |
| Peng et al. | Carbon quantum dots decorated heteroatom co-doped core-shell Fe0@ POCN for degradation of tetracycline via multiply synergistic mechanisms | |
| Sheydaei et al. | A visible-light active g-C3N4/Ce–ZnO/Ti nanocomposite for efficient photoelectrocatalytic pharmaceutical degradation: Modelling with artificial neural network | |
| CN109529892A (en) | A kind of nano strip MOA composite photo-catalyst preparation method | |
| CN102671674A (en) | Magnetically supported silver bromide photochemical catalysis material and preparation method thereof | |
| CN106824070A (en) | A kind of two tungsten selenide nitrogen-doped graphene photocatalysis sorbing materials and preparation method thereof | |
| CN107224982A (en) | Cu/Pd alloys for reduction dechlorination material modify TiO2The preparation method of catalyst | |
| CN107744821A (en) | A kind of magnetic photocatalyst with SPR responses and preparation method thereof | |
| CN104492464B (en) | Preparation method of silver iodide/beta type bismuth oxide composite material | |
| CN106111179B (en) | A kind of small size nitrogen-doped graphene photochemical catalyst and its preparation method and application | |
| Song et al. | A novel nitrogenous core-shell MIL-101 (Fe)-based nanocomposite for enhanced adsorption and photo-degradation of organic pollutant under visible light | |
| CN108543542A (en) | A kind of preparation method and application of three-dimensional porous composite photo-catalyst |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180302 |