CN106268860A - A kind of Au/Fe3o4nano load catalyst and its preparation method and application - Google Patents
A kind of Au/Fe3o4nano load catalyst and its preparation method and application Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000010931 gold Substances 0.000 claims abstract description 75
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 49
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 13
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 13
- 239000003381 stabilizer Substances 0.000 claims abstract description 13
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 5
- 229920000642 polymer Polymers 0.000 claims abstract description 4
- 239000011943 nanocatalyst Substances 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 19
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 15
- 239000002699 waste material Substances 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 10
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 9
- 239000004202 carbamide Substances 0.000 claims description 9
- 235000013877 carbamide Nutrition 0.000 claims description 9
- 229910052737 gold Inorganic materials 0.000 claims description 9
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 9
- SJUCACGNNJFHLB-UHFFFAOYSA-N O=C1N[ClH](=O)NC2=C1NC(=O)N2 Chemical compound O=C1N[ClH](=O)NC2=C1NC(=O)N2 SJUCACGNNJFHLB-UHFFFAOYSA-N 0.000 claims description 8
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000007605 air drying Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000005485 electric heating Methods 0.000 claims description 5
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 238000007790 scraping Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000012448 Lithium borohydride Substances 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 238000007146 photocatalysis Methods 0.000 claims description 3
- 230000001699 photocatalysis Effects 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 230000003252 repetitive effect Effects 0.000 claims description 3
- 239000000975 dye Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000447 pesticide residue Substances 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims 1
- 229920006316 polyvinylpyrrolidine Polymers 0.000 claims 1
- 229920002554 vinyl polymer Polymers 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 8
- 239000002105 nanoparticle Substances 0.000 abstract description 7
- 238000006731 degradation reaction Methods 0.000 abstract description 6
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 abstract 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 239000005906 Imidacloprid Substances 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- YWTYJOPNNQFBPC-UHFFFAOYSA-N imidacloprid Chemical compound [O-][N+](=O)\N=C1/NCCN1CC1=CC=C(Cl)N=C1 YWTYJOPNNQFBPC-UHFFFAOYSA-N 0.000 description 4
- 229940056881 imidacloprid Drugs 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000002122 magnetic nanoparticle Substances 0.000 description 2
- 239000002121 nanofiber Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- -1 Methyl Chemical group 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000004531 microgranule Substances 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000010792 warming Methods 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8906—Iron and noble metals
-
- B01J35/39—
-
- B01J35/393—
-
- 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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Abstract
The invention discloses a kind of Au/Fe3O4Nano load catalyst and its preparation method and application.Catalyst carrier is Fe3O4, active component is Au nanoparticle, and its mean diameter is 40 nanometers.In catalyst, the average mass fraction of Au is about 0.5%～1%, and preparation method is that hydro-thermal prepares Fe3O4, seal shady place and save backup.With polymer such as polyvinylpyrrolidones as stabilizer, prepare Au colloidal sol with reducing agent reduction gold chloride.By Fe3O4Join in Au colloidal sol, stir, filter, dry last prepared Au/Fe3O4Nano load catalyst.Catalyst prepared by the inventive method has the highest catalysis activity at light degradation organic pollution.
Description
Technical field
The present invention relates to nanocatalyst technical field, particularly relate to a kind of Au/Fe3O4Nano load catalyst and system thereof
Preparation Method and application.
Background technology
Au/Fe3O4Nano material combines Au nanoparticle and Fe due to it3O4Magnetic nano-particle two aspect highlights excellent
Gesture, is easily isolated especially as one, high conversion, stability and recuperability, is widely used in biological medicine in recent years
And chemical field, such as fields such as catalyst, pharmaceutical carrier, Separation of Proteins, heavy metal adsorptions.Wherein Au nanoparticle has height
Surface energy, is supported on carrier and can effectively be stoped reunion, improves the catalysis activity of catalyst；Magnetic nano-particle has
Specific surface area is big, good modifiability and the magnetic property of excellence and be widely used in metal supported catalyst.
As far back as the late nineteen eighties, Haruta M of Japan et al. finds, when Au nano-particle is supported on Fe2O3With
TiO2During Deng metal oxide surface, Au nano-particle shows good water-resistance and stability, also to CO under low temperature state
Oxidation performance goes out the highest catalysis activity, and from that time, research worker both domestic and external starts to have opened up relevant nanometer gold as urging
The field of agent, load type gold catalyst therewith the most just becomes the research emphasis of catalytic field.Wang Xiaohui etc. pass through electrostatic
Spin processes is prepared containing Fe3O4The TiO of nanoparticle2Nanofiber, then use immersion reduction method Au nanoparticle to be embedded into
TiO2On nanofiber, prepare one and there is relatively ferromagnetism (being easy to material separation and recycling) and the most visible light-responded
The composite photocatalyst material of ability.Visible, Au/Fe3O4Catalyst will be played a great role at catalytic field.
Summary of the invention
Present invention aim at providing a kind of Au/Fe with excellent catalytic performance3O4The preparation method of catalyst.
The present invention adopts the technical scheme that:
The Au/Fe of the present invention3O4The carrier of nano load catalyst is Fe3O4, active component is noble metal Au, and it is average
Particle diameter is 40 nanometers, and in catalyst, the average mass fraction of Au is 0.5%～1.0%.
The Au/Fe of the present invention3O4Specifically comprising the following steps that of the preparation method of nano load catalyst
(1)Fe3O4Preparation
The amount of weighing FeCl3·6H2O, polyvinylpyrrolidone and carbamide are placed in container, mix with 1,2-PD, magnetic force
Stirring or ultrasonic resonance, add in autoclave by solution after 5min, be placed in electric heating Constant pressure drying case, at 180～200 DEG C
Reaction 10～20h, is transferred to reacted solution in the glass container of cleaning, by Magnet adsorbed product from container, by it
Separate, pour out upper strata waste liquid, with the washing of dehydrated alcohol repeatedly magnetic until cleaning, scraping after natural air drying, sealing and preserving
In shady place, the Fe i.e. prepared3O4Nanocatalyst；
(2) preparation of Au colloidal sol
Accurately measure chlorauric acid solution, stabilizer and reducing agent are poured in container and mix, prepare gold nano colloidal sol；
(3)Au/Fe3O4The preparation of nanocatalyst
The Fe that step (1) prepares is added in step (2)3O4Nanocatalyst, is placed in ultrasonic vibration reaction 30min, treats Au
It is carried on nanometer Fe completely3O4After, standing, bottom small magnet contactor, pour out upper strata waste liquid, dehydrated alcohol carries out magnetic
Clean for several times until upper strata waste liquid is transparent, be dried, prepare Au/Fe3O4Catalyst.
In step (1), FeCl3·6H2O, polyvinylpyrrolidone, the mol ratio of carbamide are 1:2:2, and solvent is 1,2-third
Glycol.
In step (2), described reducing agent is sodium borohydride, potassium borohydride or lithium borohydride, preferably sodium borohydride.
In step (2), described stabilizer is polyvinylpyrrolidone, Polyethylene Glycol or polyvinyl alcohol, the most poly-second
Alkene pyrrolidone.
In step (2), described chlorauric acid solution, stabilizer (molal weight is based on the repetitive of polymer) and reduction
The mol ratio of agent is 1:5:5.
In step (3), aurosol accounts for Fe3O4The mass percent of nanocatalyst is 0.6%～1.1%.
The Au/Fe of the present invention3O4Nano load catalyst may be used for photocatalysis field.
The Au/Fe of the present invention3O4Nano load catalyst may be used for dyestuff or pesticide residue degraded aspect.
The positive effect of the present invention is as follows:
In photocatalysis aspect, the Au/Fe of the present invention3O4Nano load catalyst is compared to single Fe3O4Degraded, tool
There are good degrading effect and the advantage being easily recycled.
Accompanying drawing explanation
Fig. 1 is the Au/Fe of embodiment 1 preparation3O4Transmission electron microscope photo；
Fig. 2 is the Au/Fe of embodiment 1 preparation3O4XRD figure；
Fig. 3 is the Au/Fe of embodiment 1 preparation3O4Hysteresis curve figure.
Detailed description of the invention
The following examples are that the present invention is described in further detail.
Embodiment 1
(1)Fe3O4Preparation
Accurately weigh 0.8mmol FeCl3·6H2O, 0.1677g polyvinylpyrrolidone (PVP) and 1.68mmol carbamide are put
In clean small beaker, add the 1,2-PD mixing of 8mL, put into stirrer, magnetic stirring apparatus stirs, available
Ultrasonic resonance a few minutes, until obtaining clear solution.Then clear solution poured in autoclave and screw reactor
Guarantee not leak gas, put into electric heating Constant pressure drying case, start timing when being warming up to 195 DEG C, react 16h.After reaction terminates, take
Go out reactor, the solution that it is interior is transferred in the little reaction bulb of cleaning, utilizes Fe3O4The magnetic of Nano microsphere product, so can
By one piece of Magnet adsorbed product from beaker, to separate, to pour out upper strata waste liquid, wash by dehydrated alcohol repeatedly magnetic
Until cleaning, the sample after cleaning is poured into scrape after natural air drying inside surface plate to put into seal in clean vial and is stored in the moon
Dark place, even if we are obtained Fe3O4Nanocatalyst.
(2) preparation of gold nano colloidal sol
Accurately measure the 8.5 × 10 of 3.75mL-3The HAuCl of mol/L4, accurately weigh 17.69mg PVP, 6.03mg
NaBH4Pour in small beaker and mix, prepare gold nano colloidal sol.
(3)Au/Fe3O4The preparation of nanocatalyst
8mg Fe is added in (2)3O4Nanocatalyst, is placed in small beaker ultrasonic vibration reaction 5min, treats no longer to have little
Bubble produces i.e. reaction completely, to guarantee that Au is supported on nanometer Fe completely3O4On, due to nanometer Au/Fe3O4It is magnetic, takes out quiet
It is placed on small magnet, adsorbs beaker bottom with small magnet, pour out upper strata waste liquid, then carry out magnetic wash number with dehydrated alcohol
Secondary, until pouring out after upper strata waste liquid is transparent, the material of beaker bottom is exactly the required Au/Fe prepared3O4Catalyst.
Fig. 1 is the Au/Fe of embodiment 1 preparation3O4Transmission electron microscope photo；Known by transmission electron microscope picture, catalyst be microgranule in
Microspheroidal, its Average Particle Diameters is about 30～about 50nm.
Fig. 2 is the Au/Fe of embodiment 1 preparation3O4XRD figure；Learnt by XRD: Au 2 θ be 38.84 °, 43.38 °,
The diffraction maximum of 74.44 °, illustrates Au/Fe3O4Catalyst is successfully prepared；Its hysteresis curve figure is known, Fe3O4、Au/Fe3O4After reclaiming
Au/Fe3O4Saturated magnetization rate be respectively 85.39emu g-1, 44.91emu g-1With 61.22emu g-1, such that it is able to
Find out Fe3O4Magnetic die down after load Au, be likely to be due to load Fe after Au3O4Concentration in a disguised form reduce thus cause
Dying down of magnetic, but the Au/Fe reclaimed below3O4Magnetic become by force again, probably due to the peeling of Au causes the increasing of magnetic
By force.
Fig. 3 is the Au/Fe of embodiment 1 preparation3O4Hysteresis curve figure.30mg g is learnt through experiment-1Methyl orange (MO)
At Au/Fe3O4Under effect, the most degradable after sunlight 30min, circulate 6 times, degradation rate maintains more than 95%.Separately
Outward, this catalyst has certain degradation effect to imidacloprid (IMI), single Au to the degraded of IMI almost without effect, although
Single Fe3O4IMI is had certain degradation effect, but there is no Au/Fe3O4Degradation effect is obvious；Rubbing of Au with PVP is known in experiment
That ratio is at 1:5, C0=0.00005mol/L, Au/Fe3O4Amount when being 0.7g/L, after high voltage mercury lamp radiation 90min to pyrrole worm
Quinoline (IMI) degradation rate is up to 92%.
Embodiment 2
(1)Fe3O4Preparation
The amount of weighing FeCl3·6H2O, polyvinylpyrrolidone and carbamide are placed in container, mix with 1,2-PD, magnetic force
Stirring or ultrasonic resonance, add in autoclave by solution after 5min, be placed in electric heating Constant pressure drying case, 180 DEG C of reactions
20h, is transferred to reacted solution in the glass container of cleaning, by Magnet adsorbed product from container, separates,
Pour out upper strata waste liquid, with the washing of dehydrated alcohol repeatedly magnetic until cleaning, scraping after natural air drying, sealing and being stored in shady place,
The Fe i.e. prepared3O4Nanocatalyst；
(2) preparation of Au colloidal sol
Accurately measure chlorauric acid solution, stabilizer and reducing agent are poured in container and mix, prepare gold nano colloidal sol；
(3)Au/Fe3O4The preparation of nanocatalyst
The Fe that step (1) prepares is added in step (2)3O4Nanocatalyst, is placed in ultrasonic vibration reaction 30min, treats Au
It is carried on nanometer Fe completely3O4After, standing, bottom small magnet contactor, pour out upper strata waste liquid, dehydrated alcohol carries out magnetic
Clean for several times until upper strata waste liquid is transparent, be dried, prepare Au/Fe3O4Catalyst.
In step (1), FeCl3·6H2O, polyvinylpyrrolidone, the mol ratio of carbamide are 1:2:2, and solvent is 1,2-third
Glycol.
In step (2), described reducing agent is potassium borohydride.
In step (2), described stabilizer is Polyethylene Glycol.
In step (2), described chlorauric acid solution, is 1:5:5 by the mol ratio of stabilizer and reducing agent.
In step (3), aurosol accounts for Fe3O4The mass percent of nanocatalyst is 0.6%～1.1%.
Embodiment 3
(1)Fe3O4Preparation
The amount of weighing FeCl3·6H2O, polyvinylpyrrolidone and carbamide are placed in container, mix with 1,2-PD, magnetic force
Stirring or ultrasonic resonance, add in autoclave by solution after 5min, be placed in electric heating Constant pressure drying case, 200 DEG C of reactions
10h, is transferred to reacted solution in the glass container of cleaning, by Magnet adsorbed product from container, separates,
Pour out upper strata waste liquid, with the washing of dehydrated alcohol repeatedly magnetic until cleaning, scraping after natural air drying, sealing and being stored in shady place,
I.e. prepare Fe3O4Nanocatalyst；
(2) preparation of Au colloidal sol
Accurately measure chlorauric acid solution, stabilizer and reducing agent are poured in container and mix, prepare gold nano colloidal sol；
(3)Au/Fe3O4The preparation of nanocatalyst
The Fe that step (1) prepares is added in step (2)3O4Nanocatalyst, is placed in ultrasonic vibration reaction 30min, treats Au
It is carried on nanometer Fe completely3O4After, standing, bottom small magnet contactor, pour out upper strata waste liquid, dehydrated alcohol carries out magnetic
Clean for several times until upper strata waste liquid is transparent, be dried, prepare Au/Fe3O4Catalyst.
In step (1), FeCl3·6H2O, polyvinylpyrrolidone, the mol ratio of carbamide are 1:2:2, and solvent is 1,2-third
Glycol.
In step (2), described reducing agent is lithium borohydride.
In step (2), described stabilizer is polyvinyl alcohol.
In step (2), described chlorauric acid solution, is 1:5:5 by the mol ratio of stabilizer and reducing agent.
In step (3), aurosol accounts for Fe3O4The Theoretical Mass percentage ratio of nanocatalyst is 0.6%～1.2%.
The catalyst that embodiment 2 is prepared to embodiment 1 with the catalyst of 3 preparations has similar catalytic performance.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, permissible
Understand and these embodiments can be carried out multiple change without departing from the principles and spirit of the present invention, revise, replace
And modification, the scope of the present invention be defined by the appended.
Claims (8)
1. an Au/Fe3O4Nano load catalyst, it is characterised in that: described catalyst carrier is Fe3O4, active component is expensive
Metal Au, its mean diameter is 40 nanometers, and in catalyst, the average mass fraction of Au is 0.5%～1.0%.
2. prepare Au/Fe as claimed in claim 1 for one kind3O4The method of nano load catalyst, it is characterised in that: described side
Specifically comprising the following steps that of method
(1)Fe3O4Preparation
The amount of weighing FeCl3·6H2O, polyvinylpyrrolidone and carbamide are placed in container, add the mixing of solvent 1,2-PD, magnetic
Power stirring or ultrasonic resonance, add in autoclave by solution after 5min, be placed in electric heating Constant pressure drying case, 180～200
DEG C reaction 10～20h, is transferred to reacted solution in the glass container of cleaning, by Magnet adsorbed product from container, and general
It separates, and pours out upper strata waste liquid, with the washing of dehydrated alcohol repeatedly magnetic until cleaning, scraping after natural air drying, sealing and protecting
It is stored in shady place, the Fe i.e. prepared3O4Nanocatalyst；
(2) preparation of Au colloidal sol
Accurately measure chlorauric acid solution, stabilizer and reducing agent are poured in container and mix, prepare gold nano colloidal sol；
(3)Au/Fe3O4The preparation of nanocatalyst
The Fe that step (1) prepares is added in step (2)3O4Nanocatalyst, is placed in ultrasonic vibration reaction 30min, treats that Au is complete
It is carried on nanometer Fe3O4After, standing, bottom small magnet contactor, pour out upper strata waste liquid, dehydrated alcohol carries out magnetic wash
For several times until upper strata waste liquid is transparent, it is dried, prepares Au/Fe3O4Catalyst.
3. preparation method as claimed in claim 2, it is characterised in that: in step (1), FeCl3·6H2O, polyvinylpyrrolidine
Ketone (molal weight is based on the repetitive of polymer), mol ratio 1:2:2 of carbamide.
4. preparation method as claimed in claim 2, it is characterised in that: in step (2), described reducing agent be sodium borohydride,
Potassium borohydride or lithium borohydride.
5. preparation method as claimed in claim 2, it is characterised in that: in step (2), described stabilizer is polyvinyl pyrrole
Alkanone, Polyethylene Glycol or polyvinyl alcohol.
6. preparation method as claimed in claim 2, it is characterised in that: in step (2), described chlorauric acid solution, stabilizer
The mol ratio of (molal weight is based on the repetitive of polymer) and reducing agent is 1:5:5.
7. Au/Fe as claimed in claim 13O4Nano load catalyst is for the application of photocatalysis field.
8. Au/Fe as claimed in claim 13O4Nano load catalyst answering in terms of dyestuff or pesticide residue degraded
With.
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| CN111617777A (en) * | 2020-06-16 | 2020-09-04 | 云深(福建)环保科技有限公司 | Indoor visible light response catalyst, preparation method and application thereof |
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