CN106268860B - 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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- CN106268860B CN106268860B CN201610685141.0A CN201610685141A CN106268860B CN 106268860 B CN106268860 B CN 106268860B CN 201610685141 A CN201610685141 A CN 201610685141A CN 106268860 B CN106268860 B CN 106268860B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000010931 gold Substances 0.000 claims abstract description 73
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 16
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 16
- 239000003381 stabilizer Substances 0.000 claims abstract description 13
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 229920000642 polymer Polymers 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 20
- 239000011943 nanocatalyst Substances 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 15
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 15
- 239000002699 waste material Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 9
- 239000004202 carbamide Substances 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
- 239000005906 Imidacloprid Substances 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 7
- 229910052737 gold Inorganic materials 0.000 claims description 7
- YWTYJOPNNQFBPC-UHFFFAOYSA-N imidacloprid Chemical compound [O-][N+](=O)\N=C1/NCCN1CC1=CC=C(Cl)N=C1 YWTYJOPNNQFBPC-UHFFFAOYSA-N 0.000 claims description 7
- 229940056881 imidacloprid Drugs 0.000 claims description 7
- 238000007605 air drying Methods 0.000 claims description 5
- 238000005485 electric heating Methods 0.000 claims description 5
- 239000011521 glass Substances 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
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 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
- 238000002156 mixing Methods 0.000 claims description 2
- 229910000510 noble metal Inorganic materials 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims 1
- 229940012189 methyl orange Drugs 0.000 claims 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims 1
- 230000006641 stabilisation Effects 0.000 claims 1
- 238000011105 stabilization Methods 0.000 claims 1
- 238000006731 degradation reaction Methods 0.000 abstract description 9
- 230000015556 catabolic process Effects 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 7
- 239000002105 nanoparticle Substances 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 4
- 238000001914 filtration Methods 0.000 abstract 1
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 abstract 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 230000005389 magnetism Effects 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000002122 magnetic nanoparticle Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002121 nanofiber Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- -1 Methyl Chemical group 0.000 description 1
- 206010040844 Skin exfoliation Diseases 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000005540 biological transmission 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
- 239000000975 dye Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 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
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000447 pesticide residue Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 230000008092 positive effect 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
- 238000000926 separation method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 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
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- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
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- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- 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
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- 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
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- 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
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- Chemical Kinetics & Catalysis (AREA)
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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 average grain diameter is 40 nanometers.The average mass fraction of Au is about 0.5%~1% in catalyst, and preparation method is hydro-thermal preparation Fe3O4, seal shady place and save backup.Using polymer such as polyvinylpyrrolidones as stabilizer, Au colloidal sol is made with reducing agent reduction gold chloride.By Fe3O4It is added in Au colloidal sol, Au/Fe is finally made in stirring, filtering, drying3O4Nano load catalyst.The catalyst of the method for the present invention preparation has very high catalytic activity in light degradation organic pollutant.
Description
Technical field
The present invention relates to nanocatalyst technical field more particularly to a kind of Au/Fe3O4Nano load catalyst and its system
Preparation Method and application.
Background technique
Au/Fe3O4Nano material combines Au nanoparticle and Fe due to it3O4Protrusion is excellent in terms of magnetic nano-particle two
Gesture is easily isolated, high conversion, stability and recuperability especially as one kind, is widely used in biological medicine in recent years
And chemical field, such as catalyst, pharmaceutical carrier, Separation of Proteins, heavy metal adsorption field.Wherein Au nanoparticle has height
Surface energy, being supported on carrier can effectively prevent to reunite, and improve the catalytic activity of catalyst；Magnetic nano-particle has
Large specific surface area, good modifiability and excellent magnetic property and be widely used in metal supported catalyst.
Early in the late nineteen eighties, Japanese Haruta M et al. discovery, when Au nano particle is supported on Fe2O3With
TiO2When equal metal oxide surfaces, Au nano particle shows good water-resistance and stability, also to CO under low-temperature condition
Oxidation performance goes out very high catalytic activity, and from that time, researcher both domestic and external starts to have opened up related nanogold as urging
The field of agent, load type gold catalyst therewith also just become the research emphasis of catalytic field.Wang Xiaohui etc. passes through electrostatic
Spin processes are prepared containing Fe3O4The TiO of nanoparticle2Nanofiber, then be embedded into Au nanoparticle using immersion reduction method
TiO2On nanofiber, preparing a kind of has compared with ferromagnetism (separate and reuse convenient for material) and well visible light-responded
The composite photocatalyst material of ability.As it can be seen that Au/Fe3O4Catalyst will play a great role in catalytic field.
Summary of the invention
It is an object of that present invention to provide a kind of Au/Fe with excellent catalytic performance3O4The preparation method of catalyst.
The technical solution adopted by the present invention is that：
Au/Fe of the invention3O4The carrier of nano load catalyst is Fe3O4, active component is noble metal Au, is averaged
Partial size is 40 nanometers, and the average mass fraction of Au is 0.5%~1.0% in catalyst.
Au/Fe of the invention3O4Specific step is as follows for the preparation method of nano load catalyst：
(1)Fe3O4Preparation
The amount of weighing FeCl3·6H2O, polyvinylpyrrolidone and urea are placed in container, are mixed with 1,2-PD, magnetic
Power stirs or ultrasonic resonance, adds in autoclave solution after 5min, is placed in electric heating Constant pressure drying case, 180~200
DEG C 10~20h of reaction, the solution after reaction is transferred in clean glass container, with magnet outside container adsorbed product, will
It is separated, and upper layer waste liquid is poured out, and with dehydrated alcohol, repeatedly magnetic washing scrapes, sealing is protected up to cleaning after natural air drying
It is stored in shady place, the Fe obtained3O4Nanocatalyst；
(2) preparation of Au colloidal sol
It is accurate to measure chlorauric acid solution, stabilizer and reducing agent are poured into container and mixed, gold nano colloidal sol is made；
(3)Au/Fe3O4The preparation of nanocatalyst
To Fe made from addition step (1) in step (2)3O4Nanocatalyst is placed in ultrasonic vibration reaction 30min, to Au
It is carried on nanometer Fe completely3O4Afterwards, it stands, with small magnet contactor bottom, pours out upper layer waste liquid, dehydrated alcohol carries out magnetic
For several times until upper layer waste liquid is transparent, Au/Fe is made in drying for cleaning3O4Catalyst.
In step (1), FeCl3·6H2O, polyvinylpyrrolidone, urea molar ratio be 1：2：2, solvent 1,2- third
Glycol.
In step (2), the reducing agent is sodium borohydride, potassium borohydride or lithium borohydride, preferably sodium borohydride.
In step (2), the stabilizer is polyvinylpyrrolidone, polyethylene glycol or polyvinyl alcohol, preferably poly- second
Alkene pyrrolidone.
In step (2), the chlorauric acid solution, stabilizer (molal weight is based on the repetitive unit of polymer) and reduction
The molar ratio of agent is 1:5:5.
In step (3), aurosol accounts for Fe3O4The mass percent of nanocatalyst is 0.6%~1.1%.
Au/Fe of the invention3O4Nano load catalyst can be used for photocatalysis field.
Au/Fe of the invention3O4Nano load catalyst can be used for dyestuff or pesticide residue degradation aspect.
The positive effect of the present invention is as follows：
On in terms of photocatalysis, Au/Fe of the invention3O4Nano load catalyst is compared to single Fe3O4Degradation, tool
The advantages of having good degrading effect and being easily recycled.
Detailed description of the invention
Fig. 1 is Au/Fe prepared by embodiment 13O4Transmission electron microscope photo；
Fig. 2 is Au/Fe prepared by embodiment 13O4XRD diagram；
Fig. 3 is Au/Fe prepared by embodiment 13O4Hysteresis loop figure.
Specific embodiment
The following examples are a further detailed description of the invention.
Embodiment 1
(1)Fe3O4Preparation
Accurately weigh 0.8mmol FeCl3·6H2O, 0.1677g polyvinylpyrrolidone (PVP) and 1.68mmol urea
It is placed in clean small beaker, adds the 1,2-PD mixing of 8mL, be put into stirrer, stirred on magnetic stirring apparatus, it can
With ultrasonic resonance a few minutes, until obtaining clear solution.Then clear solution is poured into autoclave and screws reaction
Kettle ensures no gas leakage, is put into electric heating Constant pressure drying case, when being warming up to 195 DEG C of beginning timing, reacts 16h.After reaction,
Reaction kettle is taken out, the solution in it is transferred in clean small reaction flask, utilizes Fe3O4The magnetism of nanosphere product, so
One piece of magnet adsorbed product outside beaker can be used, be separated, pour out upper layer waste liquid, washed with the multiple magnetism of dehydrated alcohol
Wash until clean, the sample after cleaning pour into inside surface plate scraped after natural air drying be put into clean vial be sealed in
Shady place, even if the Fe obtained by us3O4Nanocatalyst.
(2) preparation of gold nano colloidal sol
It is accurate to measure the 8.5 × 10 of 3.75mL-3The HAuCl of mol/L4, accurately weigh 17.69 mg PVP, 6.03mg
NaBH4It pours into small beaker and mixes, gold nano colloidal sol is made.
(3)Au/Fe3O4The preparation of nanocatalyst
To addition 8mg Fe in (2)3O4Small beaker is placed in ultrasonic vibration reaction 5min, to which there is no small by nanocatalyst
It is fully reacting that bubble, which generates, to ensure 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 layer waste liquid, then carry out magnetic wash number with dehydrated alcohol
It is secondary, until being poured out after upper layer waste liquid is transparent, the substance of beaker bottom Au/Fe obtained required for being exactly3O4Catalyst.
Fig. 1 is Au/Fe prepared by embodiment 13O4Transmission electron microscope photo；Known by transmission electron microscope picture, catalyst is in particle
Microspheroidal, Average Particle Diameters are about in 30~50nm or so.
Fig. 2 is Au/Fe prepared by embodiment 13O4XRD diagram；It is learnt by XRD：Au 2 θ be 38.84 °, 43.38 °,
74.44 ° of diffraction maximum, illustrates Au/Fe3O4Catalyst is successfully prepared；Its hysteresis loop figure knows, Fe3O4、Au/Fe3O4After recycling
Au/Fe3O4Saturated magnetization rate be respectively 85.39emug-1, 44.91emug-1And 61.22emug-1, so as to
Find out Fe3O4Magnetism die down after load Au, may due to load Au after Fe3O4Concentration in a disguised form reduce so as to cause
The magnetic Au/Fe for dying down, however recycling below3O4It is magnetic become strong again, probably due to peelings of Au leads to the increasing of magnetism
By force.
Fig. 3 is Au/Fe prepared by embodiment 13O4Hysteresis loop figure.30 mgg are learnt through experiment-1Methyl orange
(MO) in Au/Fe3O4Under effect, sunlight irradiation 30min after almost degrade, recycle 6 times, degradation rate maintain 95% with
On.In addition, the catalyst has certain degradation effect to imidacloprid (IMI), single Au is to the degradation of IMI almost without effect
Fruit, although single Fe3O4There is certain degradation effect to IMI, but there is no Au/Fe3O4Degradation effect is obvious；Experiment know Au with
The molar ratio of PVP is 1：5, C0=0.00005mol/L, Au/Fe3O4Amount when being 0.7g/L, after high voltage mercury lamp radiation 90min
To imidacloprid (IMI) degradation rate up to 92%.
Embodiment 2
(1)Fe3O4Preparation
The amount of weighing FeCl3·6H2O, polyvinylpyrrolidone and urea are placed in container, are mixed with 1,2-PD, magnetic force
Solution is added in autoclave after 5min, is placed in electric heating Constant pressure drying case by stirring or ultrasonic resonance, is reacted at 180 DEG C
Solution after reaction is transferred in clean glass container by 20h, with magnet outside container adsorbed product, separated,
Upper layer waste liquid is poured out, with the multiple magnetic washing of dehydrated alcohol until cleaning, scrapes, is sealed in shady place after natural air drying,
The Fe obtained3O4Nanocatalyst；
(2) preparation of Au colloidal sol
It is accurate to measure chlorauric acid solution, stabilizer and reducing agent are poured into container and mixed, gold nano colloidal sol is made；
(3)Au/Fe3O4The preparation of nanocatalyst
To Fe made from addition step (1) in step (2)3O4Nanocatalyst is placed in ultrasonic vibration reaction 30min, to Au
It is carried on nanometer Fe completely3O4Afterwards, it stands, with small magnet contactor bottom, pours out upper layer waste liquid, dehydrated alcohol carries out magnetic
For several times until upper layer waste liquid is transparent, Au/Fe is made in drying for cleaning3O4Catalyst.
In step (1), FeCl3·6H2O, polyvinylpyrrolidone, urea molar ratio be 1：2：2, solvent 1,2- third
Glycol.
In step (2), the reducing agent is potassium borohydride.
In step (2), the stabilizer is polyethylene glycol.
In step (2), the chlorauric acid solution, the molar ratio by stabilizer and reducing agent is 1:5:5.
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 urea are placed in container, are mixed with 1,2-PD, magnetic
Power stirs or ultrasonic resonance, adds in autoclave solution after 5min, is placed in electric heating Constant pressure drying case, anti-at 200 DEG C
Answer 10h, the solution after reaction be transferred in clean glass container, with magnet outside container adsorbed product, divided
From, upper layer waste liquid is poured out, it is with the multiple magnetic washing of dehydrated alcohol until clean, it scrapes, is sealed in darkness after natural air drying
Place, obtains Fe3O4Nanocatalyst；
(2) preparation of Au colloidal sol
It is accurate to measure chlorauric acid solution, stabilizer and reducing agent are poured into container and mixed, gold nano colloidal sol is made；
(3)Au/Fe3O4The preparation of nanocatalyst
To Fe made from addition step (1) in step (2)3O4Nanocatalyst is placed in ultrasonic vibration reaction 30min, to Au
It is carried on nanometer Fe completely3O4Afterwards, it stands, with small magnet contactor bottom, pours out upper layer waste liquid, dehydrated alcohol carries out magnetic
For several times until upper layer waste liquid is transparent, Au/Fe is made in drying for cleaning3O4Catalyst.
In step (1), FeCl3·6H2O, polyvinylpyrrolidone, urea molar ratio be 1：2：2, solvent 1,2- third
Glycol.
In step (2), the reducing agent is lithium borohydride.
In step (2), the stabilizer is polyvinyl alcohol.
In step (2), the chlorauric acid solution, the molar ratio by stabilizer and reducing agent is 1:5:5.
In step (3), aurosol accounts for Fe3O4The Theoretical Mass percentage of nanocatalyst is 0.6%~1.2%.
Catalyst prepared by catalyst and embodiment 1 prepared by embodiment 2 and 3 has similar catalytic performance.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (1)
1. a kind of Au/Fe3O4Application of the nano load catalyst in visible light photocatalytic degradation methyl orange or imidacloprid, feature
It is：The catalyst carrier is Fe3O4, active component is noble metal Au, and average grain diameter is 40 nanometers, Au in catalyst
Average mass fraction is 0.5%~1.0%；The Au/Fe3O4The specific steps of the preparation method of nano load catalyst are such as
Under：
(1)Fe3O4Preparation
The amount of weighing FeCl3·6H2O, polyvinylpyrrolidone and urea are placed in container, and the mixing of solvent 1,2-PD, magnetic is added
Power stirs or ultrasonic resonance, adds in autoclave solution after 5min, is placed in electric heating Constant pressure drying case, 180~200
DEG C 10~20h of reaction, the solution after reaction is transferred in clean glass container, with magnet outside container adsorbed product, will
It is separated, and upper layer waste liquid is poured out, and with dehydrated alcohol, repeatedly magnetic washing scrapes, sealing is protected up to cleaning after natural air drying
It is stored in shady place, the Fe obtained3O4Nanocatalyst；
FeCl3·6H2O, the molar ratio 1 of polyvinylpyrrolidone, urea:2:2, wherein：The polyvinylpyrrolidone mole matter
Amount is based on the repetitive unit of polymer；
(2) preparation of Au colloidal sol
It is accurate to measure chlorauric acid solution, stabilizer and reducing agent are poured into container and mixed, gold nano colloidal sol is made；
The reducing agent is sodium borohydride, potassium borohydride or lithium borohydride；The stabilizer is polyvinylpyrrolidone, gathers
Ethylene glycol or polyvinyl alcohol；The molar ratio of the chlorauric acid solution, stabilizer and reducing agent is 1:5:5；Wherein：The stabilization
Agent molal weight is based on the repetitive unit of polymer；
(3)Au/Fe3O4The preparation of nanocatalyst
To Fe made from addition step (1) in step (2)3O4Nanocatalyst is placed in ultrasonic vibration reaction 30min, complete to Au
It is carried on nanometer Fe3O4Afterwards, it stands, with small magnet contactor bottom, pours out upper layer waste liquid, dehydrated alcohol carries out magnetic wash
It is dry for several times until upper layer waste liquid is transparent, Au/Fe is made3O4Catalyst.
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