CN106040261B - A kind of preparation method and application of silver/di-iron trioxide xerogel catalyst - Google Patents
A kind of preparation method and application of silver/di-iron trioxide xerogel catalyst Download PDFInfo
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- CN106040261B CN106040261B CN201610523881.4A CN201610523881A CN106040261B CN 106040261 B CN106040261 B CN 106040261B CN 201610523881 A CN201610523881 A CN 201610523881A CN 106040261 B CN106040261 B CN 106040261B
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- silver
- iron trioxide
- xerogel
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- xerogel catalyst
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- 229910052709 silver Inorganic materials 0.000 title claims abstract description 53
- 239000004332 silver Substances 0.000 title claims abstract description 52
- 239000003054 catalyst Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 18
- PLIKAWJENQZMHA-UHFFFAOYSA-N 4-aminophenol Chemical compound NC1=CC=C(O)C=C1 PLIKAWJENQZMHA-UHFFFAOYSA-N 0.000 claims abstract description 16
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 claims abstract description 16
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 13
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 230000032683 aging Effects 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 239000011240 wet gel Substances 0.000 claims abstract description 9
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 8
- 238000013019 agitation Methods 0.000 claims abstract description 7
- 239000000499 gel Substances 0.000 claims abstract description 7
- 150000002823 nitrates Chemical class 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 58
- 239000011259 mixed solution Substances 0.000 claims description 34
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 13
- 229910052742 iron Inorganic materials 0.000 claims description 7
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 16
- 239000000126 substance Substances 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 238000006555 catalytic reaction Methods 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 239000012279 sodium borohydride Substances 0.000 abstract description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 abstract description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 230000035484 reaction time Effects 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 description 8
- 238000009826 distribution Methods 0.000 description 8
- 230000003197 catalytic effect Effects 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 238000000975 co-precipitation Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000001802 infusion Methods 0.000 description 3
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000005457 ice water Substances 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 235000017060 Arachis glabrata Nutrition 0.000 description 1
- 241001553178 Arachis glabrata Species 0.000 description 1
- 235000010777 Arachis hypogaea Nutrition 0.000 description 1
- 235000018262 Arachis monticola Nutrition 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000001754 anti-pyretic effect Effects 0.000 description 1
- 239000002221 antipyretic Substances 0.000 description 1
- 229940125716 antipyretic agent Drugs 0.000 description 1
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 235000020232 peanut Nutrition 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 150000003378 silver Chemical class 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Substances [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000000352 supercritical drying Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 231100001234 toxic pollutant Toxicity 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
-
- 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
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/02—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reactions involving the formation of amino groups from compounds containing hydroxy groups or etherified or esterified hydroxy groups
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to derived energy chemical fields, disclose a kind of preparation method and application of silver/di-iron trioxide xerogel catalyst；Specifically includes the following steps: nine water ferric nitrates are dissolved in dehydrated alcohol, it is thoroughly mixed uniformly；Silver nitrate is dissolved in deionized water, is stirred until homogeneous and is slowly added into above-mentioned iron nitrate solution dropwise, magnetic agitation reaction stops stirring after reacting 8 ~ 10h；It is slowly added to propylene oxide dropwise again, stirs 3 ~ 5min, become cloudy to colloidal sol, stop stirring, be placed in 40 DEG C of water-baths and wait gel；After obtained wet gel in air 10 ~ 12h of aging, vacuum drying；Calcining, obtains silver-colored/di-iron trioxide xerogel catalyst.The method simple process, production cost is low, low for equipment requirements, and synthesis process is completely pollution-free, environmental-friendly, is suitable for industrial production.The available reduction paranitrophenol of catalysis at room temperature of the catalyst prepares p-aminophenol, and with water as solvent, sodium borohydride makees hydrogen source, and catalyst amount is few, and the reaction time is short, high conversion rate.
Description
Technical field
The present invention relates to a kind of silver/di-iron trioxide xerogel catalyst preparation method and applications, belong to derived energy chemical
Field.
Background technique
Nano silver grain can have with chemical activity in fields such as electronics, chemical industry, biology and pharmacy due to its high surface
It is widely applied, but simple substance Nano silver grain preparation cost is high, because having biggish specific surface area, holds under van der Waals interaction
It is easy to reunite, its catalytic activity is influenced, in addition easy-sintering leads to catalyst inactivation under high temperature, to reduce answering for silver nano-grain
With value and application range.Therefore need to find it is a kind of it is cheap, preparation is simple, stability is good, load with some strength
Body is of great significance for the application of argentum-based catalyzer.
Carrier and preparation method can all influence the distribution of the dispersion degree, active site of silver particles, to influence catalytic activity.
Compared with traditional silica, alumina support, di-iron trioxide is not only cheap to be easy to get, and itself is as a kind of reducible
Oxide is with more the potentiality as catalyst carrier.The method for commonly preparing argentum-based catalyzer has infusion process and co-precipitation
Method, process is tedious for infusion process, operating condition is harsh, and the particle size distribution range of coprecipitation preparation is big.
One important application of argentum-based catalyzer is that catalysis paranitrophenol prepares p-aminophenol, and paranitrophenol is a kind of common
Not biodegradable toxic pollutant, and p-aminophenol is a kind of important industrial chemicals and medicine intermediate, can be extensive
For synthesizing the fields such as Antipyretics, rubber chemicals, developer, feed, dyestuff, lubricating oil antiager.With to amino
The increase of phenol demand prepares p-aminophenol because it is efficient, environmental protection becomes main synthesis using the direct catalytic hydrogenation of paranitrophenol
Route.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method and application of di-iron trioxide carried silver catalyst, using ring
Ethylene Oxide synthesis, calcining two-step method preparation silver/di-iron trioxide xerogel catalyst in silver granuel diameter is smaller, size distribution is equal
It is even, add hydrogen to prepare p-aminophenol with the xerogel catalyst paranitrophenol, have process flow is simple, catalytic activity is high,
The good advantage of stability.
The present invention provides this silver/di-iron trioxide xerogel catalyst preparation methods, specifically includes the following steps:
(1) at room temperature, nine water ferric nitrates are added in dehydrated alcohol in proportion, are thoroughly mixed and are uniformly mixed
Close solution A；
(2) silver nitrate is add to deionized water in proportion, is stirred until homogeneous, obtain mixed solution B；
(3) the mixed solution B in step (2) is slowly added into dropwise in the mixed solution A of step (1), magnetic agitation
After 8 ~ 10h of lower reaction, stops stirring, obtain mixed solution C；It is slowly added to propylene oxide dropwise into mixed solution C again, stirs
3 ~ 5min becomes cloudy to colloidal sol, stops stirring, is placed in 40 ~ 50 DEG C of water-baths and waits gel, obtain wet gel；
(4) wet gel for obtaining step (3) is in air after aging, vacuum drying, calcines, can be prepared by air
Silver/di-iron trioxide xerogel catalyst.
In step (1), the mass ratio of the nine water ferric nitrate and dehydrated alcohol is 0.288 ~ 0.422；
In step (2), the volume ratio of the dehydrated alcohol in the deionized water and step (1) is 3:9 ~ 20, the nitric acid
The amount of silver is calculated according to mass fraction 1 ~ 10% silver-colored in product silver/di-iron trioxide xerogel；
In step (3), the volume ratio of dehydrated alcohol is 1:3 ~ 10 in the propylene oxide and step (1)；
In step (4), the ageing time is 10-12h；The vacuum drying temperature is 40 ~ 60 DEG C, and drying time is
24h。
In step (4), the temperature of the calcining is 600 ~ 800 DEG C, and the time of calcining is 4 ~ 6h.
Further, another object of the present invention is to provide the silver/di-iron trioxide xerogel nano materials to use
P-aminophenol (PAP) is prepared in catalysis paranitrophenol (PNP), the specific steps are as follows:
(1) the paranitrophenol 50mL for preparing 0.1mM at room temperature is spare in volumetric flask；
(2) the sodium borohydride solution 25mL of 0.25M is prepared in ice-water bath and is stored in spare in ice-water bath；
(3) measure step (1) in paranitrophenol 20mL be added in the beaker of 50mL, speed of agitator be maintained at 100 turns/
Minute；
(4) it measures freshly prepared sodium borohydride solution 1mL in step (2) to be added in above-mentioned three-necked flask, stirs 10s
The sample for taking out 3mL afterwards does ultraviolet test；
(5) homemade silver/silicon dioxide spheric catalyst is added in above-mentioned solution, it is constant in mechanical stirring revolving speed
In the case of every 10s take a sample, with ultraviolet specrophotometer survey paranitrophenol conversion situation, sample is refunded after test
It states in beaker；
(6) catalyst is recycled after the reaction was completed, is washed repeatedly, it is dry, it is used when in case being catalyzed again.
Compared to the prior art, advantage is as follows by the present invention:
(1) silver-colored simple substance due to high specific surface energy, high activity it is easy to reunite, oxidizable, affect catalytic efficiency, silver loaded
On cheap di-iron trioxide carrier, the dispersibility of silver is enhanced, agglomeration is avoided.
(2) compared with common infusion process, coprecipitation, on the one hand the propylene oxide method of use keeps silver metal element direct
In conjunction with carrier, the interaction between silver and carrier is enhanced, anti-caking power is improved, on the other hand enhances silver particles
Dispersion degree reduces the partial size of silver particles, increases the specific surface of catalyst, increases catalyst and nitro contact surface, catalysis
Efficiency enhancing.
(3) compared with supercritical drying, vacuum drying not only reduces cost, but also avoids the risk of experimentation.
(4) the method simple process, low for equipment requirements, synthesis process is completely pollution-free, environmental-friendly, and it is raw to be suitable for industry
It produces.
(5) catalytic reaction condition is mild, and catalyst stability is good, since the carrier effect catalytic activity of di-iron trioxide is bright
Aobvious to improve, the selectivity of catalyst is good, and catalyst is recyclable to be recycled, long service life.
Detailed description of the invention
Fig. 1 is silver/di-iron trioxide xerogel catalyst X-ray diffraction pattern that the embodiment of the present invention 1 obtains；
Fig. 2 is the resulting silver of embodiment 1/di-iron trioxide xerogel catalyst nitrogen adsorption-desorption curve a and aperture
Distribution map b；
Fig. 3 is the resulting silver of embodiment 1/di-iron trioxide xerogel catalyst scanning electron microscope (SEM) photograph a, energy spectrum diagram b；
Fig. 4 is the resulting silver of embodiment 1/di-iron trioxide xerogel catalyst transmission electron microscope picture a and high-resolution transmits
Electron microscope b；
Fig. 5 is nano silver grain size distribution in the resulting silver of embodiment 1/di-iron trioxide xerogel catalyst；
Fig. 6 is the resulting silver of embodiment 1/UV absorption of the di-iron trioxide xerogel catalyst when being catalyzed paranitrophenol
Spectrogram；
Fig. 7 is the resulting silver of embodiment 1/circulation figure of the di-iron trioxide xerogel catalyst when being catalyzed paranitrophenol.
Specific embodiment
The present invention is further explained in the light of specific embodiments.
Embodiment 1:
(1) at room temperature, the nine water ferric nitrates for weighing 4.8071g are added in 15mL dehydrated alcohol, are thoroughly mixed
Uniformly obtain mixed solution A；
(2) it weighs 78.7mg silver nitrate to be added in the deionized water of 3mL, is stirred until homogeneous to obtain mixed solution B；
(3) mixed solution B is slowly added into mixed solution A dropwise, with magnetic agitation reaction revolving speed be 1500 turns/
Minute, stop stirring to get mixed solution C after reacting 10h；
(4) propylene oxide for measuring 3mL is slowly added into mixed solution C dropwise, is stirred 3min, is become cloudy to colloidal sol,
Stop stirring, is placed in 40 DEG C of water-baths and waits gel；
(5) by wet gel that step (4) obtains in air aging 12h be placed in 40 DEG C of vacuum ovens it is dry for 24 hours；
(6) blocks of solid that step (5) obtains be can be prepared by into silver/tri- oxidations two after 600 DEG C of calcining 6h in air
Iron xerogel catalyst.
Fig. 1 is resulting silver/di-iron trioxide xerogel catalyst X-ray diffraction pattern, from figure line it can be observed that 2θ=38.26 °, 44.47 °, 77.74 ° of corresponding crystal faces are (111), (200), the metallic silver simple substance of the face-centred cubic structure of (311),
2θ=35.68 °, 40.92 °, 49.53 °, 54.14 °, 57.66 °, 62.53 °, 64.09 °, 72.37 ° of corresponding crystal faces
For (110), (113), (024), (116), (018), (214), (200), (300) and (119) are three oxidations two
Iron crystal phase shows that silver ion is successfully reduced into silver-colored simple substance and is supported on di-iron trioxide.
Fig. 2 is resulting silver/di-iron trioxide xerogel catalyst nitrogen adsorption-desorption curve a and graph of pore diameter distribution
B, the specific surface area of the sample are 29.423m2/ g, pore volume are 0.249 cm3/ g, pore-size distribution is between 0 ~ 8nm, average hole
Diameter is 3.026nm.
Fig. 3 is resulting silver/di-iron trioxide xerogel catalyst scanning electron microscope (SEM) photograph a and energy spectrum diagram b, can be with from Fig. 3 (a)
Di-iron trioxide carrier is found out in a length of 90nm, and wide 30nm peanut shape is of uniform size；From Fig. 3 (b) it can be seen that sample only by
Tri- kinds of elements of Ag, O and Fe are constituted, and show that sample is not incorporated into impurity element.
Fig. 4 is resulting silver/di-iron trioxide xerogel catalyst transmission electron microscope picture a and high-resolution-ration transmission electric-lens figure b,
It can be clearly seen that spherical silver nanoparticles (black dot) are evenly distributed in carrier surface from Fig. 4 (a), overcome silver
Agglomeration；It is 0.235nm, the silver of corresponding crystal face (111) according to the available spacing of lattice of Fig. 4 (b).
Fig. 5 is nano silver grain size distribution in resulting silver/di-iron trioxide xerogel catalyst, can from Fig. 5
Silver granuel diameter is distributed in 3 ~ 11nm, average grain diameter 6.04nm out.
Fig. 6 is UV absorption spectrogram of the resulting silver/di-iron trioxide xerogel catalyst when being catalyzed paranitrophenol, from
After Fig. 6 is observed that addition catalyst, wavelength corresponding nitro absorption peak at 400nm is more and more weaker, while at 300nm
There is the absorption peak of amino and gradually increase, after 130s, nitro is fully converted to amino.
Fig. 7 is cyclic curve figure of the resulting silver/di-iron trioxide xerogel catalyst in catalysis paranitrophenol, from Fig. 7
As can be seen that the conversion ratio of paranitrophenol still exists after using five times silver/di-iron trioxide xerogel catalyst circulation of preparation
85% or more.
Embodiment 2:
(1) at room temperature, the nine water ferric nitrates for weighing 4.9588g are added in 15mL dehydrated alcohol, are thoroughly mixed
Uniformly obtain mixed solution A；
(2) it weighs 31.5mg silver nitrate to be added in the deionized water of 3mL, is stirred until homogeneous to obtain mixed solution B；
(3) mixed solution B is slowly added into mixed solution A dropwise, stops stirring after 8h is reacted under magnetic agitation, obtains
To mixed solution C；
(4) propylene oxide for measuring 4mL is slowly added into mixed solution C dropwise, is stirred 5min, is become cloudy to colloidal sol,
Stop stirring, is placed in 50 DEG C of water-baths and waits gel；
(5) by wet gel that step (4) obtains in air aging 12h be placed in 60 DEG C of vacuum ovens it is dry for 24 hours；
(6) blocks of solid that step (5) obtains be can be prepared by into silver/tri- oxidations two after 600 DEG C of calcining 6h in air
Iron xerogel catalyst.
Embodiment 3:
(1) at room temperature, the nine water ferric nitrates for weighing 4.554g are added in 15mL dehydrated alcohol, are thoroughly mixed
It is even to obtain mixed solution A；
(2) it weighs 157.5mg silver nitrate to be added in the deionized water of 5mL, is stirred until homogeneous to obtain mixed solution B；
(3) mixed solution B is slowly added into mixed solution A dropwise, stops stirring after 10h is reacted under magnetic agitation,
Obtain mixed solution C；
(4) propylene oxide for measuring 2mL is slowly added into mixed solution C dropwise, is stirred 5min, is become cloudy to colloidal sol,
Stop stirring, is placed in 50 DEG C of water-baths and waits gel；
(5) by wet gel that step (4) obtains in air aging 10h be placed in 40 DEG C of vacuum ovens it is dry for 24 hours；
(6) blocks of solid that step (5) obtains be can be prepared by into silver/tri- oxidations two after 800 DEG C of calcining 4h in air
Iron xerogel catalyst.
Embodiment 4:
(1) at room temperature, the nine water ferric nitrates for weighing 5g are added in 20mL dehydrated alcohol, are thoroughly mixed uniform obtain
To mixed solution A；
(2) it weighs 15.75mg silver nitrate to be added in the deionized water of 35mL, is stirred until homogeneous to obtain mixed solution B；
(3) mixed solution B is slowly added into mixed solution A dropwise, stops stirring after 8h is reacted under magnetic agitation, obtains
To mixed solution C；
(4) propylene oxide for measuring 5mL is slowly added into mixed solution C dropwise, is stirred 5min, is become cloudy to colloidal sol,
Stop stirring, is placed in 40 DEG C of water-baths and waits gel；
(5) by wet gel that step (4) obtains in air aging 12h be placed in 40 DEG C of vacuum ovens it is dry for 24 hours；
(6) blocks of solid that step (5) obtains be can be prepared by into silver/tri- oxidations two after 600 DEG C of calcining 4h in air
Iron xerogel catalyst.
Claims (7)
1. a kind of silver/di-iron trioxide xerogel catalyst preparation method, which comprises the steps of:
(1) at room temperature, nine water ferric nitrates are added in dehydrated alcohol in proportion, be thoroughly mixed uniformly obtain mixing it is molten
Liquid A；
(2) silver nitrate is add to deionized water in proportion, is stirred until homogeneous, obtain mixed solution B；
(3) the mixed solution B in step (2) is slowly added into dropwise in the mixed solution A of step (1), it is anti-under magnetic agitation
After answering 8 ~ 10h, stops stirring, obtain mixed solution C；It is slowly added to propylene oxide dropwise into mixed solution C again, stirring 3 ~
5min becomes cloudy to colloidal sol, stops stirring, is placed in 40-50 DEG C of water-bath and waits gel, obtain wet gel；
(4) it by after step (3) resulting wet gel in air aging, is dried in vacuo, is calcined in air, can be prepared by silver/tri-
Aoxidize two iron xerogel catalyst.
2. a kind of silver according to claim 1/di-iron trioxide xerogel catalyst preparation method, which is characterized in that
In step (1), the mass ratio of the nine water ferric nitrate and dehydrated alcohol is 0.288 ~ 0.422.
3. a kind of silver according to claim 1/di-iron trioxide xerogel catalyst preparation method, which is characterized in that
In step (2), the volume ratio of the dehydrated alcohol in the deionized water and step (1) is 3:9 ~ 20；The amount root of the silver nitrate
According to mass fraction 1 ~ 10% silver-colored in product silver/di-iron trioxide xerogel.
4. a kind of silver according to claim 1/di-iron trioxide xerogel catalyst preparation method, which is characterized in that
In step (3), the volume ratio of dehydrated alcohol is 1:3 ~ 10 in the propylene oxide and step (1).
5. a kind of silver according to claim 1/di-iron trioxide xerogel catalyst preparation method, which is characterized in that
In step (4), the ageing time is 10-12h；Vacuum drying temperature is 40 ~ 60 DEG C, and drying time is for 24 hours.
6. a kind of silver according to claim 1/di-iron trioxide xerogel catalyst preparation method, which is characterized in that
In step (4), the temperature of the calcining is 600 ~ 800 DEG C, and the time of calcining is 4 ~ 6h.
7. silver/di-iron trioxide xerogel catalyst application made from any one preparation method according to claim 1 ~ 6,
It is characterized in that, being used to be catalyzed paranitrophenol for the silver/di-iron trioxide xerogel catalyst prepares p-aminophenol.
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| Catalytic performance of Ag/Fe2O3 for the low temperature oxidation of carbon monoxide;Abolfazl Biabani-Ravandi，et.al.;《Chemical Engineering Journal》;20130111;第219卷;第125页第2.1节，第3节，图1 |
| Characterization of the Sol-Gel Formation of Iron(III) Oxide/Hydroxide Nanonetworks from Weak Base Molecules;Jeremy D. Walker,et.al.;《Chem. Mater.》;20061231;第18卷(第20期);第4794页右栏Experimental Section，第4793页右栏 |
| Hydrogen production by steam reforming of liquefied natural gas (LNG) over mesoporous Ni-Al2O3 aerogel catalyst prepared by a single-step epoxide-driven sol-gel method;Yongju Bang，et. al.;《International Journal of Hydrogen Energy》;20111103;第37卷;第1437页左栏第3段-右栏第1段，图1，第1437页第2.1节，第1441页3.6节、3.7节，第1442页第4节 |
| One-pot green synthesis of silver/iron oxide composite nanoparticles for 4-nitrophenol reduction;Jau-Rung Chiou，et.al.;《Journal of Hazardous Materials》;20130124;第248-249卷;摘要、第397页第3.2节 |
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