CN105833878A - Preparation method of Fe2O3-CeO2 nano-composite catalyst - Google Patents
Preparation method of Fe2O3-CeO2 nano-composite catalyst Download PDFInfo
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
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Abstract
The invention discloses a preparation method of Fe2O3-CeO2 nano-composite catalyst. The method includes the following steps: (1) using ferric nitrate and cerous nitrate to prepare a metallic salt solution, adding a precipitant in a dropwise manner, adjusting the pH value, stirring the mixture for 3.5-4.5 hours, and performing aging for 12-18 hours; (2) performing centrifugal separation, and washing the product obtained after centrifuging the mixture and removing the solution; and (3) drying the product, and performing grinding, roasting, tabletting, crushing, and screening in order to obtain the product. The Fe2O3-CeO2 nano-composite catalyst prepared for the coprecipitation method has good conversion rate, selectivity and stability when the prepared catalyst catalyzes NO+CO disappearance. Moreover, the catalyst uses cheap iron doped metal, and does not add any surface active agent, so that the cost is reduced greatly. The catalyst is safe and non-toxic, has simple operation and short production time, and is beneficial to expand industrial production.
Description
Technical field
The present invention relates to the preparation method of a kind of nano-composite catalyst, particularly to a kind of Fe2O3-CeO2
The preparation method of nano-composite catalyst.
Background technology
The approach of NO and CO in removing vehicle exhaust has a lot, the most industrialized maximally efficient clean
The method changing these harmful gass is to use the catalyzed conversion of three-way catalyst.And due to three-way catalyst
Main active component is the noble metals such as Pt, Rh, Pd, although noble metal embodies and is preferably catalyzed activity,
But owing to it is expensive and the defect of antioxygen property difference, so in recent years, find a kind of cheap height and live
The catalyst of property is important topic.Some base metal can be hopeful to replace dilute because of its high activity shown
The noble metal lacked is as eliminating NO+CO catalyst, it has also become Many researchers perpetual object.
Ce and containing CeO2Material, because its outstanding storage oxygen release ability, is increasingly widely applied to vapour
Tail gas three-effect catalysis.The outer electronic structure of rare earth metal cerium is 4f15d16s2, have+4 to stablize with+3 two kinds
Valence state, and its standard electrode potential is low, easily realizes the mutual conversion of+3 and+4 valency ions, stores or release
Put oxygen.But pure CeO2Heat stability the highest and store oxygen and rely primarily on surface and carry out, easy-sintering during high temperature
Oxygen storage capacity is made to be greatly reduced.Therefore, in recent years, people are to CeO2Among adulterate some ions with expectation
Increasing its oxygen storage capacity, reason is to replace the brilliant position of Ce ion after the ion adulterated enters lattice, with solid
Solution and CeO2Coexist.
Coprecipitation is typically to be mixed by the material of different chemical composition, in mixed liquor under solution state
Add suitable precipitant and prepare presoma precipitate, then precipitate is dried or is calcined, thus make
Obtain corresponding powder granule.The advantage of coprecipitation is: one has that preparation technology is simple, low cost,
The advantage that preparation condition is easily controllable, synthesis cycle is short;Furthermore it is by the various chemical reactions in solution
Can directly obtain that granularity is little and the nano-powder material that is evenly distributed.
The information being disclosed in this background section is merely intended to increase the reason of the general background to the present invention
Solve, and be not construed as recognizing or imply in any form that this information structure is for this area general technology
Prior art well known to personnel.
Summary of the invention
It is an object of the invention to provide a kind of Fe2O3-CeO2The preparation method of nano-composite catalyst, from
And when obtaining a kind of catalysis NO+CO, there is higher selectivity, stability and conversion ratio.
For achieving the above object, the technical scheme that the present invention provides is as follows:
A kind of Fe2O3-CeO2The preparation method of nano-composite catalyst, comprises following operating procedure:
(1) take ferric nitrate and metal salt solution made by cerous nitrate, drip precipitant, regulate pH value, stir
Mix 3.5~4.5 hours, aging 12~18 hours;
(2) by rear gained material centrifugation aging in step (1), by gained after centrifugal segregation solution
Material washs, and washing to cleaning mixture is neutrality;
(3) gained material after washing in step (2) is dried, be ground the most successively, roasting,
Tabletting, broken, sieve and i.e. obtain product.
A kind of Fe2O3-CeO2The preparation method of nano-composite catalyst, its more detailed step is:
(1) taking ferric nitrate and cerous nitrate by the amount ratio of material is 1~4.5:2~10 to make metal salt solution,
Dropping precipitant, regulates pH value, and dropping limit, limit is stirred, and continues stirring 3.5~4.5 hours after dripping,
The most aging 12~18 hours, precipitate is had to occur;
(2) rear gained aging in step (1) is included sedimentary material centrifugation, remove centrifugal
After removing solution, gained material, i.e. taking precipitate wash, and washing to cleaning mixture is neutrality;
(3) gained precipitate after washing in step (2) is dried, obtain catalyst precursor, by institute
Catalyst precursor be ground successively, roasting, tabletting, broken, sieve and i.e. obtain product.
Preferably, in step (1), ferric nitrate and cerous nitrate make slaine by the amount of material than for 2:5
Solution.
Preferably, in step (1), dropping precipitant regulation pH value is 10.0.
Preferably, the precipitant described in step (1) is 1:1 ammonia.
Preferably, stirring 4 hours in step (1), aging 12~18 hours.
Preferably, the washing described in step (2) is first to use water to be washed 2~3 times by precipitate, then
Dehydrated alcohol is used to be washed 3~4 times by precipitate.
Preferably, the sintering temperature described in step (3) is 500 DEG C, and roasting time is 4 hours.
Preferably, the screening described in step (3) was 40~60 mesh sieves.
Preferably, the drying described in step (3) is to dry 12 hours at 80 DEG C for keeping temperature.
Compared with prior art, there is advantages that
The present invention is Fe prepared by coprecipitation2O3-CeO2Nano-composite catalyst, prepares gained catalyst
When being catalyzed NO+CO and disappearing, there is higher conversion ratio and selectivity, and excellent stability;Simultaneously
The present invention selects the most cheap Fe2O3 doping metal, does not adds any surfactant so that cost drops significantly
Low;Further safety non-toxic of the present invention, simple to operate, the production time is short, is of value to expansion industrialization
Produce.
Accompanying drawing explanation
Fig. 1 is the Fe that Fe with Ce different mol ratio is made2O3-CeO2Nano-composite catalyst and non-impurity-doped
Type CeO2Conversion ratio figure during catalyst NO reaction.
Fig. 2 is the Fe that Fe with Ce different mol ratio is made2O3-CeO2Nano-composite catalyst and non-impurity-doped
Type CeO2Selectivity figure during catalyst NO reaction.
Fig. 3 is the Fe that Fe with Ce different mol ratio is made2O3-CeO2Nano-composite catalyst and non-impurity-doped
Type CeO2Catalyst XRD figure.
Detailed description of the invention
It is described in detail below in conjunction with detailed description of the invention, it is to be understood that protection scope of the present invention is also
Do not limited by detailed description of the invention.In embodiment, ferric nitrate uses Fe (NO3)3·9H2O, for commercially available;Nitre
Acid cerium uses Ce (NO3)3·6H2O, commercially available gained;1:1 ammonia is commercially available gained.
Embodiment 1
A kind of Fe2O3-CeO2The preparation method of nano-composite catalyst, operating procedure is as follows:
(1)Fe(NO3)3·9H2O and Ce (NO3)3·6H2O presses the amount of material than for 2:5, i.e. weighs
Fe(NO3)3·9H2O1.617g and Ce (NO3)3·6H2O4.3412g, is dissolved in distilled water that to make slaine molten
Liquid, dropping 1:1 ammonia is as precipitant, and room temperature drips limit stirring below, and regulation pH value is 10.0, drips
Continue stirring 4.0 hours after adding, the most aging 15 hours, have precipitate to occur;
(2) rear gained aging in step (1) including sedimentary material be centrifuged separating, it is heavy to take
Shallow lake thing washs, and first uses water to be washed 3 times by precipitate, then uses dehydrated alcohol that precipitate is washed 3
Secondary, washing to cleaning mixture is neutrality;
(3) gained precipitate after washing in step (2) being put into holding temperature in aerator drying baker is
Dry 12 hours, obtain catalyst precursor, gained catalyst precursor is ground successively for 80 DEG C,
Keeping temperature is 500 DEG C of roastings 4 hours, then tabletting, broken, cross 40 mesh sieves and sieve and i.e. obtain product.
Embodiment 2
A kind of Fe2O3-CeO2The preparation method of nano-composite catalyst, operating procedure is as follows:
(1)Fe(NO3)3·9H2O and Ce (NO3)3·6H2O presses the amount of material than for 3:10, i.e. weighs
Fe(NO3)3·9H2O 1.213g and Ce (NO3)3·6H2O 4.3412g, is dissolved in distilled water that to make slaine molten
Liquid, dropping 1:1 ammonia is as precipitant, and room temperature drips limit stirring below, and regulation pH value is 10.0, drips
Continue stirring 4.5 hours after adding, the most aging 12 hours, have precipitate to occur;
(2) rear gained aging in step (1) including sedimentary material be centrifuged separating, it is heavy to take
Shallow lake thing washs, and first uses water to be washed 2 times by precipitate, then uses dehydrated alcohol that precipitate is washed 4
Secondary, washing to cleaning mixture is neutrality;
(3) gained precipitate after washing in step (2) being put into holding temperature in aerator drying baker is
Dry 12 hours, obtain catalyst precursor, gained catalyst precursor is ground successively for 80 DEG C,
Keeping temperature is 500 DEG C of roastings 4 hours, then tabletting, broken, cross 60 mesh sieves and sieve and i.e. obtain product.
Embodiment 3
A kind of Fe2O3-CeO2The preparation method of nano-composite catalyst, operating procedure is as follows:
(1)Fe(NO3)3·9H2O and Ce (NO3)3·6H2O presses the amount of material than for 3.5:10, i.e. weighs
Fe(NO3)3·9H2O 1.415g and Ce (NO3)3·6H2O 4.3412g, is dissolved in distilled water that to make slaine molten
Liquid, dropping 1:1 ammonia is as precipitant, and room temperature drips limit stirring below, and regulation pH value is 10.0, drips
Continue stirring 3.5 hours after adding, the most aging 18 hours, have precipitate to occur;
(2) rear gained aging in step (1) including sedimentary material be centrifuged separating, it is heavy to take
Shallow lake thing washs, and first uses water to be washed 3 times by precipitate, then uses dehydrated alcohol that precipitate is washed 4
Secondary, washing to cleaning mixture is neutrality;
(3) gained precipitate after washing in step (2) being put into holding temperature in aerator drying baker is
Dry 12 hours, obtain catalyst precursor, gained catalyst precursor is ground successively for 80 DEG C,
Keeping temperature is 500 DEG C of roastings 4 hours, then tabletting, broken, cross 50 mesh sieves and sieve and i.e. obtain product.
Embodiment 4
A kind of Fe2O3-CeO2The preparation method of nano-composite catalyst, operating procedure is as follows:
(1)Fe(NO3)3·9H2O and Ce (NO3)3·6H2O presses the amount of material than for 4.5:10, i.e. weighs
Fe(NO3)3·9H2O 1.819g and Ce (NO3)3·6H2O 4.3412g, is dissolved in distilled water that to make slaine molten
Liquid, dropping 1:1 ammonia is as precipitant, and room temperature drips limit stirring below, and regulation pH value is 10.0, drips
Continue stirring 4.0 hours after adding, the most aging 15 hours, have precipitate to occur;
(2) rear gained aging in step (1) including sedimentary material be centrifuged separating, it is heavy to take
Shallow lake thing washs, and first uses water to be washed 3 times by precipitate, then uses dehydrated alcohol that precipitate is washed 3
Secondary, washing to cleaning mixture is neutrality;
(3) gained precipitate after washing in step (2) being put into holding temperature in aerator drying baker is
Dry 12 hours, obtain catalyst precursor, gained catalyst precursor is ground successively for 80 DEG C,
Keeping temperature is 500 DEG C of roastings 4 hours, then tabletting, broken, cross 50 mesh sieves and sieve and i.e. obtain product.
Embodiment 5
A kind of Fe2O3-CeO2The preparation method of nano-composite catalyst, operating procedure is as follows:
(1)Fe(NO3)3·9H2O and Ce (NO3)3·6H2O presses the amount of material than for 1:2, i.e. weighs
Fe(NO3)3·9H2O 2.021g and Ce (NO3)3·6H2O 4.3412g, is dissolved in distilled water that to make slaine molten
Liquid, dropping 1:1 ammonia is as precipitant, and room temperature drips limit stirring below, and regulation pH value is 10.0, drips
Continue stirring 3.5 hours after adding, the most aging 14 hours, have precipitate to occur;
(2) rear gained aging in step (1) including sedimentary material be centrifuged separating, it is heavy to take
Shallow lake thing washs, and first uses water to be washed 2 times by precipitate, then uses dehydrated alcohol that precipitate is washed 3
Secondary, washing to cleaning mixture is neutrality;
(3) gained precipitate after washing in step (2) being put into holding temperature in aerator drying baker is
Dry 12 hours, obtain catalyst precursor, gained catalyst precursor is ground successively for 80 DEG C,
Keeping temperature is 500 DEG C of roastings 4 hours, then tabletting, broken, cross 60 mesh sieves and sieve and i.e. obtain product.
Embodiment 6
(1) 0g Fe (NO is weighed3)3·9H2O and 4.3412gCe (NO3)3·6H2O is dissolved in distilled water,
It is made into metal salt solution, and is 10.0 with the stirring of dropping limit, 1:1 ammonia limit to pH value;Drip complete
After, continue magnetic agitation 4h, then aged at room temperature 15h under room temperature;
(2) by aging rear gained material centrifugation, first with distilled water by precipitate cyclic washing three times,
With dehydrated alcohol, precipitate is washed three times again, until the aobvious neutrality of cleaning mixture;Then the air blast of 80 DEG C
Drying baker is dried 12h, then the catalyst precursor obtained is milled fully, roast at a temperature of 500 DEG C
Burn 4h;Fine catalyst tabletting, broken, screening, choose particle diameter 40~60 mesh catalyst, obtain product
Product.
Detection
Weigh 0.05g above-described embodiment 1 gained catalyst to be placed in stable reactor, in advance to reactor
In be passed through nitrogen gas 1h, air in reactor or foreign gas are drained, then to be passed through volume are 5% simultaneously
The He gas of CO and 85% of NO and 10%, heating is reacted.Temperature be respectively 150 DEG C,
175 DEG C, 200 DEG C, 225 DEG C, 250 DEG C, 275 DEG C time, measure the activity of each temperature spot successively, and detect
NO content in reactor, calculates NO conversion ratio, the percent value of NO before i.e. NO accounts for reaction after reaction.
Selectivity is the N that NO changes into2Account for the percentage ratio of the NO of total conversion, draw data in Fig. 1, Fig. 2.
Fe in Fig. 1, Fig. 2, Fig. 30.3-Ce-O curve is embodiment 2 gained catalyst reaction curve obtained,
Fe0.35-Ce-O curve is embodiment 3 gained catalyst reaction curve obtained, Fe0.4-Ce-O curve is for implementing
Example 1 gained catalyst reaction curve obtained, Fe0.45-Ce-O curve is embodiment 4 gained catalyst reaction institute
Obtain curve, Fe0.5-Ce-O curve is embodiment 5 gained catalyst reaction curve obtained, CeO in Fig. 32
Curve is embodiment 6 gained catalyst reaction curve obtained.
As seen from Figure 1, the Fe prepared2O3-CeO2Nano-composite catalyst is the most active, i.e. NO
All there occurs conversion, but by the selectivity figure of Fig. 2 it is obvious that the ratio of only Fe with Ce is
When 40/100 i.e. mol ratio is 2:5, conversion ratio and selectivity are all 100% when temperature is 250 DEG C, now
Catalyst is optimal choosing.
CeO2 does not occur the peak of Fe after being doped with ferrum as seen from Figure 3, but peak occurs in that partially
Move, illustrate at Fe2O3-CeO2Nano-composite catalyst is successfully mixed with ferrum.
Present invention application coprecipitation is to CeO2Middle doping Fe element, Fe unit have variable quantivalence,
When being doped into CeO by " co-precipitation " synthetic method2Time, make cell configuration change, and probability phase
To relatively big, catalysis activity is made to be greatly reinforced.
The aforementioned description to the specific illustrative embodiment of the present invention illustrates that and the purpose of illustration.
These descriptions are not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to above-mentioned
Teaching, can much change and change.The purpose selected exemplary embodiment and describe exists
In explaining the certain principles of the present invention and actual application thereof, so that those skilled in the art can be real
Now and utilize the various different exemplary of the present invention and various different selection and change.
The scope of the present invention is intended to be limited by claims and equivalents thereof.
Claims (9)
1. a Fe2O3-CeO2The preparation method of nano-composite catalyst, it is characterised in that comprise with
Lower operating procedure:
(1) take ferric nitrate and metal salt solution made by cerous nitrate, drip precipitant, regulate pH value, stir
Mix 3.5~4.5 hours, aging 12~18 hours;
(2) by rear gained material centrifugation aging in step (1), by gained after centrifugal segregation solution
Material washs;
(3) gained material after washing in step (2) is dried, be ground the most successively, roasting,
Tabletting, broken, sieve and i.e. obtain product.
Fe the most according to claim 12O3-CeO2The preparation method of nano-composite catalyst, its feature
It is: in step (1), ferric nitrate and cerous nitrate make metal salt solution by the amount of material than for 2:5.
Fe the most according to claim 12O3-CeO2The preparation method of nano-composite catalyst, its feature
It is: in step (1), dropping precipitant regulation pH value is 10.0.
Fe the most according to claim 32O3-CeO2The preparation method of nano-composite catalyst, its feature
It is: the precipitant described in step (1) is 1:1 ammonia.
Fe the most according to claim 12O3-CeO2The preparation method of nano-composite catalyst, its feature
It is: stirring 4 hours in step (1), aging 12~18 hours.
Fe the most according to claim 12O3-CeO2The preparation method of nano-composite catalyst, its feature
It is: the washing described in step (2) is for first using water to be washed 2~3 times by precipitate, then uses anhydrous
Precipitate is washed 3~4 times by ethanol.
Fe the most according to claim 12O3-CeO2The preparation method of nano-composite catalyst, its feature
Being: the sintering temperature described in step (3) is 500 DEG C, roasting time is 4 hours.
Fe the most according to claim 12O3-CeO2The preparation method of nano-composite catalyst, its feature
It is: the screening described in step (3) was 40~60 mesh sieves.
Fe the most according to claim 12O3-CeO2The preparation method of nano-composite catalyst, its feature
It is: the drying described in step (3) is to dry 12 hours at 80 DEG C for keeping temperature.
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Cited By (4)
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CN106215963A (en) * | 2016-08-16 | 2016-12-14 | 张静 | A kind of preparation method of energy-efficient pulverized coal injection combustion supporting catalyst |
CN111013597A (en) * | 2019-12-26 | 2020-04-17 | 北京工业大学 | Preparation method of cerium-based composite oxide low-temperature SCR catalyst with Ce-MOF as precursor |
CN113522265A (en) * | 2021-07-28 | 2021-10-22 | 中国科学院兰州化学物理研究所 | Metal oxide doped cerium oxide catalyst and preparation method and application thereof |
WO2022089668A1 (en) * | 2020-10-26 | 2022-05-05 | 苏州大学 | Platinum-loaded flower-like iron-cerium composite material and preparation method therefor and application thereof in low-temperature thermal catalytic treatment of toluene |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106215963A (en) * | 2016-08-16 | 2016-12-14 | 张静 | A kind of preparation method of energy-efficient pulverized coal injection combustion supporting catalyst |
CN111013597A (en) * | 2019-12-26 | 2020-04-17 | 北京工业大学 | Preparation method of cerium-based composite oxide low-temperature SCR catalyst with Ce-MOF as precursor |
WO2022089668A1 (en) * | 2020-10-26 | 2022-05-05 | 苏州大学 | Platinum-loaded flower-like iron-cerium composite material and preparation method therefor and application thereof in low-temperature thermal catalytic treatment of toluene |
CN113522265A (en) * | 2021-07-28 | 2021-10-22 | 中国科学院兰州化学物理研究所 | Metal oxide doped cerium oxide catalyst and preparation method and application thereof |
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