CN106492813A - A kind of three-dimensional ordered macroporous LaFeO of support type3/CeO2The preparation method of catalyst - Google Patents
A kind of three-dimensional ordered macroporous LaFeO of support type3/CeO2The preparation method of catalyst Download PDFInfo
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- CN106492813A CN106492813A CN201610837236.XA CN201610837236A CN106492813A CN 106492813 A CN106492813 A CN 106492813A CN 201610837236 A CN201610837236 A CN 201610837236A CN 106492813 A CN106492813 A CN 106492813A
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- lafeo
- catalyst
- ceo
- dimensional ordered
- ordered macroporous
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- 239000003054 catalyst Substances 0.000 title claims abstract description 29
- 229910017771 LaFeO Inorganic materials 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 27
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000012065 filter cake Substances 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 7
- 229910002321 LaFeO3 Inorganic materials 0.000 claims description 17
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 7
- 239000004471 Glycine Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- 230000031709 bromination Effects 0.000 claims description 2
- 238000005893 bromination reaction Methods 0.000 claims description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 16
- 238000000967 suction filtration Methods 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 4
- 238000001802 infusion Methods 0.000 abstract description 2
- 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 description 20
- 239000000243 solution Substances 0.000 description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 14
- 239000004926 polymethyl methacrylate Substances 0.000 description 14
- 239000012043 crude product Substances 0.000 description 10
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 8
- 239000001301 oxygen Substances 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 8
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 7
- 239000000084 colloidal system Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 125000003630 glycyl group Chemical group [H]N([H])C([H])([H])C(*)=O 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 230000001476 alcoholic effect Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- -1 Methyl bromide alkane Chemical class 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229940102396 methyl bromide Drugs 0.000 description 1
- GZUXJHMPEANEGY-UHFFFAOYSA-N methyl bromide Substances BrC GZUXJHMPEANEGY-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000004449 solid propellant Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/63—Pore volume
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
Abstract
The present invention relates to a kind of three-dimensional ordered macroporous LaFeO of support type3/CeO2The preparation method of catalyst, belongs to material chemistry technical field.Cerous nitrate is added in deionized water the cerous nitrate solution for preparing that concentration is 0.1 ~ 1mol/L that stirs；By 3DOMLaFeO3Carrier is added in cerous nitrate solution, is subsequently adding auxiliary agent, 30～600min of stirring reaction at 20～90 DEG C, and reaction is cooled to room temperature after terminating, and after suction filtration, deionized water and ethanol exchange washing and obtains filter cake；The filter cake for obtaining is dried, then at 300～600 DEG C, 1～10h of roasting prepares the three-dimensional ordered macroporous LaFeO of support type3/CeO2Catalyst.The method mainly prepares the three-dimensional ordered macroporous LaFeO of support type by infusion process3/CeO2Catalyst.
Description
Technical field
The present invention relates to a kind of three-dimensional ordered macroporous LaFeO of support type3/CeO2The preparation method of catalyst, belongs to materialized
Learn technical field.
Background technology
Cadmium ferrite（LaFeO3）It is the most basic oxide of rare-earth elements of lanthanum, which has typical perovskite structure
（ABO3）.Perovskite composite oxide has flexible designability so that such material is quite received in fields such as physics, chemistry
Favor, perovskite composite oxide is in catalysis burning, photocatalysis, catalytic cracking, catalytic hydrogenation, solid fuel cell, environment
The aspects such as catalysis have obtained extensive research and application.Three-dimensional ordered macroporous (Three-dimensiomlly ordered
Macroporous, 3DOM) material is macropore, the duct that be mutually communicated and hole of the class in three dimensions, with aligned orderly
New macroporous material of the footpath size more than 50 nm.Compared with pore-free material, pore passage structure and opening that 3DOM materials are mutually communicated
Inner surface be conducive to material in the diffusion of material internal, make reactive material more fully with avtive spot act on, improve reaction
Activity.
CeO2Due to there is preferably storage oxygen/oxygen release characteristic, in catalytic field especially cleaning catalyst for tail gases of automobiles
To being widely applied.Carbon monoxide (CO), hydrocarbon (HC) and nitrogen oxides (NOx) three is mainly contained in vehicle exhaust
Plant pollutant.Cleaning catalyst for tail gases of automobiles be different from general industrial catalyst, it must possess and meanwhile by tail gas this three
Plant harmful gas CO, HC and NOx conversion, be provided simultaneously with effect of catalysis oxidation and catalytic reduction reaction.
Single CeO2There is the poor easy-sintering of heat endurance and the relatively slow defect of oxygen evolution, and LaFeO3Although oxygen
Release is compared with rapid but its too small specific surface limits its application prospect.As the two is respectively provided with excellent storage put oxygen performance, will
The two is cleverly combined together, and the synergy on surface is likely to greatly enhance its catalytic performance.
Content of the invention
The problem existed for above-mentioned prior art and deficiency, it is three-dimensional ordered macroporous that the present invention provides a kind of support type
（3DOM）LaFeO3/CeO2The preparation method of catalyst.It is three-dimensional ordered macroporous that the method mainly prepares support type by infusion process
LaFeO3/CeO2Catalyst, the present invention are achieved through the following technical solutions.
A kind of three-dimensional ordered macroporous LaFeO of support type3/CeO2The preparation method of catalyst, which comprises the following steps that：
Step 1, cerous nitrate is added in deionized water stir prepare concentration for concentration for 0.1 ~ 1mol/L nitre
Sour cerium solution；
Step 2, by 3DOMLaFeO3Carrier is according to LaFeO3With cerous nitrate mol ratio it is（1～10）:1 is added in step 1
In cerous nitrate solution, auxiliary agent is subsequently adding, 30～600min of stirring reaction at 20～90 DEG C, reaction are cooled to room after terminating
Temperature, after suction filtration, deionized water and ethanol exchange washing and obtain filter cake；
Step 3, the filter cake that step 2 is obtained is dried, then at 300～600 DEG C, 1～10h of roasting prepares load
The three-dimensional ordered macroporous LaFeO of type3/CeO2Catalyst.
In the step 2, auxiliary agent is polyethylene glycol, polyvinylpyrrolidone, cetyl trimethyl bromination alkane, glycine
In one or more arbitrary proportion mixtures, the addition of auxiliary agent is 3DOMLaFeO3The 1%～50% of carrier quality.
3DOMLaFeO in above-mentioned steps 23Carrier is obtained by colloid crystal template：
（a）By lanthanum nitrate with ferric nitrate it is in molar ratio（1～9）:1 mixing, adds methyl alcohol, and it is 0.1 ~ 1mol/L that concentration is obtained
Alcoholic solution；（b）At 20～90 DEG C, 30～360min is stirred with the speed constant temperature of 300～1000r/min；（c）Press poly- methyl
Methyl acrylate（PMMA）:Slaine（Lanthanum nitrate and ferric nitrate）Mass ratio=1:（1～3）, PMMA templates are added step
（b）Solution in mixed；（d）By step（c）Mixed solution stand 2～4 hours at normal temperatures, be subsequently placed in 30～90
At DEG C, freeze-day with constant temperature obtains crude product in 12～24 hours, to remove moisture therein；（e）By step（d）Gained crude product is with 2 DEG C/min
Heating rate be warmed up to 450～600 DEG C after constant temperature 2～4 hours, obtain final product three-dimensional ordered macroporous LaFeO3Material（3DOMLaFeO3
Carrier）.
The invention has the beneficial effects as follows：
（1）3DOM materials have uniform sequential macropore duct, higher pore volume and skeleton composition as a class new material
Diversity the features such as, can as loaded catalyst in carrier part, uniform dispersion is supported on the activearm on its surface
Point, the dispersiveness of active component is improved, prevents which from reuniting；
（2）CeO2With LaFeO3It is respectively provided with excellent storage put oxygen performance, CeO2There is the poor easy-sintering of heat endurance and oxygen evolution phase
To slow defect, and LaFeO3Although oxygen evolution is compared with rapid but its too small specific surface limits its application prospect.To the two
Cleverly it is combined together, more excellent catalytic performance can be played.
Description of the drawings
Fig. 1 is the support type 3DOMLaFeO that the embodiment of the present invention 1 is prepared3/CeO2Catalyst SEM schemes, and wherein A, B are
Different angles；
Fig. 2 is the support type 3DOMLaFeO that the embodiment of the present invention 1 is prepared3/CeO2Catalyst TEM schemes, and wherein A, B be not for
Same multiplication factor.
Specific embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment 1
The three-dimensional ordered macroporous LaFeO of the support type3/CeO2The preparation method of catalyst, which comprises the following steps that：
Step 1, cerous nitrate is added in deionized water stirs（At 30 DEG C, stirred with the speed constant temperature of 300r/min
60min）Prepare the cerous nitrate solution that concentration is that concentration is 0.1mol/L；
Step 2, by 3DOMLaFeO3Carrier is according to LaFeO3It is 10 with cerous nitrate mol ratio:1 is added to the cerous nitrate in step 1
In solution, auxiliary agent is subsequently adding（Auxiliary agent is glycine, and the addition of auxiliary agent is 3DOMLaFeO3The 20% of carrier quality）, 25
With speed stirring reaction 120min of 300r/min at DEG C, reaction is cooled to room temperature after terminating, deionized water and second after suction filtration
Alcohol exchanges washing and obtains filter cake；
Step 3, the filter cake that step 2 is obtained is dried（Freeze-day with constant temperature 24h is carried out with 100 DEG C）, then roasting at 450 DEG C
4h prepares the three-dimensional ordered macroporous LaFeO of support type3/CeO2Catalyst.
The support type 3DOMLaFeO that wherein embodiment 1 is prepared3/CeO2Catalyst SEM is schemed as shown in figure 1, embodiment 1
The support type 3DOMLaFeO for preparing3/CeO2Catalyst TEM figures are as shown in Figure 2.
3DOMLaFeO in above-mentioned steps 23Carrier is obtained by conventional colloid crystal template：
（a）It is 1 in molar ratio by lanthanum nitrate and ferric nitrate:1 mixing, adds methyl alcohol, and the alcohol that concentration is obtained for 0.1mol/L is molten
Liquid；（b）At 30 DEG C, with the speed constant temperature stirring 60min of 300r/min；（c）Press polymethyl methacrylate（PMMA）:Metal
Salt（Lanthanum nitrate and ferric nitrate）Mass ratio=1:1, PMMA templates are added step（b）Solution in mixed；（d）Will step
Suddenly（c）Mixed solution stand 2 hours at normal temperatures, be subsequently placed in freeze-day with constant temperature at 60 DEG C and obtain crude product in 24 hours, with remove
Moisture therein；（e）By step（d）Gained crude product is warmed up to constant temperature 4 hours after 600 DEG C with the heating rate of 2 DEG C/min, obtains final product
Three-dimensional ordered macroporous LaFeO3Material（3DOMLaFeO3Carrier）.
Embodiment 2
The three-dimensional ordered macroporous LaFeO of the support type3/CeO2The preparation method of catalyst, which comprises the following steps that：
Step 1, cerous nitrate is added in deionized water stirs（At 30 DEG C, stirred with the speed constant temperature of 300r/min
60min）Prepare the cerous nitrate solution that concentration is that concentration is 1mol/L；
Step 2, by 3DOMLaFeO3Carrier is according to LaFeO3It is 1 with cerous nitrate mol ratio:1 is added to the cerous nitrate in step 1
In solution, auxiliary agent is subsequently adding（Auxiliary agent is glycine, and the addition of auxiliary agent is 3DOMLaFeO3The 1% of carrier quality）, at 20 DEG C
Under with speed stirring reaction 600min of 300r/min, reaction is cooled to room temperature after terminating, deionized water and ethanol after suction filtration
Exchange washing and obtain filter cake；
Step 3, the filter cake that step 2 is obtained is dried（Freeze-day with constant temperature 24h is carried out with 100 DEG C）, then roasting at 600 DEG C
1h prepares the three-dimensional ordered macroporous LaFeO of support type3/CeO2Catalyst.
3DOMLaFeO in above-mentioned steps 23Carrier is obtained by conventional colloid crystal template：
（a）It is 9 in molar ratio by lanthanum nitrate and ferric nitrate:1 mixing, adds methyl alcohol, and alcoholic solution of the concentration for 1mol/L is obtained；
（b）At 20 DEG C, with the speed constant temperature stirring 30min of 1000r/min；（c）Press polymethyl methacrylate（PMMA）:Slaine
（Lanthanum nitrate and ferric nitrate）Mass ratio=1:3, PMMA templates are added step（b）Solution in mixed；（d）By step
（c）Mixed solution stand 4 hours at normal temperatures, be subsequently placed in freeze-day with constant temperature at 90 DEG C and obtain crude product in 12 hours, to remove which
In moisture；（e）By step（d）Gained crude product is warmed up to constant temperature 2 hours after 450 DEG C with the heating rate of 2 DEG C/min, obtains final product three
Dimension ordered big hole LaFeO3Material（3DOMLaFeO3Carrier）.
Embodiment 3
The three-dimensional ordered macroporous LaFeO of the support type3/CeO2The preparation method of catalyst, which comprises the following steps that：
Step 1, cerous nitrate is added in deionized water stirs（At 30 DEG C, stirred with the speed constant temperature of 300r/min
60min）Prepare the cerous nitrate solution that concentration is that concentration is 0.8mol/L；
Step 2, by 3DOMLaFeO3Carrier is according to LaFeO3It is 8 with cerous nitrate mol ratio:1 is added to the cerous nitrate in step 1
In solution, auxiliary agent is subsequently adding（Auxiliary agent is glycine, and the addition of auxiliary agent is 3DOMLaFeO3The 50% of carrier quality）, 90
With speed stirring reaction 30min of 1000r/min at DEG C, reaction is cooled to room temperature after terminating, deionized water and second after suction filtration
Alcohol exchanges washing and obtains filter cake；
Step 3, the filter cake that step 2 is obtained is dried（Freeze-day with constant temperature 24h is carried out with 100 DEG C）, then roasting at 300 DEG C
10h prepares the three-dimensional ordered macroporous LaFeO of support type3/CeO2Catalyst.
3DOMLaFeO in above-mentioned steps 23Carrier is obtained by conventional colloid crystal template：
（a）It is 7 in molar ratio by lanthanum nitrate and ferric nitrate:1 mixing, adds methyl alcohol, and the alcohol that concentration is obtained for 0.5mol/L is molten
Liquid；（b）At 90 DEG C, with the speed constant temperature stirring 360min of 800r/min；（c）Press polymethyl methacrylate（PMMA）:Gold
Category salt（Lanthanum nitrate and ferric nitrate）Mass ratio=1:2, PMMA templates are added step（b）Solution in mixed；（d）Will
Step（c）Mixed solution stand 3 hours at normal temperatures, be subsequently placed in freeze-day with constant temperature at 30 DEG C and obtain crude product in 20 hours, to remove
Remove moisture therein；（e）By step（d）Gained crude product is warmed up to constant temperature 3 hours after 500 DEG C with the heating rate of 2 DEG C/min, i.e.,
Obtain three-dimensional ordered macroporous LaFeO3Material（3DOMLaFeO3Carrier）.
Embodiment 4
The three-dimensional ordered macroporous LaFeO of the support type3/CeO2The preparation method of catalyst, which comprises the following steps that：
Step 1, cerous nitrate is added in deionized water stirs（At 30 DEG C, stirred with the speed constant temperature of 300r/min
60min）Prepare the cerous nitrate solution that concentration is that concentration is 0.5mol/L；
Step 2, by 3DOMLaFeO3Carrier is according to LaFeO3It is 5 with cerous nitrate mol ratio:1 is added to the cerous nitrate in step 1
In solution, auxiliary agent is subsequently adding（It is 1 that auxiliary agent is mass ratio:1:1 polyethylene glycol, polyvinylpyrrolidone and cetyl three
Methyl bromide alkane mixture, the addition of auxiliary agent is 3DOMLaFeO3The 40% of carrier quality）, with 1000r/min's at 70 DEG C
Speed stirring reaction 50min, reaction are cooled to room temperature after terminating, and after suction filtration, deionized water and ethanol exchange washing and filtered
Cake；
Step 3, the filter cake that step 2 is obtained is dried（Freeze-day with constant temperature 24h is carried out with 100 DEG C）, then roasting at 400 DEG C
8h prepares the three-dimensional ordered macroporous LaFeO of support type3/CeO2Catalyst.
3DOMLaFeO in above-mentioned steps 23Carrier is obtained by conventional colloid crystal template：
（a）It is 5 in molar ratio by lanthanum nitrate and ferric nitrate:1 mixing, adds methyl alcohol, and the alcohol that concentration is obtained for 0.8mol/L is molten
Liquid；（b）At 20 DEG C, with the speed constant temperature stirring 360min of 800r/min；（c）Press polymethyl methacrylate（PMMA）:Gold
Category salt（Lanthanum nitrate and ferric nitrate）Mass ratio=1:3, PMMA templates are added step（b）Solution in mixed；（d）Will
Step（c）Mixed solution stand 4 hours at normal temperatures, be subsequently placed in freeze-day with constant temperature at 90 DEG C and obtain crude product in 12 hours, to remove
Remove moisture therein；（e）By step（d）Gained crude product is warmed up to constant temperature 2 hours after 480 DEG C with the heating rate of 2 DEG C/min, i.e.,
Obtain three-dimensional ordered macroporous LaFeO3Material（3DOMLaFeO3Carrier）.
Above in association with accompanying drawing to the present invention specific embodiment be explained in detail, but the present invention be not limited to above-mentioned
Embodiment, in the ken that those of ordinary skill in the art possess, can be with before without departing from present inventive concept
Put that various changes can be made.
Claims (2)
1. the three-dimensional ordered macroporous LaFeO of a kind of support type3/CeO2The preparation method of catalyst, it is characterised in that concrete steps are such as
Under：
Step 1, cerous nitrate is added in deionized water stir prepare concentration be 0.1 ~ 1mol/L cerous nitrate molten
Liquid；
Step 2, by 3DOMLaFeO3Carrier is according to LaFeO3It is 1～10 with cerous nitrate mol ratio:1 is added to the nitric acid in step 1
In cerium solution, auxiliary agent is subsequently adding, 30～600min of stirring reaction at 20～90 DEG C, reaction are cooled to room temperature after terminating, and take out
After filter, deionized water and ethanol exchange washing and obtain filter cake；
Step 3, the filter cake that step 2 is obtained is dried, then at 300～600 DEG C, 1～10h of roasting prepares load
The three-dimensional ordered macroporous LaFeO of type3/CeO2Catalyst.
2. the three-dimensional ordered macroporous LaFeO of support type according to claim 13/CeO2The preparation method of catalyst, its feature
It is：In the step 2 auxiliary agent be polyethylene glycol, polyvinylpyrrolidone, cetyl trimethyl bromination alkane, in glycine
One or more arbitrary proportion mixtures, the addition of auxiliary agent is 3DOMLaFeO3The 1%～50% of carrier quality.
Priority Applications (1)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022069797A1 (en) * | 2020-10-01 | 2022-04-07 | Teknologian Tutkimuskeskus Vtt Oy | Method for forming a porous structure, porous structure and use |
| CN114768812A (en) * | 2022-04-20 | 2022-07-22 | 河北科技大学 | Heterogeneous Fenton catalyst LaFeO3/3DOMCeO2And preparation method and application thereof |
| CN115193439A (en) * | 2022-04-20 | 2022-10-18 | 河北科技大学 | Three-dimensional ordered macroporous La 0.4 Ce 0.6 FeO 3 Preparation method and application of photocatalyst |
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| CN101199929A (en) * | 2007-12-24 | 2008-06-18 | 天津大学 | Macroporous Pt/CeO2 catalyst for water gas shift reaction and preparing process thereof |
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| CN101199929A (en) * | 2007-12-24 | 2008-06-18 | 天津大学 | Macroporous Pt/CeO2 catalyst for water gas shift reaction and preparing process thereof |
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| YANE ZHENG等: "Designed oxygen carriers from macroporous LaFeO3 supported CeO2 for chemical-looping reforming of methane", 《APPLIED CATALYSIS B: ENVIRONMENTAL》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022069797A1 (en) * | 2020-10-01 | 2022-04-07 | Teknologian Tutkimuskeskus Vtt Oy | Method for forming a porous structure, porous structure and use |
| CN114768812A (en) * | 2022-04-20 | 2022-07-22 | 河北科技大学 | Heterogeneous Fenton catalyst LaFeO3/3DOMCeO2And preparation method and application thereof |
| CN115193439A (en) * | 2022-04-20 | 2022-10-18 | 河北科技大学 | Three-dimensional ordered macroporous La 0.4 Ce 0.6 FeO 3 Preparation method and application of photocatalyst |
| CN115193439B (en) * | 2022-04-20 | 2024-02-20 | 北京石油化工学院 | Three-dimensional ordered macroporous La 0.4 Ce 0.6 FeO 3 Preparation method and application of photocatalyst |
| CN114768812B (en) * | 2022-04-20 | 2024-02-27 | 北京石油化工学院 | Heterogeneous Fenton catalyst LaFeO 3 /3DOMCeO 2 Preparation method and application thereof |
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