CN108855041A - A kind of preparation method of Ceria-zirconia solid solution catalyst - Google Patents
A kind of preparation method of Ceria-zirconia solid solution catalyst Download PDFInfo
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000006104 solid solution Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000003054 catalyst Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 27
- 239000000243 solution Substances 0.000 claims abstract description 13
- 239000007864 aqueous solution Substances 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 239000000725 suspension Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000032683 aging Effects 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 7
- 229910000027 potassium carbonate Inorganic materials 0.000 claims abstract description 6
- 229910004664 Cerium(III) chloride Inorganic materials 0.000 claims abstract description 3
- 229910003130 ZrOCl2·8H2O Inorganic materials 0.000 claims abstract description 3
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims abstract description 3
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims 1
- 239000006228 supernatant Substances 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 7
- 238000003786 synthesis reaction Methods 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 5
- 230000001376 precipitating effect Effects 0.000 abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 230000021615 conjugation Effects 0.000 abstract 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical group [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000010970 precious metal Substances 0.000 description 4
- 229910001868 water Inorganic materials 0.000 description 4
- 101710134784 Agnoprotein Proteins 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 239000008188 pellet Substances 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000000908 ammonium hydroxide Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 2
- 229910000420 cerium oxide Inorganic materials 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000004502 linear sweep voltammetry Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- -1 Rare earth cerium oxide Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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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
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
- B01D53/9445—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC]
- B01D53/945—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC] characterised by a specific catalyst
-
- 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
-
- 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
-
- 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
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Environmental & Geological Engineering (AREA)
- Biomedical Technology (AREA)
- Combustion & Propulsion (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
Abstract
The invention discloses a kind of preparation method of Ceria-zirconia solid solution catalyst, this method is first to weigh CeCl3·7H2O and ZrOCl2·8H2O is added deionized water and stirs to being completely dissolved, and K is then added dropwise with vigorous stirring2CO3Aqueous solution is until solution ph is 8.2-10.2；The suspension room temperature ageing 12h obtained after being added dropwise, suspension after ageing, which is then transferred in crystallizing kettle, is put into thermostatic drying chamber progress hydro-thermal reaction, after crystallizing kettle Temperature fall, it is centrifuged and is washed with deionized until chloride completely disappears, it is transferred to crucible after drying, is put into Muffle kiln roasting and obtains CeO2‑ZrO2Solid solution catalyst.The method of the present invention as precipitating reagent and is combined to be added dropwise and realized with hydro-thermal method (synthesis) using solution of potassium carbonate, the catalyst crystal degree height of preparation, the moderate length of particle, and it is good to be combined into flower-shaped conjugation, large specific surface area.
Description
Technical field
The present invention relates to a kind of Ceria-zirconia (CeO2-ZrO2) solid solution catalyst preparation method.
Background technique
Currently, environmental problem has become a global significant problem, the big model in public eye is appeared in again and again
It encloses haze weather, PM2.5 and ultra tiny floating dust particle etc. and endangers the noun of health of masses and make people on tenterhooks, this pollutant
One of main source be exactly harmful substance in motor-vehicle tail-gas.Cleaning catalyst for tail gases of automobiles mainly includes precious metal catalyst
Agent and non-precious metal catalyst two major classes.Since Precious Metals Resources are rare and expensive, develop with superior catalytic
Active non-precious metal catalyst becomes the focus of research.Rare earth cerium oxide (CeOx) net in vehicle exhaust as hydrogen-storing material
Change with being widely used in three-way catalyst (Three Way Catalyst, TWC), it improves the air-fuel ratio of catalyst
Characteristic promotes noble metal in the dispersion of catalyst surface, to improve the reactivity of three-way catalyst.Ceria
(CeO2) there is fluorite structure, good stability is all shown from room temperature to fusing point.Its major catalytic principle is CeO2Have
Excellent oxygen storage capacity, essence are derived from the variable valence i.e. Ce of Ce ion4+Ce can be changed into reducing environment3+And
The latter can reversibly restore tetravalent state in an oxidizing environment again.This reversible Ce3+/Ce4+Redox couple is automobile
Serious C is endangered in tail gasnHm, NO, CO be changed into the CO less to environmental hazard2、H2O and N2Provide crucial key.So
And CeO2Under 1000 DEG C of high temperature, it is easy to happen sintering, specific surface area reduces, and makes oxygen storage capacity (Oxygen Storage
Capacity, OSC) decline, its application range in practice is limited to a certain extent.So many scientific researchers
In research by CeO2Middle doped zirconia (ZrO2) solid solution is formed to improve CeO2Structural stability and oxygen storage capacity,
Significantly improve CeO2Oxidation-reduction quality and low-temperature catalyzed performance, become current three way conversion catalyst for purificationof tail gas of automobile
In a kind of indispensable material.According to Ce/Zr than with maturing temperature it has been determined that the crystal structure of this material have：Monoclinic crystal
System, tetragonal crystal system and cubic system.
Common CeO2-ZrO2The preparation method of solid solution has coprecipitation, sol-gel process, high-temperature roasting method, high-energy ball
Mill method etc..Different preparation methods has the crystal phase structure of solid solution, surface area, oxidation-reduction quality and Oxygen storage capacity biggish
It influences.Prepare the CeO of function admirable2-ZrO2Solid solution has great importance for expanding its application.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of CeO2-ZrO2The preparation of solid solution catalyst
Method.
CeO of the invention2-ZrO2The preparation method of solid solution catalyst, includes the following steps：
Weigh CeCl3·7H2O and ZrOCl2·8H2O is added deionized water and stirs to being completely dissolved, and then shifts solution
Into three-neck flask, K is added dropwise with constant pressure funnel with vigorous stirring2CO3Aqueous solution is until solution ph is 8.2；Drop
The suspension room temperature ageing 12h obtained after adding, the suspension after ageing, which is then transferred in crystallizing kettle, is put into thermostatic drying chamber
Middle carry out hydro-thermal reaction is centrifuged and is washed with deionized until chloride completely disappears, by sample after crystallizing kettle Temperature fall
Product are put into 80 DEG C of thermostatic drying chambers and are transferred to crucible to after being completely dried, and are put into Muffle kiln roasting and obtain CeO2-ZrO2Solid solution
Body catalyst.
The K2CO3The rate of addition of aqueous solution is 0.4ml/min, concentration 0.3M.
When suspension after ageing is then transferred to progress hydro-thermal reaction in crystallizing kettle, reaction temperature is 60 DEG C of duration 3h.
Until chloride completely disappears, method is using AgNO for the washing3It is tested, a small amount of sample is taken to survey
Examination, as addition AgNO3It is generated afterwards without precipitating, then it is assumed that Chlorine in Solution compound has completely disappeared.
The maturing temperature a length of 5h when being 350 DEG C, heating rate are 3 DEG C/min.
The present invention is successfully prepared by the synthesis for using dripping method to combine with hydro-thermal method using potassium carbonate as precipitating reagent
Flower pattern CeO2-ZrO2Solid solution, which is cubic fluorite structure, and crystallinity is high, large specific surface area.
Detailed description of the invention
Fig. 1 is the CeO using distinct methods preparation2-ZrO2The stereoscan photograph of solid solution, (a) Ammonia Process, (b) hydro-thermal
Method, (c) disposably pour into method, (d) synthesis；
Fig. 2 is the CeO of distinct methods preparation2-ZrO2Solid solution XRD diffraction pattern, (a) synthesis, (b) hydro-thermal method, (c) ammonia
Water law, (d) disposably pour into method；
Fig. 3 is the CeO of distinct methods preparation2-ZrO2The linear sweep voltammetry curve graph of solid solution；(a) synthesis, (b) water
Thermal method, (c) disposably pour into method.
Specific embodiment
Embodiment 1
Weigh 3.02gCeCl3·7H2O (8.1mmol) and 0.2898gZrOCl2·8H2O (0.9mmol) adds in beaker
Enter 10ml deionized water, is stirred with glass bar to being completely dissolved.Then it transfers the solution into three-neck flask, with vigorous stirring
The K of 0.30M is added dropwise with constant pressure funnel2CO3Aqueous solution (0.4ml/min) until reach 8.2 pH value.It is added dropwise
The suspension room temperature ageing 12h obtained afterwards, the suspension after ageing are then transferred to and are put into 60 DEG C of thermostatic drying chamber in crystallizing kettle
Middle hydro-thermal 3h is centrifuged and is washed with deionized until chloride completely disappears (AgNO after crystallizing kettle Temperature fall3It surveys
Examination).Sample is put into in 80 DEG C of thermostatic drying chamber dry 12h.It is transferred to crucible after being completely dried, is put into 350 DEG C of Muffle furnace,
It roasts 5h (3 DEG C/min of heating rate), obtains CeO2-ZrO2Solid solution.
Embodiment 2
With embodiment 1, difference is that K is added dropwise2CO3Aqueous solution until reach 9.2 pH value.
Embodiment 3
With embodiment 1, difference is that K is added dropwise2CO3Aqueous solution until reach 10.2 pH value.
CeO made from above-described embodiment2-ZrO2The pore structure parameter table of solid solution is as shown in table 1, it can be seen that with pH
Reduction, the specific surface area of solid solution is continuously increased, and the sample of the specific surface area ratio PH10.2 of the sample of pH8.2 increases
106.6%.
Table 1CeO2-ZrO2The pore structure parameter of solid solution
Embodiment 4
K2CO3Aqueous solution disposably pours into method preparation
Weigh 3.02gCeCl3·7H2O (8.1mmol) and 0.2898gZrOCl2·8H2O (0.9mmol) adds in beaker
Enter 10ml deionized water, is stirred with glass bar to being completely dissolved.Then it transfers the solution into three-neck flask, with vigorous stirring
It is added at one time the K of appropriate 0.30M2CO3Aqueous solution to pH value reaches 8.2.Suspension room temperature is aged 12h, is then centrifuged for and spends
Ion water washing completely disappears (AgNO until chloride3Test).80 DEG C of sample dry 12h.350 DEG C of roasting 5h (heating rates 3
DEG C/min), obtain CeO2-ZrO2Solid solution.
Embodiment 5
Hydro-thermal method preparation
Weigh 3.02gCeCl3·7H2O (8.1mmol) and 0.2898gZrOCl2·8H2O (0.9mmol) adds in beaker
Enter 10ml deionized water, is stirred with glass bar to being completely dissolved.Then it transfers the solution into three-neck flask, with vigorous stirring
The K of 0.30M is added dropwise with constant pressure funnel2CO3Aqueous solution (0.4ml/min) reaches 8.2 to pH.It is obtained after being added dropwise
Suspension be transferred in crystallizing kettle, be put into still aging 12h in 60 DEG C of thermostatic drying chamber, after crystallizing kettle Temperature fall,
It is centrifuged and is washed with deionized until chloride completely disappears (AgNO3Test).Sample is being put into 80 DEG C of freeze-day with constant temperature
Dry 12h in case.It is transferred to crucible after being completely dried, is put into Muffle furnace roasting and (with 3 DEG C/min temperature programming to 350 DEG C, and protects
5h is held, automatic to cool down), obtain CeO2-ZrO2Solid solution.
Embodiment 6
The preparation of ammonium hydroxide dripping method
Weigh 3.02gCeCl3·7H2O (8.1mmol) and 0.2898gZrOCl2·8H2O (0.9mmol) adds in beaker
Enter 50ml deionized water, is stirred with glass bar to being completely dissolved.It transfers the solution into three-neck flask, stirs 30min.Then exist
Be vigorously stirred it is lower with constant pressure funnel be added dropwise ammonium hydroxide until pH value be 9.5, continue after being added dropwise stirring it is 0.5 small
When.Suspension room temperature is aged 12h, is then washed 2 times with dehydrated alcohol after filtering and deionized water is sufficiently washed again, is put into 60
Dry 12h in DEG C insulating box, then 500 DEG C of roasting 4h (2 DEG C/min of heating rate) in Muffle furnace, obtain CeO2-ZrO2Solid solution
Body.
Fig. 1 is the CeO using the preparation of several distinct methods2-ZrO2The stereoscan photograph of solid solution, as seen from Figure 1 ammonia
The CeO of water law preparation2-ZrO2Solid solution pellet is diametrically 5-25 μm or so of irregular reunion shape, the preparation of 12h hydro-thermal method
CeO2-ZrO2The sliver shape that solid solution pellet is 10-20 μm or so in length disposably pours into the CeO of method preparation2-ZrO2Gu
CeO is made in the short flake that melt granules are 20-30 μm or so in length, synthesis2-ZrO2Solid solution pellet is 20- in length
30 μm or so of short flake and major part is combined into flower-shaped.
The CeO of distinct methods preparation2-ZrO2Solid solution XRD diffraction pattern is as shown in Figure 2.It can be seen that from XRD diffraction pattern
It goes out peak position at 28.5 °, 33.2 °, 47.6 °, 57.1 °, 58.6 °, 69.4 °, 76.6 °, respectively correspond (111), (200),
(220), (311), (222), (400), (331) crystal face, it is known that sample is cube fluorite structure.From the comparative experiments of distinct methods
As can be seen that the variation of method does not have an impact the crystal form of particle, particle is still cubic fluorite.The sample of dripping method preparation
Product diffraction peak intensity most most sharpens by force, illustrates that the crystallinity of particle is best.
The CeO of distinct methods preparation2-ZrO2The linear sweep voltammetry curve graph of solid solution is as shown in Figure 3.It can be seen that several
Obtained material analysis oxygen ability is it is still further preferred that the synthesis combined by dripping method with hydro-thermal method in kind method.
Claims (6)
1. a kind of CeO2-ZrO2The preparation method of solid solution catalyst, which is characterized in that include the following steps：
Weigh CeCl3·7H2O and ZrOCl2·8H2O is added deionized water and stirs to being completely dissolved, and then transfers the solution into three
In neck flask, K is added dropwise with constant pressure funnel with vigorous stirring2CO3Aqueous solution is until solution ph is 8.2-10.2；
The suspension room temperature ageing 12h obtained after being added dropwise, the suspension after ageing, which is then transferred in crystallizing kettle, is put into freeze-day with constant temperature
Hydro-thermal reaction is carried out in case, after crystallizing kettle Temperature fall, is centrifuged and is washed with deionized until chloride completely disappears, it will
Sample is put into 80 DEG C of thermostatic drying chambers and is transferred to crucible to after being completely dried, and is put into Muffle kiln roasting and obtains CeO2-ZrO2Gu
Solution catalyst.
2. CeO according to claim 12-ZrO2The preparation method of solid solution catalyst, which is characterized in that the K2CO3
The rate of addition of aqueous solution is 0.4mL/min, concentration 0.3M.
3. CeO according to claim 12-ZrO2The preparation method of solid solution catalyst, which is characterized in that the K2CO3
Aqueous solution is added dropwise dropwise until solution ph is 8.2.
4. CeO according to claim 12-ZrO2The preparation method of solid solution catalyst, which is characterized in that outstanding after ageing
When supernatant liquid is then transferred to progress hydro-thermal reaction in crystallizing kettle, reaction temperature is 60 DEG C of duration 3h.
5. CeO according to claim 12-ZrO2The preparation method of solid solution catalyst, which is characterized in that the washing
Until chloride completely disappears, method is using AgNO3It is tested.
6. CeO according to claim 12-ZrO2The preparation method of solid solution catalyst, which is characterized in that the roasting
Temperature a length of 5h when being 350 DEG C, heating rate are 3 DEG C/min.
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| CN112237910A (en) * | 2020-12-16 | 2021-01-19 | 中南大学 | Preparation method of CeZrK/rGO nano solid solution catalyst |
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