CN106430304B - A kind of preparation method of high-ratio surface high temperature resistant cerium zirconium solid solution - Google Patents
A kind of preparation method of high-ratio surface high temperature resistant cerium zirconium solid solution Download PDFInfo
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- CN106430304B CN106430304B CN201610612068.4A CN201610612068A CN106430304B CN 106430304 B CN106430304 B CN 106430304B CN 201610612068 A CN201610612068 A CN 201610612068A CN 106430304 B CN106430304 B CN 106430304B
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- RCFVMJKOEJFGTM-UHFFFAOYSA-N cerium zirconium Chemical compound [Zr].[Ce] RCFVMJKOEJFGTM-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000006104 solid solution Substances 0.000 title claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000006229 carbon black Substances 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 4
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 4
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 22
- 238000001914 filtration Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 230000032683 aging Effects 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229910001868 water Inorganic materials 0.000 claims description 5
- 150000000703 Cerium Chemical class 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 abstract description 2
- 238000000975 co-precipitation Methods 0.000 abstract description 2
- 229910052735 hafnium Inorganic materials 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 229910000420 cerium oxide Inorganic materials 0.000 abstract 1
- 229920000620 organic polymer Polymers 0.000 abstract 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 abstract 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 abstract 1
- 229910001928 zirconium oxide Inorganic materials 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 9
- 238000003756 stirring Methods 0.000 description 8
- 238000009938 salting Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 5
- 229910006213 ZrOCl2 Inorganic materials 0.000 description 4
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium nitrate Inorganic materials [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- IPCAPQRVQMIMAN-UHFFFAOYSA-L zirconyl chloride Chemical compound Cl[Zr](Cl)=O IPCAPQRVQMIMAN-UHFFFAOYSA-L 0.000 description 4
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical compound [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910009253 Y(NO3)3 Inorganic materials 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009415 formwork Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229920000428 triblock copolymer Polymers 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- BXJPTTGFESFXJU-UHFFFAOYSA-N yttrium(3+);trinitrate Chemical compound [Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O BXJPTTGFESFXJU-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
-
- 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
- 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
-
- B01J35/613—
-
- B01J35/615—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Abstract
The present invention relates to a kind of preparation methods of high-ratio surface high temperature resistant cerium zirconium solid solution, the solid solution is mainly made of cerium oxide and zirconium oxide, auxiliary element is one or more of La, Pr, Y, Al, Hf, and traditional organic polymer template is replaced using one of carbon black, activated carbon or graphene as modifying agent in co-precipitation preparation process.Of the invention preparation method is simple, and prepared cerium zirconium sosoloid specific surface area is larger, and high-temperature stability is preferable, and environmentally friendly, industrialized production easy to accomplish.
Description
Technical field
The present invention relates to a kind of preparation methods of high-ratio surface high temperature resistant cerium zirconium solid solution, belong to rare earth metallurgy technology neck
Domain.
Background technique
CeO2Specific Ce3+/Ce4+Redox cycle becomes an important group in three-way catalyst (TWCs)
At part.But CeO2Since experience high temperature can be such that particle itself is sintered, and by ZrO2CeO is added2In can improve its high-temperature stable
Property.It is well known that three-effect catalysis reaction occurs mainly in the surface of catalyst, therefore the Gao Bibiao of hydrogen-storing material cerium zirconium sosoloid
Area and good thermal stability are the prerequisites of its high catalytic capability.
102698731 A of patent CN discloses a kind of preparation method of high temperature resistant cerium zirconium solid solution, prepared doping
The cerium zirconium sosoloid high-temperature stability of La, Y, Pr, Nd are preferable, but macromolecule organic modifiers used in its preparation process are being washed
A large amount of waste water can be generated during washing, or incomplete combustion will affect the purity of cerium zirconium sosoloid in high-temperature calcination process
And performance.Patent CN103316658 A discloses a kind of nanometer composite cerium zirconium solid solution and preparation method thereof, is equally preparing
Organic structure guiding die plate agent, such as triblock copolymer P123, cetyl trimethylammonium bromide have been used in journey.Document
" nano Ce O2Carbon black additive amount, calcination temperature and calcination time have been investigated to CeO in the modification precipitation method preparation research of powder "2
The influence of partial size, although being only limitted to instead of organic formwork agent to CeO in coprecipitation process using inorganic matter carbon black2Grain
The research of diameter.
Summary of the invention
The object of the present invention is to provide it is a kind of it is at low cost, method is simple, environmental-friendly high-ratio surface high temperature resistant cerium zirconium is solid
The preparation method of solution.
The preparation method of high-ratio surface high temperature resistant cerium zirconium solid solution of the present invention includes the following steps:
It (1) is that 10-80:3.5-50:0.8-15 weighs soluble cerium salt, soluble zirconates and doped chemical according to mass ratio
Soluble-salt be dissolved in deionized water solution be made；
(2) one of carbon black, activated carbon or graphene are added in the solution of step 1 as modifying agent；
(3) H is added after the solution of step 2 is sufficiently mixed uniformly2O2, H2O2Additional amount be soluble cerium salt quality
30%-50%；
(4) solution of step 3 is added drop-wise to containing NH3•H2O or NH4HCO3In the precipitating reagent of middle one or two, keep
PH value of solution=8-10, the solidliquid mixture that then ageing reaction 4h is obtained；
(5) finally by the obtained solidliquid mixture filtering and washing of step 4, to the filtration cakes torrefaction that filtering and washing obtains, and
2h is roasted at 500 DEG C, roasting 2h obtains required cerium zirconium sosoloid at 650 DEG C.
Doped chemical described in step 1 is one or more of La, Pr, Y, Al, Hf；
The usage amount of modifying agent described in step 2 is the 10%-60% of the solution gross mass of step 1；
Drying means used in filtration cakes torrefaction is freeze-drying in step 5.
By adopting the above technical scheme, technical effect of the invention has:
Of the invention preparation method is simple, is not related to the use of macromolecule organic in preparation process, to environment friend
It is good, and industrialized production easy to accomplish.The specific surface area with higher of cerium zirconium sosoloid synthesized by the present invention and high-temperature stable
Property, the cerium zirconium sosoloid specific surface area obtained after 500 DEG C of roasting 2h, 650 DEG C of roasting 2h is 70-170 m2/ g, at 1000 DEG C
Specific surface area > 30 m after roasting 4h2/g。
Specific embodiment
Embodiment 1:
Weigh 1.083g La (NO3)3•6H2O、0.958g Y(NO3)3•6H2O、13.024g Ce(NO3)3•6H2O、
4.834g ZrOCl2•8H2O is dissolved in 150mL deionized water, and 18g carbon black is added and in above-mentioned solution and stirs 2h, molten to each salt
5mL H is added after sufficiently being adsorbed by carbon black in liquid ion2O2And continue to stir 1h, NH is added in the above-mentioned salting liquid prepared4HCO3It is molten
In liquid, a small amount of NH is added after being added dropwise3•H2O makes pH value of solution=9, ageing reaction 4h, and filtering and washing is freeze-dried, 500 DEG C
Lower roasting 2h, roasting 2h obtains required cerium zirconium sosoloid at 650 DEG C, and testing its specific surface area is 90 m2/ g, at 1000 DEG C
Its aging specific surface is 32 m after roasting 4h2/g。
Embodiment 2:
Weigh 1.326g La (NO3)3•6H2O、7.57g Ce(NO3)3•6H2O、15.66g ZrOCl2•8H2O、12.21g
Al(NO3)3•9H2O is dissolved in 100mL deionized water, and 30g carbon black is added in above-mentioned solution and stirs 2h, to each salting liquid from
3mL H is added after sufficiently being adsorbed by carbon black in son2O2And continue to stir 1h, NH is added in the above-mentioned salting liquid prepared3•H2O solution
In, and pH=9 are kept, ageing reaction 4h, filtering and washing are freeze-dried after being added dropwise, and are roasted 2h at 500 DEG C, are roasted at 650 DEG C
It burns 2h and obtains required cerium zirconium sosoloid, testing its specific surface area is 130 m2/ g, table is compared in its aging after roasting 4h at 1000 DEG C
Face is 38 m2/g。
Embodiment 3: 0.744g La (NO is weighed3)3•6H2O、14g Ce(NO3)3•6H2O、7.254g ZrOCl2•8H2O、
1.658g Pr(NO3)3•6H2O is dissolved in 100mL deionized water, and 30g active carbon is added and in above-mentioned solution and stirs 2h, to each
5mL H is added after being sufficiently tightly held by activated carbon in salting liquid ion2O2And continue to stir 1h, the above-mentioned salting liquid prepared is added
NH3•H2In O solution, and pH=9 keeping, ageing reaction 4h, filtering and washing are freeze-dried after being added dropwise, 2h is roasted at 500 DEG C,
2h is roasted at 650 DEG C and obtains required cerium zirconium sosoloid, and testing its specific surface area is 75 m2/ g roasts after 4h it at 1000 DEG C
Aging specific surface is 34 m2/g。
Embodiment 4: 0.958g Y (NO is weighed3)3•6H2O、10.853g Ce(NO3)3•6H2O、4.834g ZrOCl2•
8H2O、1.088g Pr(NO3)3•6H2O is dissolved in 100mL deionized water, and 58g carbon black is added in above-mentioned solution and stirs 2h,
5mL H is added after each salting liquid ion is sufficiently adsorbed by carbon black2O2And continue to stir 1h, the above-mentioned salting liquid prepared is added
NH4HCO3In solution, a small amount of NH is added after being added dropwise3•H2O makes pH value of solution=9, and ageing reaction 4h, filters after being added dropwise
Washing is freeze-dried, and 2h is roasted at 500 DEG C, and roasting 2h obtains required cerium zirconium sosoloid at 650 DEG C, tests its specific surface area
For 82 m2/ g, its aging specific surface is 32 m after 4h is roasted at 1000 DEG C2/g。
Claims (2)
1. a kind of preparation method of high-ratio surface high temperature resistant cerium zirconium solid solution, it is characterized in that: including the following steps:
(1) according to mass ratio be 10-80:3.5-50:0.8-15 weigh soluble cerium salt, soluble zirconates and doped chemical can
Soluble, which is dissolved in deionized water, is made solution, and the doped chemical is one or more of La, Pr, Y, Ai, Hf；
(2) one of carbon black, activated carbon or graphene are added in the solution of step 1 as modifying agent, the modifying agent
Usage amount be step 1 solution gross mass 10%-60%；
(3) H is added after the solution of step 2 is sufficiently mixed uniformly2O2, H2O2Additional amount be the 30%-of soluble cerium salt quality
50%；
(4) solution of step 3 is added drop-wise to containing NH3•H2O or NH4HCO3In the precipitating reagent of middle one or two, pH value of solution is kept
=8-10, the solidliquid mixture that then ageing reaction 4h is obtained；
(5) finally by the obtained solidliquid mixture filtering and washing of step 4, to the filtration cakes torrefaction that filtering and washing obtains, and 500
2h is roasted at DEG C, roasting 2h obtains required cerium zirconium sosoloid at 650 DEG C.
2. the preparation method of high-ratio surface high temperature resistant cerium zirconium solid solution according to claim 1, it is characterized in that: in step 5
Drying means used in filtration cakes torrefaction is freeze-drying.
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| CN108499338A (en) * | 2018-04-04 | 2018-09-07 | 成都达奇环境科技有限公司 | A kind of denitrification apparatus |
| CN108499556B (en) * | 2018-04-04 | 2021-05-04 | 成都达奇环境科技有限公司 | Low-temperature denitration catalyst and preparation method thereof |
| CN108640151B (en) * | 2018-06-11 | 2020-07-14 | 东南大学 | Aluminum-containing zirconium oxide hollow microsphere and preparation method thereof |
| CN109794252B (en) * | 2019-01-16 | 2022-06-10 | 山东国瓷功能材料股份有限公司 | Magnetic cerium-zirconium composite oxide and preparation method and application thereof |
| CN109761260B (en) * | 2019-03-27 | 2021-10-12 | 淄博加华新材料有限公司 | Rare earth and zirconium doped cerium dioxide and preparation method thereof |
| CN113117663A (en) * | 2021-04-21 | 2021-07-16 | 上海交通大学 | Porous cerium oxide doped zirconia material and preparation method and application thereof |
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| CN104437530B (en) * | 2014-12-24 | 2016-05-25 | 西安元创化工科技股份有限公司 | A kind of preparation method of denitrating catalyst |
| CN105013457B (en) * | 2015-06-19 | 2018-04-17 | 云南中烟工业有限责任公司 | A kind of high oxygen storage capacity cerium zirconium sosoloid prepared using tobacco plant as template and preparation method thereof |
| CN105771955A (en) * | 2016-04-14 | 2016-07-20 | 江门市科恒实业股份有限公司 | Preparation method of ceria-zirconia solid solution |
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