CN103350003A - Preparation method of CeO2-ZrO2-Al2O3 oxygen-storage material - Google Patents
Preparation method of CeO2-ZrO2-Al2O3 oxygen-storage material Download PDFInfo
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- CN103350003A CN103350003A CN2013102621647A CN201310262164A CN103350003A CN 103350003 A CN103350003 A CN 103350003A CN 2013102621647 A CN2013102621647 A CN 2013102621647A CN 201310262164 A CN201310262164 A CN 201310262164A CN 103350003 A CN103350003 A CN 103350003A
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Abstract
The invention discloses a preparation method of a CeO2-ZrO2-Al2O3 oxygen-storage material, and relates to a microwave calcination and coprecipitation preparation method for an oxygen-storage material for automobile exhaust catalytic purification. The preparation method is characterized in that the CeO2-ZrO2-Al2O3 oxygen-storage material is prepared from Ce(NO3)3.6H2O, ZrOCl2.8H2O and Al(NO3)3.6H2O after preparing a CeO2-ZrO2-Al2O3 precursor through coprecipitation and implementing microwave calcination. The preparation method has the effects and advantages that the CeO2-ZrO2-A12O3 solid solution oxygen-storage material, which is prepared at relatively low temperature through a microwave calcination technology, is simple in preparation process, low in cost, and remarkable in oxygen-storage capacity and thermal stability effect.
Description
Technical field
A kind of CeO
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material relates to a kind of microwave calcination co-precipitation preparation method of the hydrogen-storing material of using for catalytic cleaning of car tail gas.
Background technology
Vehicle exhaust is the one of the main reasons that causes atmosphere pollution, has caused the countries in the world great attention, drops into substantial contribution, technology and manpower and administers.All the time, to support noble metal formation three-way catalyst on the inorganic oxides such as cerium oxide the purifying and catalyzing processing is carried out in motor vehicle exhaust emission.In this three-way catalyst, noble metal plays the effect of reduction of nitrogen oxide reaction and carbon monoxide and oxidation reactions of hydrocarbons.In addition, inorganic oxide plays and increases the noble metal specific area, thereby and divergent reaction produce the agglomeration that heat has suppressed noble metal.Particularly cerium oxide has oxygen storage capacity, can optimize above-mentioned oxidation reaction and reduction reaction.But when using three-way catalyst under the hot conditions, cerium oxide meeting grain growth causes specific area to reduce, and oxygen storage capacity descends.Therefore, the heat endurance that improves cerium oxide seems particularly important, has also carried out a large amount of research both at home and abroad.
For example: domestic publication number CN101549256A discloses a kind of hydrogen-storing material for catalytic cleaning of car tail gas.Take cerous nitrate, zirconium nitrate and iron oxide as raw material, adopt the conventional calcining of sol-gel process to prepare hydrogen-storing material.Its shortcoming is: not exclusively, easily powder reuniting, complex process, crystal grain is relatively slightly and even not for the cerium zirconium composite of generation.In addition, Japanese's application publication number CN101484240A discloses a kind of hydrogen-storing material, and the 2nd particle and the conventional calcining of noble metal of the 1st particle that is made of the composite oxides of the rare earth element beyond the composite oxides of cerium and zirconium or cerium, the cerium and zirconium, the composite oxides that contain rare earth element, alkali metal and zirconium form solid solution.Its shortcoming is: mix between the particle inhomogeneous, cost is high and complex process etc.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists for above-mentioned technology, provides a kind of and can adopt cheaply industrial raw material, obtains CeO at a lower temperature
2-ZrO
2-Al
2O
3The solid solution hydrogen-storing material, preparation technology is simple, cost is low, and oxygen storage capacity and the significant CeO of thermal stability result
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material.
The objective of the invention is to be achieved through the following technical solutions.
A kind of CeO
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material is characterized in that the (NO with Ce
3)
36H
2O, ZrOCl
28H
2O and Al (NO
3)
36H
2O is raw material, obtains CeO through co-precipitation
2-ZrO
2-Al
2O
3Presoma gets CeO through microwave calcination
2-ZrO
2-Al
2O
3Hydrogen-storing material.
A kind of microwave calcination co-precipitation CeO of the present invention
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material is characterized in that the step of its preparation process comprises:
(1) preparation Ce (NO
3)
36H
2O, ZrOCl
28H
2O and Al (NO
3)
36H
2The mixing salt solution of O;
(2) close H in the salting liquid at concrete
2O
2With Ce
3+Be oxidized to Ce
4+, add again PVAC polyvinylalcohol, make A solution;
(3) preparation ammonium carbonate and ammoniacal liquor cushioning liquid B;
(4) adopt cocurrent process to mix A solution and solution B, carry out precipitation reaction, carry out again ageing, filtration, make CeO
2-ZrO
2-Al
2O
3The hydrogen-storing material presoma;
(5) with the CeO that makes
2-ZrO
2-Al
2O
3The hydrogen-storing material presoma carries out microwave sintering, makes CeO
2-ZrO
2-Al
2O
3Hydrogen-storing material.
A kind of microwave calcination co-precipitation CeO of the present invention
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material is characterized in that the preparation Ce (NO for preparing in the step (1)
3)
36H
2O, ZrOCl
28H
2O and Al (NO
3)
36H
2In the mixing salt solution of O, Ce (NO
3)
36H
2O, ZrOCl
28H
2O and Al (NO
3)
36H
2The mol ratio of O is Ce:Zr:Al=1:1:1, and concentration is 150g/L.
A kind of microwave calcination co-precipitation CeO of the present invention
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material is characterized in that step (2) is that the adding volumetric concentration is 2%-5%H
2O
2With Ce
3+Be oxidized to Ce
4+, solution becomes light yellowly by colourless, adds the PVA of 5%-10% again, and stirs 30-60min.
A kind of microwave calcination co-precipitation CeO of the present invention
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material, it is characterized in that step (3) preparation ammonium carbonate and ammoniacal liquor cushioning liquid be with ammonium carbonate and ammoniacal liquor according to mass ratio 4-3:2-3, add that deionized water is mixed with, ammonium radical ion concentration is 3mol/L.
A kind of microwave calcination co-precipitation CeO of the present invention
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material is characterized in that step (4) A solution and solution B adopt by volume 1:1 mixing of cocurrent process; Mixed process constantly stirs, and the control solution PH is 8-10.
A kind of microwave calcination co-precipitation CeO of the present invention
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material is characterized in that step (4) ageing process is at 85-95 ℃ of lower ageing 4-8h.
A kind of microwave calcination co-precipitation CeO of the present invention
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material, the microwave calcination process that it is characterized in that step (5) are the CeO that will get
2-ZrO
2-Al
2O
3Take the microwave drying heating power as 10-20kw, be 10-30min drying time to the hydrogen-storing material presoma in the industrial microwave oven of 2.45GHz frequency; The microwave calcination heating power is 15-40kw, and be 25-40min heat time heating time; Microwave sintering oxidation heating power is 45-70kw, and heating-up temperature is 550-650 ℃, and temperature retention time is 1-3h.
A kind of microwave calcination co-precipitation CeO of the present invention
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material is with technical grade Ce (NO
3)
36H
2O, ZrOCl
28H
2O and Al (NO
3)
36H
2O is primary raw material, adds an amount of oxidant H
2O
2, precipitating reagent (ammonium carbonate and NH
3H
2The cushioning liquid of O), expanding agent PVA, CeO is prepared in co-precipitation
2-ZrO
2-Al
2O
3The hydrogen-storing material presoma is prepared CeO by microwave calcination
2-ZrO
2-Al
2O
3Hydrogen-storing material.It is advantageous that: 1. need not complicated technological process, preparation process is simple, price is lower; 2. by microwave calcination CeO
2-ZrO
2-Al
2O
3The mode of hydrogen-storing material presoma realizes CeO under the lower temperature
2-ZrO
2-Al
2O
3The preparation of hydrogen-storing material has that specific area is large, oxygen storage capacity is strong, thermal stability is good, anti-aging characteristics such as strong.The present invention adopts the microwave calcination technology to prepare hydrogen-storing material, compare with conventional method for calcinating, microwave calcination have selectively add thermal material, heating rate is fast, the efficiency of heating surface is high, chemical reaction is had catalytic action, is conducive to promote solid phase reaction and homogenising, is easy to the significant advantage such as automatically control, so microwave calcination is expected to one of effective way that becomes industrial cleaner production.Aspect hydrogen-storing material, also only be confined to the preparation that microwave drying and conventional calcining presoma form hydrogen-storing material in present document and the patented technology, the research that forms hydrogen-storing material solid solution for microwave calcination technique is not also found.In sum, the present invention adopts the cheaply CeO of industrial raw material by co-precipitation is obtained
2-ZrO
2-Al
2O
3Precursor carries out calcination processing under the microwave, obtains at a lower temperature CeO
2-ZrO
2-Al
2O
3The solid solution hydrogen-storing material, not only preparation technology is simple, cost is low, and expection oxygen storage capacity and thermal stability result is remarkable.
Description of drawings
Fig. 1 is the process chart of the inventive method.
The specific embodiment
A kind of CeO
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material is with Ce (NO
3)
36H
2O, ZrOCl
28H
2O and Al (NO
3)
36H
2O is raw material, obtains CeO through co-precipitation
2-ZrO
2-Al
2O
3Presoma gets CeO through microwave calcination
2-ZrO
2-Al
2O
3Hydrogen-storing material; Specific operation process is as follows:
(1) preparation of salting liquid: with Ce (NO
3)
36H
2O, ZrOCl
28H
2O and Al (NO
3)
36H
2O adds deionized water and is mixed with salting liquid;
(2) add 2-5%H
2O
2With Ce
3+Be oxidized to Ce
4+, solution becomes light yellowly by colourless, adds the PVA of 5-10% again, and stirs 30-60min; Obtain solution A;
(3) preparation of buffer base (BB) solution: according to mass ratio 4-3:2-3, adding deionized water, to be mixed with solution B for subsequent use with ammonium carbonate and ammoniacal liquor.
(4) co-precipitation: adopt cocurrent process that solution A and solution B are mixed also constantly stirring, the control solution PH is 8-10.Until purplish red precipitation fully after, with it at 85-95 ℃ of lower ageing 4-8h; With the solution suction filtration that obtains, the filter cake of acquisition namely is required CeO
2-ZrO
2-Al
2O
3The hydrogen-storing material presoma.
(5) microwave calcination: the CeO that obtains
2-ZrO
2-Al
2O
3Take the microwave drying heating power as 10-20kw, be 10-30min drying time to the hydrogen-storing material presoma in the industrial microwave oven of 2.45GHz frequency; The microwave calcination heating power is 15-40kw, and be 25-40min heat time heating time; Microwave sintering oxidation heating power is 45-70kw, and heating-up temperature is 550-650 ℃, and temperature retention time is 1-3h, namely obtains required product.
Embodiment 1
At first will get 25%Ce (NO
3)
36H
2O, 25%Zr (NO
3)
48H
2O and 50%Al (NO
3)
36H
2O adds deionized water and is mixed with mixing salt solution, adds 2%H
2O
2With Ce
3+Be oxidized to Ce
4+, solution becomes light yellowly by colourless, adds 5% PVA again, and stirs 30min.Again ammonium carbonate and ammoniacal liquor are made into the buffer base (BB) solution for standby according to quality 1:1.Adopt cocurrent process mixing salt solution and the buffer base (BB) solution for preparing to be passed through and stream mixing and continuous stirring, the control solution PH is 8.Until purplish red precipitation fully after, with it at 85 ℃ of lower ageing 8h.The solution that ageing is complete carries out vacuum filtration and obtains CeO
2-ZrO
2-Al
2O
3Hydrogen-storing material presoma filter cake A.With the CeO that obtains
2-ZrO
2-Al
2O
3Take the microwave drying heating power as 10kw, be 30min drying time to hydrogen-storing material presoma filter cake in 2.45GHz frequency industrial microwave oven; The microwave calcination heating power is 15kw, and be 30min heat time heating time; Microwave sintering oxidation heating power is 45kw, and heating-up temperature is 650 ℃, and temperature retention time is the 3h calcining, namely obtains required product.Sample microwave calcination and conventional calcining (650 ℃ and be incubated 3h), and carry out burin-in process through 1000 ℃ of conventional calcining 12h, contrast sees the following form.
Embodiment 2
At first will get 25%Ce (NO
3)
36H
2O, 25%Zr (NO
3)
48H
2O and 50%Al (NO
3)
36H
2O adds deionized water and is mixed with mixing salt solution, adds 3%H
2O
2With Ce
3+Be oxidized to Ce
4+, solution becomes light yellowly by colourless, adds 7.5% PVA again, and stirs 45min.Again ammonium carbonate and ammoniacal liquor are made into the buffer base (BB) solution for standby according to quality 3:2.Adopt cocurrent process mixing salt solution and the buffer base (BB) solution for preparing to be led to and stream mixing and continuous stirring, the control solution PH is 9.Until purplish red precipitation fully after, with it at 90 ℃ of lower ageing 6h.The solution that ageing is complete carries out vacuum filtration and spray-drying obtains CeO
2-ZrO
2-Al
2O
3Hydrogen-storing material presoma powder B.With the CeO that obtains
2-ZrO
2-Al
2O
3Take the microwave drying heating power as 15kw, be 20min drying time to hydrogen-storing material presoma filter cake in 2.45GHz frequency industrial microwave oven; The microwave calcination heating power is 20kw, and be 25min heat time heating time; Microwave sintering oxidation heating power is 60kw, and heating-up temperature is 600 ℃, and temperature retention time is the 2h calcining, namely obtains required product.Sample microwave calcination and conventional calcining (600 ℃ and be incubated 2h),, and carry out burin-in process through 1000 ℃ of conventional calcining 12h, contrast sees the following form.
Embodiment 3
At first will get 25%Ce (NO
3)
36H
2O, 25%Zr (NO
3)
48H
2O and 50%Al (NO
3)
36H
2O adds deionized water and is mixed with mixing salt solution, adds 5%H
2O
2With Ce
3+Be oxidized to Ce
4+, solution becomes light yellowly by colourless, adds 10% PVA again, and stirs 60min.Again ammonium carbonate and ammoniacal liquor are made into the buffer base (BB) solution for standby according to quality 4:3.Adopt cocurrent process mixing salt solution and the buffer base (BB) solution for preparing to be passed through and stream mixing and continuous stirring, the control solution PH is 10.Until purplish red precipitation fully after, with it at 95 ℃ of lower ageing 4h.The solution that ageing is complete carries out vacuum filtration and carries out spray-drying obtaining CeO
2-ZrO
2-Al
2O
3Hydrogen-storing material presoma powder C.With the CeO that obtains
2-ZrO
2-Al
2O
3Take the microwave drying heating power as 20kw, be 10min drying time to hydrogen-storing material presoma filter cake in 2.45GHz frequency industrial microwave oven; The microwave calcination heating power is 40kw, and be 20min heat time heating time; Microwave sintering oxidation heating power is 70kw, and heating-up temperature is 550 ℃, and temperature retention time is the 1h calcining, namely obtains required product.Sample microwave calcination and conventional calcining (550 ℃ and be incubated 1h), and carry out burin-in process through 1000 ℃ of conventional calcining 12h, contrast sees the following form.
With the CeO that obtains
2-ZrO
2-Al
2O
3Every part of hydrogen-storing material presoma powder A, B, C get 500g, compare respectively structure such as following table with 2450MHz industrial microwave oven calcine technology and conventional calcine technology:
A kind of employing coprecipitation that the present invention proposes prepares CeO
2-ZrO
2-Al
2O
3The hydrogen-storing material presoma also carries out microwave calcination and prepares CeO
2-ZrO
2-Al
2O
3The prescription of hydrogen-storing material and method, be described by preferred embodiment, person skilled obviously can be within not breaking away from content of the present invention, spirit and scope to structure as herein described with equipment is changed or suitably change and combination, realize the technology of the present invention.Special needs to be pointed out is, the replacement that all are similar or change are apparent to the art technology talent, and they are deemed to be included in spirit of the present invention, scope and the content.
Claims (8)
1. CeO
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material is characterized in that the (NO with Ce
3)
36H
2O, ZrOCl
28H
2O and Al (NO
3)
36H
2O is raw material, obtains CeO through co-precipitation
2-ZrO
2-Al
2O
3Presoma gets CeO through microwave calcination
2-ZrO
2-Al
2O
3Hydrogen-storing material.
2. a kind of microwave calcination co-precipitation CeO according to claim 1
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material is characterized in that the step of its preparation process comprises:
(1) preparation Ce (NO
3)
36H
2O, ZrOCl
28H
2O and Al (NO
3)
36H
2The mixing salt solution of O;
(2) close H in the salting liquid at concrete
2O
2With Ce
3+Be oxidized to Ce
4+, add again PVAC polyvinylalcohol, make A solution;
(3) preparation ammonium carbonate and ammoniacal liquor cushioning liquid B;
(4) adopt cocurrent process to mix A solution and solution B, carry out precipitation reaction, carry out again ageing, filtration, make CeO
2-ZrO
2-Al
2O
3The hydrogen-storing material presoma;
(5) with the CeO that makes
2-ZrO
2-Al
2O
3The hydrogen-storing material presoma carries out microwave sintering, makes CeO
2-ZrO
2-Al
2O
3Hydrogen-storing material.
3. a kind of microwave calcination co-precipitation CeO according to claim 2
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material is characterized in that the preparation Ce (NO for preparing in the step (1)
3)
36H
2O, ZrOCl
28H
2O and Al (NO
3)
36H
2In the mixing salt solution of O, Ce (NO
3)
36H
2O, ZrOCl
28H
2O and Al (NO
3)
36H
2The mol ratio of O is Ce:Zr:Al=1:1:1, and concentration is 150g/L.
4. a kind of microwave calcination co-precipitation CeO according to claim 2
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material is characterized in that step (2) is that the adding volumetric concentration is 2%-5%H
2O
2With Ce
3+Be oxidized to Ce
4+, solution becomes light yellowly by colourless, adds the PVA of 5%-10% again, and stirs 30-60min.
5. a kind of microwave calcination co-precipitation CeO according to claim 2
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material, it is characterized in that step (3) preparation ammonium carbonate and ammoniacal liquor cushioning liquid be with ammonium carbonate and ammoniacal liquor according to mass ratio 4-3:2-3, add that deionized water is mixed with, ammonium radical ion concentration is 3mol/L.
6. a kind of microwave calcination co-precipitation CeO according to claim 2
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material is characterized in that step (4) A solution and solution B adopt by volume 1:1 mixing of cocurrent process; Mixed process constantly stirs, and the control solution PH is 8-10.
7. a kind of microwave calcination co-precipitation CeO according to claim 2
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material is characterized in that step (4) ageing process is at 85-95 ℃ of lower ageing 4-8h.
8. a kind of microwave calcination co-precipitation CeO according to claim 2
2-ZrO
2-Al
2O
3The preparation method of hydrogen-storing material, the microwave calcination process that it is characterized in that step (5) are the CeO that will get
2-ZrO
2-Al
2O
3Take the microwave drying heating power as 10-20kw, be 10-30min drying time to the hydrogen-storing material presoma in the industrial microwave oven of 2.45GHz frequency; The microwave calcination heating power is 15-40kw, and be 25-40min heat time heating time; Microwave sintering oxidation heating power is 45-70kw, and heating-up temperature is 550-650 ℃, and temperature retention time is 1-3h.
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103846089A (en) * | 2014-01-14 | 2014-06-11 | 台州欧信环保净化器有限公司 | Homogeneous solid-solution cerium-zirconium-cobalt-aluminum composite material and preparation method thereof |
| CN108325514A (en) * | 2018-05-10 | 2018-07-27 | 北京工业大学 | A kind of preparation method improving cerium base SCR catalyst low temperature active |
| CN108947570A (en) * | 2018-09-07 | 2018-12-07 | 长沙理工大学 | A kind of porous ceramics microballoon and preparation method thereof |
| CN112473575A (en) * | 2020-11-19 | 2021-03-12 | 浙江工业大学 | CeO (CeO)2-Ag2O(PdO)/SiO2Preparation method and application of composite aerogel |
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| ZHENLING WEI等: "Preparation and property investigation of CeO2-ZrO2-Al2O3 oxygen-storage compounds", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103846089A (en) * | 2014-01-14 | 2014-06-11 | 台州欧信环保净化器有限公司 | Homogeneous solid-solution cerium-zirconium-cobalt-aluminum composite material and preparation method thereof |
| CN103846089B (en) * | 2014-01-14 | 2015-12-09 | 台州欧信环保净化器有限公司 | A kind of homogeneous solid solution cerium zirconium cobalt aluminium composite material and preparation method thereof |
| CN108325514A (en) * | 2018-05-10 | 2018-07-27 | 北京工业大学 | A kind of preparation method improving cerium base SCR catalyst low temperature active |
| CN108325514B (en) * | 2018-05-10 | 2021-01-15 | 北京工业大学 | Preparation method for improving low-temperature activity of cerium-based SCR catalyst |
| CN108947570A (en) * | 2018-09-07 | 2018-12-07 | 长沙理工大学 | A kind of porous ceramics microballoon and preparation method thereof |
| CN112473575A (en) * | 2020-11-19 | 2021-03-12 | 浙江工业大学 | CeO (CeO)2-Ag2O(PdO)/SiO2Preparation method and application of composite aerogel |
| CN112473575B (en) * | 2020-11-19 | 2023-09-19 | 浙江工业大学 | CeO (CeO) 2 -Ag 2 O(PdO)/SiO 2 Preparation method and application of composite aerogel |
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Application publication date: 20131016 |