CN103861663A - Composite precipitating agent - Google Patents
Composite precipitating agent Download PDFInfo
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- CN103861663A CN103861663A CN201210545791.7A CN201210545791A CN103861663A CN 103861663 A CN103861663 A CN 103861663A CN 201210545791 A CN201210545791 A CN 201210545791A CN 103861663 A CN103861663 A CN 103861663A
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- ammonium carbonate
- ammoniacal liquor
- carbonic hydroammonium
- compound precipitants
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Abstract
The invention provides a composite precipitating agent. The composite precipitating agent comprises two or three ingredients selected from ammonium bicarbonate, ammonium carbonate, and ammonium hydroxide; can be used for preparation of novel oxygen storage materials; and is capable of stabilizing oxygen storage material preparation technology.
Description
Technical field
The present invention relates to purifying vehicle exhaust process field, relate to specifically a kind of compound precipitants.
Background technology
The discharge that reduces industry and motor vehicle pernicious gas is one of society sixty-four dollar question, and the effective way addressing this problem is to use the three-way catalyst that can simultaneously transform CO, HC, NOx.Cerium zirconium sosoloid has stronger oxygen storage capacity, becomes the important component part of preparing automobile exhaust pollution emission control three-way catalyst.
Although cerium zirconium sosoloid at high temperature can keep good storage oxygen performance, the heat endurance of texture is poor, and specific surface is lower, and the Tetragonal zirconium dioxide that easily dissociates under higher temperature makes single Emission in Cubic be transformed into multiphase coexistence.Along with the increasingly stringent of automobile emissions standards and petrol engine are to the development of lean-burn direction, what require that hydrogen-storing material has higher high temperature specific surface heat endurance and a Geng Gao stores oxygen performance.Chinese patent 1449863A discloses a kind of nano cerium zirconium based compound oxide, make by the method for hydrogen peroxide and ammoniacal liquor co-precipitation, but its specific surface is lower, imporosity.Chinese patent CN1935359A and CN1962051A also disclose the preparation of cerium zirconium compound oxide material, but these cerium zirconium base oxide solid solution specific surfaces of reporting are not high, and imporosity, complicated process of preparation, and during for catalyst carrier, catalytic activity is lower.
Summary of the invention
First the present invention provides a kind of compound precipitants, and this compound precipitants contains two or three in carbonic hydroammonium, ammoniacal liquor or ammonium carbonate;
Wherein the mass concentration of ammoniacal liquor is 20%;
Preferably, this compound precipitants comprises carbonic hydroammonium and ammoniacal liquor, and wherein the part by weight of carbonic hydroammonium and ammoniacal liquor is 1:0.6-6.5; Further preferred, the part by weight of carbonic hydroammonium and ammoniacal liquor is 1:2.2;
Preferably, this compound precipitants comprises ammonium carbonate and ammoniacal liquor, and wherein the part by weight of ammonium carbonate and ammoniacal liquor is 1:0.5-5; Further preferred, the part by weight of ammonium carbonate and ammoniacal liquor is 1:1.5;
Preferably, this compound precipitants comprises carbonic hydroammonium and ammonium carbonate, and wherein the part by weight of carbonic hydroammonium and ammonium carbonate is 1:0.6-7; Further preferred, the part by weight of carbonic hydroammonium and ammonium carbonate is 1:1;
Preferably, this compound precipitants comprises carbonic hydroammonium, ammonium carbonate and ammoniacal liquor, and wherein the part by weight of carbonic hydroammonium, ammonium carbonate and ammoniacal liquor is 0.5-1:0.6-7:0.5-5; Further preferred, the part by weight of carbonic hydroammonium, ammonium carbonate and ammoniacal liquor is 0.5:1.0:0.5.
Prepare the method for above-mentioned compound precipitants for directly each component being mixed, when use, can add water to be mixed with solution.
This compound precipitants can be used for preparing novel hydrogen-storing material, in preparation process, pH value can be controlled stablely, be beneficial to precipitation reaction, is beneficial to control process conditions, and the technique that makes to prepare hydrogen-storing material is more stable.
The present invention also provides a kind of rare earth oxygen storage material, and this rare earth oxygen storage material is made up of cerium oxide, zirconia, lanthana, yittrium oxide.
Wherein the weight percent content of cerium oxide, zirconia, lanthana and yittrium oxide is respectively: cerium oxide 20-50%, zirconia 40-75%, lanthana 1-15%, yittrium oxide 3-15%;
Further preferred, the weight percent content of cerium oxide, zirconia, lanthana and yittrium oxide is respectively: cerium oxide 25-45%, zirconia 45-65%, lanthana 5-8%, yittrium oxide 5-12%;
Further preferred, the weight percent content of cerium oxide, zirconia, lanthana and yittrium oxide is respectively: cerium oxide 30-40%, zirconia 50-60%, lanthana 2-6%, yittrium oxide 6-9%.
Above-mentioned rare earth oxygen storage material prepares by the following method:
In aforesaid compound precipitants, add the nitrate solution of cerium, zirconium, yttrium, lanthanum;
The sediment that above-mentioned reaction obtains carries out ripening 16-50 hour at 50 DEG C-150 DEG C;
The rare earth oxygen storage material obtaining can carry out press filtration, washing, roasting and pulverizing again; The rare earth oxygen storage material obtaining at 700 DEG C roasting 4 hours and at 1000 DEG C roasting after 4 hours, there is respectively at least 110m
2/ g and 40m
2the specific area of/g.
Use the synthetic hydrogen-storing material of said method, technique is simple, and synthetic hydrogen-storing material specific area is high, and storage oxygen performance is high, and during for the catalyst carrier of vehicle exhaust processing, catalytic activity is high.
Hydrogen-storing material of the present invention has higher specific area and storage oxygen performance, uses this material can improve the catalytic activity of auto-exhaust catalyst, can reduce the consumption of noble metal, thereby reduce production costs simultaneously.
Brief description of the drawings
1000 DEG C of XRD collection of illustrative plates of aging 4 hours of Fig. 1 embodiment 4 hydrogen-storing material;
1000 DEG C of hydrogen reducing collection of illustrative plates of aging 4 hours of Fig. 2 embodiment 4 hydrogen-storing material.
Detailed description of the invention
Embodiment 1
Prepare compound precipitants: get carbonic hydroammonium 51.1kg, ammoniacal liquor 50kg and a small amount of auxiliary agent (4kg hydrogen peroxide and 1.0kg n-octyl alcohol), mix.Wherein carbonic hydroammonium is white crystalline powder shape solid, and ammonia concn is 20%(mass concentration).Add 155.0kg deionized water to be mixed with mixed precipitation agent solution.
Preparation zirconium nitrate solution, gets zirconium carbonate 11.71kg, nitric acid 10.84kg.Zirconium carbonate is poured in salpeter solution, obtained product zirconium nitrate after reacting about 30min;
Preparation mixed nitrate solution: get 9.84kg cerous nitrate, 2.27kg lanthanum nitrate and 1.89kg yttrium nitrate, add 40 degrees Celsius of deionized waters of 450kg and surfactant (softex kw) 2.6kg to be stirred to completely and dissolve.Then the above-mentioned zirconium nitrate solution preparing is joined in this mixed solution and stirs 30min.
Constant rotational speed stirring under, above-mentioned mixed nitrate solution is slowly dropped to the precursor solution that obtains reaction in mixed precipitation agent solution.
Be placed in reactor static solution, temperature in the kettle risen to 90 DEG C of insulations and within 40 hours, carry out ripening.
After ripening finishes, obtain suspension.Filter this suspension with plate and frame filter press, obtain filter cake, then clean filter cake 2 times with deionization hot water, after cleaning, filter, and add specific surface activating agent (1kg softex kw) cleaning for the second time while stirring, keep stirring 30 minutes.
Washing and filter after the 180 DEG C of dry roastings 4 hours at 700 DEG C in air after 24 hours in air of the filter cake that obtains, obtain hydrogen-storing material product.Then this product roasting 4 hours at 1000 DEG C in air that takes a morsel, obtains the ageing products of this hydrogen-storing material.
Embodiment 2
The present embodiment is with embodiment 1, and difference is that the compound precipitants using comprises carbonic hydroammonium 50kg, ammoniacal liquor 75kg and a small amount of auxiliary agent (4kg hydrogen peroxide and 1.0kg n-octyl alcohol).
Embodiment 3
The present embodiment is with embodiment 1, and difference is that the compound precipitants using comprises carbonic hydroammonium 50kg, ammonium carbonate 50kg and a small amount of auxiliary agent (4kg hydrogen peroxide and 1.0kg n-octyl alcohol).
Embodiment 4
The present embodiment is with embodiment 1, and difference is that the compound precipitants using comprises carbonic hydroammonium 25kg, ammonium carbonate 75kg and a small amount of auxiliary agent (4kg hydrogen peroxide and 1.0kg n-octyl alcohol).
Embodiment 5
The present embodiment is with embodiment 1, and difference is that the compound precipitants using comprises ammonium carbonate 50kg, ammoniacal liquor 50kg and a small amount of auxiliary agent (4kg hydrogen peroxide and 1.0kg n-octyl alcohol).
Embodiment 6
The present embodiment is with embodiment 1, and difference is that the compound precipitants using comprises ammonium carbonate 50kg, ammoniacal liquor 25kg and a small amount of auxiliary agent (4kg hydrogen peroxide and 1.0kg n-octyl alcohol).
Embodiment 7
The present embodiment is with embodiment 1, and difference is that the compound precipitants using comprises carbonic hydroammonium 25kg, ammonium carbonate 25kg, ammoniacal liquor 25kg and a small amount of auxiliary agent (4kg hydrogen peroxide and 1.0kg n-octyl alcohol).
Embodiment 8
The present embodiment is with embodiment 1, and difference is that the compound precipitants using comprises carbonic hydroammonium 25kg, ammonium carbonate 25kg, ammoniacal liquor 50kg and a small amount of auxiliary agent (4kg hydrogen peroxide and 1.0kg n-octyl alcohol).
Embodiment 9
The hydrogen-storing material that embodiment 1-8 is prepared is roasting under different temperatures in air, and the specific area after heat treatment is in table 1, and unit is m
2/ g.
The specific area of hydrogen-storing material after table 1 roasting
Claims (9)
1. a compound precipitants, is characterized in that this compound precipitants contains two or three in carbonic hydroammonium, ammonium carbonate and ammoniacal liquor.
2. compound precipitants according to claim 1, is characterized in that this compound precipitants comprises carbonic hydroammonium and ammoniacal liquor, and wherein the part by weight of carbonic hydroammonium and ammoniacal liquor is 1:0.6-6.5.
3. compound precipitants according to claim 2, is characterized in that in this compound precipitants, the part by weight of carbonic hydroammonium and ammoniacal liquor is 1:2.2.
4. compound precipitants according to claim 1, is characterized in that this compound precipitants comprises ammonium carbonate and ammoniacal liquor, and wherein the part by weight of ammonium carbonate and ammoniacal liquor is 1:0.5:5.
5. compound precipitants according to claim 4, is characterized in that this compound precipitants comprises ammonium carbonate and ammoniacal liquor, and wherein the part by weight of ammonium carbonate and ammoniacal liquor is 1:1.5.
6. compound precipitants according to claim 1, is characterized in that this compound precipitants comprises carbonic hydroammonium and ammonium carbonate, and wherein the part by weight of carbonic hydroammonium and ammonium carbonate is 1:0.6-7.
7. compound precipitants according to claim 6, is characterized in that this compound precipitants comprises carbonic hydroammonium and ammonium carbonate, and wherein the part by weight of carbonic hydroammonium and ammonium carbonate is 1:1.
8. compound precipitants according to claim 1, is characterized in that this compound precipitants comprises carbonic hydroammonium, ammonium carbonate and ammoniacal liquor, and wherein the part by weight of carbonic hydroammonium, ammonium carbonate and ammoniacal liquor is 0.5-1:0.6-7:0.5-5.
9. compound precipitants according to claim 8, is characterized in that this compound precipitants comprises carbonic hydroammonium, ammonium carbonate and ammoniacal liquor, and wherein the part by weight of carbonic hydroammonium, ammonium carbonate and ammoniacal liquor is 0.5:1.0:0.5.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1449863A (en) * | 2003-04-28 | 2003-10-22 | 华东理工大学 | Nano Cerium-zirconium base compound oxide and preparation process thereof |
CN1817447A (en) * | 2006-01-05 | 2006-08-16 | 四川大学 | Hydrogen-storing material with low-cerium and production thereof |
CN101690890A (en) * | 2009-09-23 | 2010-04-07 | 中国海洋石油总公司 | Method for preparing high-thermal-stability cerium-based oxygen storage material |
CN101745375A (en) * | 2008-12-15 | 2010-06-23 | 比亚迪股份有限公司 | Cerium zirconium aluminum based multiple oxide material and preparing method thereof |
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2012
- 2012-12-14 CN CN201210545791.7A patent/CN103861663A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1449863A (en) * | 2003-04-28 | 2003-10-22 | 华东理工大学 | Nano Cerium-zirconium base compound oxide and preparation process thereof |
CN1817447A (en) * | 2006-01-05 | 2006-08-16 | 四川大学 | Hydrogen-storing material with low-cerium and production thereof |
CN101745375A (en) * | 2008-12-15 | 2010-06-23 | 比亚迪股份有限公司 | Cerium zirconium aluminum based multiple oxide material and preparing method thereof |
CN101690890A (en) * | 2009-09-23 | 2010-04-07 | 中国海洋石油总公司 | Method for preparing high-thermal-stability cerium-based oxygen storage material |
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Application publication date: 20140618 |