CN1552517A - Preparation of nano cerium-zirconium rare-earth composite fluorine compound solid solution based catalyst - Google Patents
Preparation of nano cerium-zirconium rare-earth composite fluorine compound solid solution based catalyst Download PDFInfo
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- CN1552517A CN1552517A CNA2003101174534A CN200310117453A CN1552517A CN 1552517 A CN1552517 A CN 1552517A CN A2003101174534 A CNA2003101174534 A CN A2003101174534A CN 200310117453 A CN200310117453 A CN 200310117453A CN 1552517 A CN1552517 A CN 1552517A
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Abstract
A process for preparing the catalyst based on the nano-class sosoloid of composite oxide of Ce, Zr and RE includes such steps as proportionally mixing the Ce-contained salt solution with Zr-contained one, neutralizing, depositing, filtering, washing depositing with deionized water, adding water, hydrothermal reacting in high-pressure reactor, filterint to obtain deposit, and supercritical drying. Its advantages are high crystallized level, small and uniform granularity, large specific surface area and high thermal stability.
Description
1, technical field:
The present invention relates to the catalyst based preparation method of nano-scale cerium zirconium complex rare-earth oxidate containing valuable metal solid solution, this type of catalyst is mainly used in the purifying vehicle exhaust catalyst aid, also can be used as other catalyst.
2, background technology:
Vehicle exhaust is one of main source of urban atmospheric pollution, is the important measures of guaranteeing environmental quality to the improvement of vehicle exhaust.At present, the measure of improvement is divided into emission controls by improving combustion and external purification.External purification mainly is to realize by the purifying vehicle exhaust catalytic unit, and the core of purifying vehicle exhaust catalytic unit is a catalyst.Nano-scale cerium zirconium complex rare-earth oxidate containing valuable metal solid solution is catalyst based to be a kind of catalyst aid of good purifying vehicle exhaust, because its adding, not only reduced the use amount of noble metal in the catalyst, and having improved catalytic activity, its oxygen storage capacity, mechanical strength and heat endurance all are improved.
Patent CN 1193948A discloses a kind of based on zirconia and cerium oxide composition, Preparation Method And The Use, 900 ℃ down the specific area of calcining after 6 hours be at least 30m
2/ g, and exist with the pure solid solution form of cerium oxide in zirconia.
Patent CN 1263868A discloses a kind of nanometer cerium zirconium oxide, and Preparation Method And The Use comprises the CeO of 4～98% (wt)
2ZrO with 1～95% (wt)
2, its composite oxides are to decompose and to obtain through preceding (the surpassing) that contain hydrazine or the hydrazonium salt thing that becomes under 200～1000 ℃.
Patent CN 1387943A discloses a kind of preparation technology based on cerium oxide and zirconia composite oxide solid solution, this composite oxide solid solution comprises cerium oxide 10～90% (wt), zirconia 10～90% (wt), it is characterized in that mixed reactant is behind alkali precipitation, sediment heat treatment, oven dry, calcining are made, be at least 35m in the specific area of calcining after 6 hours under 1000 ℃
2/ g, and exist with the pure solid solution form of cerium oxide in zirconia.
3, summary of the invention:
The objective of the invention is to overcome above-mentioned shortcoming and a kind of catalyst based method of Hydrothermal Preparation nano-scale cerium zirconium complex rare-earth oxidate containing valuable metal solid solution that adopts is provided.Calcine with catalyst based need not the passing through of nano-scale cerium zirconium complex rare-earth oxidate containing valuable metal solid solution that the present invention prepares, the crystal formation of the catalyst that obtains is a cubic system, crystallization degree height, crystal development are good, and particle diameter is little and be evenly distributed, specific area is big, Heat stability is good.
The present invention prepares the catalyst based method of nano-scale cerium zirconium complex rare-earth oxidate containing valuable metal solid solution, and it includes following steps:
1) salting liquid that will contain cerium mixes by goods institute's oxidation-containing cerium and zirconic molar percentage with the salting liquid that contains zirconium;
2) with alkaline matter with the mixture neutralization precipitation;
3) filter;
4) use deionized water washing sediment, wash to washing lotion and detect no chlorion existence with silver nitrate;
5) the cerium zirconium hydroxide that obtains and add water and put into autoclave and carry out hydro-thermal reaction after the washing;
6) after hydro-thermal reaction finishes, product is filtered, the sediment that obtains carries out supercritical drying and gets nano-scale cerium zirconium mixed oxide solid solution catalyst in same autoclave.
Above-mentioned steps 1) can add one or more rare earth element nitrate solution in.
Above-mentioned rare earth element nitrate can be obtained with nitric acid dissolve by lanthana, praseodymium oxide, neodymia, yittrium oxide.
Above-mentioned steps 1) except that the cerium zirconium, the molar percentage of the addition of other rare earth is 0～20% in.
Above-mentioned steps 2) adopt alkaline matter neutralization precipitation mixture, controlling its final pH value is 8.5～11.5.
Above-mentioned steps 2) alkaline matter that is adopted can be ammoniacal liquor, and the percentage by weight of its concentration is 10～28%, also can adopt the weak solution of NaOH.
Above-mentioned steps 2) precipitation temperature is 0～80 ℃.
Above-mentioned steps 5) hydrothermal reaction process control hydrothermal temperature is 140～300 ℃, and pressure is 0.6～4Mpa, and the time is 0.5～10h.
Above-mentioned steps 6) baking temperature is 100～300 ℃, and drying pressure is 7～10Mpa.
Above-mentioned steps 6) the nano-scale cerium zirconium mixed oxide solid solution catalyst of dry back gained comprises that the molar percentage of cerium oxide is 50～90%, zirconic molar percentage is 10～50%.
The present invention is owing to adopt Hydrothermal Preparation nano-scale cerium zirconium complex rare-earth oxidate containing valuable metal solid solution catalyst based, so the crystal formation of its product for preparing is a cubic system, crystallization degree height, crystal development are good, and particle diameter is little and be evenly distributed, specific area is big, Heat stability is good.Another characteristics of the present invention be after the hydro-thermal reaction in same reactor supercritical drying obtain product, need not to pass through again high-temperature calcination, thereby not only simplified operation, and the product specific area that makes is bigger, catalytic activity is better; Because reaction and drying are carried out at same reactor, have saved equipment investment, operating process is simpler, makes the powder granularity of gained controlled again, does not have reunion substantially.In addition, the present invention also is included in and can adds one or more other rare earth oxides in the cerium zirconium compound oxide solid solution, thereby further improves specific area, heat endurance, mechanical strength and the service life of catalyst, has improved its catalytic activity.The present invention not only technological process is simple, and the product quality height, and is free from environmental pollution.Catalyst based with the nano-scale cerium zirconium mixed oxide solid solution that the present invention makes, granularity is that specific area is greater than 100m between 5～20nm
2/ g, the proportioning of kind, quantity and the cerium zirconium of change additive can also make specific area up to 150～180m
2More than/the g, the specific area after 1000 ℃ calcining was worn out in 6 hours down is at least at 45m
2/ g.Should be noted that in the composite oxides of the present invention to have comprised hafnium, this is general and zirconium coexistence owing to hafnium in the mineral resources, and non-special reason does not need to separate in addition.The present invention is all significant catalyst based preparation method of nano-scale cerium zirconium complex rare-earth oxidate containing valuable metal solid solution of a kind of social benefit and economic benefit.
4, description of drawings:
Fig. 1 is the X-ray diffraction analysis chart with the product of the present invention's preparation;
Fig. 2 is the particle size distribution figure that records the product of embodiment 1 preparation with small-angle diffraction;
Fig. 3 is the particle size distribution figure that records the product of embodiment 2 preparations with small-angle diffraction;
Fig. 4 (a) is the TEM figure of the product of embodiment 3 preparations;
Fig. 4 (b) is the TEM figure of the product of embodiment 4 preparations.
5, the specific embodiment:
Embodiment 1:
Get cerous carbonate 30g, with the red fuming nitric acid (RFNA) dissolving, with mixing mutually after the basic zirconium chloride 25g dissolving, mix the back and come precipitation mixture with 25% (wt) ammoniacal liquor, control final pH=9.1, with the pure water washing, wash to washing lotion and detect no chlorion existence after precipitation is finished with silver nitrate.The cerium zirconium hydroxide that obtains after washing is good adds water, stirs into slurry with agitator, and slurry is put into autoclave carries out hydro-thermal reaction, 120 ℃ of control reaction temperatures, 8 hours time.After hydro-thermal reaction finishes, with the product cold filtration, the sediment that obtains is dissolved into slurry with ethanol, slurry is carried out supercritical drying in same autoclave, 2 hours drying times, the product that obtains after the drying is the nano cerium zirconium oxide, and the specific area of cerium Zirconium oxide after 1000 ℃ calcining was worn out in 6 hours down is 45m
2/ g.
X-ray diffraction the analysis showed that the oxide of acquisition exists with solid solution phase form, and x-ray diffraction pattern is seen a line among Fig. 1.
Small-angle diffraction records its particle size distribution and sees Fig. 2.
Embodiment 2:
Get cerous carbonate 20g, with the red fuming nitric acid (RFNA) dissolving, with mixing mutually after the basic zirconium chloride 15g dissolving, mix the back and come precipitation mixture with 25% (wt) ammoniacal liquor, control final pH=9.3, with the pure water washing, wash to washing lotion and detect no chlorion existence after precipitation is finished with silver nitrate.The cerium zirconium hydroxide that obtains after washing is good adds water, stirs into slurry with agitator, and slurry is put into autoclave carries out hydro-thermal reaction, 160 ℃ of control reaction temperatures, 5 hours time.After hydro-thermal reaction finishes, with the product cold filtration, the sediment that obtains is dissolved into slurry with ethanol, slurry is carried out supercritical drying in same autoclave, 4 hours drying times, the product that obtains after the drying is the nano cerium zirconium oxide, and the specific area of cerium Zirconium oxide after 1000 ℃ calcining was worn out in 6 hours down is 46m
2/ g.
X-ray diffraction the analysis showed that the oxide of acquisition exists with solid solution phase form, and x-ray diffraction pattern is seen the b line among Fig. 1.
Small-angle diffraction records its particle size distribution and sees Fig. 3.
Embodiment 3:
Get cerous carbonate 30g, lanthana 6g dissolves with red fuming nitric acid (RFNA) respectively, with mixing mutually after the basic zirconium chloride 25g dissolving, mix the back and come precipitation mixture with 25% (wt) ammoniacal liquor, control final pH=9.8, with the pure water washing, wash to washing lotion and detect no chlorion existence after precipitation is finished with silver nitrate.The cerium zirconium lanthanum hydroxide that obtains after washing is good adds water, stirs into slurry with agitator, and slurry is put into autoclave carries out hydro-thermal reaction, 180 ℃ of control reaction temperatures, 4.5 hours time.After hydro-thermal reaction finishes, with the product cold filtration, the sediment that obtains is dissolved into slurry with ethanol, slurry is carried out supercritical drying in same autoclave, 2 hours drying times, the product that obtains after the drying is the nano cerium zirconium lanthanum-oxides, and the specific area of cerium zirconium lanthanum-oxides after 1000 ℃ calcining was worn out in 6 hours down is 47m
2/ g.
X-ray diffraction the analysis showed that the oxide of acquisition exists with solid solution phase form, and finds that with the TEM detection product pellet of gained is evenly distributed, good dispersion, and its size is between 5～10 nanometers, and its TEM figure sees Fig. 4 (a).
Embodiment 4:
Get cerous carbonate 30g, lanthana 6g, praseodymium oxide 7g, dissolve with red fuming nitric acid (RFNA) respectively, with mixing mutually after the basic zirconium chloride 25g dissolving, mix the back and come precipitation mixture with 25% (wt) ammoniacal liquor, control final pH=10.5, with the pure water washing, wash to washing lotion and detect no chlorion existence after precipitation is finished with silver nitrate.The cerium zirconium lanthanum praseodymium hydroxide that obtains after washing is good adds water, stirs into slurry with agitator, and slurry is put into autoclave carries out hydro-thermal reaction, 250 ℃ of control reaction temperatures, 3 hours time.After hydro-thermal reaction finishes, with the product cold filtration, the sediment that obtains is dissolved into slurry with ethanol, slurry is carried out supercritical drying in same autoclave, 3 hours drying times, the product that obtains after the drying is a nano cerium zirconium lanthanum praseodymium oxide, and the specific area of cerium zirconium lanthanum praseodymium oxide after 1000 ℃ calcining was worn out in 6 hours down is 50m
2/ g.
X-ray diffraction the analysis showed that the oxide of acquisition exists with solid solution phase form, and finds that with the TEM detection product pellet of gained is evenly distributed, good dispersion, and its size is between 5～10 nanometers, and its TEM figure sees Fig. 4 (b).
Embodiment 5:
Get zirconium carbonate 30g, cerous carbonate 20g with the red fuming nitric acid (RFNA) dissolving, uses 25% (wt) ammoniacal liquor to precipitate again, controls final pH=10.5, washs with pure water after precipitation is finished.The cerium zirconium hydroxide that obtains after washing is good adds water, stirs into slurry with agitator, and slurry is put into autoclave carries out hydro-thermal reaction, 150 ℃ of control reaction temperatures, 6 hours time.After hydro-thermal reaction finishes, with the product cold filtration, the sediment that obtains is dissolved into slurry with ethanol, slurry is carried out supercritical drying in same autoclave, 2 hours drying times, the product that obtains after the drying is the nano cerium zirconium oxide, and the specific area of cerium Zirconium oxide after 1000 ℃ calcining was worn out in 6 hours down is 46m
2/ g.
X-ray diffraction the analysis showed that the oxide of acquisition exists with solid solution phase form, and x-ray diffraction pattern is seen c line among Fig. 1.
Embodiment 6:
Take by weighing a certain amount of basic zirconium chloride and cerous carbonate (is 1: 1 and 9: 1 two kinds of proportional arrangement presomas according to cerium oxide and zirconic molar percentage), step and method with reference to embodiment 1, the product that obtains after the drying is the nano cerium zirconium oxide, and the specific area of cerium Zirconium oxide after 1000 ℃ calcining was worn out in 6 hours down is respectively 49m
2/ g and 45m
2/ g.
Claims (10)
1, the catalyst based preparation method of a kind of nano-scale cerium zirconium complex rare-earth oxidate containing valuable metal solid solution is characterized in that including following steps:
1) salting liquid that will contain cerium mixes by goods institute's oxidation-containing cerium and zirconic molar percentage with the salting liquid that contains zirconium;
2) with alkaline matter with the mixture neutralization precipitation;
3) filter;
4) use deionized water washing sediment, wash to washing lotion and detect no chlorion existence with silver nitrate;
5) the cerium zirconium hydroxide that obtains and add water and put into autoclave and carry out hydro-thermal reaction after the washing;
6) after hydro-thermal reaction finishes, product is filtered, the sediment that obtains carries out supercritical drying and gets nano-scale cerium zirconium mixed oxide solid solution catalyst in same autoclave.
2, the catalyst based preparation method of nano-scale cerium zirconium complex rare-earth oxidate containing valuable metal solid solution according to claim 1 is characterized in that above-mentioned steps 1) in can add one or more rare earth element nitrate solution.
3, the catalyst based preparation method of nano-scale cerium zirconium complex rare-earth oxidate containing valuable metal solid solution according to claim 1 is characterized in that above-mentioned rare earth element nitrate can be obtained with nitric acid dissolve by lanthana, praseodymium oxide, neodymia, yittrium oxide.
4, the catalyst based preparation method of nano-scale cerium zirconium complex rare-earth oxidate containing valuable metal solid solution according to claim 1 is characterized in that above-mentioned steps 1) in except that the cerium zirconium, the molar percentage of the addition of other rare earth is 0～20%.
5, the catalyst based preparation method of nano-scale cerium zirconium complex rare-earth oxidate containing valuable metal solid solution according to claim 1 is characterized in that above-mentioned steps 2) adopt alkaline matter neutralization precipitation mixture, controlling its final pH value is 8.5～11.5.
6, the catalyst based preparation method of nano-scale cerium zirconium complex rare-earth oxidate containing valuable metal solid solution according to claim 1, it is characterized in that above-mentioned steps 2) alkaline matter that adopted can be ammoniacal liquor, the percentage by weight of its concentration is 10～28%, also can adopt the weak solution of NaOH.
7, the catalyst based preparation method of nano-scale cerium zirconium complex rare-earth oxidate containing valuable metal solid solution according to claim 1 is characterized in that above-mentioned steps 2) precipitation temperature be 0～80 ℃.
8, the catalyst based preparation method of nano-scale cerium zirconium complex rare-earth oxidate containing valuable metal solid solution according to claim 1, it is characterized in that above-mentioned steps 5) hydrothermal reaction process control hydrothermal temperature be 140～300 ℃, pressure is 0.6～4Mpa, and the time is 0.5～10h.
9, the catalyst based preparation method of nano-scale cerium zirconium complex rare-earth oxidate containing valuable metal solid solution according to claim 1 is characterized in that above-mentioned steps 6) baking temperature be 100～300 ℃, drying pressure is 7～10Mpa.
10, the catalyst based preparation method of nano-scale cerium zirconium complex rare-earth oxidate containing valuable metal solid solution according to claim 1 is characterized in that above-mentioned steps 6) the nano-scale cerium zirconium mixed oxide solid solution catalyst of dry back gained comprises that the molar percentage of cerium oxide is 50～90%, zirconic molar percentage is 10～50%.
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| CN100398199C (en) * | 2006-05-18 | 2008-07-02 | 浙江大学 | Method for preparing temperature-resisting Ce-Zr composite aluminium oxide material |
| CN100398448C (en) * | 2005-07-26 | 2008-07-02 | 中国科学院物理研究所 | Flower shape structured nano-cerium oxide and its preparation method and use |
| CN100445207C (en) * | 2005-07-22 | 2008-12-24 | 中国科学院物理研究所 | Flower structure nano cerium oxide base composite material and its preparing method and use |
| CN102513085A (en) * | 2011-11-07 | 2012-06-27 | 上海华明高纳稀土新材料有限公司 | Cerium oxide-zirconium oxide-based composite oxide and preparation method thereof |
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| TWI469926B (en) * | 2008-12-04 | 2015-01-21 | Sakai Chemical Industry Co | Zirconium oxide dispersion, production thereof and resin composition containing the dispersion |
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2003
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| CN100398448C (en) * | 2005-07-26 | 2008-07-02 | 中国科学院物理研究所 | Flower shape structured nano-cerium oxide and its preparation method and use |
| CN100398199C (en) * | 2006-05-18 | 2008-07-02 | 浙江大学 | Method for preparing temperature-resisting Ce-Zr composite aluminium oxide material |
| TWI469926B (en) * | 2008-12-04 | 2015-01-21 | Sakai Chemical Industry Co | Zirconium oxide dispersion, production thereof and resin composition containing the dispersion |
| CN103249676A (en) * | 2010-11-30 | 2013-08-14 | 罗地亚管理公司 | Composition based on zirconium oxide and on at least one oxide of a rare earth other than cerium, having a specific porosity, processes for preparing same and use thereof in catalysis |
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