CN1631522A - Binary composite mesopore oxide material making cerium as base and its preparation - Google Patents
Binary composite mesopore oxide material making cerium as base and its preparation Download PDFInfo
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- CN1631522A CN1631522A CN 200410091551 CN200410091551A CN1631522A CN 1631522 A CN1631522 A CN 1631522A CN 200410091551 CN200410091551 CN 200410091551 CN 200410091551 A CN200410091551 A CN 200410091551A CN 1631522 A CN1631522 A CN 1631522A
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- 239000000463 material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims description 14
- 229910052684 Cerium Inorganic materials 0.000 title claims description 8
- 239000011218 binary composite Substances 0.000 title claims description 8
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims description 8
- 239000000243 solution Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 6
- 239000011148 porous material Substances 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000003153 chemical reaction reagent Substances 0.000 claims description 7
- 230000001376 precipitating effect Effects 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 5
- 150000000703 Cerium Chemical class 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052775 Thulium Inorganic materials 0.000 claims description 4
- 229910052788 barium Inorganic materials 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000000839 emulsion Substances 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 150000003863 ammonium salts Chemical group 0.000 claims description 2
- QKXCAKZMAORNSR-UHFFFAOYSA-N azane 1-chlorohexadecane Chemical compound N.CCCCCCCCCCCCCCCCCl QKXCAKZMAORNSR-UHFFFAOYSA-N 0.000 claims description 2
- 230000031709 bromination Effects 0.000 claims description 2
- 238000005893 bromination reaction Methods 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- XQSBLCWFZRTIEO-UHFFFAOYSA-N hexadecan-1-amine;hydrobromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[NH3+] XQSBLCWFZRTIEO-UHFFFAOYSA-N 0.000 claims description 2
- RNYJXPUAFDFIQJ-UHFFFAOYSA-N hydron;octadecan-1-amine;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[NH3+] RNYJXPUAFDFIQJ-UHFFFAOYSA-N 0.000 claims description 2
- KKWUACQXLWHLCX-UHFFFAOYSA-N hydron;tetradecan-1-amine;chloride Chemical compound Cl.CCCCCCCCCCCCCCN KKWUACQXLWHLCX-UHFFFAOYSA-N 0.000 claims description 2
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 2
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 229910021653 sulphate ion Inorganic materials 0.000 claims description 2
- AHNISXOXSNAHBZ-UHFFFAOYSA-M tetrakis-decylazanium;bromide Chemical compound [Br-].CCCCCCCCCC[N+](CCCCCCCCCC)(CCCCCCCCCC)CCCCCCCCCC AHNISXOXSNAHBZ-UHFFFAOYSA-M 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 5
- 238000004140 cleaning Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 2
- 150000003839 salts Chemical class 0.000 abstract 2
- 230000004913 activation Effects 0.000 abstract 1
- 238000010276 construction Methods 0.000 abstract 1
- 229910017053 inorganic salt Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- 239000002699 waste material Substances 0.000 abstract 1
- 238000001354 calcination Methods 0.000 description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000013335 mesoporous material Substances 0.000 description 3
- 230000010757 Reduction Activity Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000000593 microemulsion method Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- CEYYIKYYFSTQRU-UHFFFAOYSA-M trimethyl(tetradecyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)C CEYYIKYYFSTQRU-UHFFFAOYSA-M 0.000 description 1
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- Catalysts (AREA)
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
Abstract
A oxide material based of Fei and its producing way, belongs to inorganic catalyst material technique field, used as the faci material of motor waste air cleaning catalyst. The invention increase the activation at low temperature by the change of construction.(TPR low temperature restore scope: 120-200 degC) and heat stability(after worked in 900 degC, 20--40m/g, hole vacuum0.03--0.3cm/g, hole diameter5nm--20nm). The producing way takes template way, first solute the Fei salt and metal solution salt by water of no ion, mix them by rate, then mix the inorganic salt solution and surface activate solution, add precipitate dose, water heat at 50-100 degC, wash, dry, last, fire at 400-1000 degC, then we get the oxide material.
Description
Technical field
The present invention relates to a kind of cerium Quito unit composite mesopore oxide material and preparation method thereof, belong to inorganic catalysis material technical field, be suitable for the coating material of cleaning catalyst for tail gases of automobiles.
Background technology
General vehicle exhaust is handled catalyst and mainly is made up of three parts: carrier, coating and layer of precious metal, the synergy of three parts can be handled carbon monoxide, hydrocarbon and the oxynitrides in the tail gas simultaneously, reduce the pollution to environment.CeO
2And with its be the composite oxides of base because of having the good oxygen that stores, high-temperature stability is widely used as coating material.
At present, both at home and abroad report be used to prepare CeO
2And the method for composite oxide powder mainly contains: the precipitation method, sol-gal process, template and microemulsion method etc.Though wherein precipitation method preparation technology is simple, specific area and catalytic activity are all not high; Sol-gal process and microemulsion method all need strict control reaction condition, industrially are difficult to realize large-scale production; And template adds organic macromolecule to make template based on the general precipitation method therein, is easy to industrialization, and the material of preparation not only has high-specific surface area, and catalytic activity is higher.
Mesoporous material refers to the inorganic porous material in 2nm～50nm scope.In recent years, it is with its adjustable mesopore orbit, and high specific area reaches good heat endurance and enjoys people to pay close attention to, and represented application prospects in fields such as catalysis, separation, sensors.Template is one of main method of preparation mesoporous material, uses it for preparation CeO in the document " Daniela Terribile, chem.mater., 9,2676,1997 " first
2Mesoporous material, 450 ℃ of following specific surfaces are up to 201m
2/ g, the tight burning temperature is at 1000 ℃, but its TPR (temperature programmed reduction) reduction temperature does not obtain basic change, and with directly precipitation is the same, reduction peak has just changed the oxygen storage capacity of system about 500 ℃ and 820 ℃.
Summary of the invention
The object of the invention is to provide a kind of cerium-based binary composite mesopore oxide material with high thermal stability and ultralow reduction temperature and preparation method thereof, and the present invention mainly utilizes the change on the institutional framework to improve the low-temperature reduction activity and the heat endurance of the prepared sample of template.
Technical scheme of the present invention is as follows:
A kind of binary composite mesopore oxide material of cerium-based is characterized in that:
1) developed by molecule formula: Ce
1-xB
xO
δ, wherein B is a kind of in Zr, Cu, Fe, Mn, Mg, Ba or the thulium except that Ce, 0≤x≤0.5,1≤δ≤2;
2) aperture 5nm～20nm;
3) handle specific area 100～150m through 450 ℃
2/ g, pore volume 0.5～0.8cm
3/ g; Specific area 20～40m after 900 ℃ of processing
2/ g, pore volume 0.03～0.3cm
3/ g;
4) low-temperature reduction peak temperature interval was at 120～200 ℃ during temperature programmed reduction was tested.
The preparation method of a kind of binary composite mesopore oxide material provided by the invention is characterized in that this method carries out as follows:
1) dissolve the soluble-salt of cerium salt and described metallic element respectively with deionized water, making concentration after the mixing is 0.1～3.0M solution I; In deionized water, making concentration is 0.05～1.0M solution II with surfactant dissolves; Described cerium salt is ammonium salt, nitrate or chlorate; The soluble-salt of described metallic element is the nitrate or the chlorate of Zr, Cu, Fe, Mn, Mg, Ba or the thulium except that Ce;
2) solution I and solution II are mixed, and stir;
3) precipitating reagent is added step 2) mixed solution in, or mixed solution added in the precipitating reagent, the control pH value continues reaction 1～3h 5～14 in the reaction, forms emulsion;
4) emulsion is put into autoclave, at 50～100 ℃ of following hydro-thermal reaction 5～100h;
5) with the filtration of step 4) products therefrom, washing, drying, calcine 2～4h down at 400 ℃～1000 ℃ then, make composite mesopore oxide material.
Surfactant of the present invention adopts in Tetra-n-decylammonium bromide, cetyl ammonium bromide, octadecyl bromination ammonium, tetradecyl ammonium chloride, cetyl chloride ammonium, octadecyl ammonium chloride, dodecyl sodium sulfate or the polyvinyl alcohol any.
Precipitating reagent of the present invention is urea, solubility hydroxide, soluble carbon hydrochlorate, ammoniacal liquor or soluble sulphate.
The product low-temperature reduction activity of this method preparation is very high, and TPR reduction peak position is at 120～200 ℃, well below document Daniela Terribile, and chem.mater., the result in 9,2676,1997,1000 ℃ still have 10m after the calcining down
2The specific area of/g has shown very high heat endurance.Oxide powder provided by the invention can be used as the coating material of auto-exhaust catalyst.
Description of drawings
The CeO that Fig. 1 provides for the embodiment of the invention 1
2XRD figure under different temperatures.
The Ce that Fig. 2 embodiment of the invention 2 provides
0.75Zr
0.25O
2Graph of pore diameter distribution after 450 ℃ of processing.
The Ce that Fig. 3 embodiment of the invention 2 provides
0.75Zr
0.25O
2Stereoscan photograph after 900 ℃ of processing.
The Ce that Fig. 4 embodiment of the invention 2 provides
0.75Zr
0.25O
2Temperature programmed reduction curve after 450 ℃ of processing.
The specific embodiment
Embodiment 1:
The cerium source is Ce (NO
3)
3, surfactant is a softex kw, precipitating reagent is (NH
4)
2CO
3With Ce (NO
3)
3Be dissolved in the solution that deionized water is made into 2M, the aqueous solution 0.5M with surfactant adds Ce (NO then
3)
3Solution.Wherein the ratio of component is as follows in the reaction system: Ce (NO
3)
3: 2C
16TMABr: 8NH
4HCO
3: 200H
2O.Mixed liquor is 60 ℃ through the hydrothermal treatment consists condition and handles 100h, filters, and with deionized water and absolute ethanol washing sample, dry 15h under 90 ℃ is last then, respectively at 450 ℃ and 900 ℃ of following calcining samples, obtains products molecule formula: CeO
2Specific surface after 450 ℃ of calcinings is 141m
2/ g, pore volume are 0.59cm
3/ g, the aperture is 8.3nm, TPR reduction peak temperature is 180 ℃ and 565 ℃; Specific surface after 900 ℃ of calcinings is 31m
2/ g, pore volume are 0.21cm
3/ g, the aperture is 13.1nm, TPR reduction peak temperature is 160 ℃.
Embodiment 2:
Ce (NO
3)
3Solution is 2M, Zr (NO
3)
4Solution is 0.1M, and it is pressed Ce (NO
3)
3: Zr (NO
3)
4Be mixed and made into mixed liquor at=3: 1, mixes with the 0.5M solution of softex kw then.Wherein the ratio of component is as follows in the reaction system: 0.75Ce (NO
3)
3: 0.25Zr (NO
3)
4: 2C
16TMABr: 8NH
4HCO
3: 400H
2O.Hydrothermal temperature is selected 100 ℃, carries out 10h, filters, and with deionized water and absolute ethanol washing sample, dry 15h under 90 ℃ is last then, respectively at 450 ℃ and 900 ℃ of following calcining samples, obtains products molecule formula: Ce
0.75Zr
0.25O
2Specific surface is 130m after 450 ℃ of calcinings
2/ g, pore volume are 0.54cm
3/ g, the aperture is 9.9nm, TPR reduction peak temperature: 180 ℃; Specific surface is 31m after 900 ℃ of calcinings
2/ g, pore volume are 0.21cm
3/ g, the aperture is 13.1nm, TPR reduction peak temperature: 159 ℃ of (see figure 4)s.
Embodiment 3:
Ce (NO
3)
3Solution is 3M, Zr (NO
3)
4Solution is 1M, and it is pressed Ce (NO
3)
3: Zr (NO
3)
4Be mixed and made into mixed liquor at=1: 1, mixes with the 1M solution of tetradecyl trimethyl ammonium chloride then.Formula rate 0.5Ce (NO
3)
3: 0.5Zr (NO
3)
4: 2C
16TMABr: 8NH
4HCO
3: 300H
2O.Hydrothermal temperature is selected 80 ℃, carries out 48h, filters, and with deionized water and absolute ethanol washing sample, dry 15h under 90 ℃ is last then, respectively at 450 ℃ and 900 ℃ of following calcining samples, obtains products molecule formula: Ce
0.5Zr
0.5O
2Specific surface is 118m after 450 ℃ of calcinings
2/ g, pore volume are 0.3cm
3/ g, the aperture is 7.2nm, TPR reduction peak temperature: 180 ℃; Specific surface is 31m after 900 ℃ of calcinings
2/ g, pore volume are 0.2cm
3/ g, the aperture is 9.9nm, TPR reduction peak temperature: 159 ℃.
Embodiment 4:
Ce (NO
3)
3Solution is 2M, Fe (NO
3)
4Solution is 2M, and it is pressed Ce (NO
3)
3: Fe (NO
3)
4Be mixed and made into mixed liquor at=9: 1, mixes with the 0.5M solution of softex kw then.Formula rate 0.9Ce (NO
3)
3: 0.1Fe (NO
3)
4: 2C
16TMABr: 8NH
4HCO
3: 200H
2O.Hydrothermal temperature is selected 50 ℃, carries out 100h, filters, and with deionized water and absolute ethanol washing sample, dry 15h under 90 ℃ is last then, respectively at 450 ℃ and 900 ℃ of following calcining samples, obtains products molecule formula: Ce
0.9Fe
0.1O
1.65Specific surface is 103m after 450 ℃ of calcinings
2/ g, pore volume are 0.38cm
3/ g, the aperture is 6.5nm, TPR reduction peak temperature: 138 ℃ and 482 ℃; Specific surface is 18m after 900 ℃ of calcinings
2/ g, pore volume are 0.14cm
3/ g, the aperture is 10.5nm, TPR reduction peak temperature: 121 ℃.
Embodiment 5:
CeCl
3Solution is 1M, Fe (NO
3)
4Solution is 2M, and it is pressed Ce (NO
3)
3: Fe (NO
3)
4Be mixed and made into mixed liquor at=8: 2, mixes with the 0.3M solution of polyvinyl alcohol then.Formula rate 0.8Ce (NO
3)
3: 0.2Fe (NO
3)
4: 2C
16TMABr: 8NH
4HCO
3: 400H
2O.Hydrothermal temperature is selected 50 ℃, carries out 100h, filters, and with deionized water and absolute ethanol washing sample, dry 15h under 90 ℃ is last then, respectively at 450 ℃ and 900 ℃ of following calcining samples, obtains products molecule formula: Ce
0.8Fe
0.2O
1.52Specific surface is 91m after 450 ℃ of calcinings
2/ g, pore volume are 0.3cm
3/ g, the aperture is 5.2nm, TPR reduction peak temperature: 126 ℃ and 453 ℃; Specific surface is 13m after 900 ℃ of calcinings
2/ g, pore volume are 0.12cm
3/ g, the aperture is 8.6nm, TPR reduction peak temperature: 125 ℃.
Comparing embodiment:
People such as Terribile use the CeO of template preparation
2TPR reduction peak temperature be about 530 ℃ and 760 ℃, be as good as with direct precipitation method, and our example 1 result shows that the low-temperature reduction peak has reduced about 340 ℃ than people's such as Terribile result, and the high temperature reduction peak has reduced by 195 ℃.Shown superpower low temperature active.
Claims (4)
1. the binary composite mesopore oxide material of a cerium-based is characterized in that:
1) developed by molecule formula: Ce
1-xB
xO
δ, wherein B is a kind of in Zr, Cu, Fe, Mn, Mg, Ba or the thulium except that Ce, 0≤x≤0.5,1≤δ≤2;
2) aperture 5nm-20nm;
3) specific area 100～150m after 450 ℃ of processing
2/ g, pore volume 0.5～0.8cm
3/ g; Specific area 20～40m after 900 ℃ of processing
2/ g, pore volume 0.03～0.3cm
3/ g;
4) low-temperature reduction peak temperature interval was at 120～200 ℃ during temperature programmed reduction was tested.
2. the preparation method of a binary composite mesopore oxide material as claimed in claim 1 is characterized in that this method carries out as follows:
1) dissolve the soluble-salt of cerium salt and described metallic element respectively with deionized water, by the cerium in the prepared binary composite mesopore oxide material and the mixed in molar ratio of metallic element, making concentration is 0.1～3.0M solution I; In deionized water, making concentration is 0.05～1.0M solution II with surfactant dissolves; Described cerium salt is ammonium salt, nitrate or chlorate; The soluble-salt of described metallic element is the nitrate or the chlorate of Zr, Cu, Fe, Mn, Mg, Ba or the thulium except that Ce;
2) solution I and solution II are mixed, and stir;
3) precipitating reagent is added step 2) mixed solution in, or mixed solution added in the precipitating reagent, the control pH value continues reaction 1～3h 5～14 in the reaction, forms emulsion;
4) emulsion is put into autoclave, at 50～100 ℃ of following hydro-thermal reaction 5～100h;
5) with the filtration of step 4) products therefrom, washing, drying, calcine 2～4h down at 400 ℃～1000 ℃ then, make composite mesopore oxide material.
3. according to the described preparation method of claim 2, it is characterized in that: surfactant described in the step 1) adopts in Tetra-n-decylammonium bromide, cetyl ammonium bromide, octadecyl bromination ammonium, tetradecyl ammonium chloride, cetyl chloride ammonium, octadecyl ammonium chloride, dodecyl sodium sulfate or the polyvinyl alcohol any.
4. according to the described preparation method of claim 2, it is characterized in that: the precipitating reagent described in the step 3) is urea, solubility hydroxide, soluble carbon hydrochlorate, ammoniacal liquor or soluble sulphate.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
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