CN1565724A - Cerium-titanium solid solution and its preparing method - Google Patents
Cerium-titanium solid solution and its preparing method Download PDFInfo
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- CN1565724A CN1565724A CN 03141571 CN03141571A CN1565724A CN 1565724 A CN1565724 A CN 1565724A CN 03141571 CN03141571 CN 03141571 CN 03141571 A CN03141571 A CN 03141571A CN 1565724 A CN1565724 A CN 1565724A
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- China
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- ceo
- solid solution
- titanium
- cerium
- ceti
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- 239000006104 solid solution Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 8
- NEGBOTVLELAPNE-UHFFFAOYSA-N [Ti].[Ce] Chemical compound [Ti].[Ce] NEGBOTVLELAPNE-UHFFFAOYSA-N 0.000 title claims description 11
- 239000000843 powder Substances 0.000 claims abstract description 22
- 238000002425 crystallisation Methods 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims abstract description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 230000032683 aging Effects 0.000 claims abstract description 6
- 230000008025 crystallization Effects 0.000 claims abstract description 6
- 238000009777 vacuum freeze-drying Methods 0.000 claims abstract description 6
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000010936 titanium Substances 0.000 claims description 40
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 22
- 238000002360 preparation method Methods 0.000 claims description 15
- CVORKJTWNJQPLX-UHFFFAOYSA-N [Ce].[Mg].[Ti] Chemical compound [Ce].[Mg].[Ti] CVORKJTWNJQPLX-UHFFFAOYSA-N 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 7
- 238000001556 precipitation Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 150000002823 nitrates Chemical class 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 abstract description 6
- 239000003054 catalyst Substances 0.000 abstract description 3
- 238000000151 deposition Methods 0.000 abstract 1
- 239000002243 precursor Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 description 6
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 229910052684 Cerium Inorganic materials 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- -1 titanium alkoxide Chemical class 0.000 description 2
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052717 sulfur Chemical group 0.000 description 1
- 239000011593 sulfur Chemical group 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a CeTi#-[2]O#-[6] solid solution and its preparing method. The molecular formula is CeTi#-[2]O#-[6]. The process includes the following steps : the precursor of the cerous nitrate and titanium tetrachloride solution is served as raw material, the raw material is mixed and added into strong aqua ammonia, after depositing, aging, centrifuge washing, washing away Cl#+[-], vacuum freeze drying and baking, CeO#-[2]-TiO#-[2] powder is obtained, CeO#-[2]-TiO#-[2] powder is roasted at 650,750 and 800 degrees C., and crystallization of CeTi#-[2]O#-[6] is finished.The invention is suitable for removing NO#-[x] and SO#-[x] catalyst carrier.
Description
Technical field
The present invention relates to a kind of and single CeO
2Compare have higher stability, the CeTi of oxidation-reducibility and good low temperature active
2O
6Solid solution and preparation method thereof.
Background technology
In the practical application of nitrogenous and sulfur-bearing industrial waste gas catalytic eliminating, the main active component ceria (CeO on the catalyst
2) at temperature easy-sintering during up to 750 ℃.Thereby the oxide that often need add some anti-sintering in actual application is made composite oxides or solid solution (as CeO
2-ZrO
2); Containing CeO
2In the solid solution of-MOx, CeO
2Portion C e atom in the lattice can cause CeO after being replaced by other cations
2Distortion of lattice and defective.Therefore, contain CeO
2The solid solution of-MOx is than single CeO
2Have higher stability, oxidation-reducibility and good low temperature active.In recent years, remove CeO
2-ZrO
2Outward, people are to CeO
2-SnO
2, CeO
2-TiO
2And CeO
2The preparation of systems such as-NiO and sign have been done a large amount of work.
CeO
2-TiO
2Preparation adopt sol-gel process mostly, with inorganic Ce salt and titanium alkoxide as raw material.Because Ce and Ti ion have multiple valence state, thereby the valence state of the solid solution that makes and molecular formula are also very complicated.CeTi
2O
6Be the Ce-Ti solid solution that at present unique known Ce and Ti all exist with+4 valencys.But Ce is+3 valencys in the Ce-Ti solid solution that most researchs obtain, and Ti is+4 valencys.As: Preuss A.et al., (J.Solid State Chem., 1994,110:363-369) research has obtained Ce
2TiO
5, Ce
2Ti
2O
7And Ce
4Ti
9O
24, promptly be respectively: Ce
2O
3TiO
2, Ce
2O
32TiO
2And Ce
2O
34.5TiO
2Bamger E.etal., (J.Alloys Comp., 1994,204:101-107) research has obtained Ce
2Ti
4O
11, i.e. Ce
2O
34TiO
2Wherein Ce and Ti exist with+4 two kinds of valence states with+3.More than these research explanations Ce-Ti can form a variety of compounds, but the ratio of reaction condition and Ce-Ti all can have influence on last product, this is a very complicated system.
Dauscher A.et.al., (Catal.Lett., 1992,14:171-183) with organic titanium alkoxide and CeCl
37H
2O is a presoma, adopts the Ti of hydrolysis seasoning preparation: the Ce-Ti composite oxides of Ce=1, find in acid medium, to have formed surperficial uncertain crystalline phase, and after 450-500 ℃ of roasting, formed amorphous TiO
2Last covering CeO
2Crystal; In alkaline medium, formed CeTiO
3Compound is transformed into impalpable structure after the roasting, its high-specific surface area is 95m
2/ g.RynkowskiJ.et al., (Appl.Catal.A:Gen., 2000,203:335-348) prepared the Ce-Ti composite oxides that the Ce/Ti mol ratio is 2: 8 and 5: 5, find the pretreatment condition difference, the compound difference of formation.The Ce/Ti mol ratio is 2: 8 o'clock, just begins crystallization through 600 ℃ of roastings, has occurred CeO during 800 ℃ of roastings
2, TiO
2Reach unknown compound mutually; The sample of 400 ℃ of roastings is at 800 ℃ of H
2After the reduction, Ce has appearred respectively
4Ti
9O
24Phase; The sample of 700 ℃ of roastings detects the diffraction maximum that rutile occurred through XRD; The Ce/Ti mol ratio is 5: 5 o'clock, and when sintering temperature was lower than 400 ℃, XRD detects had only CeO
2Phase; When sintering temperature is higher than 600 ℃, there is unknown compound to occur; The sample of 400 ℃ of roastings is through 900 ℃ of H
2Ce has appearred in reduction
2Ti
2O
7Phase.XPS detects and shows that Ce content is higher than the middle mutually Ce content of body in the top layer; The Ti/Ce mol ratio is 8: 2 o'clock, Ti/Ce=1.4-1.7 in the superficial layer; The Ti/Ce mol ratio is 5: 5 o'clock, Ti/Ce=0.4-0.44 in the superficial layer, even 0.28.
Summary of the invention
The purpose of this invention is to provide a kind of chemical molecular formula is CeTi
2O
6Cerium magnesium-titanium solid solution and preparation method thereof, the CeTi of preparation gained
2O
6Solid solution and single CeO
2Compare have higher stability, oxidation-reducibility and good low temperature active, be specially adapted to remove NO
xWith take off SO
xThe carrier of catalyst.
CeTi provided by the invention
2O
6Solid solution, described component cerium titanium is than being Ce=x (x=0.1-1.0), and Ti=1-x (mol ratio) by investigating the variation of Ce/Ti mol ratio x=0.-1.0, finds Ce: Ti=0.3: 0.7 (mol ratio) is one to form preferably.
A kind of CeTi provided by the invention
2O
6Solid solution and preparation method thereof is with cerous nitrate (Ce (NO
3)
36H
2O) and carbon tetrachloride (TiCl
4) presoma of solution is raw material, evenly mixes (Ce with suitable proportioning
xTi
1-xO
2, x=0.1-1.0 wherein), with 60 droplets/minute rate of addition cerium titanium material drop is added in the concentrated ammonia liquor, stir fast simultaneously, make its precipitation (pH value=10.0-11.0), room temperature ageing 24h, centrifuge washing, flush away Cl fully
-(with the no Cl of liquor argenti nitratis ophthalmicus check
-Exist), vacuum freeze drying 12-14h (decide on the drying regime of powder drying time) places 50 ℃ the dry 24h of baking oven, changes 500 ℃ of roasting 2h in the Muffle furnace over to, gets CeO
2-TiO
2Powder.With CeO
2-TiO
2Powder is respectively with 650,750 and 800 ℃ of roasting 2h.
CeO
2-TiO
2Powder is behind 650 ℃ of roasting 2h, and when x=0.1, XRD can detect CeTi
2O
6Mutually with a spot of rutile mutually; During x=0.2, still have the CeTi that mays be seen indistinctly
2O
6Mutually with rutile mutually; During x=0.3, mainly exist with amorphous state; During x=0.4-1.0, then be single CeO
2Phase; CeO
2-TiO
2Powder behind 750 ℃ of roasting 2h, CeTi
2O
6Most of crystallization; When sintering temperature reaches 800 ℃, CeTi
2O
6Crystallization process be tending towards finishing.
Technical process of the present invention is simple, but each step needs through strictness control the Ce of preparation gained
0.3Ti
0.7O
2Composite oxides find that through the suction-desorption experiment of nitrogen its specific area is respectively 207.37m under the condition of different temperatures roasting
2/ g (500 ℃ of roasting 2h); 58.78m
2/ g (650 ℃ of roasting 2h); 50.26m
2/ g (750 ℃ of roasting 2h) and 44.66m
2/ g (800 ℃ of roasting 2h).And this suction-desorption isotherm type belongs to the VI class in the BDDT classification, and pore-size distribution belongs to the meso-hole structure material.The XRD determining result is presented at 25.9 ° of 2 θ, 26.7 ° and 27.4 ° and locates to detect CeTi
2O
6The characteristic diffraction peak of solid solution.The XPS measurement result shows Ce
3d3/2Be 882.86 (eV), Ti
2P3/2Be 458.7 (eV), O
LsLattice is 529.5 (eV), Ce/Ti=1.248, u /I
Total=0.269 (Ce
4+/ Ce
3+Ratio determined intensity and the overall strength I of u
TotalRatio.Ce
3+U /I when increasing
TotalRatio descends, u '+v '/I
TotalValue rises).At Ce
0.3Ti
0.7O
2In the composite oxides, Ce
3+Account for 17.8% of surface C e total amount.The solid solution specific area that makes is also big, and (its specific area is 44.66m behind 800 ℃ of roasting 2h
2/ g),
The specific embodiment
Embodiment 1:
CeTi
2O
6Solid solution and preparation method thereof the steps include:
(1) CeTi
2O
6Solid solution, its chemical molecular formula are CeTi
2O
6It is with cerous nitrate (Ce (NO
3)
36H
2O) and titanium tetrachloride (TiCl
4) presoma of solution is raw material, evenly mixes (Ce with suitable proportioning
xTi
1-xO
2, x=0.1-1.0 wherein), again in Ce: the ratio of Ti, Ce=x (x=0.3), corresponding cerous nitrate (Ce (NO is calculated and measured to the mol ratio of Ti=1-x (0.7)
3)
36H
2O) and carbon tetrachloride (TiCl
4) amount, make its even mixing.
(2) in the 250ml beaker, add the 40ml concentrated ammonia liquor, then the above-mentioned cerium titanium material liquid that mixes is changed in the separatory funnel, with certain speed cerium titanium material drop is added in the concentrated ammonia liquor, stir fast simultaneously, make fully (pH value=10.0-11.0) of its precipitation, room temperature ageing 24h, centrifuge washing, flush away Cl
-(with the no Cl of liquor argenti nitratis ophthalmicus check
-Exist), with vacuum freeze drying 12-14h (decide on the drying regime of powder drying time), place 50 ℃ the dry 24h of baking oven again, change 500 ℃ of roasting 2h in the Muffle furnace over to, get CeO
2-TiO
2Powder.With CeO
2-TiO
2Powder is respectively with 650,750 and 800 ℃ of roasting 2h.
(3) CeO
2-TiO
2Powder is behind 650 ℃ of roasting 2h, and when x=0.1, XRD can detect CeTi
2O
6Mutually with a spot of rutile mutually; During x=0.2, still have the CeTi that mays be seen indistinctly
2O
6Mutually with rutile mutually; During x=0.3, mainly exist with amorphous state; During x=0.4-1.0, then be single CeO
2Phase; CeO
2-TiO
2Powder behind 750 ℃ of roasting 2h, CeTi
2O
6Most of crystallization; When sintering temperature reaches 800 ℃, CeTi
2O
6Crystallization process be tending towards finishing.
Embodiment 2:
(1) CeTi
2O
6Solid solution, its chemical molecular formula are CeTi
2O
6It is with cerous nitrate (Ce (NO
3)
36H
2O) and titanium tetrachloride (TiCl
4) presoma of solution is raw material, evenly mixes (Ce with suitable proportioning
xTi
1-xO
2, x=0.1-1.0 wherein), again in Ce: the ratio of Ti, Ce=x (x=0.3), the cerous nitrate (Ce (NO that concentration is 0.5mol/L is calculated and measured to the mol ratio of Ti=1-x (0.7)
3)
36H
2O) solution 30ml, and concentration is the carbon tetrachloride (TiCl of 0.333mol/L
4) solution 105ml, make its even mixing.
(2) in the 250ml beaker, add the 40ml concentrated ammonia liquor, then the above-mentioned cerium titanium material liquid that mixes is changed in the separatory funnel, with 60 droplets/minute rate of addition cerium titanium material drop is added in the concentrated ammonia liquor, stir fast simultaneously, make fully (pH value=10.0-11.0) of its precipitation, room temperature ageing 24h, centrifuge washing, flush away Cl
-(with the no Cl of liquor argenti nitratis ophthalmicus check
-Exist), with vacuum freeze drying 12-14h (decide on the drying regime of powder drying time), place 50 ℃ the dry 24h of baking oven again, change 500 ℃ of roasting 2h in the Muffle furnace over to, get CeO
2-TiO
2Powder.With CeO
2-TiO
2Powder is respectively with 650,750 and 800 ℃ of roasting 2h.
(3) CeO
2-TiO
2Powder is behind 650 ℃ of roasting 2h, and when x=0.1, XRD can detect CeTi
2O
6Mutually with a spot of rutile mutually; During x=0.2, still have the CeTi that mays be seen indistinctly
2O
6Mutually with rutile mutually; During x=0.3, mainly exist with amorphous state; During x=0.-1.0, then be single CeO
2Phase; CeO
2-TiO
2Powder behind 750 ℃ of roasting 2h, CeTi
2O
6Most of crystallization; When sintering temperature reaches 800 ℃, CeTi
2O
6Crystallization process be tending towards finishing.
Claims (7)
1. cerium magnesium-titanium solid solution, the chemical molecular formula that it is characterized in that described solid solution is CeTi
2O
6, component cerium titanium mol ratio is Ce=x (x=0.1-1.0), Ti=1-x.
2. cerium magnesium-titanium solid solution according to claim 1 is characterized in that described cerium titanium mol ratio is: Ce: Ti=0.3: 0.7.
3. the preparation method of the described cerium magnesium-titanium solid solution of claim 1 is characterized in that the presoma with six water cerous nitrates and titanium tetrachloride solution is a raw material, with Ce
xTi
1-xO
2, wherein the proportioning of x=0.1-1.0 is evenly mixed, and cerium titanium material liquid is added drop-wise in the concentrated ammonia liquor pH value of control solution, room temperature ageing, centrifuge washing, flush away Cl with certain rate of addition
-, after the vacuum freeze drying, the baking oven that places is dry, changes kiln roasting over to, gets CeO
2-TiO
2Powder is with CeO
2-TiO
2Powder is respectively with 650,750 and 800 ℃ of roasting 2h.
4. the preparation method of cerium magnesium-titanium solid solution according to claim 3 is characterized in that described sintering temperature is 750-800 ℃.
5. the preparation method of cerium magnesium-titanium solid solution according to claim 3 is characterized in that described cerium titanium mixed liquor is added drop-wise in the concentrated ammonia solution with 60 droplets/minute rate of addition, makes the pH value=10.0-11.0 of solution.
6. the preparation method of cerium magnesium-titanium solid solution according to claim 3 is characterized in that described precipitation mixture needs at room temperature ageing 24h, centrifuge washing, flush away Cl
-, with the no Cl of liquor argenti nitratis ophthalmicus check
-Exist, vacuum freeze drying 12-14h places 50 ℃ the dry 24h of baking oven, changes 500 ℃ of roasting 2h in the Muffle furnace over to, gets CeO
2-TiO
2Powder.
7. the preparation method of cerium magnesium-titanium solid solution according to claim 3 is characterized in that described CeO
2-TiO
2Powder is behind 650 ℃ of roasting 2h, and when x=0.1, XRD can detect CeTi
2O
6Mutually with a spot of rutile mutually; During x=0.2, still have the GeTi that mays be seen indistinctly
2O
6Mutually with rutile mutually; During x=0.3, mainly exist with amorphous state; During x=0.4-1.0, then be single CeO
2Phase.CeO
2-TiO
2Powder behind 750 ℃ of roasting 2h, CeTi
2O
6Most of crystallization; When sintering temperature reaches 800 ℃, CeTi
2O
6Crystallization process finish.
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|---|---|---|---|
| CN 03141571 CN1246078C (en) | 2003-07-08 | 2003-07-08 | Cerium-titanium solid solution and its preparing method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03141571 CN1246078C (en) | 2003-07-08 | 2003-07-08 | Cerium-titanium solid solution and its preparing method |
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| Publication Number | Publication Date |
|---|---|
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| CN1246078C CN1246078C (en) | 2006-03-22 |
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| CN111215085B (en) * | 2018-11-23 | 2023-02-03 | 中国科学院大连化学物理研究所 | Two-step solar thermochemical energy storage non-noble metal catalyst and preparation and application thereof |
| CN113264694A (en) * | 2021-06-11 | 2021-08-17 | 杭州杭钢三江矿业有限公司 | Environment-friendly and energy-saving lime sintering process |
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