CN109012651A - A kind of modified oxidized cerium hydrogen-storing material of indium oxide and preparation method thereof - Google Patents
A kind of modified oxidized cerium hydrogen-storing material of indium oxide and preparation method thereof Download PDFInfo
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
- B01D53/9445—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC]
- B01D53/945—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC] characterised by a specific catalyst
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- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
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Abstract
The invention discloses a kind of modified oxidized cerium hydrogen-storing material of indium oxide, the hydrogen-storing material is the composite oxides that indium oxide and cerium oxide form, and the molar ratio of indium and Ce elements is 0.05-0.45:0.55-0.95.The invention also discloses a kind of preparation methods of the modified oxidized cerium hydrogen-storing material of indium oxide.Hydrogen-storing material of the present invention passes through using the metal composite oxide that indium oxide and cerium oxide form as matrix, synergistic effect is produced between indium oxide and cerium oxide, the Oxygen storage capacity of cerium oxide, and preparation method simple process of the present invention can be significantly improved, industrialization production is conducive to.
Description
Technical field
The present invention relates to the technical field of hydrogen-storing material more particularly to a kind of modified oxidized cerium hydrogen-storing material of indium oxide and its
Preparation method.
Background technique
CeO2It is common rare earth oxygen storage material, wherein Ce3+/Ce4+Distinctive redox cycle ability, can effectively mention
Total catalytic efficiency of high vehicle maintenance service three-way catalyst, becomes the important component of three-way catalyst.In order to mention
High CeO2Thermal stability and low temperature oxygen storage capacity, researcher can generally introduce transition metal or rare earth metal etc. and carry out to it
It is modified.
A kind of patent of invention " composite cerium-zirconium solid solution with high oxygen storage capability and its preparation side of Publication No. CN101992083A
Method ", compound cerium zirconium sosoloid are combined by cerium oxide, zirconium oxide and auxiliary agent, joined polyethylene glycol table during the preparation process
Face activating agent, the addition of surfactant can significantly increase the oxygen storage capacity of material.The hair of Publication No. CN102513085A
Bright patent " cerium oxide-zirconium oxide-based composite oxide and preparation method thereof ", by Ce3+And Ce4+It forms hydroxide and precipitates pH
The difference of value, first by the Ce in mixed solution4+And Zr4+Co-precipitation mixing, reprecipitation Ce3+, the cerium oxide after high-temperature roasting
CeO is formed in cerium zirconium sosoloid surface recombination2And ZrO2The Ceria-zirconia base of the mixture of composition, this method preparation is compound
Oxide has excellent peptizaiton to noble metal platinum, while having high Oxygen storage capacity.
Currently, cerium oxide type hydrogen-storing material is essentially all multiple using zirconium oxide or rare-earth oxide as cerium oxide
Object dopant is closed, this kind of usual preparation process of hydrogen-storing material is complicated, and oxygen storage capacity is limited, it is therefore desirable to further develop new oxygen
Change cerium based composite oxide.A kind of In of the propositions such as Zhang Shizheng3+Adulterate CeO2Solid solubility and its oxygen storage capacity in (metallography
Report, 2016,52 (5), 607-613), using the mixed solution of ethylene glycol and water as solvent, Ce (NO3)3·6H2O and In
(NO3)3·4.5H2O is prepared for In as presoma, using solvent-thermal method3+The CeO of doping2Hydrogen-storing material has studied In3+Doping
CeO2Solid solubility and In3+Doping is to CeO2The influence of Oxygen storage capacity, the results showed that In3+The CeO of doping2Middle In3+Consolidate
Solubility is 1%, works as In3+When doping is saturated concentration 1%, CeO2Oxygen storage capacity is optimal.Although Zhang Shizheng etc. is substantial
A kind of completely new hydrogen-storing material using indium doping cerium oxide is proposed, but on the one hand the hydrogen-storing material passes through hydro-thermal process, need
High-tension apparatus is wanted, industrialization production is unfavorable for, on the other hand, the relatively undoped CeO of Oxygen storage capacity2Hydrogen-storing material improves journey
It spends limited.
Summary of the invention
The problem of based on background technique, the invention proposes a kind of modified oxidized cerium hydrogen-storing material of indium oxide and its
Preparation method, by being produced between indium oxide and cerium oxide using the metal composite oxide that indium oxide and cerium oxide form as matrix
Synergistic effect has been given birth to, the Oxygen storage capacity of cerium oxide, and preparation method simple process can be significantly improved, be conducive to industry metaplasia
It produces.
The modified oxidized cerium hydrogen-storing material of a kind of indium oxide proposed by the present invention, the hydrogen-storing material are indium oxide and cerium oxide
The molar ratio of the composite oxides of composition, indium and Ce elements is 0.05-0.45:0.55-0.95.
Preferably, the molar ratio of indium and Ce elements is 0.35:0.65.
The study found that the molar ratio of indium and Ce elements is to storage in the composite oxides of above-mentioned indium oxide and cerium oxide composition
The performance of oxygen material has apparent influence, and when In:Ce molar ratio is 0.35:0.65, the Oxygen storage capacity of metal composite oxide reaches
To optimal.
The present invention also proposes a kind of preparation method of modified oxidized cerium hydrogen-storing material of indium oxide, includes the following steps:
S1, the InCl for being 0.05-0.45:0.55-0.95 by molar ratio3With Ce (NO3)3·6H2O is added to volume ratio
The in the mixed solvent dissolution of dehydrated alcohol and the deionized water composition of 2-4:1 completely, obtains mixing salt solution;
S2, the precipitating reagent of dehydrated alcohol and ammonium hydroxide composition that volume ratio is 2-4:1 is added dropwise under agitation
In mixing salt solution obtained in S1, it is stirred to react 30-60min at 70-90 DEG C, is cooled to room temperature still aging 8-12h, mistake
Filter is washed, dry, and grinding obtains presoma;
S3, the presoma that S2 is obtained is roasted into 4-6h at 500-700 DEG C, obtains the modified oxidized cerium storage oxygen of the indium oxide
Material.
Preferably, in S1, the concentration of metallic element is 0.1-1mol/L in mixing salt solution.
Preferably, in S2, the concentration of ammonium hydroxide is 20-30wt%, and precipitating reagent is added dropwise to salt-mixture obtained in S1
In solution to pH be 9-11.
Preferably, in S3, the presoma that S2 is obtained is under oxygen or air atmosphere with the heating rate liter of 3-6 DEG C/min
Temperature obtains the modified oxidized cerium hydrogen-storing material of the indium oxide to heat preservation roasting 4-6h after 500-700 DEG C.
Preferably, in S2, using alternately washing 4-6 times of ethyl alcohol and deionized water when washing.
Preferably, in S2,8-12h is dried when drying at 70-90 DEG C.
The compound gold of the modified oxidized cerium hydrogen-storing material of indium oxide of the present invention, substantially indium oxide and cerium oxide composition
Belong to oxide.The preparation method of the modified oxidized cerium hydrogen-storing material of the indium oxide is by dissolution salt solvent and precipitating
The selection and compounding of agent, it is ensured that the transformation efficiency of predecessor is generated between indium oxide and cerium oxide in metal obtained oxidation
Synergistic effect, indium oxide can significantly improve the Oxygen storage capacity of cerium oxide, compare simple CeO2Hydrogen-storing material, Oxygen storage capacity can
As many as 8 times are improved, can be used as the storage oxygen functional material of car tail gas purificant and other field.
Detailed description of the invention
Fig. 1 is the XRD diffraction pattern of the hydrogen-storing material of different indium cerium molar ratios in the embodiment of the present invention;
Fig. 2 is the TPR analysis chart of the hydrogen-storing material of different indium cerium molar ratios in the embodiment of the present invention;
Fig. 3 is the Oxygen storage capacity analysis chart of the hydrogen-storing material of different indium cerium molar ratios in the embodiment of the present invention.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of preparation method of the modified oxidized cerium hydrogen-storing material of indium oxide, includes the following steps:
S1, the InCl for being 0.35:0.65 by molar ratio3With Ce (NO3)3·6H2O is added to the anhydrous second that volume ratio is 3:1
The in the mixed solvent dissolution of alcohol and deionized water composition completely, obtains mixing salt solution;
S2, the precipitating reagent of dehydrated alcohol and 25wt% ammonium hydroxide composition that volume ratio is 3:1 is added dropwise under agitation
Enter into mixing salt solution obtained in S1, reacts 30min in 80 DEG C of stirred in water bath, be cooled to room temperature still aging 12h, mistake
Filter, using ethyl alcohol and deionized water alternately washing 5 times, dry 12h, grinding obtain presoma at 80 DEG C;
S3, the presoma for obtaining S2 pour into crucible, are placed in Muffle furnace, in air atmosphere with the heating of 5 DEG C/min
Heat preservation roasting 5h, obtains the modified oxidized cerium hydrogen-storing material of the indium oxide, mole of indium and Ce elements after rate is warming up to 600 DEG C
Than for 0.35:0.65, sample is denoted as 0.35In-0.65Ce.
Embodiment 2
A kind of preparation method of the modified oxidized cerium hydrogen-storing material of indium oxide, includes the following steps:
S1, the InCl for being 0.25:0.75 by molar ratio3With Ce (NO3)3·6H2O is added to the anhydrous second that volume ratio is 3:1
The in the mixed solvent dissolution of alcohol and deionized water composition completely, obtains mixing salt solution;
S2, the precipitating reagent of dehydrated alcohol and 25wt% ammonium hydroxide composition that volume ratio is 3:1 is added dropwise under agitation
Enter into mixing salt solution obtained in S1, reacts 30min in 80 DEG C of stirred in water bath, be cooled to room temperature still aging 8h, mistake
Filter, using ethyl alcohol and deionized water alternately washing 5 times, dry 12h, grinding obtain presoma at 80 DEG C;
S3, the presoma for obtaining S2 pour into crucible, are placed in Muffle furnace, in air atmosphere with the heating of 5 DEG C/min
Heat preservation roasting 5h, obtains the modified oxidized cerium hydrogen-storing material of the indium oxide, mole of indium and Ce elements after rate is warming up to 600 DEG C
Than for 0.25:0.75, sample is denoted as 0.25In-0.75Ce.
Embodiment 3
A kind of preparation method of the modified oxidized cerium hydrogen-storing material of indium oxide, includes the following steps:
S1, the InCl for being 0.45:0.55 by molar ratio3With Ce (NO3)3·6H2O is added to the anhydrous second that volume ratio is 3:1
The in the mixed solvent dissolution of alcohol and deionized water composition completely, obtains mixing salt solution, metallic element is dense in mixing salt solution
Degree is 0.6mol/L;
S2, the precipitating reagent of dehydrated alcohol and 25wt% ammonium hydroxide composition that volume ratio is 3:1 is added dropwise under agitation
Entering into mixing salt solution obtained in S1 to pH is 10, reacts 30min in 80 DEG C of stirred in water bath, it is old to be cooled to room temperature standing
Change 10h, filtering, using ethyl alcohol and deionized water alternately washing 5 times, dry 12h, grinding obtain presoma at 80 DEG C;
S3, the presoma for obtaining S2 pour into crucible, are placed in Muffle furnace, in air atmosphere with the heating of 5 DEG C/min
Heat preservation roasting 5h, obtains the modified oxidized cerium hydrogen-storing material of the indium oxide, mole of indium and Ce elements after rate is warming up to 600 DEG C
Than for 0.45:0.55, sample is denoted as 0.45In-0.55Ce.
Embodiment 4
A kind of preparation method of the modified oxidized cerium hydrogen-storing material of indium oxide, includes the following steps:
S1, the InCl for being 0.05:0.95 by molar ratio3With Ce (NO3)3·6H2O is added to the anhydrous second that volume ratio is 2:1
The in the mixed solvent dissolution of alcohol and deionized water composition completely, obtains mixing salt solution, metallic element is dense in mixing salt solution
Degree is 1mol/L;
S2, the precipitating reagent of dehydrated alcohol and 30wt% ammonium hydroxide composition that volume ratio is 2:1 is added dropwise under agitation
Entering into mixing salt solution obtained in S1 to pH is 11, reacts 50min in 90 DEG C of stirred in water bath, it is old to be cooled to room temperature standing
Change 10h, filtering, using ethyl alcohol and deionized water alternately washing 4 times, dry 8h, grinding obtain presoma at 90 DEG C;
S3, the presoma for obtaining S2 pour into crucible, are placed in Muffle furnace, with the heating of 6 DEG C/min under oxygen atmosphere
Heat preservation roasting 6h, obtains the modified oxidized cerium hydrogen-storing material of the indium oxide, mole of indium and Ce elements after rate is warming up to 500 DEG C
Than for 0.05:0.95, sample is denoted as 0.05In-0.95Ce.
Embodiment 5
A kind of preparation method of the modified oxidized cerium hydrogen-storing material of indium oxide, includes the following steps:
S1, the InCl for being 0.15:0.85 by molar ratio3With Ce (NO3)3·6H2O is added to the anhydrous second that volume ratio is 4:1
The in the mixed solvent dissolution of alcohol and deionized water composition completely, obtains mixing salt solution, metallic element is dense in mixing salt solution
Degree is 0.1mol/L;
S2, the precipitating reagent of dehydrated alcohol and 20wt% ammonium hydroxide composition that volume ratio is 4:1 is added dropwise under agitation
Entering into mixing salt solution obtained in S1 to pH is 9, reacts 60min in 70 DEG C of stirred in water bath, it is old to be cooled to room temperature standing
Change 8h, filtering, using ethyl alcohol and deionized water alternately washing 6 times, dry 10h, grinding obtain presoma at 70 DEG C;
S3, the presoma for obtaining S2 pour into crucible, are placed in Muffle furnace, with the heating of 3 DEG C/min under oxygen atmosphere
Heat preservation roasting 4h, obtains the modified oxidized cerium hydrogen-storing material of the indium oxide, mole of indium and Ce elements after rate is warming up to 700 DEG C
Than for 0.15:0.85, sample is denoted as 0.15In-0.85Ce.
Comparative example 1
A kind of preparation method of pure zirconia cerium hydrogen-storing material, includes the following steps:
S1, by Ce (NO3)3·6H2O is added to the mixed solvent of the dehydrated alcohol that volume ratio is 3:1 and deionized water composition
Middle dissolution completely, obtains salting liquid;
S2, the precipitating reagent of dehydrated alcohol and 25wt% ammonium hydroxide composition that volume ratio is 3:1 is added dropwise under agitation
Enter into salting liquid obtained in S1, react 30min in 80 DEG C of stirred in water bath, be cooled to room temperature still aging 12h, filter,
Using alternately washing 5 times of ethyl alcohol and deionized water, dry 12h, grinding obtain presoma at 80 DEG C;
S3, the presoma for obtaining S2 pour into crucible, are placed in Muffle furnace, in air atmosphere with the heating of 5 DEG C/min
Heat preservation roasting 5h, obtains the pure zirconia cerium hydrogen-storing material, sample is denoted as CeO after rate is warming up to 600 DEG C2。
Comparative example 2
A kind of preparation method of pure zirconia indium hydrogen-storing material, includes the following steps:
S1, by InCl3The in the mixed solvent that the dehydrated alcohol that volume ratio is 3:1 is formed with deionized water is added to have dissolved
Entirely, salting liquid is obtained;
S2, the precipitating reagent of dehydrated alcohol and 25wt% ammonium hydroxide composition that volume ratio is 3:1 is added dropwise under agitation
Enter into salting liquid obtained in S1, react 30min in 80 DEG C of stirred in water bath, be cooled to room temperature still aging 12h, filter,
Using alternately washing 5 times of ethyl alcohol and deionized water, dry 12h, grinding obtain presoma at 80 DEG C;
S3, the presoma for obtaining S2 pour into crucible, are placed in Muffle furnace, in air atmosphere with the heating of 5 DEG C/min
Heat preservation roasting 5h, obtains the pure zirconia indium hydrogen-storing material, sample is denoted as In after rate is warming up to 600 DEG C2O3。
Carry out XRD, TPR and Oxygen storage capacity test respectively to the hydrogen-storing material obtained in embodiment and comparative example, as a result such as
Shown in Fig. 1-3:
(1) XRD analysis
Sample in embodiment 1-5 and comparative example 1 is used into Rigaku company SmartLab 9KW X-ray polycrystal
Diffractometer carries out XRD analysis, as a result as shown in Figure 1, it can be seen that when In:Ce ratio is less than 0.45:0.55, composition metal oxidation
The diffraction maximum of object all only shows CeO2Cubic fluorite structure diffraction peak (JCPDS card card number be 43-1002), when In:Ce ratio
When reaching 0.45:0.55, not only there is CeO in composite oxides2Cubic fluorite structure diffraction peak, have also appeared In2O3Cube
The diffraction maximum of body-centred structure (JCPDS card card number is 06-0416).With the increase of In:Ce ratio, the diffraction of metal composite oxide
Peak intensity reduces, and diffraction peaks broadening illustrates to produce apparent interaction between indium oxide and cerium oxide.
(2) TPR is analyzed
By the sample in embodiment 1-5 and comparative example 1 in Zhejiang Fan Tai Instrument Ltd. temperature programming chemical adsorption instrument
(FINESORB-3010) temperature programmed reduction experiment (H2-TPR) is carried out, as a result as shown in Figure 2.The result shows that embodiment 1-5
There is a low-temperature reduction peak, a medium temperature reduction peak and a high temperature reduction peak in sample, with increase, that is, oxygen of In:Ce ratio
Change increasing for indium content, the peak area of medium temperature reduction peak is gradually increased, and illustrates that indium oxide may conduct in metal composite oxide
Second phase exists;The low-temperature reduction peak of sample after simultaneous oxidation indium is modified is decreased obviously compared with comparative example 1, illustrates to aoxidize
Synergistic effect between indium and cerium oxide improves the redox ability of cerium oxide.
(3) Oxygen storage capacity is analyzed
0.1g or so sample is weighed in U-tube reactor, is inhaled in Zhejiang Fan Tai Instrument Ltd. temperature programming chemistry
The Oxygen storage capacity of metal composite oxide is tested on attached instrument (FINES-ORB-3010) by the method for hydroxide titration (HOT).It is real
Apply the metal composite oxide prepared in a 1-5, the cerium oxide prepared in comparative example 1, the indium oxide 200 prepared in comparative example 2
DEG C Oxygen storage capacity test result is listed in attached drawing 3.The result shows that the Oxygen storage capacity of the metal composite oxide prepared in embodiment is bright
The aobvious Oxygen storage capacity higher than the cerium oxide and indium oxide that prepare in comparative example, the i.e. modification of indium oxide can significantly improve cerium oxide
Oxygen storage capacity, when in metal composite oxide In:Ce ratio be 0.35:0.65 when hydrogen-storing material Oxygen storage capacity be optimal.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of modified oxidized cerium hydrogen-storing material of indium oxide, which is characterized in that the hydrogen-storing material is indium oxide and cerium oxide group
At composite oxides, the molar ratio of indium and Ce elements is 0.05-0.45:0.55-0.95.
2. the modified oxidized cerium hydrogen-storing material of indium oxide according to claim 1, which is characterized in that mole of indium and Ce elements
Than for 0.35:0.65.
3. a kind of preparation method of the modified oxidized cerium hydrogen-storing material of indium oxide according to claim 1 or 2, feature exist
In including the following steps:
S1, the InCl for being 0.05-0.45:0.55-0.95 by molar ratio3With Ce (NO3)3·6H2It is 2-4:1 that O, which is added to volume ratio,
Dehydrated alcohol and deionized water composition in the mixed solvent dissolution completely, obtain mixing salt solution;
S2, the precipitating reagent of dehydrated alcohol and ammonium hydroxide composition that volume ratio is 2-4:1 is added dropwise in S1 under agitation
In obtained mixing salt solution, it is stirred to react 30-60min at 70-90 DEG C, is cooled to room temperature still aging 8-12h, is filtered,
Washing, dry, grinding obtains presoma;
S3, the presoma that S2 is obtained is roasted into 4-6h at 500-700 DEG C, obtains the modified oxidized cerium storage oxygen material of the indium oxide
Material.
4. the preparation method of the modified oxidized cerium hydrogen-storing material of indium oxide according to claim 3, which is characterized in that in S1,
The concentration of metallic element is 0.1-1mol/L in mixing salt solution.
5. the preparation method of the modified oxidized cerium hydrogen-storing material of indium oxide according to claim 3 or 4, which is characterized in that S2
In, the concentration of ammonium hydroxide is 20-30wt%, and it is 9-11 that precipitating reagent, which is added dropwise in mixing salt solution obtained in S1 to pH,.
6. according to the preparation method of the modified oxidized cerium hydrogen-storing material of the described in any item indium oxides of claim 3-5, feature exists
In in S3, the presoma that S2 is obtained is warming up to 500-700 under oxygen or air atmosphere with the heating rate of 3-6 DEG C/min
Heat preservation roasting 4-6h, obtains the modified oxidized cerium hydrogen-storing material of the indium oxide after DEG C.
7. according to the preparation method of the modified oxidized cerium hydrogen-storing material of the described in any item indium oxides of claim 3-6, feature exists
In in S2, using alternately washing 4-6 times of ethyl alcohol and deionized water when washing.
8. according to the preparation method of the modified oxidized cerium hydrogen-storing material of the described in any item indium oxides of claim 3-7, feature exists
In, in S2, when dry at 70-90 DEG C dry 8-12h.
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T. YUZHAKOVA ET AL.: ""Preparation and Characterization of Me2O3-CeO2 (Me ) B, Al, Ga, In) Mixed-Oxide Catalysts"", 《CHEM. MATER.》 * |
张世政等: ""In3+掺杂CeO2的固溶度及其储氧能力"", 《金属学报》 * |
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