CN105709736A - Preparation method of embedded Pt@CeO2 nanotube composite catalyst - Google Patents
Preparation method of embedded Pt@CeO2 nanotube composite catalyst Download PDFInfo
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- CN105709736A CN105709736A CN201610183856.6A CN201610183856A CN105709736A CN 105709736 A CN105709736 A CN 105709736A CN 201610183856 A CN201610183856 A CN 201610183856A CN 105709736 A CN105709736 A CN 105709736A
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
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- B01J23/63—Platinum group metals with rare earths or actinides
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Abstract
The invention discloses a preparation method of an embedded Pt@CeO2 nanotube composite catalyst and belongs to the technical field of catalysts. The catalyst is formed by taking CeO2 hollow nanotubes as carriers and embedding Pt nanoparticles in tube walls in a highly dispersed manner. According to the preparation process, Ce(OH)CO3 precursors serve as sacrificial templates and are mixed with NaOH and H2PtCl6 solutions for reactions, Ce(OH)CO3@CeO2 is produced through a solid-liquid interface reaction, [Pt(OH)xCly]<m-> is adsorbed under the electrostatic effect, and the embedded Pt@CeO2 nanotube composite catalyst is prepared through pickling and H2 reduction finally. The method is simple, easy to implement, environment-friendly and clean, and the prepared embedded Pt@CeO2 nanotube composite catalyst has the excellent heat stability and shows superior CO oxidation catalysis performance.
Description
Technical field
The invention belongs to catalyst technical field, be specifically related to a kind of mosaic Pt@CeO2The preparation method of nano-tube composite catalyst.
Background technology
Precious metals pt base catalyst receives much concern at catalyst industry because of the catalysis of its uniqueness activity, selectivity and stability.Owing to Precious Metals Resources is poor and expensive, therefore promote noble metal utilisation and be always the key problem that noble metal catalyst is developed.Wherein by noble metal catalyst sized nanostructures, to increase their specific surface area and then to improve catalytic efficiency, it is the effective ways making full use of noble metal.But, the fusing point of noble metal nano particles is relatively low, easily sinters and affects catalysis activity.To this end, noble metal nano particles is generally combined by scientist with oxide, with the latter as carrier, by nanoparticle " grappling " in carrier surface, to improve the anti-sintering property of noble metal.
In various oxide carriers, CeO2It it is one of the material of most study.Due to Ce element is affected by environment can be at Ce3+With Ce4+Between occur reversible transition to realize storage and the release of oxygen, and CeO2Charge migration and transport of substances, therefore noble metal and CeO can be realized by contact interface between carrier and noble metal2Carrier shows strong interaction in many catalytic reactions.
In order to give full play to Pt and CeO2Synergism in catalytic reaction and the heat stability of raising catalyst, scientist have employed different strategies.Wherein oxide is coated with small size precious metals pt nanoparticle, Pt/CeO can be significantly improved2Catalysis activity and stability.Such as, the Pt/CeO that tight pure China etc. prepare by microemulsion method2@SiO2In core-shell nano, due to SiO2Shell inhibits Pt and CeO in calcination process2Grow up so that remove SiO2Pt/CeO after shell2Compound particle the most still keeps higher heat stability, and due to Pt and CeO2Sufficiently contact, strengthens interaction therebetween, thus it is shown that superior CO oxidation catalytic property (J. Am. Chem. Soc., 2010,132,4,998 4999)；Zhang Hongjie et al. utilizes Ce (OH)3In-situ reducing Pt2+, in the case of being not added with other any reducing agents, it is prepared for the Pt CeO of many core-shell structure copolymer2(J.
Am. Chem. Soc., 2013,135,15,864 15872)；Xia Younan etc. utilize styroflex for template supporting Pt nanoparticle, then at its superficial growth CeO2Shell, then high-temperature calcination removes fibrous template, thus obtains CeO2Nanotube inner surface inlays catalyst (the Angew. Chem. of Pt particle
Int. Ed., 2012,51,9,543 9546).
At the CeO reported2In/noble metal composite hollow structure, noble metal or be carried on hollow CeO2Outer surface or be only embedded in hollow CeO2Inner surface.Precious metals pt nanoparticle is embedded in CeO2Not yet report inside hollow structure material.This structure is expected to improve further the heat stability of Pt particle, strengthens Pt and CeO2Between cooperative effect.
Summary of the invention
For improving heat stability and the catalysis activity of Pt base catalyst further, the invention provides a kind of simple method, a kind of novel mosaic Pt@CeO2The preparation method of nano-tube composite catalyst.This catalyst has excellent heat stability, and illustrates superior CO oxidation catalytic property.
For solving the problems referred to above, the present invention adopts the following technical scheme that
A kind of mosaic Pt@CeO2The preparation method of nano-tube composite catalyst comprises the steps:
A, with cerium salt, carbamide as raw material, centrifugal, deionized water wash, 80 DEG C of dry 6-12 h after 80 DEG C of reaction 24 h, it is thus achieved that solid bar-shaped Ce (OH) CO3Presoma；
B, presoma step A prepared join in NaOH solution, are subsequently added H2PtCl6Solution, (200 ~ 400rpm) stirs 1 day at a slow speed, stands 2 days；After reaction terminates, through centrifugal, deionized water wash, 80 DEG C of dry 6-12 h, obtain PtOx-Ce (OH) CO3@CeO2；
C, sample step B obtained carry out pickling, are then centrifuged for, deionized water wash, 80 DEG C of dry 6-12 h, obtain PtOx-CeO2Hollow Nano pipe；
D, step C is obtained PtOx-CeO2Hollow Nano pipe is H at 250 DEG C ~ 400 DEG C2Reductase 12 ~ 4 h, obtains mosaic Pt@CeO2Nano-tube composite catalyst.
Cerium salt described in above-mentioned steps A is Ce (NO3)3·6H2O or CeCl3·7H2O。
H described in above-mentioned steps B2PtCl6The concentration of solution is 0.01 ~ 0.1 mol/L.
The concentration of the NaOH described in above-mentioned steps B is 2 ~ 6 mol/L.
Acid described in above-mentioned steps C is dilute HNO3Or dilute HCl.
H described in above-mentioned steps D2The atmosphere of reduction is N2Flow velocity: 27
Ml/min, H2Flow velocity: 3 ml/min.
Beneficial effects of the present invention: the preparation method that the present invention provides is simple, it is not necessary to surfactant or polymer auxiliary, it is not required that loaded down with trivial details preparation process, and by Ce (OH) CO3Presoma, as sacrificing template, utilizes its solid-liquid interface with NaOH solution to react and is prepared hollow-core construction, method green cleaning.The mosaic Pt@CeO obtained2In nano-tube composite catalyst, active component Pt particle size is little and is highly dispersed to be embedded in nanotube walls, greatly improves the heat stability of Pt nanoparticle and the catalysis activity of catalyst.
Accompanying drawing explanation
Fig. 1 is embodiment 1 gained mosaic Pt@CeO2The transmission electron microscope picture of nano-tube composite catalyst.
Fig. 2 is embodiment 1 gained mosaic Pt@CeO2Elementary analysis figure is swept in the angle of elevation details in a play not acted out on stage, but told through dialogues scanning transmission electron microscope figure of nano-tube composite catalyst and face thereof.
Fig. 3 is embodiment 1 and embodiment 4 gained mosaic Pt@CeO2The CO oxidation catalytic property of nano-tube composite catalyst.
Fig. 4 is embodiment 2 and embodiment 3 gained mosaic Pt@CeO2The transmission electron microscope picture of nano-tube composite catalyst.
Fig. 4 a is embodiment 2 gained mosaic Pt@CeO2The transmission electron microscope picture of nano-tube composite catalyst.
Fig. 4 b is embodiment 3 gained mosaic Pt@CeO2The transmission electron microscope picture of nano-tube composite catalyst.
Detailed description of the invention
The present invention will be further described with specific embodiment below in conjunction with the accompanying drawings, in order to those skilled in the art can be better understood by the present invention, but and is not so limited the present invention.
Embodiment 1:
Mosaic Pt@CeO2The preparation method of nano-tube composite catalyst
Take 6.95 g Ce (NO3)3·6H2O and 5.77
G carbamide is dissolved in 320 ml deionized waters, stirs 10
Transfer to after min in there-necked flask, at oil bath 80 DEG C, be incubated 24 hours；Cooling, repeatedly deionized water wash, 80 DEG C be dried, i.e. can get bar-shaped Ce (OH) CO3Presoma.
Take in the deionized water after 3.6 g NaOH are dissolved in 30 ml evacuation deoxygenations, be subsequently adding 100 above-mentioned dried Ce (OH) CO of mg3Presoma is stirred, then evacuation, and drum nitrogen carries out deoxygenation；Under nitrogen atmosphere, the H of 0.02 mol/L that 1 ml prepares is added2PtCl6Solution, (300rpm) stirs 1 day at a slow speed, stands 2 days；Centrifugal, repeatedly deionized water wash, 80 DEG C are dried；
By above-mentioned dried sample dispersion in 10 ml deionized waters, add 5 ml HNO3(1
Mol/L), concussion 30-60 minute, is then centrifuged for, repeatedly deionized water wash gently, and 80 DEG C are dried；
Above-mentioned dried sample is carried out H2Reduction, at H2Flow velocity is 3
Ml/min, N2Flow velocity is under the atmosphere of 27 ml/min, is warming up to 250 DEG C and is incubated 2 hours, and heating rate is 3 DEG C/min, final prepared mosaic Pt@CeO2Nano-tube composite catalyst.
Embodiment 2:
Mosaic Pt@CeO2The preparation method of nano-tube composite catalyst: end product pattern is affected by mixing speed
Take 6.95 g Ce (NO3)3·6H2O and 5.77
G carbamide is dissolved in 320 ml deionized waters, stirs 10
Transfer to after min in there-necked flask, at oil bath 80 DEG C, be incubated 24 hours；Cooling, repeatedly deionized water wash, 80 DEG C be dried, i.e. can get bar-shaped Ce (OH) CO3Presoma.
Take in the deionized water after 3.6 g NaOH are dissolved in 30 ml evacuation deoxygenations, be subsequently adding 100 above-mentioned dried Ce (OH) CO of mg3Presoma is stirred, then evacuation, and drum nitrogen carries out deoxygenation；Under nitrogen atmosphere, the H of 0.02 mol/L that 1 ml prepares is added2PtCl6Solution, quickly (900rpm) stirs 1 day, stands 2 days；Centrifugal, repeatedly deionized water wash, 80 DEG C are dried；
By above-mentioned dried sample dispersion in 10 ml deionized waters, add 5 ml HNO3(1
Mol/L), concussion 30-60 minute, is then centrifuged for, repeatedly deionized water wash gently, and 80 DEG C are dried；
Above-mentioned dried sample is carried out H2Reduction, at H2Flow velocity is 3
Ml/min, N2Flow velocity is under the atmosphere of 27 ml/min, is warming up to 250 DEG C and is incubated 2 hours, and heating rate is 3 DEG C/min, final prepared mosaic Pt@CeO2Nano-tube composite catalyst.
Embodiment 3:
Mosaic Pt@CeO2The preparation method of nano-tube composite catalyst: end product pattern is affected by the response time
Take 6.95 g Ce (NO3)3·6H2O and 5.77 g carbamide are dissolved in 320 ml deionized waters, transfer in there-necked flask after stirring 10 min, are incubated 24 hours at oil bath 80 DEG C；Cooling, repeatedly deionized water wash, 80 DEG C be dried, i.e. can get bar-shaped Ce (OH) CO3Presoma.
Take in the deionized water after 3.6 g NaOH are dissolved in 30 ml evacuation deoxygenations, be subsequently adding 100 above-mentioned dried Ce (OH) CO of mg3Presoma is stirred, then evacuation, and drum nitrogen carries out deoxygenation；Under nitrogen atmosphere, the H of 0.02 mol/L that 1 ml prepares is added2PtCl6Solution, (300rpm) stirs 1 day at a slow speed, stands 3 days；Centrifugal, repeatedly deionized water wash, 80 DEG C are dried；
By above-mentioned dried sample dispersion in 10 ml deionized waters, add 5 ml HNO3(1
Mol/L), concussion 30-60 minute, is then centrifuged for, repeatedly deionized water wash gently, and 80 DEG C are dried；
Above-mentioned dried sample is carried out H2Reduction, at H2Flow velocity is 3
Ml/min, N2Flow velocity is under the atmosphere of 27 ml/min, is warming up to 250 DEG C and is incubated 2 hours, and heating rate is 3 DEG C/min, final prepared mosaic Pt@CeO2Nano-tube composite catalyst.
Embodiment 4:
Mosaic Pt@CeO2The preparation method of nano-tube composite catalyst: the high-temperature calcination impact on end product catalytic performance
Take 6.95 g Ce (NO3)3·6H2O and 5.77 g carbamide are dissolved in 320 ml deionized waters, transfer in there-necked flask after stirring 10 min, are incubated 24 hours at oil bath 80 DEG C；Cooling, repeatedly deionized water wash, 80 DEG C be dried, i.e. can get bar-shaped Ce (OH) CO3Presoma.
Take in the deionized water after 3.6 g NaOH are dissolved in 30 ml evacuation deoxygenations, be subsequently adding 100 above-mentioned dried Ce (OH) CO of mg3Presoma is stirred, then evacuation, and drum nitrogen carries out deoxygenation；Under nitrogen atmosphere, the H of 0.02 mol/L that 1 ml prepares is added2PtCl6Solution, (300rpm) stirs 1 day at a slow speed, stands 2 days；Centrifugal, repeatedly deionized water wash, 80 DEG C are dried；
By above-mentioned dried sample dispersion in 10 ml deionized waters, add 5 ml HNO3(1
Mol/L), concussion 30-60 minute, is then centrifuged for, repeatedly deionized water wash gently, and 80 DEG C are dried；
Above-mentioned dried sample is carried out H2Reduction, at H2Flow velocity is 3
Ml/min, N2Flow velocity is under the atmosphere of 27 ml/min, is warming up to 250 DEG C and is incubated 2 hours, and heating rate is 3 DEG C/min, final prepared mosaic Pt@CeO2Nano-tube composite catalyst；
By prepared mosaic Pt@CeO2Nano-tube composite catalyst calcines 2 h at 700 DEG C, and heating rate is 5 DEG C/min.
From above-described embodiment 1-3 and combine accompanying drawing it follows that by Fig. 1 and Fig. 4, along with increasing response time or mixing speed, mosaic Pt@CeO2The hollow degree of nano-tube composite catalyst is more and more inconspicuous.
By above-described embodiment 4 and combine accompanying drawing it follows that from the figure 3, it may be seen that prepare mosaic Pt@CeO2Nano-tube composite catalyst still has good catalysis activity after 700 DEG C of calcinings, indicates mosaic Pt@CeO2Nano-tube composite catalyst has excellent heat stability.
Claims (7)
1. a mosaic Pt CeO2The preparation method of nano-tube composite catalyst, it is characterised in that described mosaic Pt@CeO2Nano-tube composite catalyst is with CeO2Hollow Nano pipe is carrier, and Pt nanoparticle is highly dispersed to be embedded in CeO2The composite catalyst that hollow Nano pipe is internally formed.
2. prepare mosaic Pt CeO as claimed in claim 1 for one kind2The method of nano-tube composite catalyst, it is characterised in that comprise the following steps:
A, with cerium salt, carbamide as raw material, centrifugal, deionized water wash, 80 DEG C of dry 6-12 h after 80 DEG C of reaction 24 h, it is thus achieved that solid bar-shaped Ce (OH) CO3Presoma；
B, presoma prepared by step A and NaOH solution and H2PtCl6Solution mixing is reacted；After reaction terminates, through centrifugal, deionized water wash, 80 DEG C of dry 6-12 h, obtain PtOx-Ce (OH) CO3@CeO2；
C, sample step B obtained carry out pickling, are then centrifuged for, deionized water wash, 80 DEG C of dry 6-12 h, obtain PtOx-CeO2Hollow Nano pipe；
D, step C is obtained PtOx-CeO2Hollow Nano pipe is H at 250 DEG C ~ 400 DEG C2Reductase 12 ~ 4 h, obtains mosaic Pt@CeO2Nano-tube composite catalyst.
Mosaic Pt@CeO the most according to claim 22The preparation method of nano-tube composite catalyst, it is characterised in that the cerium salt described in described step A is Ce (NO3)3·6H2O or CeCl3·7H2O。
Mosaic Pt@CeO the most according to claim 22The preparation method of nano-tube composite catalyst, it is characterised in that the H described in described step B2PtCl6The concentration of solution is 0.01 ~ 0.1 mol/L, and the concentration of described NaOH is 2 ~ 6 mol/L.
Mosaic Pt@CeO the most according to claim 22The preparation method of nano-tube composite catalyst, it is characterised in that the reaction condition described in described step B stirs 1 day for (200 ~ 400rpm) at a slow speed, stands 2 days.
Mosaic Pt@CeO the most according to claim 22The preparation method of nano-tube composite catalyst, it is characterised in that the acid described in described step C is dilute HNO3Or dilute HCl.
Mosaic Pt@CeO the most according to claim 12The application of nano-tube composite catalyst, it is characterised in that described mosaic Pt@CeO2Nano-tube composite catalyst is applied to be catalyzed CO oxidation reaction.
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Cited By (5)
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| CN107638878A (en) * | 2017-11-14 | 2018-01-30 | 济南大学 | A kind of preparation method of sandwich structure nano-tube composite catalyst |
| CN110075834A (en) * | 2019-04-26 | 2019-08-02 | 东南大学 | C-shaped cerium oxide nano fiber of Supported Pt Nanoparticles and its preparation method and application |
| CN110152658A (en) * | 2019-06-03 | 2019-08-23 | 浙江大学 | It is a kind of can anti-sintering mosaic Pd@cerium dioxide nano-tube catalyst and preparation method thereof |
| CN110152653A (en) * | 2019-05-15 | 2019-08-23 | 南京师范大学 | A kind of hollow Nano tubulose manganese-based low-temperature denitration catalyst and preparation method thereof |
| CN114284516A (en) * | 2021-12-30 | 2022-04-05 | 国网安徽省电力有限公司电力科学研究院 | Catalyst with low Pt loading capacity, preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107638878A (en) * | 2017-11-14 | 2018-01-30 | 济南大学 | A kind of preparation method of sandwich structure nano-tube composite catalyst |
| CN107638878B (en) * | 2017-11-14 | 2020-02-04 | 济南大学 | Preparation method of nanotube composite catalyst with sandwich structure |
| CN110075834A (en) * | 2019-04-26 | 2019-08-02 | 东南大学 | C-shaped cerium oxide nano fiber of Supported Pt Nanoparticles and its preparation method and application |
| CN110152653A (en) * | 2019-05-15 | 2019-08-23 | 南京师范大学 | A kind of hollow Nano tubulose manganese-based low-temperature denitration catalyst and preparation method thereof |
| CN110152658A (en) * | 2019-06-03 | 2019-08-23 | 浙江大学 | It is a kind of can anti-sintering mosaic Pd@cerium dioxide nano-tube catalyst and preparation method thereof |
| CN110152658B (en) * | 2019-06-03 | 2020-04-03 | 浙江大学 | Sintering-resistant mosaic Pd @ cerium dioxide nanotube catalyst and preparation method thereof |
| CN114284516A (en) * | 2021-12-30 | 2022-04-05 | 国网安徽省电力有限公司电力科学研究院 | Catalyst with low Pt loading capacity, preparation method and application thereof |
| CN114284516B (en) * | 2021-12-30 | 2024-04-19 | 国网安徽省电力有限公司电力科学研究院 | Low Pt-loaded catalyst, preparation method and application thereof |
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