CN106693957A - Preparation method of platinum catalyst powder - Google Patents
Preparation method of platinum catalyst powder Download PDFInfo
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- CN106693957A CN106693957A CN201710044498.5A CN201710044498A CN106693957A CN 106693957 A CN106693957 A CN 106693957A CN 201710044498 A CN201710044498 A CN 201710044498A CN 106693957 A CN106693957 A CN 106693957A
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- platinum catalyst
- catalyst powder
- aluminum sulfate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
Abstract
The invention discloses a preparation method of platinum catalyst powder. The preparation method comprises the following preparation steps: adding ammonium chlorocarbonate and aluminum sulfate into polyethyleneglycol; reacting in the presence of organic surface active agent and foaming agent to form precipitate; filtering, and passing through an ethanol solution containing sodium platinichloride and penetrating agent to obtain a suspension; performing heating reaction to obtain doped aluminum oxide granules; and finally, performing ozone oxidation treatment and hydrogen reduction treatment to obtain aluminum oxide based platinum catalyst granules. According to the invention, the method is convenient; and the catalyst has the advantages of high activity, low ignition temperature, favorable high-temperature stability and the like, thereby having high practical value.
Description
Technical field
The invention belongs to noble metal catalyst technical field, and in particular to a kind of preparation method of platinum catalyst powder.
Background technology
Loaded noble metal catalyst is widely used in the hydrogenation of all kinds of organic compounds, dehydrogenation reaction, wherein with
Supported palladium, Platinum Noble Metal Catalyst are most widely used.Support type in hydrogenation, dehydrogenation reaction process in all kinds of organic compounds
Noble metal catalyst has sulfur resistive, the ageing resistance not available for high activity, high selectivity and other metallic catalysts.
The main contributions of palladium component show the selectivity aspect for improving catalyst in noble metal catalyst, and the effect of platinum component is main
The raising of catalyst activity is shown, if the hydrogenation life-span of catalyst can be improved in carried metal iron in the catalyst.
Platinum, palladium, the height of the adding proportion of iron content have a certain impact to active, the selectivity of catalyst.
Chinese patent (CN200810225539.1) is milled to certain particle size using by catalysis material, impregnates noble metal, dries
Powder is obtained after dry, roasting, then ball milling slurrying.Slurry is coated on ceramic honeycomb carrier, is urged after drying, roasting
Agent.The advantage of this kind of method is that just load is fixed on material noble metal before refining, and noble metal will not be moved during defibrination
Move.The surface of this invention noble metal dispersion powder before non-ball milling, during defibrination, powder can be destroyed, fragmentation, produce new breaking
Face, and new surface does not have noble metal and cannot carry out catalytic action, reduces catalyst performance.
The content of the invention
It is an object of the invention to provide a kind of preparation method of platinum catalyst powder, the inventive method is easy, catalyst tool
There are high activity, low light-off temperature, good high-temperature stability, with very strong practical value.
A kind of preparation method of platinum catalyst powder, its preparation process is as follows：
Step 1, by carbonic acid ammonia, aluminum sulfate addition polyethylene glycol, strong stirring is uniform；
Step 2, organic surface active agent and foaming agent are added into polyethylene glycol, continue to stir；
Step 3, question response terminates, and after the completion of sedimentation, filtration washing obtains filter residue, and low-grade fever drying obtains aluminium oxide nano
Grain；
Step 4, aluminum oxide nanoparticle is put into ethanol, adds platinic sodium chloride and bleeding agent, and stirring forms suspended mixed liquor；
Step 5, by suspended mixed liquor addition reactor, heated sealed reaction, reaction is filtrated to get doping type oxidation after terminating
Alumina particles；
Step 6, doping type alumina particle carries out the oxidation reaction in ozone-air atmosphere, obtains platinum oxide-alumina particle；
Step 7, platinum oxide-alumina particle carries out hydrogen reducing reaction, obtains alumina base Pt catalyst granule.
Ammonium carbonate and the proportioning of aluminum sulfate in step 1 are 1.2-3.5:1, the addition of polyethylene glycol is aluminum sulfate quality
3-5 times；Using polyethylene glycol as solvent, with good dispersion effect, while relatively stable aluminium carbonate can be formed
Precipitation, dispersion effect is good, and precipitability is good.
Organic surface active agent in step 2 uses DTAC, and addition is the 2-5% of aluminum sulfate.
Foaming agent in step 2 uses two azoaminobenzenes, and addition is the 5-9% of aluminum sulfate.
Low-grade fever temperature in step 3 is 40-60 DEG C, drying time 5-8h；Dried in low-grade fever mode, can not only be gone
Except polyethylene glycol, while ensureing aluminium carbonate Stability Analysis of Structures, activating agent sticks to precipitation surface, and Stability Analysis of Structures with foaming agent, does
Dry adhesion.
Bleeding agent in step 4 uses AEO, and addition is consistent with foaming agent, and platinic sodium chloride amount is sulphur
1-1.2 times of sour aluminium；Can be adhered in nano-calcium carbonate aluminium surface using bleeding agent, while using the common work of the materials such as dispersant
With the suspension structure of formation stabilization.
Heated sealed temperature in step 5 is 130-150 DEG C, and the heat time is 2-4h；The energy by the way of heated sealed
Enough platinic sodium chloride is infiltrated into completely in alumina particle, form the granular pattern doped structure of stabilization.
Ozone content is 30-50% in ozone-air in step 6, and reaction temperature is 80-100 DEG C, and the reaction time is
2-4h；Using ozone as oxidant, the platinic sodium chloride in precipitation is converted into platinum oxide, forms the platinum oxide-oxidation of stabilization
Constructed of aluminium.
Hydrogen reducing temperature in step 7 is 150-170 DEG C, and pressure is 2-6MPa, and the reaction time is 2-4h；Using hydrogen
As reducing gas, platinum oxide can be converted into platinum element.
In the present invention, with aluminum sulfate and platinic sodium chloride as raw material, platinum catalyst material is prepared, preparing thinking is：Will
Chlorine carbonic acid ammonia, aluminum sulfate are added in polyethylene glycol, are aided with formation precipitation, filtering under conditions of organic surface active agent and foaming agent
Suspension is carried out in the ethanol by platinic sodium chloride with bleeding agent afterwards, doping type alumina particle is obtained by heating response,
Last ozone Oxidation Treatment and hydrogen reducing treatment, obtain alumina base Pt catalyst granule.
Compared with prior art, the invention has the advantages that：
The inventive method is easy, and catalyst has the advantages that high activity, low light-off temperature, good high-temperature stability, with very
Strong practical value.
Brief description of the drawings
Fig. 1 is catalyst fines picture obtained in embodiment 1.
Fig. 2 is the methane conversion curve of different comparative examples and embodiment 1.
Specific embodiment
The present invention is described further with reference to embodiment：
Embodiment 1
A kind of preparation method of platinum catalyst powder, its preparation process is as follows：
Step 1, by carbonic acid ammonia, aluminum sulfate addition polyethylene glycol, strong stirring is uniform；
Step 2, organic surface active agent and foaming agent are added into polyethylene glycol, continue to stir；
Step 3, question response terminates, and after the completion of sedimentation, filtration washing obtains filter residue, and low-grade fever drying obtains aluminium oxide nano
Grain；
Step 4, aluminum oxide nanoparticle is put into ethanol, adds platinic sodium chloride and bleeding agent, and stirring forms suspended mixed liquor；
Step 5, by suspended mixed liquor addition reactor, heated sealed reaction, reaction is filtrated to get doping type oxidation after terminating
Alumina particles；
Step 6, doping type alumina particle carries out the oxidation reaction in ozone-air atmosphere, obtains platinum oxide-alumina particle；
Step 7, platinum oxide-alumina particle carries out hydrogen reducing reaction, obtains alumina base Pt catalyst granule.
Ammonium carbonate and the proportioning of aluminum sulfate in step 1 are 1.2:1, the addition of polyethylene glycol is the 3 of aluminum sulfate quality
Times.
Organic surface active agent in step 2 uses DTAC, and addition is the 2% of aluminum sulfate.
Foaming agent in step 2 uses two azoaminobenzenes, and addition is the 5% of aluminum sulfate.
Low-grade fever temperature in step 3 is 40 DEG C, drying time 5h.
Bleeding agent in step 4 uses AEO, and addition is consistent with foaming agent, and platinic sodium chloride amount is sulphur
1 times of sour aluminium.
Heated sealed temperature in step 5 is 130 DEG C, and the heat time is 2h.
Ozone content is 30% in ozone-air in step 6, and reaction temperature is 80 DEG C, and the reaction time is 2h.
Hydrogen reducing temperature in step 7 is 150 DEG C, and pressure is 2MPa, and the reaction time is 2h.
Testing result：
Catalyst in embodiment is carried out into active evaluation test, and the loaded platinum catalyst powder that can be directly bought using market
End as a comparison case 1 and comparative example 2.Experimental condition is as follows：
Simulated engine exhaust gas volume is constituted：Methane：1000ppm, carbon monoxide：3000ppm, carbon dioxide：10%, one
Nitrogen oxide：1000ppm oxygen：6.5%, nitrogen：Balance Air；Air speed：40000h-1.Result is as shown in Figure 2.
Fig. 2 is the methane conversion curve of different comparative examples and embodiment 1.
Embodiment 2
A kind of preparation method of platinum catalyst powder, its preparation process is as follows：
Step 1, by carbonic acid ammonia, aluminum sulfate addition polyethylene glycol, strong stirring is uniform；
Step 2, organic surface active agent and foaming agent are added into polyethylene glycol, continue to stir；
Step 3, question response terminates, and after the completion of sedimentation, filtration washing obtains filter residue, and low-grade fever drying obtains aluminium oxide nano
Grain；
Step 4, aluminum oxide nanoparticle is put into ethanol, adds platinic sodium chloride and bleeding agent, and stirring forms suspended mixed liquor；
Step 5, by suspended mixed liquor addition reactor, heated sealed reaction, reaction is filtrated to get doping type oxidation after terminating
Alumina particles；
Step 6, doping type alumina particle carries out the oxidation reaction in ozone-air atmosphere, obtains platinum oxide-alumina particle；
Step 7, platinum oxide-alumina particle carries out hydrogen reducing reaction, obtains alumina base Pt catalyst granule.
Ammonium carbonate and the proportioning of aluminum sulfate in step 1 are 3.5:1, the addition of polyethylene glycol is the 5 of aluminum sulfate quality
Times.
Organic surface active agent in step 2 uses DTAC, and addition is the 5% of aluminum sulfate.
Foaming agent in step 2 uses two azoaminobenzenes, and addition is the 9% of aluminum sulfate.
Low-grade fever temperature in step 3 is 60 DEG C, drying time 8h.
Bleeding agent in step 4 uses AEO, and addition is consistent with foaming agent, and platinic sodium chloride amount is sulphur
1.2 times of sour aluminium.
Heated sealed temperature in step 5 is 150 DEG C, and the heat time is 4h.
Ozone content is 50% in ozone-air in step 6, and reaction temperature is 100 DEG C, and the reaction time is 4h.
Hydrogen reducing temperature in step 7 is 170 DEG C, and pressure is 6MPa, and the reaction time is 4h.
Embodiment 3
A kind of preparation method of platinum catalyst powder, its preparation process is as follows：
Step 1, by carbonic acid ammonia, aluminum sulfate addition polyethylene glycol, strong stirring is uniform；
Step 2, organic surface active agent and foaming agent are added into polyethylene glycol, continue to stir；
Step 3, question response terminates, and after the completion of sedimentation, filtration washing obtains filter residue, and low-grade fever drying obtains aluminium oxide nano
Grain；
Step 4, aluminum oxide nanoparticle is put into ethanol, adds platinic sodium chloride and bleeding agent, and stirring forms suspended mixed liquor；
Step 5, by suspended mixed liquor addition reactor, heated sealed reaction, reaction is filtrated to get doping type oxidation after terminating
Alumina particles；
Step 6, doping type alumina particle carries out the oxidation reaction in ozone-air atmosphere, obtains platinum oxide-alumina particle；
Step 7, platinum oxide-alumina particle carries out hydrogen reducing reaction, obtains alumina base Pt catalyst granule.
Ammonium carbonate and the proportioning of aluminum sulfate in step 1 are 2.5:1, the addition of polyethylene glycol is the 4 of aluminum sulfate quality
Times.
Organic surface active agent in step 2 uses DTAC, and addition is the 3% of aluminum sulfate.
Foaming agent in step 2 uses two azoaminobenzenes, and addition is the 8% of aluminum sulfate.
Low-grade fever temperature in step 3 is 50 DEG C, drying time 7h.
Bleeding agent in step 4 uses AEO, and addition is consistent with foaming agent, and platinic sodium chloride amount is sulphur
1.1 times of sour aluminium.
Heated sealed temperature in step 5 is 130-150 DEG C, and the heat time is 2-4h.
Ozone content is 40% in ozone-air in step 6, and reaction temperature is 90 DEG C, and the reaction time is 3h.
Hydrogen reducing temperature in step 7 is 160 DEG C, and pressure is 4MPa, and the reaction time is 3h.
Embodiment 1-3 is as follows with the activity data of comparative example 1-2：
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | |
| T50（℃） | 346 | 351 | 337 | 363 | 377 |
| T90（℃） | 405 | 412 | 401 | 444 | 530 |
One embodiment of the invention is the foregoing is only, the side of the present invention, all use equivalents or equivalent transformation is not intended to limit
The technical scheme that formula is obtained, all falls within protection scope of the present invention.
Claims (9)
1. a kind of preparation method of platinum catalyst powder, its preparation process is as follows：
Step 1, by carbonic acid ammonia, aluminum sulfate addition polyethylene glycol, strong stirring is uniform；
Step 2, organic surface active agent and foaming agent are added into polyethylene glycol, continue to stir；
Step 3, question response terminates, and after the completion of sedimentation, filtration washing obtains filter residue, and low-grade fever drying obtains aluminium oxide nano
Grain；
Step 4, aluminum oxide nanoparticle is put into ethanol, adds platinic sodium chloride and bleeding agent, and stirring forms suspended mixed liquor；
Step 5, by suspended mixed liquor addition reactor, heated sealed reaction, reaction is filtrated to get doping type oxidation after terminating
Alumina particles；
Step 6, doping type alumina particle carries out the oxidation reaction in ozone-air atmosphere, obtains platinum oxide-alumina particle；
Step 7, platinum oxide-alumina particle carries out hydrogen reducing reaction, obtains alumina base Pt catalyst granule.
2. a kind of preparation method of platinum catalyst powder according to claim 1, it is characterised in that the carbonic acid in step 1
Ammonium is 1.2-3.5 with the proportioning of aluminum sulfate:1, the addition of polyethylene glycol is 3-5 times of aluminum sulfate quality.
3. the preparation method of a kind of platinum catalyst powder according to claim 1, it is characterised in that organic in step 2
Surfactant uses DTAC, and addition is the 2-5% of aluminum sulfate.
4. a kind of preparation method of platinum catalyst powder according to claim 1, it is characterised in that the foaming in step 2
Agent uses two azoaminobenzenes, and addition is the 5-9% of aluminum sulfate.
5. a kind of preparation method of platinum catalyst powder according to claim 1, it is characterised in that the low-grade fever in step 3
Temperature is 40-60 DEG C, drying time 5-8h.
6. a kind of preparation method of platinum catalyst powder according to claim 1, it is characterised in that the infiltration in step 4
Agent uses AEO, and addition is consistent with foaming agent, and platinic sodium chloride amount is 1-1.2 times of aluminum sulfate.
7. a kind of preparation method of platinum catalyst powder according to claim 1, it is characterised in that the sealing in step 5
Heating-up temperature is 130-150 DEG C, and the heat time is 2-4h；Platinic sodium chloride can completely be infiltrated into by the way of heated sealed
In alumina particle, the granular pattern doped structure of stabilization is formed.
8. a kind of preparation method of platinum catalyst powder according to claim 1, it is characterised in that the ozone in step 6
Ozone content is 30-50% in air, and reaction temperature is 80-100 DEG C, and the reaction time is 2-4h.
9. a kind of preparation method of platinum catalyst powder according to claim 1, it is characterised in that the hydrogen in step 7
Reduction temperature is 150-170 DEG C, and pressure is 2-6MPa, and the reaction time is 2-4h.
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| CN201710044498.5A CN106693957A (en) | 2017-01-21 | 2017-01-21 | Preparation method of platinum catalyst powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108704640A (en) * | 2018-06-13 | 2018-10-26 | 李飞杰 | A kind of preparation method of porous oxidation platinum catalyst |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1350885A (en) * | 2000-10-31 | 2002-05-29 | 舒德化学公司 | Catalyst for preparing chloroform by hydrogenation dechlorination of carbon tetrachloride |
| US20060100110A1 (en) * | 2000-07-05 | 2006-05-11 | Societe D' Exploitation De Produits Pour Les Industries Chimiques Seppic | Novel hydrogen-absorbing composition, process for its preparation and use as composition for filling optical fibre cables |
| CN1964116A (en) * | 2005-11-10 | 2007-05-16 | Lg电子株式会社 | Catalyst for water gas shift reaction and preparation method thereof |
| CN104998627A (en) * | 2015-07-17 | 2015-10-28 | 西安石油大学 | Preparation method and application of mesoporous-macroporous catalyst for catalytic methane oxidation |
| CN105797766A (en) * | 2016-04-21 | 2016-07-27 | 中广核研究院有限公司 | Integrated catalyst applied to catalytic combustion of methane and preparation method thereof |
-
2017
- 2017-01-21 CN CN201710044498.5A patent/CN106693957A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060100110A1 (en) * | 2000-07-05 | 2006-05-11 | Societe D' Exploitation De Produits Pour Les Industries Chimiques Seppic | Novel hydrogen-absorbing composition, process for its preparation and use as composition for filling optical fibre cables |
| CN1350885A (en) * | 2000-10-31 | 2002-05-29 | 舒德化学公司 | Catalyst for preparing chloroform by hydrogenation dechlorination of carbon tetrachloride |
| CN1964116A (en) * | 2005-11-10 | 2007-05-16 | Lg电子株式会社 | Catalyst for water gas shift reaction and preparation method thereof |
| CN104998627A (en) * | 2015-07-17 | 2015-10-28 | 西安石油大学 | Preparation method and application of mesoporous-macroporous catalyst for catalytic methane oxidation |
| CN105797766A (en) * | 2016-04-21 | 2016-07-27 | 中广核研究院有限公司 | Integrated catalyst applied to catalytic combustion of methane and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 杨勇，: ""催化剂载体氧化铝的制备工艺及改性研究"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 杨骏英等，: ""Pt/γ-Al2O3体系氧化还原过程中PtO2和Pt分散状态的研究"", 《石油学报（石油化工）》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108704640A (en) * | 2018-06-13 | 2018-10-26 | 李飞杰 | A kind of preparation method of porous oxidation platinum catalyst |
| CN108704640B (en) * | 2018-06-13 | 2021-03-30 | 绍兴市梓昂新材料有限公司 | Preparation method of porous platinum oxide catalyst |
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