CN110639510A - Method for preparing monatomic catalyst through re-dispersion of Pt nanoparticles - Google Patents
Method for preparing monatomic catalyst through re-dispersion of Pt nanoparticles Download PDFInfo
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- CN110639510A CN110639510A CN201911003668.0A CN201911003668A CN110639510A CN 110639510 A CN110639510 A CN 110639510A CN 201911003668 A CN201911003668 A CN 201911003668A CN 110639510 A CN110639510 A CN 110639510A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 72
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000006185 dispersion Substances 0.000 title description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 69
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011865 Pt-based catalyst Substances 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 230000032683 aging Effects 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 229920006395 saturated elastomer Polymers 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 6
- 230000001172 regenerating effect Effects 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 23
- 229910052697 platinum Inorganic materials 0.000 description 9
- 239000010453 quartz Substances 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000001833 catalytic reforming Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000000731 high angular annular dark-field scanning transmission electron microscopy Methods 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000001307 helium Substances 0.000 description 3
- 229910052734 helium Inorganic materials 0.000 description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 3
- 238000002407 reforming Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000005865 ionizing radiation Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002699 waste material 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
- 229910002835 Pt–Ir Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Classifications
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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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/394—Metal dispersion value, e.g. percentage or fraction
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a method for preparing a monatomic catalyst by redispersing Pt nanoparticles, and belongs to the technical field of Pt catalysts. The method comprises the following steps: (1) preparing a catalyst containing Pt nanoparticles; (2) and (3) carrying out redispersion treatment on the catalyst containing the Pt nano particles by using a mixture of air, water and HCl at a high temperature to obtain the Pt monatomic catalyst. The method for preparing the monatomic catalyst by redispersing the Pt nanoparticles has the advantages of simple operation and obvious effect, can effectively disperse the Pt nanoparticles into the Pt monatomic, and is suitable for not only newly preparing the monatomic Pt catalyst but also regenerating the deactivated Pt-based catalyst after use.
Description
Technical Field
The invention belongs to the technical field of Pt catalysts, and relates to a method for preparing a monatomic catalyst by redispersing Pt nanoparticles.
Background
The platinum catalyst is a catalyst frequently used in the reaction process of chemistry, petroleum and chemical industry, has higher catalytic activity and good selectivity, is simple and convenient to manufacture, has small using amount, and can improve the performance of the catalyst by changing and improving the manufacturing method. Therefore, the catalyst is widely used in the reaction processes of ammonia oxidation, petroleum hydrocarbon reforming, unsaturated compound oxidation and hydrogenation, carbon monoxide and nitrogen oxide removal in gas and the like.
Catalytic reforming is one of petroleum refining processes, i.e. hydrocarbon molecular structures in gasoline fractions are rearranged into new molecules under the action of a catalyst, so that light gasoline fractions obtained by crude oil distillation are converted into high-octane gasoline rich in aromatic hydrocarbons. Although the platinum catalyst is an excellent catalyst in catalytic reforming reaction, Pt is seriously accumulated under high temperature and water-containing atmosphere along with the progress of the reaction, and researches by mazeck et al find that Pt is seriously accumulated in the catalyst which runs for 1967 days in naphtha catalytic reforming reaction, the maximum grain diameter of Pt reaches 90nm, the activity of the catalyst is greatly reduced, and the accumulated Pt particles need to be redispersed in order to recover the activity of the catalyst.
USP 44897 discloses a redispersion process for Pt-Ir based catalysts by reducing the catalyst, treating it with helium containing HCl and water in an oxygen-free atmosphere, and finally with a gas containing HCl and oxygen to redisperse the active component.
CN 106268883B discloses a method for dispersing high Pt, which comprises the steps of carrying out ionizing radiation treatment on an alumina carrier loaded with active components, and then carrying out water chlorine activation and reduction to obtain a platinum-based agent with higher platinum dispersion degree.
CN107362834A discloses a method for recovering the activity of a catalyst used in continuous reforming, which comprises the steps of burning the used catalyst, soaking in hydrochloric acid at 30 ℃ for 2h, removing waste liquid, drying, and finally performing chlorine activation at 510 ℃ for 4h to obtain an activated catalyst. The method can effectively recover the activity of the continuous reforming catalyst through experimental tests.
The existing catalyst redispersion method has various defects and shortcomings, and the USP 44897 uses helium containing HCl and water under an oxygen-free atmosphere for treatment, so that the cost of the helium used industrially is higher; in patent CN 106268883B, the alumina carrier loaded with active components needs to be subjected to ionizing radiation treatment in advance, and the steps are complicated; patent CN107362834A is soaked in hydrochloric acid at 30 ℃ for 2h, the waste liquid is removed, and the drying is carried out, so that the steps are complicated and the online treatment is difficult.
Disclosure of Invention
The invention aims to provide a method for redispersing Pt clusters into monoatomic groups or preparing a monoatomic Pt catalyst, which is simple to operate, does not need to carry out special treatment on a carrier and a catalyst, uses air as a treatment medium, has low cost, can be operated on line and can effectively redisperse the Pt clusters into monoatomic groups. The invention can provide technical support for the deactivation and regeneration (redispersion) of the platinum-based catalyst in the industrial catalytic reforming. The purpose of the invention is realized by the following technical scheme.
A method for preparing a monatomic catalyst by re-dispersing Pt nanoparticles is characterized by comprising the following steps: (1) preparing a catalyst containing Pt nanoparticles; (2) and (3) carrying out redispersion treatment on the catalyst containing the Pt nano particles by using a mixture of air, water and HCl at a high temperature to obtain the Pt monatomic catalyst.
Further, the content of Pt in the Pt-based catalyst is 0.01-3 wt.%.
Further, the temperature used for the redispersion treatment is 400 to 600 ℃, preferably 450 to 550 ℃.
Further, the preparation method of the medium used for the redispersion treatment comprises the following steps: the air was passed through an aqueous HCl solution to obtain saturated air containing HCl.
Further, the concentration of the aqueous HCl solution of the medium used for the redispersion preparation treatment was: 0.01 to 0.5mol/L, preferably 0.01 to 0.2 mol/L.
Further, the ratio of the medium gas agent used in the redispersion treatment is 1000: 0.5-1000: 10. Gas-agent ratio: the ratio of the amount of gas passing through the catalyst bed per hour to the volume of catalyst.
Furthermore, the redispersion time is 2-15 h.
In order to simulate a catalyst deactivated by severe accumulation of Pt in a reaction, the present invention hydrothermally ages a newly prepared catalyst to obtain a catalyst containing Pt nanoparticles. Carrying out hydrothermal aging treatment on the Pt nanoparticle-containing catalyst obtained in the step (1), and then carrying out redispersion treatment in the step (2); the hydrothermal aging conditions are as follows: the hydrothermal aging temperature is 400-700 ℃, the water content of the hydrothermal aging medium is 5-40 v%, the aging time is 10-72 h, and the gas-to-agent ratio is 1000: 0.5-1000: 10.
The method for preparing the monatomic catalyst by redispersing the Pt nanoparticles has the advantages of simple operation and obvious effect, can effectively disperse the Pt nanoparticles into the Pt monatomic, and is suitable for not only newly preparing the monatomic Pt catalyst but also regenerating the deactivated Pt-based catalyst after use.
Drawings
FIG. 1 is a HAADF STEM plot of a platinum catalyst after 24h hydrothermal aging.
FIG. 2 is a HAADF STEM plot of platinum catalyst after 8h of redispersion.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
Example 1
Aging of the catalyst
The catalyst prepared by the dipping method is put in a quartz tube reactor, the filling amount of the catalyst is 100ml, the hydrothermal aging temperature is 500 ℃, the water content of an aging medium is 20 v%, the gas-agent ratio is 1000:1, and the hydrothermal aging time is 24 h.
The HAADF STEM graph of the aged platinum catalyst is shown in FIG. 1, from which it can be seen that Pt on the platinum catalyst is heavily accumulated in a large particle form after hydrothermal aging for 24 hours.
Example 2
Redispersion treatment of Pt nanoparticles
Placing the aged catalyst, namely the catalyst containing Pt nano particles, in a quartz tube, wherein the loading amount of the catalyst is 100ml, the heating temperature is set to 400 ℃, the gas-to-agent ratio is 1000:0.5, the concentration of an HCl solution is 0.02mol/L, air passes through the HCl solution in advance to prepare saturated air containing HCl, then the saturated air enters the quartz tube to contact with the catalyst, and the redispersion treatment time is 2 h.
Example 3
Redispersion treatment of Pt nanoparticles
Placing the aged catalyst, namely the catalyst containing Pt nano particles, in a quartz tube, wherein the loading amount of the catalyst is 100ml, the heating temperature is set to be 500 ℃, the gas-to-agent ratio is 1000:1, the concentration of an HCl solution is 0.05mol/L, air passes through the HCl solution in advance to prepare saturated air containing HCl, then the saturated air enters the quartz tube to contact with the catalyst, and the redispersion treatment time is 5 h.
Example 4
Redispersion treatment of Pt nanoparticles
Placing the aged catalyst, namely the catalyst containing Pt nano particles, in a quartz tube, wherein the loading amount of the catalyst is 100ml, the heating temperature is set to be 500 ℃, the gas-to-agent ratio is 1000:1, the concentration of the HCl solution is 0.2mol/L, air passes through the HCl solution in advance to prepare saturated air containing HCl, then the saturated air enters the quartz tube to contact with the catalyst, and the redispersion treatment time is 8 h.
The HAADF STEM diagram of the redispersed platinum catalyst is shown in FIG. 2, from which it can be seen that the Pt particles are effectively dispersed in a monoatomic state. It is fully demonstrated by combining fig. 1 and 2 that the redispersion treatment process of the present invention can effectively disperse Pt particles into monoatomic particles for Pt particles that accumulate more heavily.
Example 5
Redispersion treatment of Pt nanoparticles
Placing the aged catalyst, namely the catalyst containing Pt nano particles, in a quartz tube, wherein the loading amount of the catalyst is 100ml, the heating temperature is set to be 550 ℃, the gas-to-agent ratio is 1000:2, the concentration of an HCl solution is 0.01mol/L, air passes through the HCl solution in advance to prepare saturated air containing HCl, then the saturated air enters the quartz tube to contact with the catalyst, and the redispersion treatment time is 10 hours.
Claims (10)
1. A method for preparing a monatomic catalyst by re-dispersing Pt nanoparticles is characterized by comprising the following steps: (1) preparing a catalyst containing Pt nanoparticles; (2) and (3) carrying out redispersion treatment on the catalyst containing the Pt nano particles by using a mixture of air, water and HCl at a high temperature to obtain the Pt monatomic catalyst.
2. The method according to claim 1, wherein the Pt content in the Pt-based catalyst is 0.01 to 3 wt.%.
3. The method according to claim 1, wherein the temperature used for the redispersion treatment is 400 to 600 ℃.
4. The method according to claim 1, wherein the temperature used for the redispersion treatment is 450 to 550 ℃.
5. The method according to claim 1, wherein the media used for redispersion is prepared by: the air was passed through an aqueous HCl solution to obtain saturated air containing HCl.
6. The process according to claim 5, wherein the aqueous HCl concentration of the medium used in the redispersion preparation is: 0.01 to 0.5 mol/L.
7. The process according to claim 5, wherein the aqueous HCl concentration of the medium used in the redispersion preparation is: 0.01 to 0.2 mol/L.
8. The method according to claim 1, wherein the ratio of the medium gas to the medium gas is 1000:0.5 to 1000: 10.
9. The method according to claim 1, wherein the redispersion time is 2 to 15 hours.
10. The method according to claim 1, wherein the catalyst containing Pt nanoparticles obtained in step (1) is subjected to a hydrothermal aging treatment, and then subjected to a redispersion treatment in step (2); the hydrothermal aging conditions are as follows: the hydrothermal aging temperature is 400-700 ℃, the water content of the hydrothermal aging medium is 5-40 v%, the aging time is 10-72 h, and the gas-to-agent ratio is 1000: 0.5-1000: 10.
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| CN201911003668.0A CN110639510A (en) | 2019-10-22 | 2019-10-22 | Method for preparing monatomic catalyst through re-dispersion of Pt nanoparticles |
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| CN201911003668.0A CN110639510A (en) | 2019-10-22 | 2019-10-22 | Method for preparing monatomic catalyst through re-dispersion of Pt nanoparticles |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114618476A (en) * | 2022-02-16 | 2022-06-14 | 中国科学院大连化学物理研究所 | Monoatomic platinum-based catalyst, and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108325523A (en) * | 2018-02-02 | 2018-07-27 | 华东理工大学 | A kind of propane dehydrogenation catalyst and preparation method thereof |
| CN110252337A (en) * | 2019-06-05 | 2019-09-20 | 北京氦舶科技有限责任公司 | A kind of monatomic catalyst of Pt/CoO and its preparation method and application |
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2019
- 2019-10-22 CN CN201911003668.0A patent/CN110639510A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108325523A (en) * | 2018-02-02 | 2018-07-27 | 华东理工大学 | A kind of propane dehydrogenation catalyst and preparation method thereof |
| CN110252337A (en) * | 2019-06-05 | 2019-09-20 | 北京氦舶科技有限责任公司 | A kind of monatomic catalyst of Pt/CoO and its preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| FRANÇOIS LE NORMAND等: ""Redispersion of Sintered Pt/Al2O3 Naphtha Reforming Catalysts: An in Situ Study Monitored by X-ray Absorption Spectroscopy"", 《J. PHYS. CHEM.》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114618476A (en) * | 2022-02-16 | 2022-06-14 | 中国科学院大连化学物理研究所 | Monoatomic platinum-based catalyst, and preparation method and application thereof |
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Application publication date: 20200103 |