CN112657492A - Ir-GaOx-based propane dehydrogenation catalyst and preparation method and application thereof - Google Patents
Ir-GaOx-based propane dehydrogenation catalyst and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides an Ir-GaOx propane dehydrogenation catalyst, which is prepared from iridium metal or iridium oxide, gallium oxide and Al2O3Carrier composition, wherein the iridium element content is Al2O30.03-1.5 wt% of carrier, gallium element content is Al2O31-10 wt% of the carrier. The preparation method of the Ir-GaOx-based propane dehydrogenation catalyst comprises the following steps: loading the gallium metal precursor solution and the iridium metal precursor solution on an alumina carrier step by step, or mixing the gallium metal precursor solution and the iridium metal precursor solution uniformly in proportion in advance and then loading the mixture on the alumina carrier; standing and aging the obtained sample, drying and roasting to obtain Ir-GaOxPropane-based dehydrogenation catalysts. Compared with the prior artThe catalyst of the invention has the advantages of good stability and high propylene selectivity.
Description
Technical Field
The invention belongs to the field of olefin preparation by low-carbon alkane dehydrogenation, and particularly relates to an Ir-GaOx-based propane dehydrogenation catalyst, and a preparation method and application thereof.
Background
In the chemical industry, olefins are an intermediate in the production of a range of chemical products such as polymers and are of irreplaceable importance. Among them, propylene plays a very important role in the production of polypropylene, acrylonitrile, oxo alcohols, propylene oxide, and other compounds. Propylene is mainly from steam cracking and catalytic cracking of naphtha. However, with the increasing demand for propylene, the traditional propylene production process has been unable to meet the increasing demand for propylene year after year. In recent years, shale gas is developed to provide a large amount of cheap propane, so that the process for preparing propylene by propane dehydrogenation becomes an effective way for filling up the gaps of supply and demand of propylene.
The preparation of propylene by propane catalytic dehydrogenation is a strong endothermic reaction and is limited by thermodynamic equilibrium, and the reaction needs to be carried out under a high temperature condition. And a series of side reactions such as deep dehydrogenation, cracking and the like are initiated at high temperature, so that the selectivity of propylene is reduced, and in addition, the catalyst is rapidly deactivated along with the increase of surface carbon deposition. Currently, commercial propane dehydrogenation catalysts mainly include both alumina-supported platinum-based and chromium-based catalysts. Wherein, although the platinum-based catalyst has higher dehydrogenation activity, platinum particles are easy to sinter under the high-temperature condition to quickly reduce the activity of the platinum particles, and the platinum-based catalyst needs to be repeatedly regenerated; chromium-based catalysts face heavy metal contamination problems, thus limiting the further development of these catalysts in propane dehydrogenation processes.
Therefore, there is a need to develop a propane dehydrogenation catalyst having high activity, selectivity, stability and environmental friendliness. The present novel propane dehydrogenation catalyst is mostly composed of bimetallic alloy, high-dispersion metal monoatomic and metal oxide. For bimetallic alloy catalyst, CN109939688A discloses an iron gallium based propane dehydrogenation catalyst, which exhibits superior catalytic performance, and the main active component of the catalyst may be iron gallium alloy, however, the propylene selectivity of the catalyst is only 95%, which is higher than 99% compared with industrial catalystThe selectivity of propylene still has a great space for improvement. For the highly dispersed metal monatomic catalyst, CN108325523A discloses a highly dispersed platinum-based catalyst, in which platinum exists in the form of monatomic or sub-nanocluster having a particle size of less than 1nm and containing only 1 to 10 platinum atoms, and although the catalytic performance of the catalyst is improved to some extent, the catalyst is still rapidly deactivated during the reaction process, and the stability is yet to be improved. Similarly, CN109718764A discloses a highly dispersed noble metal catalyst prepared from magnesium gallium composite oxide MgO-Ga2O3As a carrier, the noble metal relates to Rh, Ir and Pt, wherein the noble metal is highly dispersed, the particle size is distributed in the range of monoatomic to 3nm, however, the catalyst can be quickly deactivated in the reaction process, the propylene selectivity is only about 90 percent, and a very large promotion space still exists. In the case of oxide catalysts, gallium oxide, vanadium oxide, zirconium oxide, zinc oxide, cerium oxide, titanium oxide, etc. all exhibit certain activity and selectivity in the propane dehydrogenation reaction, but these catalysts are rapidly deactivated by being reduced or being coked in the reaction. In order to solve this problem, metals can be introduced into the oxide system, and the synergistic catalytic action of the metals and the oxides is exerted through the electronic structure modulation mechanism between the metals and the oxides. For example, Weckhuysen et Al (Angew. chem. int. Ed.2014, 53, 9251-2O3Compared with the catalyst only loaded with Pt and Ga, the supported catalyst with 0.1 wt% of Pt and 3 wt% of Ga has greatly improved propane conversion rate and propylene selectivity, but the catalyst is obviously deactivated and needs repeated scorching regeneration at high temperature. It follows that improving the stability and propylene selectivity of propane dehydrogenation catalysts remains an important research topic.
Disclosure of Invention
Aiming at the problems faced by the propane dehydrogenation catalyst, the invention provides Ir-GaOxThe catalyst has the characteristics of good stability and high propylene selectivity.
The technical scheme for solving the technical problems is as follows: an Ir-GaOx-based propane dehydrogenation catalyst, the Ir-GaOx-based propaneThe dehydrogenation catalyst is prepared from iridium metal or iridium oxide, gallium oxide and Al2O3Carrier composition, wherein the iridium element content is Al2O30.03-1.5 wt% of carrier, gallium element content is Al2O31-10 wt% of the carrier.
The invention also provides a preparation method of the Ir-GaOx-based propane dehydrogenation catalyst, which comprises the following steps:
(1) loading the gallium metal precursor solution and the iridium metal precursor solution on an alumina carrier step by step, or mixing the gallium metal precursor solution and the iridium metal precursor solution uniformly in proportion in advance and then loading the mixture on the alumina carrier;
(2) standing and aging the sample obtained in the step (1), drying and roasting to obtain Ir-GaOxPropane-based dehydrogenation catalysts.
The invention is further arranged that the gallium metal precursor solution in the step (1) is an aqueous solution of gallium salt.
The invention is further provided that the iridium metal precursor solution in the step (1) is an aqueous solution of a salt or acid containing iridium element.
The invention is further set that the aging time in the step (2) is 5-20 h.
The invention is further set that the drying temperature in the step (2) is 80-120 ℃, and the drying time is 6-24 h.
The invention is further set that the roasting temperature in the step (2) is 200-.
The alumina carrier in the preparation method can be a commercial alumina carrier, and alumina carriers with different morphologies and crystal phase structures prepared by other methods can also be used. Such as gamma-Al2O3、δ-Al2O3、θ-Al2O3The material is formed by calcining the pseudo-boehmite at the temperature of 650-750 ℃, 850-950 ℃ and 1000-1100 ℃ for 4-6h respectively.
The catalyst of the invention has simple preparation process and good repeatability. Ir-GaO prepared by the preparation method of the inventionxPropane-based dehydrogenation catalyst, produced in comparison with the prior art processes, in terms of stability and propylene selectivityThe prepared catalyst is obviously improved. Particularly in the aspect of stability, the conversion rate of propane and the selectivity of propylene are not reduced within 240min of a test, even if the reaction time is prolonged to 480min, the conversion rate of propane is only slightly reduced, and the selectivity of propylene can be always kept at about 99 percent, which shows that the catalyst has longer service life and does not need repeated high-temperature scorching regeneration, thereby greatly reducing the production operation cost, improving the production efficiency and having good application prospect.
Drawings
FIG. 1 is Ir-GaO of example 1 of the present inventionx/Al2O3Catalyst and comparative sample Ir/Al2O3、GaOx/Al2O3And Pt-GaOx/Al2O3Comparative results of catalyst propane conversion.
FIG. 2 is Ir-GaO of example 1 of the present inventionx/Al2O3Catalyst and comparative sample Ir/Al2O3、GaOx/Al2O3And Pt-GaOx/Al2O3Comparative results of catalyst propylene selectivity.
FIG. 3 is Ir-GaO of example 1 of the present inventionx/Al2O3The catalyst can obtain the conversion rate of propane and the selectivity of propylene after long-time reaction.
FIG. 4 is Ir-GaO of example 1 of the present inventionx/Al2O3High angle annular dark field scanning transmission electron microscopy of the catalyst.
FIGS. 5 and 6 are Ir-GaO of example 1 of the present inventionx/Al2O3The X-ray photoelectron spectra of Ir4f, Ga3d and O2s of the catalyst.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
Ir-GaOxPropane-based dehydrogenation catalyst consisting of metal Ir or its oxide, Ga oxide and gamma-Al2O3And (3) a carrier. (1) gamma-Al in terms of Ir content2O30.08 wt% of the carrier and a Ga content of gamma-Al2O34.8 wt% of the carrier, and a chloroiridic acid solution and a gallium nitrate solution are taken as metal precursor solutions. (2) Dipping the gallium nitrate solution in the step (1) into gamma-Al by adopting an isometric dipping method2O3The carrier is placed and aged for 12h, dried for 8h at 120 ℃ and then roasted for 4h at 630 ℃. (3) And (3) dipping the chloroiridic acid solution obtained in the step (1) onto the sample obtained in the step (2) by adopting an isometric dipping method, standing and aging for 14h, and drying at 100 ℃ for 12h to obtain the propane dehydrogenation catalyst.
The high-angle annular dark-field scanning transmission electron microscope photograph of the sample is shown in FIG. 4, and the X-ray photoelectron spectra of Ir4f, Ga3d and O2s are shown in FIGS. 5 and 6.
Example 2:
Ir-GaOxPropane-based dehydrogenation catalyst consisting of metal Ir or its oxide, Ga oxide and gamma-Al2O3And (3) a carrier. (1) gamma-Al in terms of Ir content2O30.5 wt% of the carrier and a Ga content of gamma-Al2O36.0 wt% of the carrier, and uniformly mixing the chloroiridic acid solution and the gallium nitrate solution to obtain a mixed precursor solution. (2) Dipping the mixed precursor solution in the step (1) into gamma-Al by adopting an isometric dipping method2O3And (3) standing and aging the carrier for 8h, drying the carrier at 110 ℃ for 16h, and then roasting the carrier at 650 ℃ for 3h to prepare the propane dehydrogenation catalyst.
Example 3:
Ir-GaOxPropane-based dehydrogenation catalyst consisting of metal Ir or its oxide, Ga oxide and gamma-Al2O3And (3) a carrier. (1) gamma-Al in terms of Ir content2O30.03 wt% of the carrier and a Ga content of gamma-Al2O31.0 wt% of carrier, taking chloroiridic acid solution and gallium nitrate solution as raw materialsIs a metal precursor solution. (2) Dipping the gallium nitrate solution in the step (1) into gamma-Al by adopting an isometric dipping method2O3The carrier is placed and aged for 5h, dried for 6h at 80 ℃ and then roasted for 24h at 800 ℃. (3) And (3) dipping the chloroiridic acid solution obtained in the step (1) onto the sample obtained in the step (2) by adopting an isometric dipping method, standing and aging for 5h, drying at 80 ℃ for 6h, and then roasting at 200 ℃ for 1h to obtain the propane dehydrogenation catalyst.
Example 4:
Ir-GaOxPropane-based dehydrogenation catalyst consisting of metal Ir or its oxide, Ga oxide and gamma-Al2O3And (3) a carrier. (1) gamma-Al in terms of Ir content2O31.5 wt% of the support, Ga content being gamma-Al2O310.0 wt% of the carrier, and uniformly mixing the chloroiridic acid solution and the gallium nitrate solution to obtain a mixed precursor solution. (2) Dipping the mixed precursor solution in the step (1) into gamma-Al by adopting an isometric dipping method2O3And (3) standing and aging the carrier for 20h, drying the carrier at 120 ℃ for 24h, and then roasting the carrier at 800 ℃ for 24h to prepare the propane dehydrogenation catalyst.
Comparative example 1:
Ir/γ-Al2O3the preparation of (1): (1) gamma-Al in terms of Ir content2O30.08 wt% of the carrier, and a chloroiridic acid solution was taken as a metal precursor solution. (2) Dipping the chloroiridic acid solution in the step (1) into gamma-Al by adopting an equal-volume dipping method2O3And (3) standing and aging the carrier for 14h, and drying the carrier at 100 ℃ for 12h to obtain the required catalyst.
Comparative example 2:
GaOx/γ-Al2O3the preparation of (1): (1) according to the Ga content of gamma-Al2O34.8 wt% of the carrier, and taking gallium nitrate solution as metal precursor solution. (2) Dipping the gallium nitrate solution in the step (1) into gamma-Al by adopting an isometric dipping method2O3And (3) standing and aging the carrier for 12h, drying the carrier at 120 ℃ for 8h, and then roasting the carrier at 630 ℃ for 4h to obtain the required catalyst.
Comparative example 3:
Pt-GaOx/γ-Al2O3the preparation of (1): (1) according to the Pt content of gamma-Al2O30.08 wt% of the carrier and a Ga content of gamma-Al2O34.8 wt% of the carrier, and taking a chloroplatinic acid solution and a gallium nitrate solution as metal precursor solutions. (2) Dipping the gallium nitrate solution in the step (1) into gamma-Al by adopting an isometric dipping method2O3The carrier is placed and aged for 12h, dried for 8h at 120 ℃ and then roasted for 4h at 630 ℃. (3) And (3) dipping the chloroplatinic acid solution obtained in the step (1) onto the sample obtained in the step (2) by adopting an isometric dipping method, standing and aging for 14h, and drying at 100 ℃ for 12h to obtain the propane dehydrogenation catalyst.
The catalyst samples obtained in example 1, comparative example 2 and comparative example 3 were subjected to a propane dehydrogenation reaction performance test under the following test conditions: 0.1g of the catalysts obtained in example 1, comparative example 2 and comparative example 3 were respectively loaded into a fixed bed reactor, the reaction pressure was set to be 0.1MPa, the reaction temperature was 575 ℃, the reaction gas was a mixed gas of propane, hydrogen and argon, the volume fractions of propane, hydrogen and argon were respectively 20%, 16% and 64%, the total gas flow was 78mL/min, the gas mass space velocity was 780 mL/(g.min), and the reaction time was 240 min.
The reaction results are shown in FIGS. 1 and 2, and it can be seen from FIGS. 1 and 2 that Ir/. gamma. -Al is used as a comparative sample2O3、GaOx/γ-Al2O3And Pt-GaOx/γ-Al2O3Compared with Ir-GaO prepared by the preparation method of the inventionx/γ-Al2O3The catalyst has greatly improved conversion rate and high selectivity and stability. Reacting at 575 deg.c for 240min and Ir-GaOx/γ-Al2O3The propane conversion rate of the catalyst is always kept at about 11.6%, the propylene selectivity is kept at about 99%, and no obvious decrease occurs, which shows that the Ir-GaOx-based propane dehydrogenation catalyst has good stability.
In addition, the sample of example 1 was tested for propane dehydrogenation performance under the same test conditions for a longer period of 480 min.
The reaction results are shown in FIG. 3As can be seen from FIG. 3, Ir-GaO prepared according to the preparation method of the present inventionx/γ-Al2O3The catalyst stability is very good. Within 480min of reaction, Ir-GaOx/γ-Al2O3The propane conversion rate of the catalyst is only slightly reduced, and the propylene selectivity is always maintained at about 99 percent, which shows that the catalyst has strong coking inhibition effect and is difficult to inactivate, so that frequent high-temperature coking regeneration is not needed during use, the production operation cost can be greatly reduced, and the production efficiency is improved.
Ir-GaOx/γ-Al2O3The catalyst has excellent catalytic performance because of its special geometry and electronic structure. As can be seen from the high-angle annular dark-field scanning transmission electron microscope photograph of fig. 4, the metal Ir is in an atomically dispersed state (bright spots in the figure) and is not aggregated into nanoparticles. The X-ray photoelectron spectra of fig. 5 and 6 show that Ir mainly exhibits two different valence states of 0 and +4, which may be Ir dispersed on the surface of the support and doped into the ionic lattice of the support, respectively. Ga is present in the form of +3 valences, indicating that Ga is present in the form of gallium oxide, with no metallic Ga or IrGa alloy present. Thus, Ir-GaOx/γ-Al2O3Special geometrical and electronic structure, and Ir and GaOxThe synergistic catalysis is the main reason of the excellent catalytic performance of the catalyst of the invention.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. An Ir-GaOx-based propane dehydrogenation catalyst, wherein the Ir-GaOx-based propane dehydrogenation catalyst is prepared from iridium metal or iridium oxide, gallium oxide and Al2O3Carrier composition, wherein the iridium element content is Al2O30.03-1.5 wt% of carrier, gallium element content is Al2O31-10 wt% of the carrier.
2. The method of making an Ir-GaOx-based propane dehydrogenation catalyst of claim 1, comprising the steps of:
(1) loading the gallium metal precursor solution and the iridium metal precursor solution on an alumina carrier step by step, or mixing the gallium metal precursor solution and the iridium metal precursor solution uniformly in proportion in advance and then loading the mixture on the alumina carrier;
(2) standing and aging the sample obtained in the step (1), drying and roasting to obtain Ir-GaOxPropane-based dehydrogenation catalysts.
3. The method according to claim 2, wherein the gallium metal precursor solution in step (1) is an aqueous solution of a gallium salt.
4. The production method according to claim 2, wherein the iridium metal precursor solution in step (1) is an aqueous solution of a salt or acid containing iridium element.
5. The method according to claim 2, wherein the aging time in the step (2) is 5 to 20 hours.
6. The method according to claim 2, wherein the drying temperature in the step (2) is 80 to 120 ℃ and the drying time is 6 to 24 hours.
7. The preparation method as claimed in claim 2, wherein the calcination temperature in step (2) is 200-800 ℃ and the calcination time is 1-24 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117696079A (en) * | 2024-02-05 | 2024-03-15 | 浙江师范大学杭州校区 | Nickel oxide composite PbBiO 2 Br S-type heterojunction catalyst and preparation method and application thereof |
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