CN109926067B - Platinum-palladium-cobalt ternary metal hydrogenation dearomatization catalyst and preparation method thereof - Google Patents
Platinum-palladium-cobalt ternary metal hydrogenation dearomatization catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention provides a platinum-palladium-cobalt ternary metal hydrogenation dearomatization catalyst and a preparation method thereof, wherein the preparation process of the catalyst adopts a method of stepwise impregnation of an active metal precursor, and specifically, the prepared carrier is firstly impregnated with the palladium-cobalt metal precursor, and then is impregnated with the platinum-palladium metal precursor after reduction and post-treatment. The catalyst prepared by the method has high utilization rate of platinum and palladium noble metals and strong capability of a synergistic catalyst, and the introduction of platinum and palladium leads to the enhancement of the aromatic hydrogenation performance of non-noble metal cobalt. The catalyst is especially suitable for the hydrofining process of preparing clean diesel oil, high-quality lubricant base oil and white oil by deeply dearomatizing raw oil with high sulfur content.
Description
Technical Field
The invention relates to a platinum-palladium-cobalt ternary metal hydrogenation dearomatization catalyst and a preparation method thereof.
Background
The deep hydrogenation dearomatization technology is widely applied to the refining and upgrading process of petroleum refining products, and is mainly characterized in that aromatic hydrocarbon in oil products, particularly polycyclic aromatic hydrocarbon difficult to remove, is subjected to deep hydrogenation saturation by using a reduction metal hydrogenation catalyst, so that various products with excellent product performance and meeting the environmental protection requirement, such as diesel oil with high cetane index, low-smoke point aviation kerosene, lubricating oil base oil or white oil with good photothermal oxidation stability and the like, are obtained.
From the thermodynamics of the reaction, the low reaction temperature and the high reaction pressure are favorable for the hydrogenation saturation of the aromatic hydrocarbon to the alkane, which requires that the prepared catalyst has good low-temperature hydrogenation activity. The VIII transition metal (such as nickel, cobalt, ruthenium, rhodium, palladium, platinum and the like) reduced catalyst has the aromatic hydrocarbon hydrogenation saturation capacity. In contrast, the non-noble metal nickel and cobalt-based catalyst has poor aromatic hydrogenation activity but low price; the noble metals of ruthenium, rhodium, palladium and platinum based catalysts have good arene hydrogenation activity, but the cost is high. Especially in the process of hydrofining aromatic hydrocarbon of a sulfur-containing system with complex raw materials, the synergistic catalysis of various noble metals is often used. Patents CN106466601A, CN1245204A, CN104826650B, US5391291A, US5393408, US5879539 and the like report that noble metal platinum-palladium bimetallic catalysts show good synergistic catalyst effect in the deep hydrogenation saturation process of aromatics with sulfur system. Researches show that platinum-palladium alloy nanoparticles with strong electron interaction exist on the surface of the platinum-palladium bimetallic catalyst, platinum can transfer electrons to palladium, and an electron cloud structure on the surface of the platinum-palladium metal is optimized, so that the bonding effect of metal active sites and sulfides is weakened, and the sulfur-resistant hydrogenation activity of the bimetallic catalyst is improved.
Although the precious metal platinum-palladium bimetallic catalyst shows good deep hydrogenation activity of aromatic hydrocarbon, the platinum-palladium alloy nano-particles in the traditional preparation process of the platinum-palladium catalyst are not high in proportion, and the platinum and the palladium mostly exist as single metal particles, so that the synergistic catalytic action of the platinum-palladium bimetallic catalyst is difficult to fully exert. Patent CN1205316C discloses a preparation method of a multi-element metal hydrogenation saturation catalyst in which platinum-palladium noble metal and non-noble metal are loaded on a carrier containing porous silica-alumina, but the acting force between non-noble metal components and noble metal components in the multi-element metal catalyst prepared by the method is weak, and the intrinsic hydrogenation activity of the noble metal components is not significantly improved. Therefore, the synergistic catalytic action of the non-noble metal component and the noble metal component is enhanced by further regulating and controlling the preparation method of the catalyst, and the catalyst has very important significance for developing a non-noble metal substituted or semi-substituted platinum-palladium aromatic hydrogenation catalyst with high-efficiency hydrogenation activity.
Disclosure of Invention
The invention aims to provide a preparation method of a novel platinum-palladium-cobalt ternary metal hydrofining dearomatization catalyst. The preparation process of the catalyst adopts a method of stepwise impregnation of an active metal precursor, and specifically, the prepared carrier is firstly impregnated with a palladium-cobalt metal precursor, and then is impregnated with a platinum-palladium metal precursor after reduction and post-treatment. The catalyst prepared by the method has high utilization rate of platinum and palladium noble metals and strong capability of a synergistic catalyst, and the introduction of platinum and palladium leads to the enhancement of the aromatic hydrogenation performance of non-noble metal cobalt. The catalyst is especially suitable for the hydrofining process of preparing clean diesel oil, high-quality lubricant base oil and white oil by deeply dearomatizing raw oil with high sulfur content.
In order to achieve the purpose, the invention adopts the following technical scheme:
an improved preparation method of an aromatic deep hydrogenation saturation catalyst comprises the following steps:
(a) preparing a silicon-aluminum mixed oxide carrier;
(b) preparing a cobalt-palladium mixed precursor salt solution, and controlling the concentration of cobalt in the solution to be 1.0 multiplied by 10 -2 g/ml~3.0×10 -2 g/ml and a palladium concentration of 1.7X 10 -3 g/ml ~1.0×10 -2 g/ml;
(c) impregnating the cobalt-palladium mixed precursor salt solution prepared in the step (b) on the carrier prepared in the step (a);
(d) drying, roasting and reducing the impregnated sample in the step (c);
(e) preparing a platinum-palladium mixed precursor salt solution, and controlling the concentration of platinum in the solution to be 0.5 multiplied by 10 -3 g/ml~6.7×10 -3 g/ml and a palladium concentration of 0.2X 10 -3 g/ml ~1.0×10 -2 g/ml;
(f) impregnating the sample obtained in the step (d) with the platinum-palladium mixed precursor salt solution prepared in the step (e);
(g) and (f) drying, roasting and reducing the impregnated sample to obtain the platinum-palladium-cobalt ternary metal catalyst.
Preferably, the alumina-silica component precursor of the support prepared in (a) may be at least two of alumina sol, silica sol, pseudo-boehmite, amorphous silica-alumina, silica-alumina molecular sieve;
preferably, the carrier in (a) can be prepared by a sol-gel or mechanical mixing method, and the extruded shape of the carrier can be any one of three Chinese herbs, four-leaf clover, cylindrical and spherical;
Preferably, the mass fraction of the oxides of the metal component in the carrier prepared in (a) is as follows: 20-80% of aluminum oxide and 20-40% of silicon oxide, wherein the sum of the total mass fraction is 100%;
preferably, the cobalt salt precursor used in (b) may be any one of cobalt chloride, cobalt nitrate, cobalt sulfate, cobalt acetate and cobalt oxalate; the palladium salt precursor can be any one of palladium chloride, palladium nitrate, ammonium chloropalladate and tetraammine palladium nitrate;
preferably, the cobalt-palladium mixed salt solution used in (b) is controlled to have a weight ratio of cobalt to palladium of 6.0: 1.0 to 3.0: 1.0;
preferably, (d) the drying treatment is performed at 60-150 ℃ for 1-12 hours, the roasting treatment is performed at 350-550 ℃ for 1-5 hours, and the reduction treatment is performed at 200-400 ℃ for 1-5 hours;
preferably, the platinum salt precursor used in (e) may be any one of chloroplatinic acid, ammonium chloroplatinate, tetraammineplatinum chloride and tetraammineplatinum nitrate; the palladium salt precursor can be any one of palladium chloride, palladium nitrate, ammonium chloropalladate and tetraammine palladium nitrate;
preferably, (e) the weight ratio of the platinum to palladium precursor salt solution, converted to platinum and palladium, is controlled to be 0.2: 1.0 to 2.0: 1.0;
preferably, (c) and (f) the aging temperature is controlled to be 20-120 ℃ and the aging time is controlled to be 1-12 hours when the carrier is impregnated;
Preferably, (f) impregnating the carrier under vacuum or under the protection of inert gas (such as nitrogen);
preferably, the drying treatment in (g) is at 60-150 ℃ for 1-12 hours, the roasting treatment is at 350-550 ℃ for 1-5 hours, and the reduction treatment is at 250-400 ℃ for 1-5 hours;
preferably, the total noble metal loading of platinum and palladium in the catalyst obtained in (g) is from 0.3 to 1.0 wt% and the cobalt metal loading is from 0.5 to 3.0 wt%.
When the catalyst is applied to raw oil hydrofining, the reaction conditions are as follows: the reaction temperature is 190 ℃ and 350 ℃, the reaction pressure is 14-18 MPa, and the space velocity is 0.3-1.0 h -1 The hydrogen-oil volume ratio is 500-800.
The invention has the advantages that: the preparation process of the catalyst prepared by the method adopts a step-by-step impregnation method, namely, the prepared carrier is firstly impregnated with the cobalt-palladium metal precursor mixed solution, and is then impregnated with the platinum-palladium metal precursor after reduction and treatment. In the first step, a cobalt-palladium mixed solution is immersed, and the reduction of cobalt can be promoted by introducing palladium in the reduction process. The obtained reduction sample can provide a catalyst carrier with cobalt nanoparticles as an anchoring source and palladium nanoparticles as seed crystals, and the platinum-palladium solution impregnated in the second step can be further induced to be dispersed on the surface of the catalyst carrier in the form of platinum-palladium alloy due to the high surface free energy and electrochemical displacement of the metal nanoparticles. The catalyst prepared by the method has high concentration of the platinum-palladium alloy nanoparticles, and exists in a form of taking palladium as a core and platinum as a shell, so that the catalyst has strong synergistic catalytic capability. In addition, due to the introduction of the platinum and the palladium, the aromatic hydrogenation performance of the non-noble metal cobalt is further improved. In the platinum-palladium-cobalt ternary catalyst prepared by the method, the platinum-palladium-cobalt active metals show good synergistic catalytic action, and the method is suitable for removing aromatic hydrocarbon of raw oil with high sulfur content. The invention provides a preparation method of an aromatic deep hydrofining catalyst with strong raw material adaptability, and the preparation method is simple in preparation process, good in reproducibility and convenient for industrial production.
Detailed Description
The preparation and use of the present invention are further described with reference to the following specific examples, but the specific embodiments described herein are only for illustrating and explaining the present invention and are not intended to limit the present invention.
The specific surface area and the pore volume of the catalyst material are measured by a low-temperature liquid nitrogen adsorption method.
Example 1
130 g of amorphous silica-alumina (pore volume 0.9 mL/g, specific surface area 490 m) 2 80% of dry basis), 60 g of pseudo-boehmite (70% of dry basis, 0.7 mL/g of pore volume and 280m of specific surface area 2 (g), 4.5 g of sesbania powder was put into a roll mill and mixed, 170 g of a dilute nitric acid solution (containing 3% by mass of nitric acid based on the dry weight of pseudo-boehmite) was added and then rolled into a paste, and extruded strips (diameter of about 1.6 mm) were dried at 120 ℃ for 12 hours and then calcined at 500 ℃ for 4 hours to obtain a carrier SCAT.
The CoCl is impregnated by a conventional method with equal volume 2 (analytically pure) and PdCl 2 (analytically pure) mixed solution (the weight ratio of cobalt to palladium in cobalt-palladium mixed salt solution is 5.31: 1.00) is soaked on a carrier SCAT, aged for 3 hours at 50 ℃, dried for 10 hours at 120 ℃, roasted for 3 hours at 500 ℃ and reduced for 3 hours at 300 ℃ by hydrogen to obtain an MCAT-1 sample; continuously adopting an equal-volume impregnation method to prepare PdCl 2 (analytically pure) and H 2 PtCl 6 (analytically pure) mixed solution (platinum-palladium mixed salt solution with weight ratio of platinum to palladium of 0.75: 1.00) is soaked on a carrier MCAT-1 under vacuum condition, aged for 3 hours at 50 ℃, dried for 10 hours at 120 ℃, roasted for 3 hours at 500 ℃ and reduced for 3 hours by hydrogen at 350 ℃ to obtain CAT-1 catalyst. The metal loading of the prepared catalyst according to the final platinum, palladium and cobalt is controlled to be 0.12wt%, 0.32wt% and 0.85wt% relative to the carrier respectively.
Example 2
Co (NO) is impregnated by a conventional equal volume impregnation method 3 ) 2 (analytically pure) and PdCl 2 (analytically pure) mixed solution (the weight ratio of cobalt to palladium in cobalt-palladium mixed salt solution is 5.31: 1.00) is soaked on a carrier SCAT, aged for 3 hours at 50 ℃, dried for 10 hours at 120 ℃, roasted for 3 hours at 500 ℃ and reduced for 3 hours at 300 ℃ by hydrogen to obtain an MCAT-2 sample; continuously adopting an equal-volume impregnation method to prepare PdCl 2 (analytically pure) and H 2 PtCl 6 (analytically pure) mixed solution (platinum-palladium mixed salt solution with weight ratio of platinum to palladium of 0.75: 1.00) is soaked on a carrier MCAT-2 under vacuum condition, aged for 3 hours at 50 ℃, dried for 10 hours at 120 ℃, roasted for 3 hours at 500 ℃ and reduced for 3 hours by hydrogen at 350 ℃ to obtain CAT-2 catalyst. The metal loading of the prepared catalyst according to the final platinum, palladium and cobalt is controlled to be 0.12wt%, 0.32wt% and 0.85wt% relative to the carrier respectively.
Example 3
Co (NO) is impregnated by a conventional equal volume impregnation method 3 ) 2 (analytically pure) PdCl 2 (analytically pure) mixed solution (cobalt-palladium mixed salt solution with a weight ratio of cobalt to palladium of 4.25: 1.0) dipping on a carrier SCAT, aging for 3 hours at 50 ℃, then drying for 10 hours at 120 ℃, roasting for 3 hours at 500 ℃, and reducing by hydrogen at 300 ℃ for 3 hours to obtain an MCAT-3 sample; continuously adopting an equal-volume impregnation method to prepare PdCl 2 (analytically pure) and [ Pt (NH) 3 ) 4 ] (NO 3 ) 2 (analytically pure) mixed solution (platinum-palladium mixed salt solution with weight ratio of platinum to palladium being 1.00: 1.00) is soaked on carrier MCAT-3 under vacuum condition, aged for 3 hours at 50 ℃, dried for 10 hours at 120 ℃, roasted for 3 hours at 500 ℃ and reduced for 3 hours at 350 ℃ by hydrogen to obtain CAT-3 catalyst. The metal loading of the prepared catalyst according to the final platinum, palladium and cobalt is controlled to be 0.12wt%, 0.32wt% and 0.85wt% relative to the carrier respectively.
Example 4
Co (NO) is impregnated by a conventional equal volume impregnation method 3 ) 2 (analytically pure) and PdCl 2 (analytically pure) mixed solution (the weight ratio of cobalt to palladium in cobalt-palladium mixed salt solution is 3.27: 1.00) is soaked on a carrier SCAT, aged for 3 hours at 50 ℃, dried for 10 hours at 120 ℃, roasted for 3 hours at 500 ℃ and reduced for 3 hours at 300 ℃ by hydrogen to obtain an MCAT-4 sample; continuously adopting an equal-volume impregnation method to prepare PdCl 2 (analytically pure) and H 2 PtCl 6 (analytically pure) mixed solution (platinum-palladium mixed salt solution with weight ratio of platinum to palladium of 2.00: 1.00) is soaked on a carrier MCAT-4 under vacuum condition, aged for 3 hours at 50 ℃, dried for 10 hours at 120 ℃, roasted for 3 hours at 500 ℃ and reduced for 3 hours at 350 ℃ by hydrogen to obtain CAT-4 catalyst. The metal loading of the prepared catalyst according to the final platinum, palladium and cobalt is controlled to be 0.12wt%, 0.32wt% and 0.85wt% relative to the carrier respectively.
Comparative example 1
Co (NO) is impregnated by a conventional equal volume impregnation method 3 ) 2 Soaking the (analytically pure) solution on a carrier SCAT, aging at 50 ℃ for 3 hours, then drying at 120 ℃ for 10 hours, roasting at 500 ℃ for 3 hours, and reducing at 400 ℃ for 3 hours to obtain an MCAT-5 sample; continuously adopting the method of equal-volume impregnationPdCl is prepared from PdCl 2 (analytically pure) and H 2 PtCl 6 The mixed solution (analytically pure) is soaked on a carrier MCAT-5 under the vacuum condition, aged for 3 hours at 50 ℃, dried for 10 hours at 120 ℃, roasted for 3 hours at 500 ℃ and reduced for 3 hours at 350 ℃ by hydrogen to obtain the CAT-5 catalyst. The metal loading of the prepared catalyst according to the final platinum, palladium and cobalt is controlled to be 0.12wt%, 0.32wt% and 0.85wt% relative to the carrier respectively.
Comparative example 2
Co (NO) is impregnated by a conventional equal volume impregnation method 3 ) 2 (analytically pure) H 2 PtCl 6 (analytically pure) mixed solution (the weight ratio of cobalt to palladium in cobalt-platinum mixed salt solution is 14.17: 1.0) is soaked on a carrier SCAT, aged for 3 hours at 50 ℃, dried for 10 hours at 120 ℃, roasted for 3 hours at 500 ℃ and reduced for 3 hours at 300 ℃ by hydrogen to obtain an MCAT-6 sample; continuously adopting an equal-volume impregnation method to prepare PdCl 2 (analytically pure) and [ Pt (NH) 3 ) 4 ] (NO 3 ) 2 (analytically pure) mixed solution (platinum-palladium mixed salt solution with weight ratio of platinum to palladium of 0.19: 1.00) is soaked on carrier MCAT-6 under vacuum condition, aged for 3 hours at 50 ℃, dried for 10 hours at 120 ℃, roasted for 3 hours at 500 ℃ and reduced for 3 hours at 350 ℃ by hydrogen to obtain CAT-6 catalyst. The metal loading of the prepared catalyst according to the final platinum, palladium and cobalt is controlled to be 0.12wt%, 0.32wt% and 0.85wt% relative to the carrier respectively.
Comparative example 3
Using a conventional equal-volume impregnation method to contain Co (NO) 3 ) 2 (analytically pure) PdCl 2 (analytically pure) and H 2 PtCl 6 The mixed solution is soaked on a carrier SCAT, aged for 3 hours at 50 ℃, dried for 10 hours at 120 ℃, roasted for 3 hours at 500 ℃ and reduced for 3 hours at 350 ℃ to obtain the CAT-7 catalyst. The metal loading of the prepared catalyst according to the final platinum, palladium and cobalt is controlled to be 0.12wt%, 0.32wt% and 0.85wt% relative to the carrier respectively.
Comparative example 4
Adopting a conventional equal-volume impregnation method to impregnate PdCl 2 (analytically pure) and H 2 PtCl 6 The mixed solution (analytically pure) is soaked on a carrier SCAT, aged for 3 hours at 50 ℃, dried for 10 hours at 120 ℃, roasted for 3 hours at 500 ℃ and reduced by hydrogen at 350 ℃ for 3 hours to obtain the CAT-8 catalyst. The metal loading of the final platinum and palladium in the prepared catalyst is controlled to be 0.20wt% and 0.40wt% relative to the carrier respectively.
The CAT-1 to CAT-8 catalysts were used for evaluation of the hydrorefining performance of feed oil No. 1, feed oil No. 2 and feed oil No. 3 (physical properties of feed oil are shown in Table 1). The evaluation operating conditions are that 30mL of catalyst (particles are crushed to 14-20 meshes) and 60mL of quartz sand (14-20 meshes) are mixed and filled, the reaction temperature is 190- -1 Hydrogen to oil volume ratio of 700.
The physicochemical properties of the above catalysts are shown in Table 2, and the properties of the hydrogenated oils corresponding to the performance evaluations are shown in tables 3 to 5.
TABLE 1 physical Properties of hydrogenated feedstock
TABLE 2 physicochemical Properties of the catalysts prepared
Physical Properties of hydrogenated product oil No. Table 31
Hydrogenation product oil physical Properties of Table 42
Hydrogenation of TABLE 53 oils physical Properties
The performance of the prepared catalyst is inspected by selecting three different raw materials, and the evaluation result shows that the platinum-palladium-cobalt ternary metal catalyst has excellent sulfur-resistant deep dearomatization performance by adopting non-noble metal cobalt nanoparticles as an anchoring point and palladium nanoparticles as seed crystals and is particularly suitable for producing high-quality white oil from lubricating oil fractions. The catalyst prepared by the method still shows good deep hydrofining performance under the condition that the platinum content can be reduced by 40% and the palladium content can be reduced by 20% by using low non-noble metal cobalt.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (1)
1. A preparation method of a platinum-palladium-cobalt ternary metal hydrogenation dearomatization catalyst is characterized by comprising the following steps:
(1) placing 130 g of amorphous silica-alumina, 60 g of pseudo-boehmite and 4.5 g of sesbania powder into a rolling machine for mixing and rolling, adding 170 g of dilute nitric acid solution, wherein the mass of the nitric acid is 3% of the dry basis weight of the pseudo-boehmite, rolling into paste, drying extruded strips at 120 ℃ for 12 hours, and roasting at 500 ℃ for 4 hours to obtain a carrier SCAT;
(2) the CoCl is impregnated by a conventional method with equal volume 2 And PdCl 2 The mixed solution of (A) is impregnated on a carrier SCAT, and the weight ratio of cobalt to palladium in the cobalt-palladium mixed salt solution is 5.31: 1.00, aging at 50 ℃ for 3 hours, then drying at 120 ℃ for 10 hours, roasting at 500 ℃ for 3 hours, and reducing with hydrogen at 300 ℃ for 3 hours to obtain an MCAT-1 sample; continuously adopting an equal-volume impregnation method to prepare PdCl 2 And H 2 PtCl 6 The mixed solution of (a) was impregnated on the support MCAT-1 under vacuum, and the weight ratio of platinum to palladium in the platinum-palladium mixed salt solution was 0.75: 1.00, aging at 50 ℃ for 3 hours, then drying at 120 ℃ for 10 hours, roasting at 500 ℃ for 3 hours, and reducing at 350 ℃ for 3 hours to obtain the catalyst The final metal loading of platinum, palladium and cobalt in the prepared catalyst was controlled at 0.12wt%, 0.32wt% and 0.85wt% respectively relative to the carrier.
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| CN105521797A (en) * | 2014-09-28 | 2016-04-27 | 中国石油化工股份有限公司 | Supported double-metal-component catalyst, preparation method and application thereof, and aromatic hydrocarbon saturation hydrogenation method |
| CN108745349A (en) * | 2018-05-28 | 2018-11-06 | 中国中化股份有限公司 | The preparation method of platinum-palladium bimetallic catalytic hydro-dearomatization catalyst |
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| CN105521797A (en) * | 2014-09-28 | 2016-04-27 | 中国石油化工股份有限公司 | Supported double-metal-component catalyst, preparation method and application thereof, and aromatic hydrocarbon saturation hydrogenation method |
| CN108745349A (en) * | 2018-05-28 | 2018-11-06 | 中国中化股份有限公司 | The preparation method of platinum-palladium bimetallic catalytic hydro-dearomatization catalyst |
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