CN110935445A - PdGa for selective hydrogenation of acetyleneX/Ga2O3Preparation method and application of catalyst - Google Patents
PdGa for selective hydrogenation of acetyleneX/Ga2O3Preparation method and application of catalyst Download PDFInfo
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
- B01J37/18—Reducing with gases containing free hydrogen
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- C07C5/00—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
- C07C5/02—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation
- C07C5/08—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation of carbon-to-carbon triple bonds
- C07C5/09—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by hydrogenation of carbon-to-carbon triple bonds to carbon-to-carbon double bonds
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Abstract
The invention discloses PdGa for selective hydrogenation of acetyleneX/Ga2O3A preparation method and application of a catalyst, belonging to the technical field of gas phase catalysis of supported catalysts. According to the method, a gallium oxide carrier is synthesized and prepared by a hydrothermal method, palladium particles are loaded on gallium oxide by an immersion method, permeation doping of gallium atoms in the carrier to palladium nanoparticles is realized by adjusting the pretreatment temperature of hydrogen, and then the reaction performance test of selective hydrogenation of acetylene is carried out. The results show that hydrogen pre-treatment of the formed Pd2The Ga structure has better reaction activity and ethylene selectivity to the reaction, and the synthesis method is generalThe controllable adjustment of the structure of the nano particles can be realized through the pretreatment temperature and the atmosphere, the preparation method is simple, and the performance is excellent.
Description
Technical Field
The invention relates to the technical field of supported nanoparticle catalysts, in particular to a preparation method of an acetylene selective hydrogenation catalyst.
Background
The petroleum cracking industry produces a large amount of chemical raw materials, wherein ethylene is widely applied, and polyethylene products with various structures and specifications can be produced through the polymerization of ethylene. However, ethylene obtained by petroleum cracking contains small amounts of acetylene (0.5% to 2%) which poisons and deactivates the Ziegler-Natta catalyst which catalyzes the polymerization of ethylene, seriously affecting the quality of the ethylene feed gas. Therefore, trace acetylene in the ethylene atmosphere needs to be removed, the acetylene content is reduced to the level of less than 5ppm, and at present, the industry mainly introduces a catalyst for catalyzing selective hydrogenation of acetylene to purify the ethylene gas.
The palladium-based catalyst is widely applied to acetylene selective hydrogenation reaction due to excellent reaction activity and ethylene selectivity. However, due to the high price of palladium and the low selectivity to ethylene, a second component needs to be introduced for regulation.
Disclosure of Invention
The invention aims to provide a catalyst PdGa for selective hydrogenation of acetyleneX/Ga2O3The preparation method and the application of the supported catalyst are that the gallium oxide nanorod is designed and synthesized, palladium salt is supported on the gallium oxide nanorod, when the supported catalyst is applied, reducing atmosphere is introduced, and the structure of the active component of the catalyst is regulated and controlled by regulating and controlling the pretreatment temperature (reduction temperature) of the catalyst in the reducing atmosphere, so that the performance of the catalyst is regulated and controlled.
In order to achieve the purpose, the invention adopts the technical scheme that:
PdGa for acetylene selective hydrogenationX/Ga2O3The preparation method of the catalyst comprises the steps of firstly preparing a gallium oxide carrier, and then loading palladium salt on the gallium oxide carrier by an impregnation method; roasting the palladium-loaded gallium oxide carrier at high temperature, and then carrying out reduction treatment in a reducing atmosphere to obtain the PdGa for selective hydrogenation of acetyleneX/Ga2O3A catalyst.
In the reduction treatment process, the reducing atmosphere is H2And inert gas, H in the mixed atmosphere2And inert gas in a volume ratio of 1: 5-5: 1, the reduction time is 1-5 hours.
The method comprises the following steps:
(1) dissolving palladium salt in an organic solvent to obtain a palladium salt solution, then adding the gallium oxide carrier into the palladium salt solution, and uniformly dispersing the carrier in the solution under the stirring condition to obtain a mixed material; wherein: the weight ratio of palladium to the carrier in the mixed material is (1-10): 100, respectively;
(2) removing the organic solvent in the mixed material by using a rotary evaporator, and drying to obtain solid powder, namely the palladium-loaded gallium oxide carrier;
(3) roasting the solid powder obtained in the step (2) at the temperature of 450-750 ℃ for more than 2 hours to obtain a catalyst with palladium oxide nano particles loaded on gallium oxide;
(4) reducing the catalyst of the palladium oxide nanoparticles loaded on gallium oxide obtained in the step (3) for 2-4 hours at 250-350 ℃ in a reducing atmosphere to obtain the PdGa for selective hydrogenation of acetyleneX/Ga2O3A catalyst.
In the step (1), the gallium oxide carrier is a gallium oxide nanorod carrier synthesized by a hydrothermal method, and the diameter of the gallium oxide nanorod carrier is 20-100 nanometers.
The preparation method of the gallium oxide nanorod carrier comprises the following steps: dissolving a surfactant in water, and violently stirring until the surfactant is uniformly mixed; then adding gallium salt into the mixed solution under the stirring condition, stirring until large floccules appear, and adjusting the pH value of the mixed solution to 7-8 to obtain flocculent colloidal solution; placing the colloidal solution in a closed container, and placing the closed container at the temperature of 100 ℃ and 200 ℃ for more than 8 hours; centrifuging and washing the obtained product to obtain white powder, and roasting the white powder at the temperature of 400-550 ℃ to obtain the gallium oxide nanorod carrier (Ga)2O3A carrier).
In the step (1), the content of the palladium salt in the palladium salt solution is 0.02 to 0.2 wt.%, the palladium salt is palladium acetylacetonate, palladium nitrate or palladium chloride, and the organic solvent is absolute methanol or absolute ethanol.
In the step (3), the prepared palladium oxide nanoparticles are loaded in the catalyst on gallium oxide, and the particle size of the palladium oxide nanoparticles is 4-10 nanometers.
The prepared supported PdGaX/Ga2O3In the catalyst, PdGaXThe particles are uniformly loaded on a gallium oxide carrier, PdGaXThe value of X in the particles is 0.1-1.
Subjecting the PdGa to oxidationX/Ga2O3The catalyst is applied to acetylene selective hydrogenation reaction.
The application conditions of the catalyst are as follows: the reaction gases are acetylene, ethylene, hydrogen and helium, wherein: acetylene content 0.5 vol.%, ethylene content 20 vol.%, hydrogen 5 vol.%, helium as balance gas; the total flow rate of gas is 40 ml/min; amount of catalyst and reaction gas (C)2H2、C2H4And H2) The airspeeds are respectively as follows: 0.01-0.5mg and 24480-1224000 L.h-1·g-1The reaction temperature is 100-250 ℃, and the reaction temperature is 100-250 ℃.
The invention has the following advantages and beneficial effects:
1. the invention prepares PdGa for selective hydrogenation of acetyleneX/Ga2O3The catalyst is prepared by reducing the palladium oxide-gallium oxide catalyst in a reducing atmosphere, and the structure and the surface structure of the catalyst can be accurately regulated and controlled by controlling the reducing temperature.
2. The invention carries out reduction treatment on the palladium oxide-gallium oxide catalyst at the temperature of 350 ℃ in the reducing atmosphere, and the treatment temperature realizes the infiltration doping of gallium atoms in the carrier to palladium nano particles to obtain PdGaX/Ga2O3A catalyst; pd formed by hydrogen pretreatment2The Ga structure has better reaction activity and ethylene selectivity for acetylene selective hydrogenation, the method can realize controllable adjustment of the nano-particle structure through pretreatment temperature and atmosphere, and the preparation method is simple and has excellent performance.
3. The method of the invention synthesizes and prepares PdGaX/Ga2O3Catalyst at higher BThe selectivity of the ethylene of 82 percent can be kept under the condition of alkyne conversion rate (more than 90 percent), and better stability is kept.
4. Under reducing atmosphere and different pretreatment temperatures, the surface structure of the active site nano-particles of the catalyst can be regulated, and the activity of the catalyst and the selectivity of byproduct species can be obviously regulated. This provides a reference for the design of similar catalysts.
Drawings
FIG. 1 is a graph showing the comparison of the acetylene conversion and ethylene selectivity of catalysts obtained by reduction at different reduction temperatures at 100 ℃ and 200 ℃ respectively; wherein: (a) the performance of the catalyst obtained by treatment at different reduction temperatures in a catalytic reaction at 100 ℃; (b) the performance of the catalyst obtained by treating at different reduction temperatures in a catalytic reaction at 200 ℃.
FIG. 2 shows the long-term stability test of the catalyst obtained by the reduction treatment at 300 ℃; in the figure: acetylene conversion (squares), ethylene selectivity (circles), ethane selectivity (triangles), butene species selectivity (inverted triangles).
FIG. 3 is a histogram showing the morphology of the catalyst obtained after reduction treatment at different temperatures and the corresponding particle size distribution of nanoparticles; wherein: (a) and (f) a morphology chart of the catalyst after reduction treatment at 100 ℃ and a corresponding particle size statistical histogram respectively; (b) and (g) a morphology chart of the catalyst after reduction treatment at 200 ℃ and a corresponding particle size statistical histogram respectively; (c) and (h) a morphology chart of the catalyst after reduction treatment at 300 ℃ and a corresponding particle size statistical histogram respectively; (d) and (i) a morphology chart of the catalyst after reduction treatment at 400 ℃ and a corresponding particle size statistical histogram respectively; (e) and (j) a morphology chart of the catalyst after reduction treatment at 400 ℃ and a corresponding particle size statistical histogram respectively.
Detailed Description
The present invention will be described in detail with reference to examples.
The invention is further described below with reference to the accompanying drawings. In order to compare the performance of the catalyst prepared by the method, the catalyst treated at different reduction temperatures is used for carrying out acetylene selective hydrogenation reaction performance test. Oxidizing the prepared catalyst with oxygenThe gallium carrier is diluted by 100 times and then is loaded into a reaction tube for testing. The reaction gas composition is: 0.5 vol.% C2H2，20vol.％C2H4，5vol.％H2And He balance. In the following examples and comparative examples, when the catalyst was used for the catalytic reaction, the amount of the catalyst was 0.1mg, the total flow rate of the gas was 40ml/min, the amount of the catalyst and the reaction gas (C)2H2、C2H4And H2) The airspeeds are respectively as follows: 0.1mg and 122400 Lh-1·g-1。
Example 1:
this example preparation of PdGaX/Ga2O3The catalyst process is as follows:
1. synthesis and preparation of Ga by hydrothermal method2O3Dissolving sodium dodecyl benzene sulfonate in water, and stirring vigorously to mix uniformly. Gallium nitrate hydrate is added into the solution under the condition of stirring, the solution becomes turbid, and after stirring for a period of time, massive floccules appear. Then, a sodium hydroxide solution (0.1mol/L) was added dropwise to the mixed solution to adjust the pH to 8, thereby obtaining a flocculent colloidal solution. The colloidal solution is placed in a closed container for more than 8 hours at 140 ℃ by a hydrothermal method. Centrifuging, washing with water to obtain white powder, and calcining at 500 deg.C to obtain Ga2O3The diameter of the nanorod carrier of gallium oxide is 20-100 nanometers, and the particle size of gallium oxide nanoparticles in the catalyst is 4-10 nanometers.
2. The dipping method comprises the following steps: 21mg of palladium acetylacetonate was sufficiently dissolved in 30g of anhydrous methanol, and 140mg of Ga prepared in the step (1) was added2O3And ultrasonically stirring the nano-rods for 30 minutes to ensure uniform dispersion, removing the solvent anhydrous methanol by a rotary evaporator, and drying in an oven at 20 ℃ for 2 hours to obtain solid powder, namely the palladium-loaded gallium oxide carrier.
3. Roasting the solid powder obtained in the step (2) at 500 ℃ for 2.5 hours to obtain a catalyst with palladium oxide nano particles loaded on gallium oxide;
4. reducing the catalyst of the palladium oxide nano particles obtained in the step (3) loaded on gallium oxide in reducing atmosphere to obtain the catalystTo the PdGa for selective hydrogenation of acetyleneX/Ga2O3A catalyst. Wherein: the reducing atmosphere consists of hydrogen and argon, and the volume ratio of the hydrogen to the argon is 1: 1, during reduction treatment, raising the temperature to 300 ℃ at the heating rate of 5 ℃/min for reduction treatment for 2 hours, and reducing the temperature to room temperature to obtain PdGaX/Ga2O3A catalyst.
The supported PdGa prepared in this exampleX/Ga2O3The loading of Pd in the catalyst was about 5 wt.%. In the catalyst, PdGaXParticles supported on Ga2O3On the support (FIG. 3(c) and FIG. 3(h)), the value of X was 1/2, as tested. The catalyst was subjected to a stability test for 20 hours (fig. 2), and as a result, the catalyst showed 95% acetylene selectivity and 82% ethylene selectivity, and showed good stability.
Comparative example 1:
the difference from the embodiment 1 is that: the reduction treatment temperature in the step (3) was 100 ℃ and 200 ℃.
FIG. 1 shows PdGa obtained by reduction at different temperatures in example 1 and comparative example 1X/Ga2O3As a result of performance tests of the catalyst on acetylene conversion rate and ethylene selectivity under the reaction temperature conditions of 100 ℃ and 200 ℃, respectively, it can be found that the acetylene conversion rate is reduced along with the increase of the reduction temperature, and the ethylene selectivity reaches an optimal value at a certain treatment temperature. Fig. 3 is a histogram showing the morphology of the catalyst and the corresponding particle size distribution of nanoparticles obtained after the reduction treatment at different temperatures in the example and the comparative example, and it can be found that the catalyst shows good dimensional stability during the pretreatment (reduction) at different temperatures.
Reducing the catalyst at 100 ℃ to obtain the catalyst mainly comprising palladium nanoparticles loaded on gallium oxide nanorods. The catalyst under the treatment condition has low selectivity to ethylene in the process of catalyzing selective hydrogenation reaction of acetylene, and the main reason is that the active sites of the catalyst are mainly palladium nanoparticles which have strong hydrogenation capacity to acetylene gas and ethylene gas, so that the reaction product is mainly an over-hydrogenation product ethane gas under the condition. And (3) reducing the pretreated catalyst at 200 ℃, wherein the gallium oxide carrier has a tendency of migrating towards palladium nanoparticles as can be seen from transmission electron microscope data, and the XRD data still shows that the loaded nanoparticles are still palladium nanoparticles. The catalyst obtained under these conditions exhibited 80% conversion of acetylene and 58% selectivity to ethylene at a reaction temperature of 100 ℃.
The catalyst prepared in example 1 is used for acetylene selective hydrogenation reaction, when the reaction temperature is 200 ℃, the obtained catalyst has 93% acetylene conversion rate and 82% ethylene selectivity, and after 20 hours of stability test, the reaction activity of the catalyst is reduced to be within 3 percentage points, and the ethylene selectivity is very stable. This indicates that the catalyst synthesized by the method of the present invention has good stability.
Comparative example 2:
when the pretreatment temperature is above 400 ℃, the catalyst has no catalytic activity at the reaction temperature of 100 ℃, which is probably because the surface of the nano particles is mainly a gallium-rich surface at the reduction treatment temperature, so that the catalyst is deactivated at the temperature.
By combining the comparative examples with the examples, it can be confirmed that the catalyst prepared according to the present invention has excellent catalytic performance.
The above description should not be taken as limiting the invention, and any modification, equivalent replacement, or improvement made within the spirit and principle of the invention should be included in the protection scope of the invention.
Claims (10)
1. PdGa for acetylene selective hydrogenationX/Ga2O3The preparation method of the catalyst is characterized by comprising the following steps: firstly, preparing a gallium oxide carrier, and then loading palladium salt on the gallium oxide carrier by an impregnation method; roasting the palladium-loaded gallium oxide carrier at high temperature, and then carrying out reduction treatment in a reducing atmosphere to obtain the PdGa for selective hydrogenation of acetyleneX/Ga2O3A catalyst.
2. PdGa for selective hydrogenation of acetylene according to claim 1X/Ga2O3The preparation method of the catalyst is characterized by comprising the following steps: in the reduction treatment process, the reducing atmosphere is H2And inert gas, H in the mixed atmosphere2And inert gas in a volume ratio of 1: 5-5: 1, the reduction time is 1-5 hours.
3. PdGa for selective hydrogenation of acetylene according to claim 2X/Ga2O3The preparation method of the catalyst is characterized by comprising the following steps: the method comprises the following steps:
(1) dissolving palladium salt in an organic solvent to obtain a palladium salt solution, then adding the gallium oxide carrier into the palladium salt solution, and uniformly dispersing the carrier in the solution under the stirring condition to obtain a mixed material; wherein: the weight ratio of palladium to the carrier in the mixed material is (1-10): 100, respectively;
(2) removing the organic solvent in the mixed material by using a rotary evaporator, and drying to obtain solid powder, namely the palladium-loaded gallium oxide carrier;
(3) roasting the solid powder obtained in the step (2) at the temperature of 450-750 ℃ for more than 2 hours to obtain a catalyst with palladium oxide nano particles loaded on gallium oxide;
(4) reducing the catalyst of the palladium oxide nanoparticles loaded on gallium oxide obtained in the step (3) for 2-4 hours at 250-350 ℃ in a reducing atmosphere to obtain the PdGa for selective hydrogenation of acetyleneX/Ga2O3A catalyst.
4. PdGa for selective hydrogenation of acetylene according to claim 3X/Ga2O3The preparation method of the catalyst is characterized by comprising the following steps: in the step (1), the gallium oxide carrier is a gallium oxide nanorod carrier synthesized by a hydrothermal method, and the diameter of the gallium oxide nanorod carrier is 20-100 nanometers.
5. The process of claim 4 for the selective hydrogenation of acetylenePdGa of (2)X/Ga2O3The preparation method of the catalyst is characterized by comprising the following steps: the preparation method of the gallium oxide nanorod carrier comprises the following steps: dissolving a surfactant in water, and violently stirring until the surfactant is uniformly mixed; then adding gallium salt into the mixed solution under the stirring condition, stirring until large floccules appear, and adjusting the pH value of the mixed solution to 7-8 to obtain flocculent colloidal solution; placing the colloidal solution in a closed container, and placing the closed container at the temperature of 100 ℃ and 200 ℃ for more than 8 hours; and centrifuging and washing the obtained product to obtain white powder, and roasting the white powder at the temperature of 400-550 ℃ to obtain the gallium oxide nanorod carrier.
6. PdGa for selective hydrogenation of acetylene according to claim 3X/Ga2O3The preparation method of the catalyst is characterized by comprising the following steps: in the step (1), the content of palladium salt in the palladium salt solution is 0.02-0.2 wt.%, the palladium salt is palladium acetylacetonate, palladium nitrate or palladium chloride, and the organic solvent is absolute methanol or absolute ethanol.
7. PdGa for selective hydrogenation of acetylene according to claim 3X/Ga2O3The preparation method of the catalyst is characterized by comprising the following steps: in the step (3), the prepared palladium oxide nanoparticles are loaded in the catalyst on gallium oxide, and the particle size of the palladium oxide nanoparticles is 4-10 nanometers.
8. PdGa for selective hydrogenation of acetylene according to claim 3X/Ga2O3The preparation method of the catalyst is characterized by comprising the following steps: the prepared supported PdGaX/Ga2O3In the catalyst, PdGaXThe particles are uniformly loaded on a gallium oxide carrier, PdGaXThe value of X in the particles is 0.1-1.
9. PdGa for selective hydrogenation of acetylene, prepared by the process according to any one of claims 1 to 8X/Ga2O3The application of the catalyst is characterized in that: subjecting the PdGa to oxidationX/Ga2O3The catalyst is applied to acetylene selective hydrogenation reaction.
10. PdGa for selective hydrogenation of acetylene according to claim 9X/Ga2O3The application of the catalyst is characterized in that: the application conditions of the catalyst are as follows: the reaction gases are acetylene, ethylene, hydrogen and helium, wherein: acetylene content 0.5 vol.%, ethylene content 20 vol.%, hydrogen 5 vol.%, helium as balance gas; the total flow rate of gas is 40 ml/min; amount of catalyst and reaction gas (C)2H2、C2H4And H2) The airspeeds are respectively as follows: 0.01-0.5mg and 24480-1224000 L.h-1·g-1(ii) a The reaction temperature is 100 ℃ and 250 ℃.
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| CN115212878A (en) * | 2022-07-06 | 2022-10-21 | 四川大学 | Method for preparing high-performance Pd-Ga2O3 catalyst by recycling waste palladium catalyst |
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