CN112871157B - Preparation method of mesoporous catalyst based on active alumina - Google Patents
Preparation method of mesoporous catalyst based on active alumina Download PDFInfo
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- CN112871157B CN112871157B CN202110195244.XA CN202110195244A CN112871157B CN 112871157 B CN112871157 B CN 112871157B CN 202110195244 A CN202110195244 A CN 202110195244A CN 112871157 B CN112871157 B CN 112871157B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 57
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 43
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 33
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 32
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002245 particle Substances 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 238000005507 spraying Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 11
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 11
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims abstract description 11
- 238000010926 purge Methods 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 10
- 229910052763 palladium Inorganic materials 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000010410 layer Substances 0.000 claims description 5
- 239000002344 surface layer Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 7
- 239000011148 porous material Substances 0.000 abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000011065 in-situ storage Methods 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- TYMLOMAKGOJONV-UHFFFAOYSA-N 4-nitroaniline Chemical compound NC1=CC=C([N+]([O-])=O)C=C1 TYMLOMAKGOJONV-UHFFFAOYSA-N 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- WDCYWAQPCXBPJA-UHFFFAOYSA-N 1,3-dinitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC([N+]([O-])=O)=C1 WDCYWAQPCXBPJA-UHFFFAOYSA-N 0.000 description 1
- FYFDQJRXFWGIBS-UHFFFAOYSA-N 1,4-dinitrobenzene Chemical compound [O-][N+](=O)C1=CC=C([N+]([O-])=O)C=C1 FYFDQJRXFWGIBS-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
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
- B01J23/44—Palladium
-
- 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
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/30—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds
- C07C209/32—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups
- C07C209/36—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups by reduction of nitro groups bound to carbon atoms of six-membered aromatic rings in presence of hydrogen-containing gases and a catalyst
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to the field of catalysts, and particularly relates to a preparation method of a mesoporous catalyst based on active alumina, which comprises the following steps: step 1, adding aluminum isopropoxide and palladium chloride into absolute ethyl alcohol, and stirring at a low temperature to obtain a dissolving solution; then adding sodium dodecyl sulfate, heating and stirring to obtain a mixed solution; step 2, distilling the mixed solution under reduced pressure to form viscous liquid, and then putting the viscous liquid into a mold to be dried at constant temperature to obtain prefabricated particles; step 3, adding aluminum isopropoxide into chloroform, uniformly stirring, adding diethyl ether, uniformly spraying on the surface of the prefabricated particles, and standing at constant temperature to form a liquid film to obtain coated particles; and 4, placing the coated particles into a reaction kettle, standing for 2-4h, then heating for 30-60min, and reducing after purging to obtain the mesoporous catalyst. The invention solves the difficulty of hydrogenation catalyst, ensures the internal and external temperature stability of the catalyst by utilizing the thermal conductivity of the alumina, and realizes the protection effect of active molecules by utilizing the low pore structure of the mesoporous alumina.
Description
Technical Field
The invention belongs to the field of catalysts, and particularly relates to a preparation method of a mesoporous catalyst based on activated alumina.
Background
The hydrogenation catalyst has a deactivation phenomenon along with the long-time running of the catalyst. The prior hydrogenation catalyst mainly comprises a noble metal hydrogenation catalyst, and the hydrogenation effect is realized by utilizing the activity of the surface of the noble metal, but under the normal reaction condition, the stability of the activity of the surface of the catalyst is poor based on the nonuniformity of the reaction temperature, and the performance of the catalyst is difficult to be maximized.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a mesoporous catalyst based on active alumina, which solves the difficulty of hydrogenation catalysts, ensures the internal and external temperature stability of the catalyst by utilizing the thermal conductivity of the alumina, and realizes the protection effect of active molecules by utilizing the low pore structure of the mesoporous alumina.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a preparation method of a mesoporous catalyst based on active alumina comprises the following steps:
step 1, adding aluminum isopropoxide and palladium chloride into absolute ethyl alcohol, and stirring at a low temperature to obtain a dissolving solution; then adding sodium dodecyl sulfate, heating and stirring to obtain a mixed solution; the concentration of the aluminum isopropoxide in the absolute ethyl alcohol is 50-70g/L, the addition amount of the palladium chloride is 30-50% of the mass of the aluminum isopropoxide, the low-temperature stirring temperature is 4-10 ℃, and the stirring speed is 1000-2000 r/min; the adding amount of the sodium dodecyl sulfate is 30-60% of the mass of the aluminum isopropoxide, the temperature raising and stirring temperature is 60-70 ℃, and the stirring speed is 1000-;
step 2, distilling the mixed solution under reduced pressure to form viscous liquid, and then putting the viscous liquid into a mold to be dried at constant temperature to obtain prefabricated particles; the temperature of the reduced pressure distillation is 70-80 ℃, the pressure is 70-80% of the atmospheric pressure, the temperature of the constant temperature drying is 90-100 ℃, and the pressure is 0.3-0.5 MPa;
step 3, adding aluminum isopropoxide into chloroform, uniformly stirring, adding diethyl ether, uniformly spraying on the surface of the prefabricated particles, and standing at constant temperature to form a liquid film to obtain coated particles; the concentration of the aluminum isopropoxide in the chloroform is 80-100g/L, the stirring speed is 1000-2000r/min, the addition amount of the diethyl ether is 50-300 percent of the volume of the chloroform, and the spraying amount of the uniform spraying is 2-6ml/cm 2 Standing at constant temperature of 60-65 deg.C and pressure of 0.2-0.4 MPa;
step 4, placing the coated particles into a reaction kettle, standing for 2-4h, then heating for 30-60min, and reducing after purging to obtain a mesoporous catalyst; the reaction kettle is filled with mixed gas, the mixed gas consists of 20-30% of ammonia gas, 20-40% of water vapor and the rest of nitrogen, and the standing temperature is 100-110 ℃; the temperature of the constant temperature treatment is 160-180 ℃; the purging adopts 100-120 ℃ nitrogen at the speed of 5-10 mL/min; the reduction is carried out by using hydrogen at a temperature of 90-100 ℃.
The mesoporous catalyst is composed of an inner layer of porous alumina-based palladium catalyst and a surface layer of mesoporous alumina.
The mesoporous catalyst is used for hydrogenation reaction.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the difficulty of hydrogenation catalyst, ensures the internal and external temperature stability of the catalyst by utilizing the thermal conductivity of the alumina, and realizes the protection effect of active molecules by utilizing the low pore structure of the mesoporous alumina.
2. The method ensures the stable conversion of the palladium source and the aluminum source by utilizing the in-situ hydrolysis polymerization characteristic, and rapidly carries out in-situ polymerization under the temperature condition to hinder the agglomeration of materials.
Detailed Description
The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.
Example 1
A preparation method of a mesoporous catalyst based on active alumina comprises the following steps:
step 1, adding aluminum isopropoxide and palladium chloride into 1L of absolute ethyl alcohol, and stirring at a low temperature to obtain a dissolved solution; then adding sodium dodecyl sulfate, heating and stirring to obtain a mixed solution; the concentration of the aluminum isopropoxide in the absolute ethyl alcohol is 50g/L, the adding amount of the palladium chloride is 30% of the mass of the aluminum isopropoxide, the low-temperature stirring temperature is 4 ℃, and the stirring speed is 1000 r/min; the adding amount of the sodium dodecyl sulfate is 30 percent of the mass of the aluminum isopropoxide, the temperature raising and stirring temperature is 60 ℃, and the stirring speed is 1000 r/min;
step 2, distilling the mixed solution under reduced pressure to form viscous liquid, and then putting the viscous liquid into a mold to dry at constant temperature to obtain prefabricated particles; the temperature of the reduced pressure distillation is 70 ℃, the pressure is 70% of the atmospheric pressure, the temperature of the constant temperature drying is 90 ℃, and the pressure is 0.3 MPa;
step 3, adding aluminum isopropoxide into 1L of chloroform, uniformly stirring, adding diethyl ether, uniformly spraying on the surface of the prefabricated particles after expanding and dissolving, and standing at constant temperature to form a liquid film to obtain coated particles; the concentration of the aluminum isopropoxide in the chloroform is 80g/L, the stirring speed is 1000r/min, the addition amount of the diethyl ether is 50 percent of the volume of the chloroform, and the spraying amount of the uniform spraying is 2ml/cm 2 Standing at a constant temperature of 60 ℃ and a pressure of 0.2 MPa;
step 4, placing the coated particles into a reaction kettle, standing for 2 hours, then heating for 30min, and reducing after purging to obtain a mesoporous catalyst; the reaction kettle is filled with mixed gas, the mixed gas consists of 20% of ammonia gas, 20% of water vapor and the rest of nitrogen, and the standing temperature is 100 ℃; the temperature of the constant temperature treatment is 160 ℃; the purging adopts 100 ℃ nitrogen at the speed of 5 mL/min; the reduction was carried out with hydrogen at a temperature of 90 ℃.
The mesoporous catalyst prepared in this example was composed of an inner layer of porous alumina-based palladium catalyst and a surface layer of mesoporous alumina, and the catalyst diameter was 2 mm.
Example 2
A preparation method of a mesoporous catalyst based on active alumina comprises the following steps:
step 1, adding aluminum isopropoxide and palladium chloride into 1L of absolute ethyl alcohol, and stirring at a low temperature to obtain a dissolved solution; then adding sodium dodecyl sulfate, heating and stirring to obtain a mixed solution; the concentration of the aluminum isopropoxide in the absolute ethyl alcohol is 70g/L, the addition amount of the palladium chloride is 50 percent of the mass of the aluminum isopropoxide, the low-temperature stirring temperature is 10 ℃, and the stirring speed is 2000 r/min; the adding amount of the sodium dodecyl sulfate is 60 percent of the mass of the aluminum isopropoxide, the temperature raising and stirring temperature is 70 ℃, and the stirring speed is 1500 r/min;
step 2, distilling the mixed solution under reduced pressure to form viscous liquid, and then putting the viscous liquid into a mold to be dried at constant temperature to obtain prefabricated particles; the temperature of the reduced pressure distillation is 80 ℃, the pressure is 80% of the atmospheric pressure, the temperature of the constant temperature drying is 100 ℃, and the pressure is 0.5 MPa;
step 3, adding aluminum isopropoxide into 1L of chloroform, uniformly stirring, adding diethyl ether, uniformly spraying on the surface of the prefabricated particles after diffusion and dissolution, and standing at constant temperature to form a liquid film to obtain coated particles; the concentration of the aluminum isopropoxide in the chloroform is 100g/L, the stirring speed is 2000r/min, the adding amount of the diethyl ether is 300 percent of the volume of the chloroform, and the spraying amount of the uniform spraying is 6ml/cm 2 The temperature of constant temperature standing is 65 ℃, and the pressure is 0.4 MPa;
step 4, placing the coated particles into a reaction kettle, standing for 4 hours, then heating for 60 minutes, and reducing after purging to obtain a mesoporous catalyst; the reaction kettle is filled with mixed gas, the mixed gas consists of 30% of ammonia gas, 40% of water vapor and the rest of nitrogen, and the standing temperature is 110 ℃; the temperature of the constant temperature treatment is 180 ℃; the purging adopts nitrogen at 120 ℃ and the speed is 10 mL/min; the reduction was carried out with hydrogen at a temperature of 100 ℃.
The mesoporous catalyst prepared in this example is composed of an inner layer of porous alumina-based palladium catalyst and a surface layer of mesoporous alumina, and the diameter of the catalyst is 5 mm.
Example 3
A preparation method of a mesoporous catalyst based on active alumina comprises the following steps:
step 1, adding aluminum isopropoxide and palladium chloride into 1L of absolute ethyl alcohol, and stirring at a low temperature to obtain a dissolved solution; then adding sodium dodecyl sulfate, heating and stirring to obtain a mixed solution; the concentration of the aluminum isopropoxide in the absolute ethyl alcohol is 60g/L, the adding amount of the palladium chloride is 40% of the mass of the aluminum isopropoxide, the low-temperature stirring temperature is 8 ℃, and the stirring speed is 1500 r/min; the adding amount of the sodium dodecyl sulfate is 50 percent of the mass of the aluminum isopropoxide, the temperature raising and stirring temperature is 65 ℃, and the stirring speed is 1300 r/min;
step 2, distilling the mixed solution under reduced pressure to form viscous liquid, and then putting the viscous liquid into a mold to be dried at constant temperature to obtain prefabricated particles; the temperature of the reduced pressure distillation is 75 ℃, the pressure is 75% of the atmospheric pressure, the temperature of the constant temperature drying is 95 ℃, and the pressure is 0.4 MPa;
step 3, adding aluminum isopropoxide into 1L of chloroform, uniformly stirring, adding diethyl ether, uniformly spraying on the surface of the prefabricated particles after diffusion and dissolution, and standing at constant temperature to form a liquid film to obtain coated particles; the concentration of the aluminum isopropoxide in the chloroform is 90g/L, the stirring speed is 1500r/min, the addition amount of the diethyl ether is 200 percent of the volume of the chloroform, and the spray amount of the uniform spray is 4ml/cm 2 The temperature of constant temperature standing is 63 ℃, and the pressure is 0.3 MPa;
step 4, placing the coated particles into a reaction kettle, standing for 3 hours, then heating for 50min, and reducing after purging to obtain a mesoporous catalyst; the reaction kettle is filled with mixed gas, the mixed gas consists of 25% of ammonia gas, 30% of water vapor and the rest of nitrogen, and the standing temperature is 105 ℃; the temperature of the constant temperature treatment is 170 ℃; the purging adopts nitrogen at 110 ℃, and the speed is 8 mL/min; the reduction was carried out with hydrogen at a temperature of 95 ℃.
The mesoporous catalyst prepared in this example was composed of an inner layer of porous alumina-based palladium catalyst and a surface layer of mesoporous alumina, and the catalyst diameter was 3 mm.
Examples of the invention
The catalyst of example 3 was used for the hydrogenation reaction as follows:
150g of p-dinitrobenzene, 200g of methanol and 1.2g of the catalyst of example 3 were charged into a 500mL autoclave, and the mixture was replaced with 1MPa of nitrogen for 3 times, then with 1MPa of hydrogen for 3 times, heated to 150 ℃ and kept at 2MPa for 1.5 hours. And (3) cooling, distilling and recovering methanol under the protection of nitrogen at normal pressure, and separating to obtain a p-nitroaniline crude product. The product was analyzed for its composition by gas chromatography, with a conversion of 99.3% for dinitrobenzene, a selectivity of 99.2% for p-nitroaniline and a yield of 92.3% for p-nitroaniline.
In summary, the invention has the following advantages:
1. the invention solves the difficulty of hydrogenation catalyst, ensures the internal and external temperature stability of the catalyst by utilizing the thermal conductivity of the alumina, and realizes the protection effect of active molecules by utilizing the low pore structure of the mesoporous alumina.
2. The method ensures the stable conversion of the palladium source and the aluminum source by utilizing the in-situ hydrolysis polymerization characteristic, and rapidly carries out in-situ polymerization under the temperature condition to hinder the agglomeration of materials.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (9)
1. A preparation method of a mesoporous catalyst based on active alumina is characterized by comprising the following steps: the method comprises the following steps:
step 1, adding aluminum isopropoxide and palladium chloride into absolute ethyl alcohol, and stirring at a low temperature to obtain a dissolving solution; then adding sodium dodecyl sulfate, heating and stirring to obtain a mixed solution;
step 2, distilling the mixed solution under reduced pressure to form viscous liquid, and then putting the viscous liquid into a mold to be dried at constant temperature to obtain prefabricated particles;
step 3, adding aluminum isopropoxide into chloroform, uniformly stirring, adding diethyl ether, uniformly spraying on the surfaces of the prefabricated particles, and standing at constant temperature to form a liquid film to obtain coated particles;
step 4, placing the coated particles into a reaction kettle, standing for 2-4h, then heating for 30-60min, and reducing after purging to obtain a mesoporous catalyst;
the mesoporous catalyst is composed of an inner layer of porous alumina-based palladium catalyst and a surface layer of mesoporous alumina.
2. The method for preparing a mesoporous catalyst based on activated alumina according to claim 1, comprising: the concentration of the aluminum isopropoxide in the absolute ethyl alcohol in the step 1 is 50-70g/L, the addition amount of the palladium chloride is 30-50% of the mass of the aluminum isopropoxide, the low-temperature stirring temperature is 4-10 ℃, and the stirring speed is 1000-2000 r/min.
3. The method for preparing a mesoporous catalyst based on activated alumina according to claim 1, comprising: the adding amount of the sodium dodecyl sulfate in the step 1 is 30-60% of the mass of the aluminum isopropoxide, the temperature raising and stirring temperature is 60-70 ℃, and the stirring speed is 1000-1500 r/min.
4. The method for preparing an activated alumina-based mesoporous catalyst according to claim 1, wherein: the temperature of reduced pressure distillation in the step 2 is 70-80 ℃, the pressure is 70-80% of the atmospheric pressure, the temperature of constant temperature drying is 90-100 ℃, and the pressure is 0.3-0.5 MPa.
5. The method for preparing a mesoporous catalyst based on activated alumina according to claim 1, comprising: the concentration of the aluminum isopropoxide in the chloroform in the step 3 is 80-100g/L, and the stirring speed is 1000-2000 r/min.
6. The method for preparing a mesoporous catalyst based on activated alumina according to claim 1, comprising: the addition amount of diethyl ether in the step 3 is 50-300% of the volume of chloroform, and the spraying amount of the uniform spraying is 2-6ml/cm 2 The temperature of constant temperature standing is 60-65 ℃, and the pressure is 0.2-0.4 MPa.
7. The method for preparing a mesoporous catalyst based on activated alumina according to claim 1, comprising: and (4) filling mixed gas in the reaction kettle in the step (4), wherein the mixed gas consists of 20-30% of ammonia gas, 20-40% of water vapor and the rest of nitrogen.
8. The method for preparing a mesoporous catalyst based on activated alumina according to claim 1, comprising: the standing temperature in the step 4 is 100-110 ℃; the temperature of the constant temperature treatment is 160-180 ℃; the purging adopts 100-120 ℃ nitrogen at the speed of 5-10 mL/min; the reduction is carried out by using hydrogen at a temperature of 90-100 ℃.
9. The method for preparing a mesoporous catalyst based on activated alumina according to claim 1, comprising: the mesoporous catalyst is used for hydrogenation reaction.
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