CN106944119B - Preparation method of carbon nitride supported monoatomic metal catalytic material - Google Patents
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 55
- 239000002184 metal Substances 0.000 title claims abstract description 53
- 239000000463 material Substances 0.000 title claims abstract description 32
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 16
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 7
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 6
- 229910052703 rhodium Inorganic materials 0.000 claims abstract description 5
- 229910052709 silver Inorganic materials 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 26
- 239000007787 solid Substances 0.000 claims description 20
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 15
- 229920000877 Melamine resin Polymers 0.000 claims description 14
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 claims description 5
- NWAHZABTSDUXMJ-UHFFFAOYSA-N platinum(2+);dinitrate Chemical compound [Pt+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O NWAHZABTSDUXMJ-UHFFFAOYSA-N 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 239000010948 rhodium Substances 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 239000010944 silver (metal) Substances 0.000 claims description 3
- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000000197 pyrolysis Methods 0.000 claims description 2
- VXNYVYJABGOSBX-UHFFFAOYSA-N rhodium(3+);trinitrate Chemical compound [Rh+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VXNYVYJABGOSBX-UHFFFAOYSA-N 0.000 claims description 2
- 229910001958 silver carbonate Inorganic materials 0.000 claims description 2
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- WHQSYGRFZMUQGQ-UHFFFAOYSA-N n,n-dimethylformamide;hydrate Chemical compound O.CN(C)C=O WHQSYGRFZMUQGQ-UHFFFAOYSA-N 0.000 claims 1
- 229910002804 graphite Inorganic materials 0.000 abstract description 8
- 239000010439 graphite Substances 0.000 abstract description 8
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract description 2
- 230000003993 interaction Effects 0.000 abstract description 2
- 239000003446 ligand Substances 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 24
- 239000000919 ceramic Substances 0.000 description 18
- 239000003054 catalyst Substances 0.000 description 8
- 230000005484 gravity Effects 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 238000002390 rotary evaporation Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
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- 239000003570 air Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000001833 catalytic reforming Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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Abstract
The invention mainly relates to a preparation method of a carbon nitride loaded monoatomic metal catalytic material, in particular to a preparation method of a layered graphite phase carbon nitride loaded monoatomic metal M catalytic material (M is one or more than two of Ag, Pd, Rh and Pt), belonging to the field of catalytic materials. According to the method, the metal precursor and the carbon-nitrogen precursor are complexed, the agglomeration of metal atoms is inhibited through the interaction between the metal center and the ligand, the carbon-nitrogen precursor and the metal precursor are pyrolyzed in one step to prepare the carbon-nitride-loaded monoatomic metal catalytic material, and the stability and the dispersibility of the monoatomic metal catalytic material are improved. The metal in the material prepared by the method is loaded on the surface of the layered graphite phase carbon nitride in a form of zero-valence monoatomic dispersion, and the type and the components of the loaded metal atom can be regulated and controlled according to the requirement.
Description
Technical Field
The invention mainly relates to a preparation method of a carbon nitride loaded monoatomic metal catalytic material, in particular to a preparation method of a layered graphite phase carbon nitride loaded monoatomic metal M catalytic material (M is one or more than two of Ag, Pd, Rh and Pt), belonging to the field of catalytic materials.
Background art:
monatomic catalysis is of great importance for the practical application of catalysts (X.Yang, A.Wang, B.Qiao, J.Li, J.Liu, T.Zhang.accounts of Chemical Research,2013,46, 1740-. 50% of the worldwide annual platinum production is used in three-way converters for automotive exhaust gas purification systems. Fuel cell electrode catalysts, catalytic reforming selective hydrogenation in petrochemical industry, and the synthesis of various fine chemicals all rely on high-efficiency supported noble metal catalysts such as platinum and palladium. Ag. Elements such as Pd, Rh, Pt and the like have important application in catalytic conversion reactions in multiple fields such as petrochemical industry and the like, and the research and development of the preparation method of the monatomic catalyst of the elements can greatly reduce the cost of the catalyst and improve the production efficiency.
When the metal single atom is easy to agglomerate in the preparation and reaction processes, the catalyst is deactivated. Therefore, the preparation of metal monatomic catalysts must be carried out with a support having excellent properties. g-C3N4Is a polymer material consisting of only C and N, the simple composition being such that for g-C3N4Can be carried out by a simple method without significantly changing the total composition. g-C3N4Polymer properties of (2) to g-C3N4The surface chemistry control can be carried out by molecular level modification and surface engineering, and simultaneously, the structure of the material is ensured to have enough flexibility to ensure that the g-C has enough elasticity3N4Can be used as the main matrix of various inorganic nano particles, thereby preparing g-C3N4Base composite (W.Ong, L.Tan, Y.Ng, S.Yong, S.Chai.chemical reviews,2016,116, 7159-.
Therefore, we developed a new method for preparing a carbon nitride supported monatomic metal catalytic material by pyrolyzing a carbon-nitrogen precursor and a metal precursor in one step. The metal in the material is loaded on the surface of the layered graphite phase carbon nitride in a form of zero valence monoatomic dispersion, and the type and the components of the loaded metal atom can be regulated and controlled according to the requirement.
Disclosure of Invention
The invention provides a preparation method of a carbon nitride loaded monoatomic metal catalytic material. The prepared catalyst has good single metal atom dispersibility and high stability. The method has the characteristics of simplicity and easy control, and can be used for preparing a large amount of carbon nitride supported monoatomic metal catalytic material.
The technical scheme adopted by the invention is as follows: a preparation method of a carbon nitride loaded monoatomic metal catalytic material is characterized by comprising the following steps:
(1) dissolving a carbon-nitrogen precursor in a solvent to prepare a solution A, and dissolving a metal precursor in the solvent to prepare a solution B;
(2) adding the solution B into the solution A, heating to 20-150 ℃ under a special atmosphere, mixing and stirring for 6-36h, and then naturally cooling to room temperature;
(3) removing the solvent from the solution obtained in the step (2) to obtain a solid metal carbon nitrogen adduct, and grinding the solid metal carbon nitrogen adduct to be below 80 meshes;
(4) putting the solid powder obtained in the step (3) into a muffle furnace or a tubular furnace, carrying out temperature programming pyrolysis treatment under a special atmosphere, naturally cooling to room temperature, and grinding to below 80 meshes;
(5) placing the solid powder obtained in the step (4) in a muffle furnace or a tubular furnace, heating to 450-550 ℃ at the speed of 10 ℃/min under a special atmosphere, keeping for 1h, and then naturally cooling to room temperature to obtain the carbon nitride loaded monoatomic metal catalytic material;
the method of the invention is characterized in that: the carbon-nitrogen precursor is one or a mixture of two of melamine, dicyandiamide and urea, the metal precursor is one or more of silver nitrate, silver carbonate, palladium nitrate, rhodium nitrate and platinum nitrate, the solvent is an alkaline or neutral solvent such as water, acetonitrile, ethanol, methanol, acetone, N-dimethylformamide and the like, the concentration of the solution A is 1-500g/L, the concentration of the solution B is 1-100mg/mL, the special atmosphere is under the protection of air, nitrogen and argon, the temperature programming is that the solution A is heated to 300 ℃ at the speed of 1-5 ℃/min and is kept for 1-2h, and then the solution B is heated to 400-850 ℃ at the speed of 5-10 ℃/min and is kept for 2-6 h.
The mass percent of the metal M in the prepared laminar graphite phase carbon nitride loaded monoatomic metal M catalytic material (M is one or more than two of Ag, Pd, Rh and Pt) is 0.1-3%, and the metal M exists in a form of a zero valence monoatomic atom.
The method adopts a metal precursor and carbon nitrogen precursor complexing mode, inhibits the agglomeration of metal atoms through the interaction between a metal center and a ligand, and improves the stability and the dispersibility of the monatomic metal catalytic material. The preparation method has the advantages of simple process conditions, cheap materials, mild reaction conditions, capability of obtaining materials with more excellent performance at lower preparation cost, and wide application range. Therefore, the method for preparing the carbon nitride supported monatomic metal catalytic material is simple, convenient, rapid, economical and environment-friendly.
Detailed Description
Example 1
2g of melamine was dispersed in 100mL of N, N-dimethylformamide and stirred at room temperature for 3 hours to obtain a melamine solution. 10mg of palladium nitrate was dispersed in 10mL of N, N-dimethylformamide and subjected to ultrasonic treatment for 30min to obtain a palladium nitrate solution. Transferring the melamine solution into a 250mL round-bottom flask, adding 5mL palladium nitrate solution into the melamine solution, configuring a reflux condenser pipe, heating to 120 ℃ under the protection of nitrogen, stirring for 36 hours in a dark place, and naturally cooling to room temperature. The solvent was removed from the mixed solution by rotary evaporation to give a solid metal carbon nitrogen adduct, which was dried under vacuum for 24h and then ground to 80 mesh. And (3) placing the solid powder into a ceramic crucible, placing the ceramic crucible into a tubular furnace, and heating under the protection of nitrogen. First heated to 300 ℃ at a rate of 2 ℃/min for 2h, then heated to 500 ℃ at a rate of 7 ℃/min for 2 h. Naturally cooling to room temperature, and grinding the obtained solid to 80 meshes again. And finally, placing the solid powder into a ceramic crucible, placing the ceramic crucible into a tubular furnace, heating the ceramic crucible to 550 ℃ at the speed of 10 ℃/min under the protection of nitrogen, keeping the temperature for 1h, and naturally cooling the ceramic crucible to room temperature to obtain the carbon nitride supported monatomic metal Pd catalytic material. The actual load specific gravity of Pd in the prepared material is 0.51 percent, and the metal Pd is dispersed on the layered graphite phase carbon nitride by a single atom with a zero valence state.
Example 2
2g of melamine was dispersed in 100mL of N, N-dimethylformamide and stirred at room temperature for 3 hours to obtain a melamine solution. 10mg of platinum nitrate was dispersed in 10mL of N, N-dimethylformamide, and subjected to ultrasonic treatment for 30min to obtain a platinum nitrate solution. Transferring the melamine solution into a 250mL round-bottom flask, adding 5mL of platinum nitrate solution into the melamine solution, configuring a condensation reflux pipe, heating to 120 ℃ under the protection of nitrogen, stirring for 24 hours in a dark place, and naturally cooling to room temperature. The solvent was removed from the mixed solution by rotary evaporation to give a solid metal carbon nitrogen adduct, which was dried under vacuum for 24h and then ground to 80 mesh. And (3) placing the solid powder into a ceramic crucible, placing the ceramic crucible into a tubular furnace, and heating under the protection of nitrogen. First heated to 300 ℃ at a rate of 2 ℃/min for 2h, then heated to 550 ℃ at a rate of 5 ℃/min for 4 h. Naturally cooling to room temperature, and grinding the obtained solid to 80 meshes again. And finally, placing the solid powder into a ceramic crucible, placing the ceramic crucible into a tubular furnace, heating the ceramic crucible to 550 ℃ at the speed of 10 ℃/min under the protection of nitrogen, keeping the temperature for 1h, and naturally cooling the ceramic crucible to room temperature to obtain the carbon nitride supported monoatomic metal Pt catalytic material. The actual load specific gravity of Pt in the prepared material is 0.47%, and metal Pt is dispersed on the layered graphite phase carbon nitride by a single atom with a zero valence state.
Example 3
2g of melamine was dispersed in 100mL of methanol and stirred at room temperature for 3 hours to obtain a melamine solution. 20mg of silver nitrate is dispersed in 10mL of methanol, and ultrasonic treatment is carried out for 30min to obtain a silver nitrate solution. Transferring the melamine solution into a 250mL round-bottom flask, adding the silver nitrate solution into the melamine solution, configuring a condensation reflux pipe, heating to 60 ℃ under the protection of nitrogen, stirring for 24 hours in a dark place, and naturally cooling to room temperature. The solvent was removed from the mixed solution by rotary evaporation to give a solid metal carbon nitrogen adduct, which was dried under vacuum for 24h and then ground to 80 mesh. And (3) placing the solid powder into a ceramic crucible, placing the ceramic crucible into a tubular furnace, and heating under the protection of nitrogen. First heated to 200 ℃ at a rate of 1 ℃/min for 2h, then heated to 450 ℃ at a rate of 5 ℃/min for 2 h. Naturally cooling to room temperature, and grinding the obtained solid to 80 meshes again. And finally, placing the solid powder into a ceramic crucible, placing the ceramic crucible into a tubular furnace, heating the ceramic crucible to 550 ℃ at the speed of 10 ℃/min under the protection of nitrogen, keeping the temperature for 1h, and naturally cooling the ceramic crucible to room temperature to obtain the carbon nitride supported monoatomic metal Ag catalytic material. The actual load specific gravity of Ag in the prepared material is 1.89%, and the metal Ag is dispersed on the layered graphite phase carbon nitride by a single atom with a zero valence state.
Claims (2)
1. A preparation method of a carbon nitride loaded monoatomic metal catalytic material is characterized by comprising the following steps:
(1) dissolving a carbon-nitrogen precursor in a solvent to prepare a solution A, dissolving a metal precursor in the solvent, and carrying out ultrasonic treatment for 30min to prepare a solution B;
(2) adding the solution B into the solution A, heating to 20-150 ℃ under nitrogen, mixing and stirring for 6-36h, and then naturally cooling to room temperature;
(3) removing the solvent from the solution obtained in the step (2) to obtain a solid metal carbon nitrogen adduct, and grinding the solid metal carbon nitrogen adduct to be below 80 meshes;
(4) putting the solid powder obtained in the step (3) into a muffle furnace or a tubular furnace, carrying out temperature programming pyrolysis treatment under nitrogen, then naturally cooling to room temperature, and grinding to below 80 meshes;
(5) placing the solid powder obtained in the step (4) in a muffle furnace or a tubular furnace, heating to 450-550 ℃ at the speed of 10 ℃/min under nitrogen, keeping for 1h, and then naturally cooling to room temperature to obtain the carbon nitride-loaded monatomic metal catalytic material, wherein the metal is dispersed on the layered graphite-phase carbon nitride in a zerovalent state and monatomic state;
the concentration of the solution A is 1-500 g/L;
the concentration of the solution B is 1-100 mg/mL;
the solvent is one or more than two of water, acetonitrile, ethanol, methanol, acetone and N, N-dimethylformamide;
the temperature programming is that the temperature is heated to 200-300 ℃ at the speed of 1-5 ℃/min and kept for 1-2h, then the temperature is heated to 400-850 ℃ at the speed of 5-10 ℃/min and kept for 2-6 h;
the mass percent of metal M in the laminated graphite phase carbon nitride loaded monoatomic metal M catalytic material is 0.1-3%, and M is one or more than two of Ag, Pd, Rh and Pt;
the carbon-nitrogen precursor is one or a mixture of melamine, dicyandiamide and urea.
2. The method of claim 1, wherein:
the metal precursor is one or more than two of silver nitrate, silver carbonate, palladium nitrate, rhodium nitrate and platinum nitrate.
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