CN110586151B - Preparation method of ordered mesoporous transition metal nitride - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
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- 238000000034 method Methods 0.000 claims abstract description 18
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- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
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- DMTIXTXDJGWVCO-UHFFFAOYSA-N iron(2+) nickel(2+) oxygen(2-) Chemical compound [O--].[O--].[Fe++].[Ni++] DMTIXTXDJGWVCO-UHFFFAOYSA-N 0.000 description 5
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- 238000001308 synthesis method Methods 0.000 description 2
- 229910000863 Ferronickel Inorganic materials 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
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- 229910052721 tungsten 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
-
- 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
- B01J35/61—Surface area
-
- 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
- B01J35/64—Pore diameter
- B01J35/647—2-50 nm
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Abstract
The invention provides a preparation method of ordered mesoporous transition metal nitride, which comprises the following steps: filling transition metal ions in a silicon dioxide SBA-15 mesoporous template, removing the template by using alkali after high-temperature oxidation to generate a mesoporous oxide with a mesoporous structure, and then performing high-temperature nitridation treatment on the mesoporous oxide to synthesize an ordered mesoporous transition metal nitride; the present invention is based on SBA-15 template-derived precursors, useful for various types of TMN materials. In one aspect, by promoting NH 3 The gas diffusion of (2) can effectively reduce the reaction time, and is beneficial to synthesizing a rigid mesoporous structure with high crystallinity. On the other hand, the rapid nitridation process can save the time for programming heating and cooling at common temperature, thereby inhibiting the closing and collapse of the mesoporous structure.
Description
Technical Field
The invention relates to the field of nano-structure functional materials, in particular to a preparation method of ordered mesoporous transition metal nitride.
Background
Transition Metal Nitrides (TMN) are intermetallic filling compounds produced by insertion of nitrogen into a transition metal lattice, having properties of covalent compounds, ionic crystals and transition metals. TMN has unique physical and chemical properties, such as high strength, strong acid and alkali resistance, high chemical stability, good conductivity, etc., and thus has wide applications in the fields of superhard materials, protective materials, superconductors, and structural materials. In addition, a great deal of research shows that TMN shows good catalytic activity in a plurality of hydrogen-involved reactions, and even has the performance which is not inferior to the performance of noble metals such as Pt, rh and the like, so that the TMN has important significance for carrying out extensive and intensive research on the formation mechanism, the preparation condition and the catalytic performance of the TMN and developing the application prospect.
It is well known that specific surface area and pore structure have a great influence on the catalytic reaction, whereas a large number of metal active sites and increased pore volume are provided by a high specific surface area and a regular pore structure. The preparation of the transition metal nitride is a local regular reaction, and particularly when a material with high specific surface area is synthesized, the transition metal nitride with high specific surface area can be generated under the condition that the crystal structure of a transition metal oxide precursor is not basically damaged by strictly controlling the reaction conditions. However, most of the existing methods for preparing Transition Metal Nitrides (TMN) involve high temperature heating or high pressure for a long time, and high interfacial energy and pressure exist in such reaction systems, so that the porous structure is inevitably aggregated, closed and collapsed during the transformation and recrystallization processes. Therefore, it is very necessary to use a new method to prepare ordered porous TMN with high specific surface area.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art: provides a new method for preparing ordered mesoporous transition metal nitride by a rapid nitridation synthesis method. The method is based on SBA-15 template-derived precursors and can be used for various types of TMN materials. In one aspect, by promoting NH 3 The gas diffusion of (2) can effectively reduce the reaction time, and is beneficial to synthesizing a rigid mesoporous structure with high crystallinity. On the other hand, the rapid nitridation process can save the time for programming heating and cooling at common temperature, thereby inhibiting the closing and collapse of the mesoporous structure.
The technical solution of the invention is as follows: a method for preparing ordered mesoporous transition metal nitride comprises the following steps: filling transition metal ions in a silicon dioxide SBA-15 mesoporous template, removing the template by alkali after high-temperature oxidation to generate a mesoporous oxide with a mesoporous structure, and then performing high-temperature nitridation treatment on the mesoporous oxide to synthesize the ordered mesoporous transition metal nitride.
The transition metal ions are one or more of cobalt ions, tungsten ions, chromium ions, nickel ions and iron ions.
The mesoporous oxide is one or more of cobalt oxide, tungsten oxide, chromium oxide and nickel iron oxide.
The preparation method of the silicon dioxide SBA-15 mesoporous template comprises the following steps:
1) Adding a nonionic triblock copolymer Pluronic P123 into hydrochloric acid with the pH value of less than 1, and stirring at the temperature of 30-50 ℃ until the solute is completely dissolved;
2) Adding tetraethyl orthosilicate into the solution prepared in the step 1) under the condition of stirring, uniformly mixing and standing for 10-30h; heating in an oven at 80-90 ℃ for 10-24h under the standing condition, filtering, washing and drying the filtered precipitate by using deionized water, and finally calcining at the temperature of more than 500 ℃ to obtain the silicon dioxide SBA-15 mesoporous template.
The preparation method of the mesoporous oxide comprises the following steps:
1) Adding a silicon dioxide SBA-15 mesoporous template and an oxide precursor into ethanol, uniformly mixing, stirring at room temperature for 30-50min, heating to 60-80 ℃, and evaporating to remove ethanol to obtain a mesoporous silicon composite material;
2) Putting the mesoporous silicon composite material into a porcelain boat, heating for 3-4h at 230-250 ℃ in a muffle furnace, removing the silicon dioxide SBA-15 mesoporous template by using NaOH solution, washing by using deionized water and ethanol, and drying in vacuum at 60-80 ℃ to obtain the mesoporous oxide.
The oxide precursor is metal salt corresponding to metal oxide; the metal oxide is one or more of cobalt oxide, chromium oxide, tungsten oxide and nickel iron oxide.
The invention has the beneficial effects that: the invention can synthesize a series of binary and ternary TMN materials (CoN, WN, crN and Ni) within 30min 3 FeN) and avoid pore collapse,the mesoporous structure is kept to be perfect, so that the mesoporous structure has high specific surface area and can provide more active sites in catalytic reaction. The successful preparation of the series of materials shows that the invention has universality and wide application prospect. In addition, the preparation method has the advantages of simple operation, simple equipment, uniform product and short overall reaction time.
Drawings
FIG. 1: the X-ray diffraction pattern of the example is shown.
FIG. 2: the X-ray diffraction pattern spectrum in the example is shown.
FIG. 3: coN, WN, crN and Ni prepared in the examples 3 A mesoporous morphology map of a FeN transmission electron microscope.
FIG. 4 is a schematic view of: coN, WN, crN and Ni prepared in the examples 3 FeN high resolution transmission electron microscope lattice diagram.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the present invention is not limited to the following examples.
Examples
1. Preparing a silicon dioxide SBA-15 mesoporous template:
1) 16.5mL of hydrochloric acid (HCl content 12 mol/L) was mixed with 112mL of water, 3g of the nonionic triblock copolymer Pluronic P123 was added, and the solution was stirred vigorously at 40 ℃ for 3h;
2) After complete dissolution of P123, 7.427g of tetraethyl orthosilicate was rapidly added to the acidic solution with rapid stirring and kept at 40 ℃ for 24h to obtain a synthetic gel.
3) And then heating the synthesized gel at 90 ℃ for 24h under a static condition, filtering, washing, drying and filtering to obtain a precipitate, and finally calcining at the temperature of more than 500 ℃ to obtain the silica SBA-15 mesoporous template.
2. Preparing cobalt oxide, tungsten oxide, chromium oxide and nickel iron oxide with mesoporous structures:
1) Weighing 0.5g of silicon dioxide SBA-15 mesoporous template and 0.8mol/L of metal nitrate solution as a precursor, wherein the cobalt oxide adopts Co (NO) 3 ) 2 6H 2 The O and the chromium oxide adopt Cr (NO) 3 ) 3 ·9H 2 O, tungsten oxide adopt acid hydrate H 3 [P(W 3 O 10 ) 4 ]·xH 2 O), for mixed mesoporous ferronickel oxide, ni (NO) is adopted 3 ) 3 ·6H 2 O and Fe (NO) 3 ) 3 ·9H 2 O is a mixture of 3; adding the mixed raw materials into 3.6mL of ethanol, stirring for 30min at room temperature, heating to 60 ℃, and evaporating to remove the ethanol to obtain the mesoporous silicon composite material.
2) Putting the mesoporous silicon composite material into a porcelain boat, heating for 4h at 250 ℃ in a muffle furnace, removing the silicon dioxide SBA-15 mesoporous template by using 2mol/L NaOH solution, washing by using deionized water and ethanol, and drying in vacuum at 60 ℃ to respectively prepare cobalt oxide, tungsten oxide, chromium oxide and nickel iron oxide with mesoporous structures.
3. The ordered mesoporous transition metal nitride is prepared according to the following method:
1) Loading 10mg of cobalt oxide, tungsten oxide, chromium oxide and nickel iron oxide with mesoporous structures by quartz boats respectively, putting the quartz boats into a pipeline of a temperature programming furnace with a slide rail, connecting two sections of the quartz boats with an ammonia pipeline, evacuating air in the pipeline, filling the pipeline with ammonia, and repeating the operation for 3 times.
2) And (4) sliding the furnace to a position which does not influence the sample, starting heating, and waiting for 10min to stabilize when the temperature reaches the set temperature. The furnace is then pushed towards the sample, centering the sample in the heating zone, and the reaction time is recorded until the furnace is pushed away from the sample. The following conditions were used: coN 330 deg.C, 15min, WN 600 deg.C, 10min,800 deg.C, crN 30min,380 deg.C, ni 3 FeN was 30min.
As shown in fig. 1-4, fig. 1: the X-ray diffraction pattern of the example is shown. FIG. 2: the X-ray diffraction pattern spectrum in the example is shown. FIG. 3: coN, WN, crN and Ni prepared in the examples 3 A mesoporous morphology map of a FeN transmission electron microscope. FIG. 4 is a schematic view of: coN, WN, crN and Ni prepared in the examples 3 FeN high resolution transmission electron microscope lattice diagram.
As can be seen from fig. 1-4, the transition metal mesoporous nitride prepared by the method has a good pore structure, and both small-angle XRD and TEM images show that the nanopore structure of the transition metal mesoporous nitride is well maintained; the composition of the material is pure phase, and XRD and high-resolution TEM lattice images show that the synthesis of the nitride is successful. These results indicate that the rapid nitridation synthesis method can effectively prepare transition metal nitrides having ordered pore structures.
The above are merely exemplary embodiments of the features of the present invention, and do not limit the scope of the present invention in any way. All technical solutions formed by equivalent exchanges or equivalent substitutions fall within the protection scope of the present invention.
Claims (6)
1. The preparation method of the ordered mesoporous transition metal nitride is characterized by comprising the following steps of: filling a silicon dioxide SBA-15 mesoporous template with transition metal ions, removing the template by using alkali after high-temperature oxidation to generate a mesoporous oxide with a mesoporous structure, and then performing high-temperature nitridation treatment on the mesoporous oxide to synthesize an ordered mesoporous transition metal nitride, wherein the ordered mesoporous transition metal nitride is CoN and CrN, and is prepared according to the following method:
1) Loading 10mg of mesoporous oxide with a mesoporous structure by a quartz boat, putting the quartz boat into a pipeline of a programmed temperature furnace with a slide rail, connecting two sections of pipelines with ammonia gas, evacuating air in the pipeline, filling the air with ammonia gas, and repeating the operation for 3 times;
2) Sliding the furnace to a position which does not affect the sample, starting temperature rise, waiting for 10min to stabilize when the temperature reaches a set temperature, then pushing the furnace to the sample to enable the sample to be in the center of a heating area, and starting to record reaction time until the furnace is pushed away from the sample, wherein the reaction time is less than or equal to 30min; coN is 330 ℃ and 15min; crN is 800 deg.C, 30min.
2. The method for preparing ordered mesoporous transition metal nitride according to claim 1, wherein the transition metal ions are one or more of cobalt ions and chromium ions, and the cobalt ions are Co (NO) 3 ) 2 6H 2 The O and Cr ions are Cr (NO) 3 ) 3 ·9H 2 O。
3. The method of preparing an ordered mesoporous transition metal nitride according to claim 1, wherein the mesoporous oxide is one or more of cobalt oxide and chromium oxide.
4. The method for preparing the ordered mesoporous transition metal nitride according to claim 1, wherein the method for preparing the mesoporous template of silicon dioxide SBA-15 comprises:
1) Adding a nonionic triblock copolymer Pluronic P123 into hydrochloric acid with the pH value less than 1, and stirring at 30-50 ℃ until the solute is completely dissolved;
2) Adding tetraethyl orthosilicate into the solution prepared in the step 1) under the condition of stirring, uniformly mixing and standing for 10-30h; heating in an oven at 80-90 ℃ for 10-24h under the standing condition, filtering, washing and drying the precipitate obtained by filtering by using deionized water, and finally calcining at the temperature of more than 500 ℃ to obtain the silicon dioxide SBA-15 mesoporous template.
5. The method for preparing an ordered mesoporous transition metal nitride according to claim 1, wherein the method for preparing the mesoporous oxide comprises:
1) Adding a silicon dioxide SBA-15 mesoporous template and an oxide precursor into ethanol, uniformly mixing, stirring at room temperature for 30-50min, heating to 60-80 ℃, and evaporating to remove ethanol to obtain a mesoporous silicon composite material;
2) Putting the mesoporous silicon composite material into a porcelain boat, heating for 3-4h at 230-250 ℃ in a muffle furnace, removing the silicon dioxide SBA-15 mesoporous template by using NaOH solution, washing by using deionized water and ethanol, and drying in vacuum at 60-80 ℃ to obtain the mesoporous oxide.
6. The method of preparing an ordered mesoporous transition metal nitride according to claim 5, wherein the oxide precursor is a metal salt corresponding to a metal oxide; the metal oxide is one or more of cobalt oxide and chromium oxide.
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