CN114367670A - Carbon-platinum-cobalt composite material and preparation method thereof - Google Patents
Carbon-platinum-cobalt composite material and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 42
- QEUZUDZQOIKYIC-UHFFFAOYSA-N [Pt].[Co].[C] Chemical compound [Pt].[Co].[C] QEUZUDZQOIKYIC-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
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- 239000005977 Ethylene Substances 0.000 claims abstract description 16
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 12
- 239000010941 cobalt Substances 0.000 claims abstract description 12
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 7
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- 239000002105 nanoparticle Substances 0.000 claims abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 16
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- 150000001875 compounds Chemical class 0.000 claims description 12
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- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B7/00—Preservation or chemical ripening of fruit or vegetables
- A23B7/14—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10
- A23B7/144—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10 in the form of gases, e.g. fumigation; Compositions or apparatus therefor
- A23B7/152—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10 in the form of gases, e.g. fumigation; Compositions or apparatus therefor in a controlled atmosphere comprising other gases in addition to CO2, N2, O2 or H2O ; Elimination of such other gases
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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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8913—Cobalt and noble metals
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/396—Distribution of the active metal ingredient
- B01J35/399—Distribution of the active metal ingredient homogeneously throughout the support particle
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/086—Decomposition of an organometallic compound, a metal complex or a metal salt of a carboxylic acid
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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Abstract
The invention relates to a carbon-platinum-cobalt composite material PtCo-C and a preparation method thereof. A cobalt-based precursor is prepared on the basis of a Metal Organic Framework (MOF) material, and a composite material of porous carbon matrix loaded PtCo nanoparticles is prepared by adopting a simple chemical reduction method. The cobalt-based precursor has a regular polyhedral structure, the nano cobalt particles are uniformly dispersed in the porous carbon skeleton, the PtCo-C material is prepared without adopting a reducing agent for reaction, the PtCo particles are uniformly dispersed in the porous carbon matrix, and the agglomeration of the nano particles in the reaction process is prevented, so that the performance of the material is improved, the material preparation process is simple, the ethylene removing effect is good, and the popularization and application values are good.
Description
Technical Field
The invention relates to a carbon-platinum-cobalt composite material PtCo-C, a preparation method thereof and application of the composite material in the aspect of ethylene removal.
Background
Along with the continuous development of national economy and the continuous improvement of the living standard of people in China, the consumption of vegetables and fruits is also increased year by year, so that the supply and consumption of the fruit and vegetable market are seen to be full year by year, and the quality requirements of people on the fruits and vegetables are also stricter. During the storage and transportation of the picked fruits and vegetables, the influence of the hormone ethylene on the respiration of the fruits and vegetables is very severe, and even one thousandth of the concentration can induce the ripening and aging of the fruits and vegetables. The measures for further fresh-keeping of fruits and vegetables are further improved, the use of ethylene removing agents for fresh-keeping of fruits and vegetables tends to be common gradually, and the types of ethylene removing agents are more and more abundant. Researches find that the porous carbon material composite platinum-based bimetal can absorb ethylene at room temperature and simultaneously can convert trace ethylene into carbon dioxide and water by using ultraviolet rays under the action of sunlight, so that the influence of the ethylene on fruit and plants is reduced.
Disclosure of Invention
The invention aims to provide a carbon-platinum-cobalt composite material PtCo-C, which consists of a carbon skeleton with a dodecahedron structure and PtCo nano-particles.
The invention prepares a cobalt-based precursor on the basis of a Metal Organic Framework (MOF) material, and prepares the composite material of the porous carbon matrix loaded PtCo nanoparticles by adopting a simple chemical reduction method. The cobalt-based precursor has a regular polyhedral structure, and the nano cobalt particles are uniformly dispersed in the porous carbon skeleton, so that the structure can ensure that the platinum-based active substance particles are uniformly dispersed in the porous carbon matrix after the chemical reduction reaction, and the agglomeration of the nano particles in the reaction process is prevented, thereby improving the performance of the material.
The preparation method of the bimetal phosphide composite material comprises the following steps:
1) weighing Co (NO) according to the mass ratio of 1: 1-33)2·6H2O and 2-methylimidazole, dissolving in 100ml methanol, stirring for dissolving, and adding Co (NO) into the 2-methylimidazole solution3)2Stirring the solution, aging the solution at room temperature for 24 hours after stopping stirring, and then centrifugally separating, cleaning and drying the product to obtain the cobalt-based metal organic framework compound with a dodecahedron structure.
2) Placing the cobalt-based metal organic framework compound obtained in the step 1) into a quartz boat, placing the quartz boat into a tubular resistance furnace, heating to 550-900 ℃ in an argon atmosphere, and preserving heat for 1-8 hours to obtain the dodecahedral porous carbon composite material Co-C containing the cobalt metal simple substance.
3) Adding the Co-C composite material obtained in the step 2) into H2PtCl4And (3) ultrasonically stirring the solution without adding any reducing agent, reacting for a certain time, and then cleaning and drying to obtain the PtCo-C composite material.
The cleaning and drying in the step 1) are carried out by washing for 3 times by using methanol and then vacuum drying for 8h at the temperature of 60 ℃.
In the step 2), the temperature is raised to 600 ℃ at the temperature raising rate of 5 ℃/min, and the temperature is kept for 2 h.
Said H in step 3)2PtCl4The concentration of the solution was 0.05 mol/L.
The method of the invention has the following characteristics:
(1) the dodecahedral porous carbon matrix material containing a cobalt simple substance is obtained after the cobalt-based metal organic framework compound with the dodecahedral structure is carbonized, and the PtCo active substance particles are ensured to be uniformly dispersed in the porous carbon matrix.
(2) The PtCo-C material is prepared by spontaneous in-situ reaction without adopting an external reducing agent, and the preparation process is simple and has good popularization and application values.
Drawings
FIG. 1 is an XRD pattern of the PtCo-C composite material obtained in example 1.
FIG. 2 is an SEM photograph of the PtCo-C composite material obtained in example 1.
FIG. 3 is a graph comparing the ethylene change of the PtCo-C material obtained in example 1 added to a fruit storage bin, the Co-C material obtained in comparative example 1 added to a fruit storage bin, and a fruit storage bin without any material added.
FIG. 4 shows the preservation time of bananas in a polyethylene sealed bag, wherein PtCo-C material of example 1, Co-C material of comparative example 1 and activated carbon of comparative example 2 are added into the polyethylene sealed bag.
Detailed Description
Example 1
1) Weigh 0.498g Co (NO)3)2·6H2O and 0.656g 2-methylimidazole respectively dissolved in 50ml methanol, stirred for 10 minutes, and after the solution is stirred and dissolved, the 2-methylimidazole solution is poured into Co (NO) rapidly3)2And (3) continuing stirring for 10min in the solution, aging for 24h at room temperature after stopping stirring, then centrifugally separating the product, washing for 3 times by using methanol, and finally drying for 8h in vacuum at 60 ℃ to obtain the cobalt-based metal organic framework compound with the dodecahedron structure.
2) Placing the cobalt-based metal organic framework compound with the dodecahedron structure into a quartz boat, placing the quartz boat into a tubular resistance furnace, raising the temperature from the room to the target temperature of 600 ℃ at the temperature rise rate of 5 ℃/min in the argon atmosphere, and keeping the temperature constant for 2 hours to prepare the dodecahedron porous carbon composite material Co-C containing the cobalt metal simple substance.
3) Putting the prepared 50mg of composite Co-C in 10ml of deionized water, performing ultrasonic treatment until the composite Co-C is uniform and has no precipitate, and adding the composite Co-C into 10ml of H with the concentration of 0.05mol/L2PtCl4And uniformly stirring the solution, standing for 12h, washing and drying by using ethanol and deionized water, and carrying out vacuum drying on the collected particles for 24h at the temperature of 60 ℃ to obtain PtCo-C powder.
Example 2
1) Synthesis of cobalt-based metal organic framework compounds with dodecahedral structure: weighing 1gCo (NO)3)2·6H2O and 3g of 2-methylimidazole respectively dissolved in 800ml of methanol, stirred for 10 minutes, and after the 2-methylimidazole solution is dissolved by stirring, the 2-methylimidazole solution is poured into Co (NO) rapidly3)2And (3) continuing stirring for 10min in the solution, aging for 12h at room temperature after stopping stirring, then centrifugally separating the product, washing for 3 times by using methanol, and finally drying for 12h in vacuum at 60 ℃ to obtain the cobalt-based metal organic framework compound with the dodecahedron structure.
2) Placing the cobalt-based metal organic framework compound with the dodecahedron structure into a quartz boat, placing the quartz boat into a tubular resistance furnace, heating the quartz boat to a target temperature of 800 ℃ from room temperature at a heating rate of 5 ℃/min in an argon atmosphere, and keeping the temperature constant for 4 hours to prepare the dodecahedron porous carbon composite material Co-C containing the cobalt metal simple substance.
3) Putting the prepared 50mg of composite Co-C in 10ml of deionized water, performing ultrasonic treatment until the composite Co-C is uniform and has no precipitate, and adding the composite Co-C into 10ml of H with the concentration of 0.05mol/L2PtCl4And uniformly stirring the solution, adding sodium borohydride, standing for 12h, washing and drying by using ethanol and deionized water, and carrying out vacuum drying on the collected particles for 24h at the temperature of 60 ℃ to obtain the PtCo-C composite material.
Comparative example 1
1) Weigh 0.498g Co (NO)3)2·6H2O and 0.656g 2-methylimidazole respectively dissolved in 50ml methanol, stirred for 10 minutes, and after the solution is stirred and dissolved, the 2-methylimidazole solution is poured into Co (NO) rapidly3)2Stirring for 10min, aging at room temperature for 24 hr, and agingAnd (3) centrifugally separating the product, washing the product for 3 times by using methanol, and finally drying the product for 8 hours in vacuum at the temperature of 60 ℃ to obtain the cobalt-based metal organic framework compound with the dodecahedron structure.
2) Placing the cobalt-based metal organic framework compound with the dodecahedron structure into a quartz boat, placing the quartz boat into a tubular resistance furnace, raising the temperature from the room to the target temperature of 600 ℃ at the temperature rise rate of 5 ℃/min in the argon atmosphere, and keeping the temperature constant for 2 hours to prepare the dodecahedron porous carbon composite material Co-C containing the cobalt metal simple substance.
Comparative example 2
The specific surface area of the commercial product is more than or equal to 850m2Powder activated carbon per gram.
And (3) performance testing:
the material obtained in example 1 above was characterized and tested for its performance in comparison with comparative example 1. Powder X-ray diffraction (XRD) patterns were measured using a bruker D8Advance tester. Scanning Electron Microscope (SEM) images were collected using Hitachi SU 8020. Transmission Electron Microscope (TEM) images were collected using JEM 1200 EX. Selecting bananas of the same variety, the same batch, the same size, the same hardness, the same color and the same maturity as a test product at room temperature, wherein every five bananas form a group, and the banana seeds with the mass of about 600g-750g are placed in a transparent sealing box with the volume of 45 x 25 x 35 cm. 15mg of PtCo-C material was placed on 5X 5cm of rice paper in a transparent sealed box, and ethylene changes in the sealed environment were detected with an EST-2000 hand-held gas detector. The banana with similar peel state and color, proper and similar smell and hardness to ensure the consistency of maturity is selected, and meanwhile, the banana has the same shape and similar quality in the whole appearance and does not have mechanical damage and plant diseases and insect pests and is used as an experimental material. And selecting a commercially available common polyethylene freshness protection package to store each group of bananas, the bananas in the embodiment 1, the comparative example 1 and the comparative example 2 in a sealing way, and observing the influence of different materials on the banana freshness protection time at normal temperature.
FIG. 1 is an XRD pattern of the PtCo-C composite material obtained in example 1. The Pt diffraction peak and the Co diffraction peak are obvious in the figure. In addition, a diffraction peak of C is also present in the figure.
FIG. 2 is an SEM of the PtCo-C composite material obtained in example 1. As can be seen from the figure, the PtCo-C composite material obtained by the reaction keeps dodecahedron, and does not have any structural collapse and particle agglomeration phenomenon.
FIG. 3 is a graph showing the change of ethylene between a fruit storage box containing PtCo-C material and Co-C material and a fruit storage box without adding any material (blank group), and it can be seen that the fruit storage box containing PtCo-C ethylene remover has a smaller total amount of ethylene and a faster decrease, while the fruit storage box containing Co-C material and no material has a higher total amount of ethylene and no faster decrease, compared with the PtCo-C material group, so that the PtCo-C material has a better ethylene inhibition effect.
FIG. 4 shows the time of banana retention in sealed polyethylene bags with PtCo-C material of example 1, Co-C material of comparative example 1, and activated carbon of comparative example 2. The preservation time of bananas in the packaging bag added with the PtCo-C material at normal temperature can reach 10 days, the preservation time of bananas in the packaging bag added with the Co-C material and the activated carbon material is 6 days, and the preservation time of bananas in a pure polyethylene packaging bag is 5 days.
Claims (7)
1. A carbon-platinum cobalt composite material is characterized in that: the composite material is composed of a carbon skeleton with a dodecahedron structure and PtCo nano-particles.
2. The preparation method of the carbon-platinum-cobalt composite material as claimed in claim 1, which is characterized by comprising the following steps:
1) weighing Co (NO) according to the mass ratio of 1: 1-33)2·6H2O and 2-methylimidazole, dissolving in methanol, stirring for dissolving, and adding Co (NO) into the 2-methylimidazole solution3)2Stirring the solution, aging the solution at room temperature after stopping stirring, and then centrifugally separating, cleaning and drying the product to obtain a cobalt-based metal organic framework compound with a dodecahedron structure;
2) placing the cobalt-based metal organic framework compound obtained in the step 1) into a quartz boat, placing the quartz boat into a tubular resistance furnace, heating to 550-900 ℃ in an argon atmosphere, and preserving heat for 1-8 hours to obtain a dodecahedral porous carbon composite material Co-C containing a cobalt metal simple substance;
3) adding the Co-C composite material obtained in the step 2) into H2PtCl4And (3) ultrasonically stirring the solution without adding any reducing agent, reacting for a certain time, and then cleaning and drying to obtain the carbon-platinum-cobalt composite material.
3. The method of preparing a carbon-platinum-cobalt composite material of claim 2, wherein: the cleaning and drying in the step 1) are carried out by washing for 3 times by using methanol and then vacuum drying for 8h at the temperature of 60 ℃.
4. The method of preparing a carbon-bimetallic phosphide composite material as set forth in claim 2, wherein: in the step 2), the temperature is raised to 600 ℃ at the temperature raising rate of 5 ℃/min, and the temperature is kept for 2 h.
5. The method of preparing a carbon-bimetal composite of claim 2, wherein: said H in step 3)2PtCl4The concentration of the solution was 0.05 mol/L.
6. Use of a carbon-platinum cobalt composite material according to claim 1 or a carbon-platinum cobalt composite material prepared by a method according to any one of claims 2 to 5, wherein: the carbon-platinum-cobalt composite material is applied to the field of ethylene removal and the field of electrocatalysis.
7. A catalyst, characterized by: the catalyst comprises the carbon-platinum cobalt composite material as defined in claim 1 or the carbon-platinum cobalt composite material prepared by the method as defined in any one of claims 2 to 5.
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| CN202011114897.2A CN114367670A (en) | 2020-10-16 | 2020-10-16 | Carbon-platinum-cobalt composite material and preparation method thereof |
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| CN202011114897.2A CN114367670A (en) | 2020-10-16 | 2020-10-16 | Carbon-platinum-cobalt composite material and preparation method thereof |
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| CN115602862A (en) * | 2022-10-24 | 2023-01-13 | 同济大学（Cn） | Low-platinum catalyst with high electrocatalytic activity and preparation method and application thereof |
| CN115602862B (en) * | 2022-10-24 | 2024-03-26 | 同济大学 | Low-platinum catalyst with high electrocatalytic activity and preparation method and application thereof |
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