CN111468121A - Preparation and application of MXene modified biomass carbon nano metal catalyst - Google Patents
Preparation and application of MXene modified biomass carbon nano metal catalyst Download PDFInfo
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- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
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- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/38—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D307/40—Radicals substituted by oxygen atoms
- C07D307/42—Singly bound oxygen atoms
- C07D307/44—Furfuryl alcohol
Abstract
The invention relates to preparation and application of an MXene modified biomass carbon nano metal catalyst, and belongs to the technical field of catalyst synthesis. The metal active components in the catalyst are metal nickel, cobalt, molybdenum, iron and tungsten, the carrier is graphite carbon and graphene, and the modifier is multilayer MXene. The preparation method comprises the following steps: adding multiple layers of MXene and single-layer graphene into water for ultrasonic treatment to obtain MXene/graphene suspension; dissolving sodium carboxymethylcellulose in water, stirring, adding metal salt solution, and performing ultrasonic treatment; mixing MXene/graphene suspension with the solution, performing ultrasonic treatment, freezing, and performing freeze drying to obtain a catalyst precursor; calcining the obtained precursor in a nitrogen atmosphere, and reducing in a hydrogen/nitrogen mixed gas atmosphere to obtain the MXene modified biomass nano metal catalyst. The catalyst synthesis method has the advantages of cheap raw materials, stable structure and performance and high active component content. The catalyst can be used for hydrogenation reaction of bio-oil model compounds, and has extremely high catalytic efficiency and stability.
Description
Technical Field
The invention relates to preparation and application of an MXene modified biomass carbon nano metal catalyst, and belongs to the technical field of catalyst synthesis.
Background
Since the industrial revolution, the search for renewable alternative energy has become a major issue related to human fate due to the limited reserves, non-renewable properties of fossil energy, and environmental pollution caused by burning. As a natural renewable resource, biomass energy is a research hotspot of contemporary researchers due to the advantages of low price, wide distribution, rich reserves, cyclic renewable property, low sulfur content and the like. At present, biomass is cracked into bio-oil, and then the bio-oil is converted into hydrocarbon fuel which can be directly used through upgrading and upgrading means, so that the biomass energy is an important utilization mode. For the upgrading process of the bio-oil, the upgrading process of the real bio-oil is gradually expanded to the upgrading process of the real bio-oil by a mode of catalyzing and converting model compounds (phenol, furfural, guaiacol and the like) by synthesizing efficient catalysts. He et al used zirconium dioxide loaded noble metal rhodium as a catalyst to catalytically convert guaiacol at 300 deg.C and 7MPa, and after 4h reaction, 100% conversion and 70% selectivity (to cyclohexane) were obtained [1 ]. However, the reaction conditions of the reaction are too harsh to realize industrial production. Chinese patent CN 107812523A discloses a catalyst for catalyzing bio-oil model compounds to prepare aromatic hydrocarbons, which takes CoAl hydrotalcite-like oxides as a carrier, and is used for catalytic reaction of model compounds such as p-phenol, anisole and the like after molybdenum disulfide is loaded by a hydration method. When the catalyst is used for the catalytic reaction of phenol, the conversion rate of phenol is 96.5%, and the selectivity of cyclohexanone reaches 94%. However, the catalyst needs to be roasted at high temperature in the preparation process, so that the sulfur element inevitably causes certain environmental pollution and increases the environmental protection cost. Therefore, it is a very urgent task to design and develop non-noble metal, non-sulfided catalysts for the catalytic conversion of bio-oil model compounds.
In recent years, MXene, a novel two-dimensional nanomaterial with a graphene-like structure, has attracted much attention. MXene is obtained by removing element A in MAX phase with binary metal carbide MAX phase (M represents transition metal element such as Ti, V, Cr, Mo, Nb, etc., A represents Al or Si element, and X represents C element) as precursor, and hydrofluoric acid or mixed solution of hydrochloric acid and lithium fluoride as etchant. MXene has the characteristics of good chemical stability, large specific surface area and the like, and abundant functional groups on the surface of MXene can be used as anchor points of active metal components.
Aiming at the problems existing at present, the invention develops an MXene (titanium aluminum carbide) modified biomass carbon nano metal catalyst for catalytic conversion of a bio-oil model compound.
Disclosure of Invention
The invention provides preparation and application of an MXene modified biomass carbon nano metal catalyst, which comprises the steps of taking a biomass derivative and graphene (GO for short) as a carrier, taking metal salt as an active center, taking MXene (aluminum titanium carbide) as a modifier, uniformly mixing, freezing by using liquid nitrogen, carrying out freeze drying at a low temperature to obtain a catalyst precursor, finally calcining in a nitrogen atmosphere, and reducing in a nitrogen and hydrogen mixed gas atmosphere to obtain the MXene modified biomass carbon nano metal catalyst. The catalyst can be used in hydrogenation reaction of partial bio-oil model compounds to finally obtain hydrogenation products. On one hand, the MXene modified biomass carbon nano metal catalyst has cheap raw materials and simple, convenient and efficient production process; on the other hand, the MXene modified biomass carbon nano metal catalyst can adjust the structural parameters such as the porosity of the catalyst and the like by changing the using amounts of metal salt, sodium carboxymethyl cellulose and the modifier MXene, has good selectivity for the hydrogenation reaction of the bio-oil model compound, and improves the conversion rate. In addition, the catalyst is not added with a sulfur-containing component and a noble metal component in the preparation process, so that the environmental maintenance cost and the preparation cost are greatly reduced.
The invention provides a preparation method of an MXene modified biomass carbon nano metal catalyst, which comprises the following steps:
the method comprises the following steps: dispersing the multiple layers of MXene and the single layer of graphene oxide in water according to a ratio of 4:1, and performing ultrasonic treatment for 10-30 min at room temperature; dissolving sodium carboxymethylcellulose in water, stirring uniformly, adding metal salt, and performing ultrasonic treatment for 10-30 min at room temperature, wherein the mass concentration of MXene and graphene suspension is 0.1-5%, the mass concentration of the sodium carboxymethylcellulose solution is 1-5%, and the mass fraction of the metal salt is 0.1-10%;
step two: mixing the suspension obtained in the first step with the solution, performing ultrasonic treatment at room temperature for 10-30 min, and then freezing in liquid nitrogen for 0.5-2 min; freezing and drying the liquid mixture frozen by the liquid nitrogen at the temperature of-15-10 ℃ to obtain MXene/GO/biochar catalyst precursor;
step three: and (2) placing the MXene/GO/biochar catalyst precursor into a sintering furnace, calcining for 1-5 h at the temperature of 250-600 ℃ at the flow rate of 15-50 ml/min of nitrogen, reducing the cooled MXene/GO/biochar catalyst precursor for 0.5-5 h at the temperature of 150-450 ℃ at the flow rate of 30-100 ml/min of hydrogen/nitrogen mixed gas (hydrogen: nitrogen: 1:9), and cooling to obtain the MXene modified biomass carbon nano metal catalyst.
The metal salt in the first step comprises one of nickel nitrate, cobalt nitrate, ferric nitrate, ammonium molybdate, ammonium tungstate, ammonium metatungstate and phosphotungstic acid.
In the third step, the heating rate in the calcining process in the nitrogen atmosphere is 1-10 ℃/min; in the third step, the heating rate in the reduction process of the hydrogen/nitrogen mixed atmosphere is 1-10 ℃/min.
The MXene modified biomass carbon nano metal catalyst can be used for preparing a hydrogenation product of a bio-oil model compound, and the specific steps of the MXene modified biomass carbon nano metal catalyst comprise: placing the MXene modified biomass carbon nano metal catalyst into a reaction kettle, adding 1-10 ml of a biological oil model compound solution containing n-tetradecane (internal standard substance), and reacting for 0.5-3 h under the conditions of temperature of 70-150 ℃, hydrogen partial pressure of 0.5-3 MPa and stirring at 200-500 r/min to finally obtain a hydrogenation product of the biological oil model compound.
The MXene modified biomass carbon nano metal catalyst can be used for preparing a hydrogenation product of a bio-oil model compound, and the dosage of the MXene modified biomass carbon nano metal catalyst is 5-30 mg; the solvent of phenol is one of n-heptane, n-hexane and ethanol; the bio-oil model compound is one of furfural, phenol and vanillin; the concentration of the bio-oil model compound solution is 0.5-10 mg/ml.
The invention has the advantages that:
1. the invention provides an MXene modified biomass carbon nano metal catalyst, which innovatively uses MXene as a modifier, and the proportion of mesopores is adjusted by changing the material proportion of MXene and metal salt, so that the distribution position of active sites is flexibly changed, and the catalytic activity and the applicability of the catalyst are obviously improved.
2. The MXene modified biomass carbon nano metal catalyst provided by the invention uses cheap biomass material sodium carboxymethyl cellulose as a carbon-based carrier, so that the preparation cost of the catalyst is remarkably reduced, and sulfur element and precious metal are not added in the catalytic hydrogenation process, so that pollutants generated by catalytic reaction are avoided, and the environmental protection cost and the preparation cost are reduced.
Drawings
FIG. 1: the invention provides a preparation method and an application flow chart of an MXene modified biomass carbon nano metal catalyst.
FIG. 2: scanning electron microscope photos of the MXene modified biomass carbon nano metal catalyst synthesized in example 1.
FIG. 3: the catalytic effect diagram of the MXene modified biomass carbon nano metal catalyst synthesized in the example 1 is shown.
FIG. 4: XRD detection pattern of MXene modified biomass carbon nano metal catalyst synthesized in example 1.
Detailed Description
The technical features of the present invention will be described in detail below with reference to the accompanying drawings and specific embodiments, as shown in fig. 1.
Example 1:
the invention designs preparation and application of an MXene modified biomass carbon nano metal catalyst, which specifically comprises the following steps:
the method comprises the following steps: dispersing the multilayer MXene and the single-layer graphene oxide in water according to the ratio of 4:1, and performing ultrasonic treatment for 30min at room temperature; dissolving sodium carboxymethylcellulose in water, stirring uniformly, adding nickel nitrate, and performing ultrasound treatment at room temperature for 30min, wherein the mass concentration of MXene and graphene suspension is 1%, the mass concentration of the sodium carboxymethylcellulose solution is 5%, and the mass fraction of nickel nitrate is 10%;
step two: mixing the suspension and the solution obtained in the first step, performing ultrasonic treatment at room temperature for 30min, and freezing in liquid nitrogen for 1 min; freezing and drying the mixed solution frozen by the liquid nitrogen at the temperature of-10 ℃ to obtain MXene/GO/biochar catalyst precursor;
step three: placing the MXene/GO/biochar catalyst precursor into a sintering furnace at a nitrogen flow rate of 25ml/min and a temperature of 500 ℃ (V)Rate of temperature rise3 ℃/min), the cooled catalyst is calcined for 3h at the flow rate of 100ml/min in a hydrogen/nitrogen mixed gas (hydrogen: nitrogen: 1:9) and the temperature of 300 ℃ (V)Rate of temperature riseReducing for 1h under the condition of 5 ℃/min), and cooling to obtain the MXene modified biomass carbon nano metal catalyst.
The MXene modified biomass carbon nano metal catalyst can be used for preparing a hydrogenation product of a bio-oil model compound, and the specific steps of the MXene modified biomass carbon nano metal catalyst comprise: placing MXene modified biomass carbon nano metal catalyst into a reaction kettle, adding 10ml of phenol solution containing n-tetradecane (internal standard substance), and reacting for 1h under the conditions of 100 ℃ temperature, 1MPa of hydrogen partial pressure and 300r/min stirring to finally obtain cyclohexanol.
Wherein the phenol solution is dissolved in n-heptane, the concentration of the phenol solution is 1mg/ml, the dosage of the MXene modified biomass carbon nano metal catalyst is 5mg, the conversion rate of the phenol is 98.94%, and the selectivity of the cyclohexanol is 100%.
The result shows that the scanning electron microscope photo of the MXene modified biomass carbon nano metal catalyst in the attached figure 2 shows that: the MXene/GO/biochar catalyst is in an amorphous state and has high dispersity and a multi-level structure, so that the substrate and the active site of the catalyst have more sufficient contact conditions.
In the specific implementation process, besides preparing MXene/GO/biochar catalyst, biomass carbon catalyst, MXene/biomass carbon catalyst and GO/biomass carbon catalyst are prepared respectively and are used for catalytic reaction of phenol respectively, so as to compare the influence of MXene and GO on the performance of catalyst. The preparation steps of the three catalysts are basically the same as those described in example 1, and the differences are that MXene and GO do not need to be added in the preparation process of the biomass carbon catalyst, GO does not need to be added in the preparation process of the MXene/biomass carbon catalyst, and MXene does not need to be added in the preparation process of the GO/biomass carbon catalyst.
The four catalysts are respectively applied to the hydrogenation catalysis process of phenol, and the conversion result is shown in figure 3. As shown in the attached figure 3, the MXene modified biomass carbon nano metal catalyst has the optimal performance, has the highest conversion rate of 98.94% on phenol and has 100% selectivity on cyclohexanol. As can be seen from the attached FIG. 4, after MXene and GO are added, a sharp active metal crystal peak appears in the MXene/GO/biochar catalyst.
Example 2:
the invention designs preparation and application of an MXene modified biomass carbon nano metal catalyst, which specifically comprises the following steps:
the method comprises the following steps: dispersing the multilayer MXene and the single-layer graphene oxide in water according to the ratio of 4:1, and performing ultrasonic treatment for 30min at room temperature; dissolving sodium carboxymethylcellulose in water, stirring uniformly, adding cobalt nitrate, and performing ultrasound at room temperature for 20min, wherein the mass concentration of MXene and graphene suspension is 3%, the mass concentration of the sodium carboxymethylcellulose solution is 3%, and the mass fraction of metal salt is 7%;
step two: mixing the suspension and the solution obtained in the first step, performing ultrasonic treatment at room temperature for 20min, and freezing in liquid nitrogen for 1 min; freezing and drying the mixed solution frozen by the liquid nitrogen at the temperature of-10 ℃ to obtain MXene/GO/biochar catalyst precursor;
step three: placing the MXene/GO/biochar catalyst precursor into a sintering furnace at a nitrogen flow rate of 50ml/min and a temperature of 450 ℃ (V)Rate of temperature rise3 ℃/min) for 2h, cooling the catalyst, and reacting in a hydrogen/nitrogen mixed gas (hydrogen: nitrogen: 1:9) at a flow rate of 100ml/min and a temperature ofDegree of 350 ℃ (V)Rate of temperature riseReducing for 1h under the condition of 5 ℃/min), and cooling to obtain the MXene modified biomass carbon nano metal catalyst.
The MXene modified biomass carbon nano metal catalyst can be used for preparing a hydrogenation product of a bio-oil model compound, and the specific steps of the MXene modified biomass carbon nano metal catalyst comprise: placing the MXene modified biomass carbon nano metal catalyst into a reaction kettle, adding 10ml of n-tetradecane (internal standard substance) vanillin-containing solution, and reacting for 1h under the conditions of temperature of 150 ℃, hydrogen partial pressure of 0.5MPa and stirring at 300r/min to finally obtain a hydrogenation product.
Wherein the dissolving of the vanillin solution is normal hexane, the concentration of the vanillin solution is 2.5mg/ml, the dosage of the MXene modified biomass carbon nano metal catalyst is 5mg, the conversion rate of the vanillin is 84.4%, and the selectivity of the vanillyl alcohol is 70.8%.
Example 3:
the invention designs preparation and application of an MXene modified biomass carbon nano metal catalyst, which specifically comprises the following steps:
the method comprises the following steps: dispersing the multilayer MXene and the single-layer graphene oxide in water according to the ratio of 4:1, and performing ultrasonic treatment for 30min at room temperature; dissolving sodium carboxymethylcellulose in water, stirring uniformly, adding ammonium molybdate, and performing ultrasound at room temperature for 20min, wherein the mass concentration of MXene and graphene suspension is 3%, the mass concentration of the sodium carboxymethylcellulose solution is 3%, and the mass fraction of metal salt is 5%;
step two: mixing the suspension and the solution obtained in the first step, performing ultrasonic treatment at room temperature for 20min, and freezing in liquid nitrogen for 1 min; freezing and drying the mixed solution frozen by the liquid nitrogen at the temperature of-10 ℃ to obtain MXene/GO/biochar catalyst precursor;
step three: placing the MXene/GO/biochar catalyst precursor into a sintering furnace at a nitrogen flow rate of 50ml/min and a temperature of 500 ℃ (V)Rate of temperature rise3 ℃/min) for 1.5h, and the cooled catalyst is calcined under the condition of hydrogen/nitrogen mixed gas (hydrogen: nitrogen: 1:9) flow rate of 100ml/min and temperature of 350 ℃ (V)Rate of temperature riseReducing for 1.5h under the condition of 5 ℃/min), and cooling to obtain MXene modified biomass carbon nanoA metal catalyst.
The MXene modified biomass carbon nano metal catalyst can be used for preparing a hydrogenation product of a bio-oil model compound, and the specific steps of the MXene modified biomass carbon nano metal catalyst comprise: placing the MXene modified biomass carbon nano metal catalyst into a reaction kettle, adding 10ml of furfural solution containing n-tetradecane (internal standard substance), and reacting for 1h under the conditions of 100 ℃ temperature, 1MPa of hydrogen partial pressure and 300r/min stirring to finally obtain furfuryl alcohol.
Wherein the furfural solution is dissolved by ethanol, the concentration of the furfural solution is 1mg/ml, the dosage of the MXene modified biomass carbon nano metal catalyst is 10mg, the conversion rate of the furfural is 90.97%, and the selectivity of furfuryl alcohol is 100%.
The numbers in [ ] in the present invention are respectively expressed correspondingly as the following references. The entire contents of these documents are incorporated herein in their entirety as part of the present specification.
1.He,Y.F.,et al.,Hydrodeoxygenation of guaiacol as a model compoundof lignin-derived pyrolysis bio-oil over zirconia-supported Rh catalyst:Process optimization and reaction kinetics.Fuel,2019.239:p.1015-1027.
Claims (9)
1. The preparation method of the MXene modified biomass carbon nano metal catalyst comprises the following steps;
the method comprises the following steps: dispersing the multiple layers of MXene and the single layer of graphene oxide in water according to a ratio of 4:1, and performing ultrasonic treatment for 10-30 min at room temperature; dissolving sodium carboxymethylcellulose in water, stirring uniformly, adding metal salt, and performing ultrasonic treatment for 10-30 min at room temperature, wherein the mass concentration of MXene and graphene suspension is 0.1-5%, the mass concentration of the sodium carboxymethylcellulose solution is 1-5%, and the mass fraction of the metal salt is 0.1-10%;
step two: mixing the suspension obtained in the first step with the solution, performing ultrasonic treatment at room temperature for 10-30 min, and then freezing in liquid nitrogen for 0.5-2 min; freezing and drying the liquid mixture frozen by the liquid nitrogen at the temperature of-15-10 ℃ to obtain MXene/GO/biochar catalyst precursor;
step three: and (2) placing the MXene/GO/biochar catalyst precursor into a sintering furnace, calcining for 1-5 h at the nitrogen flow rate of 15-50 ml/min and the temperature of 250-600 ℃, reducing the cooled catalyst for 0.5-5 h at the hydrogen/nitrogen mixed gas (hydrogen: nitrogen is 1:9) flow rate of 30-100 ml/min and the temperature of 150-450 ℃, and cooling to obtain the MXene modified biomass carbon nano metal catalyst.
2. The preparation method of the MXene modified biomass carbon nano-metal catalyst according to claim 1, wherein the preparation method comprises the following steps: the metal salt in the first step comprises one of nickel nitrate, cobalt nitrate, ferric nitrate, ammonium molybdate, ammonium tungstate, ammonium metatungstate and phosphotungstic acid.
3. The preparation method of the MXene modified biomass carbon nano-metal catalyst according to claim 1, wherein the preparation method comprises the following steps: and in the third step, the heating rate in the calcining process in the nitrogen atmosphere is 1-10 ℃/min.
4. The preparation method of the MXene modified biomass carbon nano-metal catalyst according to claim 1, wherein the preparation method comprises the following steps: in the third step, the heating rate in the reduction process of the hydrogen/nitrogen mixed atmosphere is 1-10 ℃/min.
5. The MXene modified biomass carbon nanometal catalyst according to claim 1 can be used for preparing hydrogenation products of bio-oil model compounds, and the specific steps comprise: placing the MXene modified biomass carbon nano metal catalyst into a reaction kettle, adding 1-10 ml of a biological oil model compound solution containing n-tetradecane (internal standard substance), and reacting for 0.5-3 h under the conditions of temperature of 70-150 ℃, hydrogen partial pressure of 0.5-3 MPa and stirring at 200-500 r/min to finally obtain a hydrogenation product.
6. The MXene modified biomass carbon nano-metal catalyst in claim 5 can be used for preparing hydrogenation products of bio-oil model compounds, and is characterized in that: the dosage of the MXene modified biomass carbon nano metal catalyst is 5-30 mg.
7. The MXene modified biomass carbon nano-metal catalyst in claim 5 can be used for preparing hydrogenation products of bio-oil model compounds, and is characterized in that: the solvent of phenol is one of n-heptane, n-hexane and ethanol.
8. The MXene modified biomass carbon nano-metal catalyst in claim 5 can be used for preparing hydrogenation products of bio-oil model compounds, and is characterized in that: the bio-oil model compound is one of furfural, phenol and vanillin.
9. The MXene modified biomass carbon nano-metal catalyst in claim 5 can be used for preparing hydrogenation products of bio-oil model compounds, and is characterized in that: the concentration of the bio-oil model compound solution is 5-50 mg/ml.
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| CN113457701A (en) * | 2021-06-08 | 2021-10-01 | 西安交通大学 | MXene-based catalyst and preparation method and application thereof |
| CN113877614A (en) * | 2021-10-27 | 2022-01-04 | 北京石墨烯技术研究院有限公司 | Modified graphene roll and preparation method and application thereof |
| CN115286898A (en) * | 2022-08-26 | 2022-11-04 | 北京航空航天大学 | Preparation method of imitated nacreous layer MXene/epoxy nano composite material |
| CN115286898B (en) * | 2022-08-26 | 2023-07-21 | 北京航空航天大学 | Preparation method of pearl layer-like MXene/epoxy nanocomposite |
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