CN113457701A - MXene-based catalyst and preparation method and application thereof - Google Patents
MXene-based catalyst and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
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- 239000006185 dispersion Substances 0.000 claims abstract description 95
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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
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- 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
-
- B01J35/61—
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
Abstract
The invention provides an MXene-based catalyst and a preparation method and application thereof, wherein the MXene-based catalyst comprises MXene and graphene oxide, and the mass ratio of the MXene to the graphene oxide is (0.5-5): 1. adding the graphene oxide dispersion liquid into the MXene dispersion liquid, uniformly mixing to obtain a mixed liquid A, and freeze-drying the mixed liquid A to obtain the MXene-based catalyst. The catalyst has good selectivity for the generation of levoglucosan, and can overcome the problems of poor selectivity, equipment corrosion, difficult recovery, environmental pollution and the like of the existing catalyst.
Description
Technical Field
The invention relates to the field of levoglucosan preparation, and particularly relates to an MXene-based catalyst and a preparation method and application thereof.
Background
The fast pyrolysis technology is one of the important ways for biomass energy utilization, and can convert biomass into bio-oil containing various high value-added chemicals rapidly and efficiently. However, the content of biomass components (i.e., cellulose, hemicellulose, and lignin) can significantly affect the distribution of chemicals in the bio-oil. The introduction of suitable catalysts is an effective means of increasing the yield of the target chemical in the bio-oil. Levoglucosan (Levoglucosan, LG, 1, 6-anhydro- β -D-glucopyranose) is an important chemical in bio-oil and has been identified by the united states department of energy (US DoE) as one of the most potential "sugar-based biorieffenery" chemicals. The levoglucosan can be metabolized by microorganisms, so that the levoglucosan can be used as an important raw material for producing biodegradable materials, such as plastics, resins and other related products. The conventional method for promoting the thermal conversion of biomass into levoglucosan mainly comprises raw material pretreatment and a method for loading a liquid acid catalyst, wherein the pretreatment method has the defects of high cost, large energy consumption, complex process and the like, and the loaded liquid acid catalyst can further dehydrate the levoglucosan to generate a byproduct levoglucosan ketone along with the increase of acid amount. Meanwhile, the liquid acid can corrode equipment and is difficult to recycle, and the strong volatility of the liquid acid can cause certain environmental pollution. Therefore, the search for a novel, efficient and green catalyst to realize the large-scale production of levoglucosan is an urgent problem to be solved at present.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an MXene-based catalyst and a preparation method and application thereof, the MXene-based catalyst has good selectivity for the generation of levoglucosan, and can overcome the problems of poor selectivity, equipment corrosion, difficult recovery, environmental pollution and the like of the existing catalyst.
The invention is realized by the following technical scheme:
an MXene-based catalyst comprises MXene and graphene oxide, wherein the mass ratio of the MXene to the graphene oxide is (0.5-5): 1.
preferably, MXene is Ti3C2Tx。
The preparation method of the MXene-based catalyst comprises the steps of adding the graphene oxide dispersion liquid into the MXene dispersion liquid, uniformly mixing to obtain a mixed liquid A, and carrying out freeze drying on the mixed liquid A to obtain the MXene-based catalyst.
Preferably, the concentration of the MXene dispersion liquid is 0.5-10mg/mL, and the concentration of the graphene oxide dispersion liquid is 0.5-10 mg/mL.
Preferably, the freeze-drying time is 20-100 h.
Preferably, the preparation method of the MXene dispersion liquid comprises the following steps:
step 1, dispersing lithium fluoride in hydrochloric acid, and stirring to obtain a mixed solution B;
step 2, MXene (Ti)3C2Tx) MAX (Ti) precursor of (2)3AlC2) Slowly adding the phases into the mixed solution B, and stirring and reacting at 25-70 ℃ to obtain a mixed solution C;
and 3, washing the precipitate after the centrifugation of the mixed solution C until the pH value of the supernatant is neutral, then diluting the obtained substrate with water or ethanol, performing ultrasonic treatment, centrifuging the liquid after the ultrasonic treatment, and taking the supernatant to obtain MXene dispersion liquid.
Further, the concentration of the hydrochloric acid is 6-12M, and the mass volume ratio of the lithium fluoride to the hydrochloric acid is (1-4) g: (30-60) mL; the mass-volume ratio of the MAX to the mixed solution B is (1-10) g (20-80) mL.
The MXene-based catalyst is applied to preparation of levoglucosan by catalytic biomass pyrolysis.
Preferably, biomass is used as a raw material, the MXene-based catalyst of any one of claims 1 or 2 is used as a catalyst, the pyrolysis reaction is carried out for 8-12s at the temperature of 400 ℃ and 600 ℃, and the liquid product is collected.
Preferably, the biomass is populus tomentosa, cotton straw and corn straw.
Compared with the prior art, the invention has the following beneficial technical effects:
MXene is a new type of two-dimensional transition metal carbide/nitride or carbonitride, available in the general formula Mn+ 1XnTxWherein M represents a transition metal, X represents C or N, TxThen represents MXene functional group-OH, ═ O, and-F). The invention constructs a heterostructure based on graphene oxide and MXene. In the heterostructure, electrons between the two can change electron distribution due to interaction, and further influence the electronic structure of a reaction site-OH, so that-OH reaction activity is enhanced. When the catalyst is used for catalyzing biomass pyrolysis, cellulose in biomass macromolecules and-OH functional groups in the MXene-based catalyst form a six-membered ring with a low energy barrier through-H proton transfer, so that the MXene-based catalyst has good selectivity for the generation of levoglucosan. MXene is a potentially recyclable and high-performance thermochemical catalyst due to its good hydrophilicity, high thermal stability, large specific surface area and easy large-scale preparation.
The invention introduces MXene-based catalyst into the field of thermal catalysis for preparing levoglucosan with high selectivity for the first time, and can overcome the problems of poor selectivity, equipment corrosion, difficult recovery, environmental pollution and the like of the existing catalyst.
Drawings
FIG. 1 is a Raman spectrum of the present invention.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
The MXene-based catalyst comprises MXene and graphene oxide, wherein the mass ratio of the MXene to the graphene oxide is (0.5-5): 1, MXene is preferably Ti3C2Tx。
The preparation method of the MXene-based catalyst comprises the following steps:
adding graphene oxide dispersion liquid into MXene dispersion liquid, uniformly mixing to obtain mixed liquid A, and freeze-drying the mixed liquid A for 20-100h to obtain the MXene-based catalyst with high selectivity.
The concentration of the MXene dispersion liquid is 0.5-10mg/mL, the concentration of the graphene oxide dispersion liquid is 0.5-10mg/mL, and the volume ratio of the MXene dispersion liquid to the graphene oxide dispersion liquid is (1-10): 1. the graphene oxide dispersion liquid is a common single-layer graphene oxide dispersion liquid.
The preparation method of the MXene dispersion liquid comprises the following steps:
step 1, dispersing lithium fluoride in hydrochloric acid, and fully stirring for 1-10min at 25-70 ℃ by using a magnetic stirrer at 200-2400rpm to obtain a mixed solution B; the concentration of the hydrochloric acid is 6-12M, and the mass volume ratio of the lithium fluoride to the hydrochloric acid is (1-4) g: (30-60) mL.
Step 2, MAX (preferably Ti)3AlC2) Slowly adding the phase into the mixed solution B, and magnetically stirring and reacting at the temperature of between 25 and 70 ℃ and 2000rpm for 0.5 to 48 hours to obtain a mixed solution C; the mass-volume ratio of the MAX to the mixed solution B is (1-10) g (20-80) mL.
And 3, repeatedly centrifuging and cleaning the precipitate after the mixed solution C is centrifuged by using distilled water until the pH value of the supernatant is neutral, then diluting the obtained substrate by using water or ethanol, carrying out ultrasonic treatment for 5-60min at the power of 200-.
Example 1:
MXene(Ti3C2Tx) A method of preparing a dispersion comprising the steps of:
step 1: adding 40mL of 9M hydrochloric acid into a plastic bottle, then dispersing 3.2g of lithium fluoride into the hydrochloric acid, and fully stirring the mixture for 5min at room temperature by using a magnetic stirrer at the speed of 1000rpm to obtain a mixed solution B;
step 2: mixing MAX (Ti)3AlC2) Gradually and slowly adding the phases into the mixed solution B, and then magnetically stirring and reacting at the speed of 1000rpm at 35 ℃ for 36 hours to obtain mixed solution C; the volume mass ratio of the MAX to the mixed liquid B is 2g:40 mL;
and step 3: and (3) repeatedly centrifuging and cleaning the precipitate obtained after the mixed solution C is centrifuged by using distilled water until the pH value of the supernatant is neutral, then adding 100mL of water into the obtained substrate for dilution, carrying out ultrasonic treatment in a nitrogen ice bath environment for 30min under the power of 200W, and finally centrifuging the diluted solution at the rotating speed of 4000r/min for 10min to obtain the supernatant, thus obtaining the MXene dispersion liquid. And (3) taking 5mL of the MXene dispersion liquid for suction filtration, tearing off the prepared MXene film, weighing to calculate the concentration of the dispersion liquid, and adding water to adjust the concentration of the MXene dispersion liquid to 1.2 mg/mL.
The preparation method of the MXene-based catalyst comprises the following steps:
step 1: taking 25mL of MXene dispersion liquid with the concentration of 1.2mg/mL, and mechanically stirring for 2 min;
step 2: dissolving 60mg of graphene oxide in 20mL of water, and mechanically stirring for 5 min;
and step 3: mixing the solutions prepared in the step 1 and the step 2 in proportion, and mechanically stirring for 3min to form a uniform mixed solution A with the mass ratio of MXene to graphene oxide being 1: 2;
and 4, step 4: freeze-drying the mixed solution A for 72h to obtain the MXene-based catalyst with high selectivity;
and 5: the method takes populus tomentosa as a raw material, adopts the catalyst of the invention to carry out pyrolysis reaction for 10s at 500 ℃, and collects a liquid product.
Example 2:
MXene(Ti3C2Tx) A method of preparing a dispersion comprising the steps of:
step 1: adding 40mL of 9M hydrochloric acid into a plastic bottle, then dispersing 3.2g of lithium fluoride into the hydrochloric acid, and fully stirring for 5min at room temperature at the speed of 200rpm by using a magnetic stirrer to obtain a mixed solution B;
step 2: mixing MAX (Ti)3AlC2) Gradually and slowly adding the phases into the mixed solution B, and then magnetically stirring and reacting at the speed of 300rpm at 35 ℃ for 36 hours to obtain mixed solution C; the volume mass ratio of the MAX to the mixed liquid B is 2g:40 mL;
and step 3: and (3) repeatedly centrifuging and cleaning the precipitate obtained after the mixed solution C is centrifuged by using distilled water until the pH value is neutral, then adding 100mL of water into the obtained product for dilution, carrying out ultrasonic treatment in a nitrogen ice bath environment for 5min under 1200W of power, and finally centrifuging the diluted solution at the rotating speed of 4000r/min for 10min to obtain a supernatant, thus obtaining the MXene dispersion liquid. And (3) taking 5mL of the MXene dispersion liquid for suction filtration, tearing off the prepared MXene film, weighing to calculate the concentration of the dispersion liquid, and adding water to adjust the concentration of the MXene dispersion liquid to 6 mg/mL.
The preparation method of the MXene-based catalyst comprises the following steps:
step 1: taking 10mL of MXene dispersion liquid with the concentration of 6mg/mL, and mechanically stirring for 3 min;
step 2: dissolving 30mg of graphene oxide in 10mL of water, and mechanically stirring for 4 min;
and step 3: mixing the solutions prepared in the step 1 and the step 2 in proportion, and mechanically stirring for 4min to form a uniform mixed solution A with the mass ratio of MXene to graphene oxide being 2: 1;
and 4, step 4: carrying out freeze drying on the mixed solution A for 48 hours to obtain the MXene-based catalyst with high selectivity;
and 5: the cotton straw is used as a raw material, the catalyst is adopted to carry out pyrolysis reaction for 8s at 550 ℃, and a liquid product is collected.
Example 3:
MXene(Ti3C2Tx) A method of preparing a dispersion comprising the steps of:
step 1: adding 40mL of 9M hydrochloric acid into a plastic bottle, then dispersing 3.2g of lithium fluoride into the hydrochloric acid, and fully stirring at room temperature for 5min by using a magnetic stirrer at the speed of 2400rpm to obtain a mixed solution B;
step 2: mixing MAX (Ti)3AlC2) Gradually and slowly adding the phases into the mixed solution B, and then magnetically stirring and reacting at the temperature of 35 ℃ at the speed of 2000rpm for 36 hours to obtain mixed solution C; the volume mass ratio of the MAX to the mixed liquid B is 2g:40 mL;
and step 3: and (3) repeatedly centrifuging and cleaning the precipitate obtained after the mixed solution C is centrifuged by using distilled water until the pH value of the supernatant is neutral, then adding 100mL of water into the obtained substrate for dilution, carrying out ultrasonic treatment in a nitrogen ice bath environment for 30min under the power of 500W, and finally centrifuging the diluted solution at the rotating speed of 4000r/min for 10min to obtain the supernatant, thus obtaining the MXene dispersion liquid. And (3) taking 5mL of the MXene dispersion liquid for suction filtration, tearing off the prepared MXene film, weighing to calculate the concentration of the dispersion liquid, and adding water to adjust the concentration of the MXene dispersion liquid to 0.5 mg/mL.
The preparation method of the MXene-based catalyst comprises the following steps:
step 1: 40mL of MXene dispersion with the concentration of 0.5mg/mL, and mechanically stirring for 5 min;
step 2: dissolving 20mg of graphene oxide in 20mL of water, and mechanically stirring for 6 min;
and step 3: mixing the solutions prepared in the step 1 and the step 2 in proportion, and mechanically stirring for 5min to form a uniform mixed solution A with the mass ratio of MXene to graphene oxide being 1: 1;
and 4, step 4: freeze-drying the mixed solution A for 96h to obtain the MXene-based catalyst with high selectivity;
and 5: the method takes corn straws as raw materials, adopts the catalyst of the invention to carry out pyrolysis reaction for 12s at 400 ℃, and collects liquid products.
Example 4:
MXene(Ti3C2Tx) A method of preparing a dispersion comprising the steps of:
step 1: adding 60mL of 6M hydrochloric acid into a plastic bottle, then dispersing 4g of lithium fluoride into the hydrochloric acid, and fully stirring for 1min at 60 ℃ by using a magnetic stirrer at the speed of 2400rpm to obtain a mixed solution B;
step 2: mixing MAX (Ti)3AlC2) Gradually and slowly adding the phases into the mixed solution B, and then magnetically stirring and reacting at the temperature of 70 ℃ at the speed of 300rpm for 48 hours to obtain mixed solution C; the volume mass ratio of the MAX to the mixed liquid B is 1g:80 mL;
and step 3: and (3) repeatedly centrifuging and cleaning the precipitate obtained after the mixed solution C is centrifuged by using distilled water until the pH value of the supernatant is neutral, then adding 100mL of ethanol into the obtained substrate for dilution, carrying out ultrasonic treatment in a nitrogen ice bath environment for 60min under 800W of power, and finally centrifuging the diluted solution for 60min at 2000r/min to obtain the supernatant, thus obtaining the MXene dispersion liquid. And (3) taking 5mL of the MXene dispersion liquid for suction filtration, tearing off the prepared MXene film, weighing to calculate the concentration of the dispersion liquid, and adding water to adjust the concentration of the MXene dispersion liquid to 3 mg/mL.
The preparation method of the MXene-based catalyst comprises the following steps:
step 1: 100mL of MXene dispersion with the concentration of 3mg/mL, and mechanically stirring for 10 min;
step 2: dissolving 100mg of graphene oxide in 10mL of water, and mechanically stirring for 5 min;
and step 3: mixing the solutions prepared in the step 1 and the step 2 in proportion, and mechanically stirring for 8min to form a uniform mixed solution A with the mass ratio of MXene to graphene oxide being 3: 1;
and 4, step 4: freeze-drying the mixed solution A for 100h to obtain the MXene-based catalyst with high selectivity;
and 5: the method takes populus tomentosa as a raw material, adopts the catalyst of the invention to carry out pyrolysis reaction for 10s at 600 ℃, and collects liquid products.
Example 5:
MXene(Ti3C2Tx) A method of preparing a dispersion comprising the steps of:
step 1: adding 30mL of 12M hydrochloric acid into a plastic bottle, then dispersing 1g of lithium fluoride into the hydrochloric acid, and fully stirring for 10min at 45 ℃ by using a magnetic stirrer at the speed of 2000rpm to obtain a mixed solution B;
step 2: mixing MAX (Ti)3AlC2) Gradually and slowly adding the phases into the mixed solution B, and then magnetically stirring and reacting at the speed of 2000rpm for 1h at the temperature of 25 ℃ to obtain a mixed solution C; the volume mass ratio of the MAX to the mixed liquid B is 10g:20 mL;
and step 3: and (3) repeatedly centrifuging and cleaning the precipitate obtained after the mixed solution C is centrifuged by using distilled water until the pH value of the supernatant is neutral, then adding 100mL of ethanol into the obtained substrate for dilution, carrying out ultrasonic treatment in a nitrogen ice bath environment for 30min under 1000W of power, and finally centrifuging the diluted solution for 30min at the rotating speed of 5000r/min to obtain the supernatant, thus obtaining the MXene dispersion liquid. And (3) taking 5mL of the MXene dispersion liquid for suction filtration, tearing off the prepared MXene film, weighing to calculate the concentration of the dispersion liquid, and adding water to adjust the concentration of the MXene dispersion liquid to 10 mg/mL.
The preparation method of the MXene-based catalyst comprises the following steps:
step 1: 20mL of MXene dispersion with the concentration of 10mg/mL, and mechanically stirring for 8 min;
step 2: dissolving 50mg of graphene oxide in 20mL of water, and mechanically stirring for 6 min;
and step 3: mixing the solutions prepared in the step 1 and the step 2 in proportion, and mechanically stirring for 8min to form a uniform mixed solution A with the mass ratio of MXene to graphene oxide being 4: 1;
and 4, step 4: freeze-drying the mixed solution A for 20h to obtain the MXene-based catalyst with high selectivity;
and 5: the cotton straw is used as a raw material, the catalyst is adopted to carry out pyrolysis reaction for 10s at the temperature of 600 ℃, and a liquid product is collected.
Example 6:
MXene(Ti3C2Tx) A method of preparing a dispersion comprising the steps of:
step 1: adding 60mL of 12M hydrochloric acid into a plastic bottle, then dispersing 1g of lithium fluoride into the hydrochloric acid, and fully stirring for 10min at 45 ℃ by using a magnetic stirrer at the speed of 2000rpm to obtain a mixed solution B;
step 2: mixing MAX (Ti)3AlC2) Gradually and slowly adding the phases into the mixed solution B, and then magnetically stirring and reacting at the speed of 2000rpm for 1h at the temperature of 25 ℃ to obtain a mixed solution C; the volume mass ratio of the MAX to the mixed liquid B is 10g:80 mL;
and step 3: and (3) repeatedly centrifuging and cleaning the precipitate obtained after the mixed solution C is centrifuged by using distilled water until the pH value of the supernatant is neutral, then adding 100mL of ethanol into the obtained substrate for dilution, carrying out ultrasonic treatment in a nitrogen ice bath environment for 30min under 1000W of power, and finally centrifuging the diluted solution for 30min at the rotating speed of 5000r/min to obtain the supernatant, thus obtaining the MXene dispersion liquid. And (3) taking 5mL of the MXene dispersion liquid for suction filtration, tearing off the prepared MXene film, weighing to calculate the concentration of the dispersion liquid, and adding water to adjust the concentration of the MXene dispersion liquid to 5 mg/mL.
The preparation method of the MXene-based catalyst comprises the following steps:
step 1: 10mL of MXene dispersion with the concentration of 5mg/mL, and mechanically stirring for 7 min;
step 2: dissolving 10mg of graphene oxide in 10mL of water, and mechanically stirring for 5 min;
and step 3: mixing the solutions prepared in the step 1 and the step 2 in proportion, and mechanically stirring for 7min to form a uniform mixed solution A with the mass ratio of MXene to graphene oxide being 5: 1;
and 4, step 4: freeze-drying the mixed solution A for 60 hours to obtain the MXene-based catalyst with high selectivity;
and 5: the method takes corn straws as raw materials, adopts the catalyst of the invention to carry out pyrolysis reaction for 8s at 450 ℃, and collects liquid products.
Comparative example 1-1:
MXene(Ti3C2Tx) A method of preparing a dispersion comprising the steps of:
step 1: adding 40mL of 9M hydrochloric acid into a plastic bottle, then dispersing 3.2g of lithium fluoride into the hydrochloric acid, and fully stirring the mixture for 5min at room temperature by using a magnetic stirrer at the speed of 1000rpm to obtain a mixed solution B;
step 2: mixing MAX (Ti)3AlC2) Gradually and slowly adding the phases into the mixed solution B, and then magnetically stirring and reacting at the speed of 1000rpm at 35 ℃ for 36 hours to obtain mixed solution C; the volume mass ratio of the MAX to the mixed liquid B is 2g:40 mL;
and step 3: and (3) repeatedly centrifuging and cleaning the precipitate obtained after the mixed solution C is centrifuged by using distilled water until the pH value of the supernatant is neutral, then adding 100mL of water into the obtained substrate for dilution, carrying out ultrasonic treatment in a nitrogen ice bath environment for 30min under the power of 200W, and finally centrifuging the diluted solution at the rotating speed of 4000r/min for 10min to obtain the supernatant, thus obtaining the MXene dispersion liquid. And (3) taking 5mL of the MXene dispersion liquid for suction filtration, tearing off the prepared MXene film, weighing to calculate the concentration of the dispersion liquid, and adding water to adjust the concentration of the MXene dispersion liquid to 1.2 mg/mL.
The pyrolysis reaction application steps of the pure MXene catalyst are as follows:
the method comprises the steps of taking populus tomentosa as a raw material, carrying out freeze drying on 25mL of pure MXene dispersion liquid with the concentration of 1.2mg/mL for 72h to obtain a catalyst with high selectivity, carrying out pyrolysis reaction for 10s at 500 ℃, and collecting a liquid product.
Comparative examples 1 to 2:
the application steps of the pure graphene oxide catalyst pyrolysis reaction are as follows:
the method comprises the steps of taking populus tomentosa as a raw material, adding 60mg of graphene oxide, carrying out freeze drying for 72h to serve as a catalyst, carrying out pyrolysis reaction for 10s at 500 ℃, and collecting a liquid product.
Comparative example 2-1:
MXene(Ti3C2Tx) A method of preparing a dispersion comprising the steps of:
step 1: adding 40mL of 9M hydrochloric acid into a plastic bottle, then dispersing 3.2g of lithium fluoride into the hydrochloric acid, and fully stirring for 5min at room temperature at the speed of 200rpm by using a magnetic stirrer to obtain a mixed solution B;
step 2: mixing MAX (Ti)3AlC2) Gradually and slowly adding the phases into the mixed solution B, and then magnetically stirring and reacting at the speed of 300rpm at 35 ℃ for 36 hours to obtain mixed solution C; the volume mass ratio of the MAX to the mixed liquid B is 2g:40 mL;
and step 3: and (3) repeatedly centrifuging and cleaning the precipitate obtained after the mixed solution C is centrifuged by using distilled water until the pH value is neutral, then adding 100mL of water into the obtained product for dilution, carrying out ultrasonic treatment in a nitrogen ice bath environment for 5min under 1200W of power, and finally centrifuging the diluted solution at the rotating speed of 4000r/min for 10min to obtain a supernatant, thus obtaining the MXene dispersion liquid. And (3) taking 5mL of the MXene dispersion liquid for suction filtration, tearing off the prepared MXene film, weighing to calculate the concentration of the dispersion liquid, and adding water to adjust the concentration of the MXene dispersion liquid to 6 mg/mL.
The pyrolysis reaction application steps of the pure MXene catalyst are as follows:
the method comprises the steps of taking cotton straws as raw materials, carrying out freeze drying on 10mL of pure MXene dispersion liquid with the concentration of 6mg/mL for 48 hours to serve as a catalyst, carrying out pyrolysis reaction for 8s at 550 ℃, and collecting liquid products.
Comparative examples 2 to 2:
the application steps of the pure graphene oxide catalytic pyrolysis reaction agent are as follows:
the method comprises the steps of taking cotton straws as raw materials, adding 30mg of graphene oxide, carrying out freeze drying for 48 hours to serve as a catalyst, carrying out pyrolysis reaction for 8s at 550 ℃, and collecting liquid products.
Comparative example 3-1:
MXene(Ti3C2Tx) A method for preparing a dispersion liquid, comprising the steps of,the method comprises the following steps:
step 1: adding 40mL of 9M hydrochloric acid into a plastic bottle, then dispersing 3.2g of lithium fluoride into the hydrochloric acid, and fully stirring at room temperature for 5min by using a magnetic stirrer at the speed of 2400rpm to obtain a mixed solution B;
step 2: mixing MAX (Ti)3AlC2) Gradually and slowly adding the phases into the mixed solution B, and then magnetically stirring and reacting at the temperature of 35 ℃ at the speed of 2000rpm for 36 hours to obtain mixed solution C; the volume mass ratio of the MAX to the mixed liquid B is 2g:40 mL;
and step 3: and (3) repeatedly centrifuging and cleaning the precipitate obtained after the mixed solution C is centrifuged by using distilled water until the pH value of the supernatant is neutral, then adding 100mL of water into the obtained substrate for dilution, carrying out ultrasonic treatment in a nitrogen ice bath environment for 30min under the power of 500W, and finally centrifuging the diluted solution at the rotating speed of 4000r/min for 10min to obtain the supernatant, thus obtaining the MXene dispersion liquid. And (3) taking 5mL of the MXene dispersion liquid for suction filtration, tearing off the prepared MXene film, weighing to calculate the concentration of the dispersion liquid, and adding water to adjust the concentration of the MXene dispersion liquid to 0.5 mg/mL.
The pyrolysis reaction application steps of the pure MXene catalyst are as follows:
taking corn straws as a raw material, carrying out freeze drying on 40mL of pure MXene dispersion liquid with the concentration of 0.5mg/mL for 96h as a catalyst, carrying out pyrolysis reaction for 12s at 400 ℃, and collecting a liquid product.
Comparative example 3-2:
the application steps of the pure graphene oxide catalytic pyrolysis reaction agent are as follows:
the method comprises the steps of taking corn straws as raw materials, adding 20mg of pure graphene oxide, freeze-drying for 96 hours to serve as a catalyst, carrying out pyrolysis reaction for 12s at 400 ℃, and collecting liquid products.
Comparative example 4-1:
the preparation method of the MXene dispersion liquid comprises the following steps:
step 1: adding 60mL of 6M hydrochloric acid into a plastic bottle, then dispersing 4g of lithium fluoride into the hydrochloric acid, and fully stirring for 1min at 60 ℃ by using a magnetic stirrer at 2400rpm to obtain a mixed solution B;
step 2: gradually and slowly adding the MAX phase into the mixed solution B, and then magnetically stirring and reacting at the temperature of 70 ℃ at the speed of 300rpm for 48 hours to obtain a mixed solution C; the volume mass ratio of the MAX to the mixed liquid B is 1g:80 mL;
and step 3: and (3) repeatedly centrifuging and cleaning the precipitate obtained after the mixed solution C is centrifuged by using distilled water until the pH value of the supernatant is neutral, then adding 100mL of ethanol into the obtained substrate for dilution, carrying out ultrasonic treatment in a nitrogen ice bath environment for 60min under 800W of power, and finally centrifuging the diluted solution for 60min at 2000r/min to obtain the supernatant, thus obtaining the MXene dispersion liquid. And (3) taking 5mL of the MXene dispersion liquid for suction filtration, tearing off the prepared MXene film, weighing to calculate the concentration of the dispersion liquid, and adding water to adjust the concentration of the MXene dispersion liquid to 3 mg/mL.
The pyrolysis reaction application steps of the pure MXene catalyst are as follows:
the method comprises the steps of taking populus tomentosa as a raw material, carrying out freeze drying on 100mL of pure MXene dispersion liquid with the concentration of 3mg/mL for 100h as a catalyst, carrying out pyrolysis reaction for 10s at 600 ℃, and collecting a liquid product.
Comparative example 4-2:
the application steps of the pure graphene oxide catalytic pyrolysis reaction agent are as follows:
the method comprises the steps of taking populus tomentosa as a raw material, carrying out pyrolysis reaction on 100mg of pure graphene oxide as a catalyst for 100h at 600 ℃ for 10s, and collecting a liquid product.
Comparative example 5-1:
the preparation method of the MXene dispersion liquid comprises the following steps:
step 1: adding 30mL of 12M hydrochloric acid into a plastic bottle, then dispersing 1g of lithium fluoride into the hydrochloric acid, and fully stirring for 10min at 45 ℃ by using a magnetic stirrer at the speed of 2000rpm to obtain a mixed solution B;
step 2: gradually and slowly adding the MAX phase into the mixed solution B, and then magnetically stirring and reacting at the speed of 2000rpm for 1h at the temperature of 25 ℃ to obtain a mixed solution C; the volume mass ratio of the MAX to the mixed liquid B is 10g:20 mL;
and step 3: and (3) repeatedly centrifuging and cleaning the precipitate obtained after the mixed solution C is centrifuged by using distilled water until the pH value of the supernatant is neutral, then adding 100mL of ethanol into the obtained substrate for dilution, carrying out ultrasonic treatment in a nitrogen ice bath environment for 30min under 1000W of power, and finally centrifuging the diluted solution for 30min at the rotating speed of 5000r/min to obtain the supernatant, thus obtaining the MXene dispersion liquid. And (3) taking 5mL of the MXene dispersion liquid for suction filtration, tearing off the prepared MXene film, weighing to calculate the concentration of the dispersion liquid, and adding water to adjust the concentration of the MXene dispersion liquid to 10 mg/mL.
The pyrolysis reaction application steps of the pure MXene catalyst are as follows:
the method comprises the steps of taking cotton straws as raw materials, carrying out freeze drying on 20mL of pure MXene dispersion liquid with the concentration of 10mg/mL for 20h as a catalyst, carrying out pyrolysis reaction for 10s at 600 ℃, and collecting liquid products.
Comparative example 5-2:
the application steps of the pure graphene oxide catalytic pyrolysis reaction agent are as follows:
taking cotton straws as a raw material, carrying out pyrolysis reaction on 50mg of pure graphene oxide at 600 ℃ for 10s by taking the pure graphene oxide as a catalyst after freeze drying for 20h, and collecting a liquid product.
Comparative example 6-1:
MXene(Ti3C2Tx) A method of preparing a dispersion comprising the steps of:
step 1: adding 60mL of 12M hydrochloric acid into a plastic bottle, then dispersing 1g of lithium fluoride into the hydrochloric acid, and fully stirring for 10min at 45 ℃ by using a magnetic stirrer at the speed of 2000rpm to obtain a mixed solution B;
step 2: gradually and slowly adding the MAX phase into the mixed solution B, and then magnetically stirring and reacting at the speed of 2000rpm for 1h at the temperature of 25 ℃ to obtain a mixed solution C; the volume mass ratio of the MAX to the mixed liquid B is 10g:80 mL;
and step 3: and (3) repeatedly centrifuging and cleaning the precipitate obtained after the mixed solution C is centrifuged by using distilled water until the pH value of the supernatant is neutral, then adding 100mL of ethanol into the obtained substrate for dilution, carrying out ultrasonic treatment in a nitrogen ice bath environment for 30min under 1000W of power, and finally centrifuging the diluted solution for 30min at the rotating speed of 5000r/min to obtain the supernatant, thus obtaining the MXene dispersion liquid. And (3) taking 5mL of the MXene dispersion liquid for suction filtration, tearing off the prepared MXene film, weighing to calculate the concentration of the dispersion liquid, and adding water to adjust the concentration of the MXene dispersion liquid to 5 mg/mL.
The pyrolysis reaction application steps of the pure MXene catalyst are as follows:
taking corn straws as a raw material, carrying out freeze drying on 10mL of pure MXene dispersion liquid with the concentration of 5mg/mL for 60h as a catalyst, carrying out pyrolysis reaction for 8s at 450 ℃, and collecting a liquid product.
Comparative example 6-2:
the application steps of the pure graphene oxide catalytic pyrolysis reaction agent are as follows:
taking corn straws as a raw material, carrying out pyrolysis reaction for 8s at 450 ℃ by taking 10mg of pure graphene oxide as a catalyst after freeze drying for 60h, and collecting a liquid product.
Comparative examples 1-1 and 1-2 are comparative examples of example 1, i.e. the catalytic conditions are the same, except that the catalysts are different; comparative examples 2-1 and 2-2 are comparative examples of example 2, i.e. the catalytic conditions are the same, except that the catalysts are different; comparative examples 3-1 and 3-2 are comparative examples of example 3, i.e. the catalytic conditions are the same, except that the catalysts are different. Comparative examples 4-1 and 4-2 are comparative examples of example 4, i.e. the catalytic conditions are the same, except that the catalysts are different. Comparative examples 5-1 and 5-2 are comparative examples of example 5, i.e., the catalytic conditions are the same except that the catalysts are different. Comparative example 6-1 and comparative example 6-2 are comparative examples of example 6, i.e., the catalytic conditions are the same, except that the catalysts are different. The catalytic results of examples 1-6 and comparative example were tested and are shown in table 1.
TABLE 1 test results of MXene-based catalyst catalytic pyrolysis of biomass to produce levoglucosan
As can be seen from Table 1, the MXene-based catalyst prepared by the method can obviously improve the yield of the levoglucosan, and especially when the mass ratio of MXene to graphene oxide in the MXene-based catalyst is 2:1, the yield of the levoglucosan is obviously improved.
The Raman spectrum of each substance of the invention is shown in figure 1, wherein figure a is the spectrum of the substance Chinese white poplar, figure b is the spectrum of MXene in the comparative example 1-1, and the Raman characteristic derivative peak of pure MXene appears at 500-1000 cm--1FIG. c shows graphite oxide in comparative examples 1 to 2The Raman characteristic derivative peak of the graphene oxide appears at 1000-1700cm-1In the embodiment 1, as shown in the diagram d, the spectrum of the mixture of the biomass, the MXene and the graphene oxide is obtained, and characteristic derivative peaks of the MXene and the graphene oxide are shifted, it can be proved that the MXene and the graphene oxide form a heterostructure, so that a synergistic effect is generated between the catalytic performances of the MXene and the graphene oxide.
Claims (10)
1. An MXene-based catalyst is characterized by comprising MXene and graphene oxide, wherein the mass ratio of the MXene to the graphene oxide is (0.5-5): 1.
2. the MXene-based catalyst of claim 1, wherein MXene is Ti3C2Tx。
3. The method for preparing the MXene-based catalyst according to any one of claims 1 or 2, wherein the MXene-based catalyst is obtained by adding the graphene oxide dispersion liquid into the MXene dispersion liquid, uniformly mixing to obtain a mixed liquid A, and freeze-drying the mixed liquid A.
4. The method for preparing the MXene-based catalyst according to claim 3, wherein the concentration of the MXene dispersion is 0.5-10mg/mL, and the concentration of the graphene oxide dispersion is 0.5-10 mg/mL.
5. The method of claim 3, wherein the freeze-drying time is 20-100 h.
6. The method of preparing an MXene-based catalyst according to claim 3, wherein the method of preparing the MXene dispersion comprises the steps of:
step 1, dispersing lithium fluoride in hydrochloric acid, and stirring to obtain a mixed solution B;
step 2, slowly adding a MAX phase of MXene into the mixed solution B, and stirring and reacting at 25-70 ℃ to obtain a mixed solution C;
and 3, washing the precipitate after the centrifugation of the mixed solution C until the pH value of the supernatant is neutral, then diluting the obtained substrate with water or ethanol, performing ultrasonic treatment, centrifuging the liquid after the ultrasonic treatment, and taking the supernatant to obtain MXene dispersion liquid.
7. The method for preparing MXene-based catalyst according to claim 6, wherein the concentration of hydrochloric acid is 6-12M, the mass volume ratio of lithium fluoride to hydrochloric acid is (1-4) g: (30-60) mL; the mass-volume ratio of the MAX to the mixed solution B is (1-10) g (20-80) mL.
8. Use of the MXene-based catalyst according to any one of claims 1 or 2, characterized in that the catalyst is used for catalytic pyrolysis of biomass for the preparation of L-glucan.
9. The use of claim 8, wherein biomass is used as raw material, the MXene-based catalyst of any one of claims 1 or 2 is used as catalyst, the pyrolysis reaction is carried out at 400-600 ℃ for 8-12s, and the liquid product is collected.
10. Use according to claim 8, wherein the biomass is populus tomentosa, cotton straw and corn straw.
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