CN110615439A - Preparation method of ultrathin chitin/two-dimensional layered titanium carbide flexible film - Google Patents

Preparation method of ultrathin chitin/two-dimensional layered titanium carbide flexible film Download PDF

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Publication number
CN110615439A
CN110615439A CN201910021416.4A CN201910021416A CN110615439A CN 110615439 A CN110615439 A CN 110615439A CN 201910021416 A CN201910021416 A CN 201910021416A CN 110615439 A CN110615439 A CN 110615439A
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chitin
solution
dimensional layered
titanium carbide
ultrasonic treatment
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CN201910021416.4A
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Inventor
吴海江
朱家乐
杨飞英
龚晨
刘志勇
何世杰
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Shaoyang University
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Shaoyang University
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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
    • 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
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/921—Titanium carbide
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a preparation method of an ultrathin chitin/two-dimensional layered titanium carbide flexible film, which is prepared by mixing Ti3AlC2Slowly pouring ceramic powder into mixed solution of LiF and HCl for etching to prepare two-dimensional layered nano material Ti3C2TxObtaining uniformly dispersed single-layer ultrathin carbon after ultrasonic treatment in argon atmosphereTitanium nano sheets are formed; mixing chitin solution and Ti3C2TxMixing colloid and ultrasonic treatment to obtain uniformly dispersed mixed solution, and filtering to form a film. The invention adopts nontoxic and easily obtained raw materials, has simple preparation process, controllable process and low cost, and the prepared ultrathin chitin/two-dimensional layered titanium carbide flexible film has the advantages of super-strong flexibility, large specific surface area, good conductivity and good hydrophilicity, and can be widely applied to the fields of energy storage, catalysis, adsorption and the like.

Description

Preparation method of ultrathin chitin/two-dimensional layered titanium carbide flexible film
Technical Field
The invention relates to the field of composite material preparation, in particular to a preparation method of an ultrathin chitin/two-dimensional layered titanium carbide flexible film.
Background
The two-dimensional layered titanium carbide is a novel two-dimensional transition metal carbide and has a two-dimensional structure similar to graphene. Selective etching of the precursor Ti by means of chemical etching3AlC2Al atomic layer to obtain two-dimensional layered titanium carbide. The two-dimensional layered titanium carbide has the performance of the traditional two-dimensional material, also has larger specific surface area, good conductivity, stability, magnetic performance and mechanical performance, and is widely applied to the fields of energy storage, catalysis, adsorption and the like.
The storage amount of chitin in nature is second to cellulose, and the chitin is widely derived from shells of crustaceans such as shrimps and crabs, and has good biocompatibility, degradability, heavy metal adsorption and hydrophilicity. Has wide application prospect in the fields of biomedical materials, food processing, water treatment and the like.
Therefore, the ultrathin chitin/two-dimensional layered titanium carbide flexible film has ultrahigh flexibility and is expected to have better application in the fields of energy storage, catalysis, adsorption and the like.
Disclosure of Invention
The invention aims to compound chitin and titanium carbide to ensure that the chitin and titanium carbide have the performance characteristics of lightness, thinness and flexibility.
The invention also aims to provide a preparation method of the ultrathin chitin/two-dimensional layered titanium carbide flexible film, which has the advantages of simple preparation process and low cost.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an ultrathin chitin/two-dimensional layered titanium carbide flexible film comprises the following steps:
step 1: 2g LiF is added into 20ml HCl and stirred for 20min, so that the LiF and the HCl react fully to obtain the etching solution.
Step 2 to the solution of step 12 g ~ 3.5.5 g Ti was slowly added3AlC2Stirring the powder at 35 deg.C for 24 ~ 48h, centrifuging with deionized water to neutral, and drying at 60 deg.C under vacuum for 12h to obtain multilayer Ti3C2TxNanosheet powder.
Step 3, taking 1g ~ 2.5.5 g of multilayer Ti in the step 23C2TxAdding 200ml of deionized water into the nanosheet powder, performing ultrasonic treatment for 4h in an argon introducing environment, and centrifuging for 1h at 3500r/min in a freeze-drying centrifuge to obtain single-layer Ti3C2TxA nanosheet colloid solution.
Step 4, a drop of glacial acetic acid solution is dripped into 40ml of distilled water, 20mg of ~ 35mg of chitin is added into 40ml of distilled water, and the chitin solution is prepared by probe ultrasonic treatment for 10 ~ 40 min.
Step 5, adding 1.6ml ~ 4ml of chitin solution obtained in step 4 into Ti obtained in step 33C2TxAnd stirring with a glass rod in a colloidal solution to enable the nanosheets to be adsorbed on the chitin, then uniformly dispersing in the solution through probe ultrasound, finally obtaining a required film through suction filtration, and drying in a vacuum drying oven at the temperature of 45 ℃ and ~ 60 ℃ to obtain the chitin/two-dimensional layered titanium carbide flexible film.
The invention has the beneficial effects that: the raw materials for preparation are easy to obtain, the preparation process is simple, the process is controllable, and the cost is low. The prepared ultrathin chitin/two-dimensional layered titanium carbide flexible film has the advantages of super-strong flexibility, large specific surface area, good conductivity and good hydrophilicity, and can be widely applied to the fields of energy storage, catalysis, adsorption and the like.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Fig. 2 is an SEM image of the chitin/two-dimensional layered titanium carbide flexible film.
Detailed Description
The following describes a method for preparing an ultra-thin chitin/two-dimensional layered titanium carbide flexible film according to an embodiment of the present invention.
The specific embodiment 1 of the present invention comprises the steps of:
step 1: 2g LiF was added to 20ml HCl and stirred for 20min, followed by the slow addition of 2g Ti3AlC2Stirring the powder at 35 ℃ for 24h, then centrifugally washing the powder with deionized water to neutrality, and drying the powder at 60 ℃ for 12h in a vacuum environment to obtain multilayer Ti3C2TxNanosheet powder.
Step 2: taking 1g of the multilayer Ti in the step 13C2TxAdding 200ml of deionized water into the nanosheet powder, performing ultrasonic treatment for 4 hours in an argon introducing environment, and centrifuging for 1 hour at 3500r/min in a refrigerated centrifuge to obtain single-layer Ti3C2TxA nanosheet colloid solution.
And step 3: dripping a drop of glacial acetic acid solution into 40ml of distilled water, adding 20mg of chitin into 40ml of distilled water, and performing ultrasonic treatment for 10min by using a probe to prepare the chitin solution.
And 4, step 4: adding 1.6ml of chitin solution obtained in the step 3 into 15ml of Ti obtained in the step 23C2TxAnd stirring with a glass rod in a colloidal solution to enable the nanosheets to be adsorbed on the chitin, then uniformly dispersing in the solution through probe ultrasound, finally obtaining a required film through suction filtration, and drying in a vacuum drying oven at 45 ℃ for 12 hours to obtain the chitin/two-dimensional layered titanium carbide flexible film. The morphology is shown in fig. 2.
The specific embodiment 2 of the present invention comprises the steps of:
step 1: 2g LiF was added to 20ml HCl and stirred for 20min, followed by slow addition of 2.5g Ti3AlC2Stirring the powder at 35 ℃ for 32h, then centrifugally washing the powder with deionized water to neutrality, and drying the powder at 60 ℃ for 12h in a vacuum environment to obtain multilayer Ti3C2TxNanosheet powder.
Step 2: taking 1.5g of multilayer Ti in the step 13C2TxAdding 200ml of deionized water into the nanosheet powder, performing ultrasonic treatment for 4 hours in an argon introducing environment, and centrifuging for 1 hour at 3500r/min in a refrigerated centrifuge to obtain single-layer Ti3C2TxA nanosheet colloid solution.
And step 3: dripping a drop of glacial acetic acid solution into 40ml of distilled water, adding 25mg of chitin into 40ml of distilled water, and performing ultrasonic treatment for 20min by using a probe to prepare the chitin solution.
And 4, step 4: adding 2.4ml of chitin solution obtained in the step 3 into 15ml of Ti obtained in the step 23C2TxAnd stirring with a glass rod in a colloidal solution to enable the nanosheets to be adsorbed on the chitin, then uniformly dispersing in the solution through probe ultrasound, finally obtaining a required film through suction filtration, and drying in a vacuum drying oven at 50 ℃ for 12 hours to obtain the chitin/two-dimensional layered titanium carbide flexible film.
The specific embodiment 3 of the present invention comprises the steps of:
step 1: 2g LiF was added to 20ml HCl and stirred for 20min, followed by slow addition of 3g Ti3AlC2Stirring the powder at 35 ℃ for 40h, then centrifugally washing the powder with deionized water to neutrality, and drying the powder at 60 ℃ for 12h in a vacuum environment to obtain multilayer Ti3C2TxNanosheet powder.
Step 2: taking 2g of the multilayer Ti in the step 13C2TxAdding 200ml of deionized water into the nanosheet powder, performing ultrasonic treatment for 4 hours in an argon introducing environment, and centrifuging for 1 hour at 3500r/min in a refrigerated centrifuge to obtain single-layer Ti3C2TxA nanosheet colloid solution.
And step 3: dripping a drop of glacial acetic acid solution into 40ml of distilled water, adding 30mg of chitin into 40ml of distilled water, and performing ultrasonic treatment for 30min by using a probe to prepare the chitin solution.
And 4, step 4: adding 3.2ml of chitin solution obtained in the step 3 into 15ml of Ti obtained in the step 23C2TxAnd stirring the nano sheets in a colloidal solution by using a glass rod to enable the nano sheets to be adsorbed on the chitin, uniformly dispersing the nano sheets in the solution by using probe ultrasound, finally obtaining a required film by suction filtration, and drying the film in a vacuum drying oven at 55 ℃ for 12 hours to obtain the chitin/two-dimensional layered titanium carbide flexible film.
The specific embodiment 4 of the present invention includes the steps of:
step 1: 2g LiF was added to 20ml HCl and stirred for 20min, followed by slow addition of 3.5g Ti3AlC2Stirring the powder at 35 ℃ for 48h, then centrifugally washing the powder with deionized water to neutrality, and drying the powder at 60 ℃ for 12h in a vacuum environment to obtain multilayer Ti3C2TxNanosheet powder.
Step 2: taking 2.5g of multilayer Ti in the step 13C2TxAdding 200ml of deionized water into the nanosheet powder, performing ultrasonic treatment for 4 hours in an argon introducing environment, and centrifuging for 1 hour at 3500r/min in a refrigerated centrifuge to obtain single-layer Ti3C2TxA nanosheet colloid solution.
And step 3: dripping a drop of glacial acetic acid solution into 40ml of distilled water, adding 35mg of chitin into 40ml of distilled water, and performing ultrasonic treatment on a probe for 40min to prepare the chitin solution.
And 4, step 4: adding 4ml of chitin solution obtained in the step 3 into 15ml of Ti obtained in the step 23C2TxAnd stirring with a glass rod in a colloidal solution to enable the nanosheets to be adsorbed on the chitin, then uniformly dispersing in the solution through probe ultrasound, finally obtaining a required film through suction filtration, and drying in a vacuum drying oven at 60 ℃ for 12 hours to obtain the chitin/two-dimensional layered titanium carbide flexible film.
The principles and embodiments of the present invention are explained herein using specific examples, which are presented only to assist in understanding the method and its core concepts of the present invention. The foregoing is only a preferred embodiment of the present invention, and it should be noted that there are objectively infinite specific structures due to the limited character expressions, and it will be apparent to those skilled in the art that a plurality of modifications, decorations or changes may be made without departing from the principle of the present invention, and the technical features described above may be combined in a suitable manner; such modifications, variations, combinations, or adaptations of the invention using its spirit and scope, as defined by the claims, may be directed to other uses and embodiments.

Claims (8)

1. A preparation method of an ultrathin chitin/two-dimensional layered titanium carbide flexible film is characterized by comprising the following steps:
(1) mixing Ti3AlC2Slowly adding the powder into a mixed solution of HCl and LiF, stirring, centrifugally washing with deionized water to be neutral, and drying in a vacuum drying oven at 60 ℃ for 12 hours to obtain the multilayer Ti3C2TxNanosheets; then a plurality of layers of Ti3C2TxAdding the nanosheets into deionized water, introducing argon gas into the deionized water, performing water bath ultrasonic treatment, and centrifuging the nanosheets for 1h at 3500r/min in a freeze-drying centrifuge to prepare single-layer nanosheets;
(2) dripping a drop of glacial acetic acid solution into 40ml of distilled water, then adding chitin powder into the distilled water, and carrying out probe ultrasonic treatment to prepare chitin solution;
(3) adding Ti obtained in the step (1)3C2TxAnd (3) dripping the chitin solution obtained in the step (2) into the nanosheet colloidal solution, stirring with a glass rod to enable the nanosheets to be adsorbed on the chitin, ultrasonically dispersing the nanosheets into the solution through a probe, finally preparing the required film through suction filtration, and drying in a vacuum drying oven to obtain the chitin/two-dimensional layered titanium carbide flexible film.
2. The method of claim 1, wherein: in step (1), Ti3AlC2The powder mass was 2g ~ 3.5.5 g, LiF 2g, HCl 20 ml.
3. The preparation method according to claim 1, wherein the reaction temperature of the stirring in the step (1) is 35 ℃, the stirring time is 24 ~ 48 hours, and the duration of the water bath ultrasonic treatment is 4 hours.
4. The method of claim 1, wherein: multilayer Ti in step (1)3C2The Tx nano-sheet content is 1g ~ 2.5.5 g, and the deionized water content is 200 ml.
5. The method of claim 1, wherein the chitin content in step (2) is 20mg ~ 35 mg.
6. The method according to claim 1, wherein the probe ultrasonic treatment time in the step (2) is 10 ~ 40 min.
7. The method according to claim 1, wherein the chitin solution in step (3) is 1.6ml ~ 4 ml.
8. The process according to claim 1, wherein the temperature in the vacuum drying oven in the step (3) is 45 ℃ to ~ 60 ℃.
CN201910021416.4A 2019-01-10 2019-01-10 Preparation method of ultrathin chitin/two-dimensional layered titanium carbide flexible film Withdrawn CN110615439A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112233914A (en) * 2020-10-15 2021-01-15 哈尔滨工业大学 Preparation method and application of micronized cellulose/MXene composite film
CN113104850A (en) * 2021-05-17 2021-07-13 青岛理工大学 Preparation method of double-loss type electromagnetic wave-absorbing material and electromagnetic wave-absorbing material
CN113493207A (en) * 2021-08-09 2021-10-12 辽宁大学 Ti3C2Tx-MXene flexible self-supporting film and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107128922A (en) * 2017-04-27 2017-09-05 陕西科技大学 A kind of titanium carbide flexible paper and preparation method thereof
WO2017184957A1 (en) * 2016-04-22 2017-10-26 Drexel University Two-dimensional metal carbide, nitride, and carbonitride films and composites for emi shielding

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017184957A1 (en) * 2016-04-22 2017-10-26 Drexel University Two-dimensional metal carbide, nitride, and carbonitride films and composites for emi shielding
CN107128922A (en) * 2017-04-27 2017-09-05 陕西科技大学 A kind of titanium carbide flexible paper and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112233914A (en) * 2020-10-15 2021-01-15 哈尔滨工业大学 Preparation method and application of micronized cellulose/MXene composite film
CN113104850A (en) * 2021-05-17 2021-07-13 青岛理工大学 Preparation method of double-loss type electromagnetic wave-absorbing material and electromagnetic wave-absorbing material
CN113493207A (en) * 2021-08-09 2021-10-12 辽宁大学 Ti3C2Tx-MXene flexible self-supporting film and preparation method thereof

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Application publication date: 20191227