CN110171831A - Hydrophobicity two dimension Ti under a kind of room temperature3C2TxThe preparation method of-MXene film - Google Patents
Hydrophobicity two dimension Ti under a kind of room temperature3C2TxThe preparation method of-MXene film Download PDFInfo
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- CN110171831A CN110171831A CN201910357771.9A CN201910357771A CN110171831A CN 110171831 A CN110171831 A CN 110171831A CN 201910357771 A CN201910357771 A CN 201910357771A CN 110171831 A CN110171831 A CN 110171831A
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Abstract
The invention discloses hydrophobicity two dimension Ti under a kind of room temperature3C2TxThe preparation method of-MXene film, which, which specifically includes that, prepares Ti using the method for selecting hydrofluoric acid in situ first3C2Tx- MXene then prepares Ti by the method being filtered by vacuum3C2TxIsocyanate-modified agent solution is then sprayed at Ti by-MXene film3C2TxThe two sides of-MXene film washes unreacted modifying agent with acetone after reaction.This method is reacted under room temperature can be completed, and be suitable for large-scale industrially prepared, be able to solve because of Ti3C2TxThe chemical instability of-MXene lamella leads to material, and performance sharply fails in actual use.
Description
Technical field
The present invention relates to hydrophobicity two dimension Ti under a kind of room temperature3C2TxThe preparation method of-MXene film, belongs to materials chemistry
Field.
Background technique
The discovery of graphene is so that two-dimension nano materials become research hotspot nearly ten years.In addition to classical graphene,
Two-dimension nano materials further include black phosphorus, boron nitride, transient metal sulfide and transition metal oxide.Univ Drexel, the U.S.
The Yury Gogotsi professor and Michel W.Barsoum professor of (Drexel University) et al. sent out in cooperation in 2011
A kind of existing New Two Dimensional structural material, to add newcomer in the family of two-dimensional material: transition metal carboritride,
Referred to as --- it steps section's alkene (MXene).By selecting suitable acid as etching agent, selective dissolves presoma MAX phase
In A atomic layer, obtain general formula be Mn+1XnTx(M represents early stage transition metal, and X represents carbon or nitrogen, and T representative is attached to surface
Functional group) MXene.Integrate the MXenes of high conductivity and functional group once it has been observed that causing that people's is extensive
Concern, has subsequently formed the research whirlpool of MXenes.And in this whirlpool, MXenes constantly achieves infusive prominent
Broken, such as: the research in super capacitor in 2014 finds Ti3C2TxIts volumetric capacitance of-MXene reaches surprising 900F cm-3；Two
Science reports Ti after year3C2Tx- MXene makes substantial progress i.e. in electromagnetic shielding field: in two-dimentional Ti3C2Tx-
MXene film thickness only 45 μm when, electromagnet shield effect is up to 92dB.This discovery is expected to break traditional electromagnetic shielding material
Limitation: metal material since the electromagnet shield effect of superelevation occupies always irresistible advantage in electromagnetic shielding field,
But with the rise of nearest flexible electronic, metal material is difficult to meet it because of the disadvantages of its perishable, difficult processing and big density
The demand of next-generation electromagnetic shielding material, and Ti3C2TxThe opportunity that-MXene occurs is just right.However, Ti3C2Tx- MXene exists
It brings and also brings puzzlement i.e. chemical instability to researcher while breakthrough.Research is found: if Ti3C2Tx-MXene
Water and oxygen are touched simultaneously, lamella edge will take the lead in being oxidized to titanium dioxide and carbon, and then oxidation process is gradually to piece
The development of layer center, eventually leads to entire Ti3C2Tx- MXene material property degradation even fails.
In view of the foregoing, it is necessary to Ti3C2Tx- MXene material carries out more in-depth study, to solve above-mentioned skill
Art problem.
Summary of the invention
To solve the deficiencies in the prior art, the purpose of the present invention is to provide hydrophobicity two dimension is prepared under a kind of room temperature
Ti3C2TxThe method of-MXene film, to solve because of Ti3C2TxThe chemical instability of-MXene lamella causes material actually to make
The problems such as capable of sharply being failed with process neutrality.
In order to achieve the above objectives, the present invention adopts the following technical scheme that:
Hydrophobicity two dimension Ti under a kind of room temperature3C2TxThe preparation method of-MXene film, comprising the following steps:
S1, preparation Ti3C2Tx- MXene:
1) it etches: lithium fluoride being added in hydrochloric acid and after stirring and dissolving, Ti is added thereto3AlC2, in 30~40 DEG C of conditions
Lower reaction, to after reaction, the Ti that is centrifugated in reactant3C2Tx- MXene particle and liquid are washed repeatedly with deionized water
It is multiple to wash reactant, until supernatant pH is 5.5~6.5；
2) it removes: deionized water is rejoined into the sediment after washing, with 20~30h of whirlpool blending instrument mechanical oscillation
Afterwards, then 0.5~1.5h of centrifugal treating, after centrifugation, the Ti of lower layer not etched is isolated3AlC2With the single layer on upper layer
Ti3C2Tx- MXene slurry.Wherein, the Ti that lower layer does not etch3AlC2Gray, and the Ti on upper layer3C2Tx- MXene amount of slurry compared with
It is few, color and the Ti not etched3AlC2Difference, most handy plastic key carries out careful separation when operation.
S2, preparation Ti3C2Tx- MXene film:
To Ti3C2Tx- MXene colloidal solution is separated by solid-liquid separation, by Ti3C2Tx- MXene nanometer sheet is deposited on water system filter membrane
On prepare Ti3C2Tx- MXene film；
S3, modifying agent is prepared:
Isocyanates and catalyst are dissolved in acetone, modifying agent is made；
S4, preparation hydrophobicity two dimension Ti3C2Tx- MXene film:
The prepared modifying agent of step S3 is placed in room with the two sides of spray gun even application film made from step S2
After 20~30h of the lower reaction of temperature, by unreacted modifying agent with acetone washing completely to get.
Preferably, aforementioned lithium fluoride and Ti3AlC2Mass ratio be 1: 1, the molal weight of the hydrochloric acid is 9M, hydrochloric acid
As long as dosage can sufficiently dissolve lithium fluoride, no specific demand, recommending dosage is that 1g lithium fluoride is dissolved in 20mL hydrochloric acid.
Preferably, in abovementioned steps S1, the reaction time at 35 DEG C is 18~30h.
It is highly preferred that centrifuge separation revolving speed is 3000~4500r/min in abovementioned steps S1.
More preferably, in abovementioned steps S1, after washing repeatedly, until supernatant pH value is 6, after guaranteeing sufficiently removal reaction
Residual acid.
It is further preferred that being separated by solid-liquid separation by the way of vacuum filtration in abovementioned steps S2.
It is highly preferred that isocyanates is octadecylisocyanate in above mentioned step S3, without being limited thereto, all contain
The organic reagent of isocyanate group；Catalyst is organic tin catalyst or amines catalyst, such as di lauric dibutyl
Tin or triethanolamine.
It is further preferred that in abovementioned steps S4, the formula rate of modifying agent are as follows: 100mg octadecylisocyanate
It is dissolved in the organic solvent of 20ml with 0.2mg dibutyl tin dilaurate, organic solvent selection can dissolve isocyanate reagents
Organic solvent, such as acetone.
The invention has the beneficial effects that:
Preparation method through the invention can be realized prepares hydrophobicity two dimension Ti at normal temperature3C2Tx- MXene film, benefit
With the functional group and Ti in the-NCO of isocyanates3C2TxThe hydroxyl on the surface-MXene reacts, and grafting long chain alkane changes
Ti3C2TxThe hydrophilicity of-MXene；By modification, be conducive to Ti3C2Tx- MXene stable dispersion in non-polar organic solvent,
To improve Ti3C2TxAgeing-resistant performance of-the MXene in actual environment use avoids performance generation in use process from sharply moving back
Change；Moreover, spraying modification technology is creatively applied in modified technique, and it is easy to operate and easy to accomplish, be conducive to scale
Change popularization and prepares hydrophobic t i3C2Tx- MXene film.
Detailed description of the invention
Fig. 1 is X ray diffracting spectrum of the invention, sequentially consists of Ti3AlC2, comparative example hydrophily Ti3C2Tx-
The hydrophobic t i of MXene film, embodiment 13C2Tx- MXene film, the hydrophobic t i after three week of aging3C2Tx-MXene
Film；
Fig. 2 is the hydrophily Ti of (a) comparative example of the invention3C2TxThe hydrophobicity of-MXene film and (b) embodiment 1
Ti3C2TxThe contact angle photo of-MXene film；
Fig. 3 is Ti rear before modified of the invention3C2TxThe fourier infrared map of-MXene film；
Fig. 4 is the hydrophobic t i of the embodiment of the present invention 23C2TxTi after three week of-MXene film and aging3C2Tx-
The electromagnetic shielding performance comparison diagram of MXene film；
Fig. 5 is the flow diagram of preparation method of the invention.
Specific embodiment
Specific introduce is made to the present invention below in conjunction with the drawings and specific embodiments.
If raw materials used is commercially available without specified otherwise in the present invention.
Embodiment 1
Referring to Fig. 5, preparation method process of the invention is as follows:
S1, preparation Ti3C2Tx- MXene:
Etching: under stirring conditions, take 1g lithium fluoride be dissolved in 20ml molal weight be 9M hydrochloric acid in, after five minutes to
1g Ti is wherein added3AlC2, reacted 24 hours under the conditions of 35 DEG C, to after reaction, using (3500 revs/min of centrifugation technique
Clock, 5 minutes/time) separation reactant in Ti3C2Tx- MXene particle and liquid, and continue using centrifugation technique deionization
Washing reaction object is repeated 8 times water repeatedly, is washed till supernatant pH to 6 or so.
Removing: 20ml deionized water is rejoined to the sediment for being washed till pH to 6 or so, with whirlpool blending instrument mechanical oscillation
After 24 hours, it is centrifuged 1 hour under 3500 revs/min of revolving speeds, goes out lower layer not with plastic key careful separation after centrifugation
The Ti of etching3AlC2The single layer Ti on (grey) and upper layer3C2Tx- MXene slurry (amount is less).
S2, preparation Ti3C2Tx- MXene film: by Ti3C2Tx- MXene colloidal solution carries out in such a way that vacuum filters
It is separated by solid-liquid separation, by Ti3C2Tx- MXene nanometer sheet is deposited on water system filter membrane and prepares Ti3C2Tx- MXene film.
S3, modifying agent is prepared: 100mg octadecylisocyanate and 0.2mg catalyst dibutyltin dilaurylate is molten
In 20ml acetone.
S4, hydrophobicity two dimension Ti3C2TxThe preparation of-MXene film: by the prepared formula of modifier of step S3, spray gun is used
It uniformly sprays on the two sides of film, it is after being placed in room temperature reaction 24 hours, unreacted modifying agent acetone washing is clean.
Embodiment 2
S1, preparation Ti3C2Tx- MXene:
Etching: under stirring conditions, take 5g lithium fluoride be dissolved in 80ml molal weight be 9M hydrochloric acid in, after five minutes to
5g Ti is wherein added3AlC2, reacted 30 hours under the conditions of 30 DEG C, to after reaction, using (3000 revs/min of centrifugation technique
Clock, 5 minutes/time) separation reactant in Ti3C2Tx- MXene particle and liquid, and continue using centrifugation technique deionization
Washing reaction object is repeated 10 times water repeatedly, is washed till supernatant pH to 6 or so.
Removing: 50ml deionized water is rejoined to the sediment for being washed till pH to 6 or so, with whirlpool blending instrument mechanical oscillation
After 30 hours, it is centrifuged 1 hour under 3000 revs/min of revolving speeds, goes out lower layer not with plastic key careful separation after centrifugation
The Ti of etching3AlC2The single layer Ti on (grey) and upper layer3C2Tx- MXene slurry (amount is less).
S2, preparation Ti3C2Tx- MXene film: by Ti3C2Tx- MXene colloidal solution carries out in such a way that vacuum filters
It is separated by solid-liquid separation, by Ti3C2Tx- MXene nanometer sheet is deposited on water system filter membrane and prepares Ti3C2Tx- MXene film.
S3, modifying agent is prepared: 100mg octadecylisocyanate and 0.2mg catalyst dibutyltin dilaurylate is molten
In 20ml acetone.
S4, hydrophobicity two dimension Ti3C2TxThe preparation of-MXene film: by the prepared formula of modifier of step S3, spray gun is used
It uniformly sprays on the two sides of film, it is after being placed in room temperature reaction 20 hours, unreacted modifying agent acetone washing is clean.
Embodiment 3
S1, preparation Ti3C2Tx- MXene:
Etching: under stirring conditions, take 5g lithium fluoride be dissolved in 80ml molal weight be 9M hydrochloric acid in, after five minutes to
5g Ti is wherein added3AlC2, reacted 18 hours under the conditions of 40 DEG C, to after reaction, using (4500 revs/min of centrifugation technique
Clock, 5 minutes/time) separation reactant in Ti3C2Tx- MXene particle and liquid, and continue using centrifugation technique deionization
Washing reaction object is repeated 10 times water repeatedly, is washed till supernatant pH to 6 or so.
Removing: 50ml deionized water is rejoined to the sediment for being washed till pH to 6 or so, with whirlpool blending instrument mechanical oscillation
After 20 hours, it is centrifuged 1 hour under 4500 revs/min of revolving speeds, goes out lower layer not with plastic key careful separation after centrifugation
The Ti of etching3AlC2The single layer Ti on (grey) and upper layer3C2Tx- MXene slurry (amount is less).
S2, preparation Ti3C2Tx- MXene film: by Ti3C2Tx- MXene colloidal solution carries out in such a way that vacuum filters
It is separated by solid-liquid separation, by Ti3C2Tx- MXene nanometer sheet is deposited on water system filter membrane and prepares Ti3C2Tx- MXene film.
S3, it prepares modifying agent: 100mg octadecylisocyanate and 0.2mg catalyst triethanolamine is dissolved in 20ml third
In ketone.
S4, hydrophobicity two dimension Ti3C2TxThe preparation of-MXene film: by the prepared formula of modifier of step S3, spray gun is used
It uniformly sprays on the two sides of film, it is after being placed in room temperature reaction 30 hours, unreacted modifying agent acetone washing is clean.
Comparative example uses commercially available hydrophily Ti3C2Tx- MXene film.
Performance detection
Shown in FIG. 1 is X ray diffracting spectrum of the invention, sequentially consists of Ti3AlC2, hydrophily Ti3C2Tx-
The hydrophobic t i of MXene film (comparative example), embodiment 13C2Tx- MXene film, embodiment 1 after three week of aging are dredged
Aqueous Ti3C2Tx- MXene film.It can be seen that proving Ti in the X ray diffracting spectrum of hydrophilic film3C2Tx- MXene quilt
It is successfully prepared out, hydrophobic t i3C2TxModified Ti is proved in the X ray diffracting spectrum of-MXene film3C2Tx- MXene's
Crystal phase structure does not change, shows in modifying process that oxidation behavior do not occur for material, three week of aging rear film X-ray
Diffracting spectrum illustrates Ti3C2TxOxidation behavior does not occur yet for-MXene.
Fig. 2 is the hydrophily Ti of (a) comparative example3C2TxThe hydrophobicity of-MXene film and (b) the embodiment of the present invention 1
Ti3C2TxThe contact angle photo of-MXene film, it can be seen that Ti after before modified3C2TxThe contact angle of-MXene film is from 39 °
Become 139 °, this shows that, by modified, film surface becomes hydrophobicity by hydrophily.
Fig. 3 is Ti rear before modified of the invention3C2TxThe fourier infrared map of-MXene film, it can be seen that comparison
The hydrophily Ti of example3C2Tx- MXene film is in 3481em-1And 1651cm-1Wavelength represents the vibration absorption peak of hydroxyl；And
The 3481cm after octadecylisocyanate is handled-1Hydroxyl vibration absworption peak disappear, then there is the vibration of nitrogen hydrogen singly-bound
Dynamic absorption peak: 3347cm-1；2964cm simultaneously-1And 2921cm-1Represent the hydrocarbon singly-bound of octadecylisocyanate long chain alkane
In plane vibration absorption peak, 1736cm-1The vibration absorption peak of C=O bond in wavelengths representative octadecylisocyanate.
Fig. 4 is the hydrophobic t i of the embodiment of the present invention 23C2TxTi after three week of-MXene film and aging3C2Tx-
The electromagnetic shielding performance comparison diagram of MXene film, it can be seen that Ti after three week of aging3C2TxThe electromagnetism of-MXene film
Shield effectiveness, which is not decayed, still maintains 50dB, has excellent performance.
To sum up, preparation method of the invention can be realized prepares hydrophobicity two dimension Ti at normal temperature3C2Tx- MXene film,
Utilize the functional group and Ti in the-NCO of isocyanates3C2TxThe hydroxyl on the surface-MXene reacts, and grafting long chain alkane changes
Ti3C2TxThe hydrophilicity of-MXene；By modification, be conducive to Ti3C2Tx- MXene stable dispersion in non-polar organic solvent,
To improve Ti3C2TxAgeing-resistant performance of-the MXene in actual environment use avoids performance generation in use process from sharply moving back
Change, keeps its excellent performance.
The basic principles, main features and advantages of the invention have been shown and described above.The technical staff of the industry should
Understand, the above embodiments do not limit the invention in any form, all obtained by the way of equivalent substitution or equivalent transformation
Technical solution is fallen within the scope of protection of the present invention.
Claims (10)
1. hydrophobicity two dimension Ti under a kind of room temperature3C2TxThe preparation method of-MXene film, which comprises the following steps:
S1, preparation Ti3C2Tx- MXene:
1) it etches: lithium fluoride being added in hydrochloric acid and after stirring and dissolving, Ti is added thereto3AlC2, anti-under the conditions of 30~40 DEG C
It answers, the Ti after reacting 18~30 hours, in centrifuge separation reactant3C2Tx- MXene particle and liquid, repeatedly with deionized water
Washing reaction object is multiple, until supernatant pH is 5.5~6.5；
2) it removes: rejoining deionized water into the sediment after washing, after 20~30h of whirlpool blending instrument mechanical oscillation,
0.5~1.5h of centrifugal treating again after centrifugation, isolates the Ti of lower layer not etched3AlC2With the single layer Ti on upper layer3C2Tx-
MXene slurry；
S2, preparation Ti3C2Tx- MXene film:
To Ti3C2Tx- MXene slurry is separated by solid-liquid separation, using vacuum filtration method by Ti3C2Tx- MXene nanometer sheet is deposited on water
It is that Ti is prepared on filter membrane3C2Tx- MXene film；
S3, modifying agent is prepared:
Isocyanates and catalyst are dissolved in acetone, modifying agent is made；
S4, preparation hydrophobicity two dimension Ti3C2Tx- MXene film:
The prepared modifying agent of step S3 is placed at room temperature with the two sides of spray gun even application film made from step S2
React 20~30h after, by unreacted modifying agent with acetone washing completely to get.
2. hydrophobicity two dimension Ti under a kind of room temperature according to claim 13C2TxThe preparation method of-MXene film, it is special
Sign is, the lithium fluoride and Ti3AlC2Mass ratio be 1: 1, the molal weight of the hydrochloric acid is 9M.
3. hydrophobicity two dimension Ti under a kind of room temperature according to claim 13C2TxThe preparation method of-MXene film, it is special
Sign is, in the step S1, the reaction time at 35 DEG C is 18~30h.
4. hydrophobicity two dimension Ti under a kind of room temperature according to claim 13C2TxThe preparation method of-MXene film, it is special
Sign is, in the step S1, centrifuge separation revolving speed is 3000-4500r/min.
5. hydrophobicity two dimension Ti under a kind of room temperature according to claim 13C2TxThe preparation method of-MXene film, it is special
Sign is, in the step S1, after washing repeatedly, until supernatant pH value is 6.
6. hydrophobicity two dimension Ti under a kind of room temperature according to claim 13C2TxThe preparation method of-MXene film, it is special
Sign is, in the step S2, is separated by solid-liquid separation by the way of vacuum filtration.
7. hydrophobicity two dimension Ti under a kind of described in any item room temperature according to claim 1~63C2TxThe preparation of-MXene film
Method, which is characterized in that in the step S3, isocyanates is the organic reagent containing isocyanate group, and catalyst is organic
Tin catalyst or amines catalyst.
8. hydrophobicity two dimension Ti under a kind of room temperature according to claim 73C2TxThe preparation method of-MXene film, it is special
Sign is that the isocyanates is octadecylisocyanate, and the catalyst is dibutyl tin dilaurate or triethanolamine.
9. hydrophobicity two dimension Ti under a kind of room temperature according to claim 73C2TxThe preparation method of-MXene film, it is special
Sign is, the formula rate of modifying agent are as follows: 100mg octadecylisocyanate and 0.2mg dibutyl tin dilaurate are dissolved in
In 20ml organic solvent.
10. hydrophobicity two dimension Ti under a kind of room temperature according to claim 73C2TxThe preparation method of-MXene film, it is special
Sign is that the organic solvent is acetone.
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| CN111298731A (en) * | 2020-03-05 | 2020-06-19 | 清华大学 | Light-driven liquid marble and preparation method and movement method thereof |
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| CN116482184A (en) * | 2023-06-21 | 2023-07-25 | 国网浙江省电力有限公司湖州供电公司 | Early warning hydrogen sensor gas-sensitive layer of lithium battery energy storage system and application thereof |
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| CN110868842A (en) * | 2019-11-29 | 2020-03-06 | 北京林业大学 | Mechanically-enhanced ultrathin semitransparent electromagnetic shielding film and preparation method thereof |
| CN110868842B (en) * | 2019-11-29 | 2021-03-05 | 北京林业大学 | Mechanically-enhanced ultrathin semitransparent electromagnetic shielding film and preparation method thereof |
| CN111298731A (en) * | 2020-03-05 | 2020-06-19 | 清华大学 | Light-driven liquid marble and preparation method and movement method thereof |
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| CN111822028A (en) * | 2020-07-21 | 2020-10-27 | 西安工业大学 | Bismuth-based photocatalytic composite film based on MXene and preparation method thereof |
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| CN113457448B (en) * | 2021-08-05 | 2023-01-17 | 重庆工商大学 | Preparation method of double-layer MXene film based on different interlayer distances |
| CN113493207A (en) * | 2021-08-09 | 2021-10-12 | 辽宁大学 | Ti3C2Tx-MXene flexible self-supporting film and preparation method thereof |
| CN114479154A (en) * | 2022-03-01 | 2022-05-13 | 南京航空航天大学 | Multifunctional durable film with hierarchical structure and preparation method thereof |
| CN116482184A (en) * | 2023-06-21 | 2023-07-25 | 国网浙江省电力有限公司湖州供电公司 | Early warning hydrogen sensor gas-sensitive layer of lithium battery energy storage system and application thereof |
| CN116482184B (en) * | 2023-06-21 | 2023-09-29 | 国网浙江省电力有限公司湖州供电公司 | Early warning hydrogen sensor gas-sensitive layer of lithium battery energy storage system and application thereof |
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