CN110204898A - A kind of preparation method of MXene- Kevlar fento laminated film - Google Patents
A kind of preparation method of MXene- Kevlar fento laminated film Download PDFInfo
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- CN110204898A CN110204898A CN201910548663.XA CN201910548663A CN110204898A CN 110204898 A CN110204898 A CN 110204898A CN 201910548663 A CN201910548663 A CN 201910548663A CN 110204898 A CN110204898 A CN 110204898A
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- mxene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids
Abstract
A kind of preparation method of MXene- Kevlar fento laminated film, the present invention relates to a kind of preparation methods of MXene film.The technical problem that the present invention is to solve the preparation process of existing MXene film is cumbersome, electromagnetic shielding performance is low.This method: one, aramid nano-fiber is prepared；Two, single layer sheet Ti is prepared3C2MXene powder；Three, by single layer sheet Ti3C2MXene powder is distributed in dimethyl sulfoxide, is then added in aramid nano-fiber solution and is stirred evenly, and then decompression is filtered into film, obtains MXene- Kevlar fento laminated film after dry.Laminated film electromagnetic shielding performance SSE/t can reach 1500~22000dB cm2g‑1, can achieve 40~120MPa with a thickness of the tensile strength of 12~30 μm of film, resist bending folds, and preparation process is simple, can be used for supercapacitor, Li battery, hydrogen storage, adsorbing domain.
Description
Technical field
The present invention relates to a kind of preparation methods of MXene film.
Background technique
MXene is a kind of New Two Dimensional material into discovery in several years, has that large specific surface area, electric conductivity be strong, physical chemistry
The characteristics of haveing excellent performance, have been widely used supercapacitor, Li battery, hydrogen storage, in terms of.Due to the multilayer of MXene
Two-dimensional structure and excellent electric conductivity make it possible it in electro-magnetic wave absorption and the application of shielding field.In order to be suitable for answering
With, MXene is prepared into MXene film by many researchers, but the MXene film or electromagnetic shielding performance that prepare are low, or
Person's preparation process is cumbersome, can not practical application.MXene is mixed with cellulose fibre such as, is obtained in the way of suction filtration later
Composite membrane, although the tensile strength of gained film has promotion, but electromagnetic shielding performance seriously glides, the electromagnetism of unit mass
Shielding properties SSE/t is only capable of reaching 2000~3000dB cm2g-1, so that electromagnetic shielding performance and mechanical property can not obtain
It is combined to perfect, the application of material is by great limitation.In addition, have scholar by MXene with carbon nanotube (CNT) is compound does
At semitransparent thin film, the excellent MXene/CNT laminated film of electromagnetic shielding performance is obtained, but its preparation process is too cumbersome,
Practical application is little.
Summary of the invention
The technical problem that the present invention is to solve the preparation process of existing MXene film is cumbersome, electromagnetic shielding performance is low,
And provide a kind of preparation method of MXene- carbonization Kevlar fento laminated film.
The preparation method of MXene- carbonization Kevlar fento laminated film of the invention, sequentially includes the following steps:
One, Kafra fiber, potassium hydroxide the preparation of aramid nano-fiber: are added to anhydrous dimethyl sulphoxide (DMSO)
In, stirring and dissolving obtains aramid nano-fiber solution；
Two, single layer sheet Ti3C2The preparation of MXene powder:
LiF is added in the hydrochloric acid solution that concentration is 6~12mol/L and is stirred evenly；Then Ti is added dropwise thereto3AlC2,
24~36h is reacted at 45~60 DEG C；Be washed with water after completion of the reaction to supernatant pH value be 5.5~6.5, be then added to from
In sub- water, it is ultrasonically treated 30~45min under protection of argon gas；After being centrifugated again, upper layer suspension is freeze-dried, list is obtained
Lamellar Ti3C2MXene powder；
Three, prepared by MXene- Kevlar fento laminated film:
A, by single layer sheet Ti3C2MXene powder is added in dimethyl sulfoxide, and ultrasonic disperse is uniform, obtains single layer sheet
Ti3C2MXene colloidal solution；Wherein single layer sheet Ti3C2The concentration of MXene is 0.1~0.6mg/mL；
B, by single layer sheet Ti3C2MXene colloidal solution is added to 12~18h of stirring in aramid nano-fiber solution, obtains
Mixed solution；The wherein quality of the aramid nano-fiber in aramid nano-fiber solution and single layer sheet Ti3C2MXene colloid is molten
Ti in liquid3C2Mass ratio be 1:(10~0.5)；
C, mixed solution is depressurized and is filtered, obtain film；Film is impregnated in methyl alcohol sub- to remove dimethyl therein
Sulfone applies pressure to film after taking-up and is kept at room temperature to methanol volatilizing, obtains MXene- Kevlar fento laminated film.
The method comprises the steps of firstly, preparing single layer Ti out3C2MXene utilizes single layer MXene and aramid nano-fiber (Aramid later
Nanofibers, ANFs) it is compound, nanofiber is present between MXene layers and surface, play the role of support and connection,
On the basis of improving film dynamic performance, while retaining the multilayered structure of MXene in laminated film, so that entering the electromagnetic wave come in
There is numerous loss paths inside film, to reach good shield effectiveness.
The thickness of MXene- Kevlar fento laminated film of the invention is adjustable, with a thickness of the drawing of 12~30 μm of film
Stretching intensity can achieve 40~120MPa, the tensile strength of 15MPa of significantly larger than pure MXene film or so.It is electromagnetically shielded simultaneously
Function admirable, can achieve 5~40dB, and unit mass electromagnetic shielding performance SSE/t can reach 1500~22000dB cm2g-1。
Gained composite film preparation technology of the invention is simple, and toughness is good, and resist bending folds, and can be applied to supercapacitor, Li
Battery, hydrogen storage, adsorbing domain.
Detailed description of the invention
Fig. 1 is the single layer sheet Ti that 1 step 2 of embodiment obtains3C2The stereoscan photograph of MXene powder；
Fig. 2 is the stereoscan photograph of the section of MXene- carbonization Kevlar fento laminated film prepared by embodiment 1；
Fig. 3 is the electromagnet shield effect in X-band of MXene- carbonization Kevlar fento laminated film prepared by embodiment 1
Figure；
Fig. 4 is the stereoscan photograph of the section of MXene- carbonization Kevlar fento laminated film prepared by embodiment 2；
Fig. 5 is the electromagnet shield effect in X-band of MXene- carbonization Kevlar fento laminated film prepared by embodiment 2
Figure.
Specific embodiment
Specific embodiment 1: the preparation method of the MXene- carbonization Kevlar fento laminated film of present embodiment, is pressed
Following steps carry out:
One, Kafra fiber, potassium hydroxide the preparation of aramid nano-fiber: are added to anhydrous dimethyl sulphoxide (DMSO)
In, stirring and dissolving obtains aramid nano-fiber solution；
Two, single layer sheet Ti3C2The preparation of MXene powder:
LiF is added in the hydrochloric acid solution that concentration is 6~12mol/L and is stirred evenly；Then Ti is added dropwise thereto3AlC2,
24~36h is reacted at 45~60 DEG C；Be washed with water after completion of the reaction to supernatant pH value be 5.5~6.5, be then added to from
In sub- water, it is ultrasonically treated 30~45min under protection of argon gas；After being centrifugated again, upper layer suspension is freeze-dried, list is obtained
Lamellar Ti3C2MXene powder；
Three, prepared by MXene- Kevlar fento laminated film:
A, by single layer sheet Ti3C2MXene powder is added in dimethyl sulfoxide, and ultrasonic disperse is uniform, obtains single layer sheet
Ti3C2MXene colloidal solution；Wherein single layer sheet Ti3C2The concentration of MXene is 0.1~0.6mg/mL；
B, by single layer sheet Ti3C2MXene colloidal solution is added to 12~18h of stirring in aramid nano-fiber solution, obtains
Mixed solution；The wherein quality of the aramid nano-fiber in aramid nano-fiber solution and single layer sheet Ti3C2MXene colloid is molten
Ti in liquid3C2Mass ratio be 1:(10~0.5)；
C, mixed solution is depressurized and is filtered, obtain film；Film is impregnated in methyl alcohol sub- to remove dimethyl therein
Sulfone applies pressure to film after taking-up and is kept at room temperature to methanol volatilizing, obtains MXene- Kevlar fento laminated film.
Specific embodiment 2: the present embodiment is different from the first embodiment in that Kafra fiber is in step 1
Chopped strand；It is other same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that Kev is towed in step 1
The mass ratio of dimension and potassium hydroxide is 1:(1.5~4)；It is other the same as one or two specific embodiments.
Specific embodiment 4: Kev in step 1 unlike one of present embodiment and specific embodiment one to three
The ratio of the volume of the quality and anhydrous dimethyl sulphoxide for dimension of towing is 1g:(500~1000) mL；Other and specific embodiment one
It is identical to one of three.
Specific embodiment 5: being stirred in step 1 unlike one of present embodiment and specific embodiment one to four
Temperature be 20~25 DEG C, mixing time be 7~10 days；It is other identical as one of specific embodiment one to four.
Specific embodiment 6: LiF in step 2 unlike one of present embodiment and specific embodiment one to five
Quality and concentration be 6~12mol/L the ratio of volume of hydrochloric acid solution be 1g:(10~30) mL；Other and specific embodiment party
One of formula one to five is identical.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six in step 2
Ti3AlC2Mass ratio with LiF is 1:(1~2)；It is other identical as one of specific embodiment one to six.
Specific embodiment 8: being soaked in step 3 c unlike one of present embodiment and specific embodiment one to seven
Steeping the time is 1.5~2.5 days；It is other identical as one of specific embodiment one to seven.
Beneficial effects of the present invention are verified with the following examples:
Embodiment 1: the present embodiment MXene- carbonization Kevlar fento laminated film preparation method, according to the following steps into
Row:
One, the preparation of aramid nano-fiber: by 1g Kevlar chopped strand, that 1.5g potassium hydroxide is added to 500mL is anhydrous
In dimethyl sulfoxide (DMSO), is stirred 7 days under conditions of 20~22 DEG C of room temperature, obtain aramid nano-fiber solution；The solution
For reddish brown；
Two, single layer sheet Ti3C2The preparation of MXene powder:
Taking 60ml concentration is that the hydrochloric acid of 9mol/L is placed in tetrafluoroethene beaker, and 4.8gLiF is added and stirs evenly；Then
3.0gTi is added dropwise thereto3AlC2, reacted for 24 hours at 50 DEG C；Being washed with water after completion of the reaction to the pH value of supernatant is 6.0, then plus
After entering the dilution of 500ml deionized water, it is ultrasonically treated 45min under protection of argon gas；After being centrifugated again, by upper layer suspension in temperature
Degree is freeze-dried 48 hours for -50 DEG C of condition, obtains single layer sheet Ti3C2MXene；
Three, prepared by MXene- Kevlar fento laminated film:
A, by 20mg single layer sheet Ti3C2MXene powder is added in 50mL dimethyl sulfoxide, and ultrasonic disperse is uniform, is obtained
Single layer sheet Ti3C2MXene colloidal solution；
B, the aramid nano-fiber solution for taking 1ml step 1 to prepare is added to the single layer sheet Ti of step 3 a3C2MXene glue
18h is stirred in liquid solution, obtains mixed solution；
C, mixed solution is depressurized and is filtered, obtain film；Film is impregnated to 2 days in methyl alcohol to remove dimethyl therein
Sulfoxide applies pressure to film after taking-up and is kept for 2 days at room temperature, and methanol volatilizees completely, and it is multiple to obtain MXene- Kevlar fento
Close film.
The single layer sheet Ti that the present embodiment step 2 obtains3C2The stereoscan photograph of MXene powder is as shown in Figure 1, from figure
1 as can be seen that Ti3C2For laminated structure.
Stereoscan photograph such as Fig. 2 of the section for the MXene- Kevlar fento laminated film that the present embodiment step 3 obtains
It is shown, figure it is seen that aramid nano-fiber is distributed in the interlayer of MXene.
MXene- Kevlar fento laminated film manufactured in the present embodiment with a thickness of 12 μm, in the electromagnetic shielding of X-band
Efficiency figure can achieve 34dB as shown in figure 3, from figure 3, it can be seen that the electromagnet shield effect of film is excellent, pass through calculate it is single
Position quality electromagnet shield effect SSE/t can reach 22000dB cm2g-1。
The tensile strength of MXene- Kevlar fento laminated film manufactured in the present embodiment can achieve 45MPa, be much higher than
The tensile strength of the 15MPa of pure MXene film or so.
Embodiment 2: the present embodiment MXene- carbonization Kevlar fento laminated film preparation method, according to the following steps into
Row:
One, the preparation of aramid nano-fiber: by 1g Kevlar chopped strand, that 1.5g potassium hydroxide is added to 500mL is anhydrous
In dimethyl sulfoxide (DMSO), is stirred 7 days under conditions of 20~22 DEG C of room temperature, obtain aramid nano-fiber solution；The solution
For reddish brown；
Two, single layer sheet Ti3C2The preparation of MXene powder:
Taking 60ml concentration is that the hydrochloric acid of 9mol/L is placed in tetrafluoroethene beaker, and 4.8gLiF is added and stirs evenly；Then
3.0gTi is added dropwise thereto3AlC2, reacted for 24 hours at 50 DEG C；Being washed with water after completion of the reaction to the pH value of supernatant is 6.0, then plus
After entering the dilution of 500ml deionized water, it is ultrasonically treated 45min under protection of argon gas；After being centrifugated again, by upper layer suspension in temperature
Degree is freeze-dried 48 hours for -50 DEG C of condition, obtains single layer sheet Ti3C2MXene；
Three, prepared by MXene- Kevlar fento laminated film:
A, by 20mg single layer sheet Ti3C2MXene powder is added in 50mL dimethyl sulfoxide, and ultrasonic disperse is uniform, is obtained
Single layer sheet Ti3C2MXene colloidal solution；
B, the aramid nano-fiber solution for taking 1.25ml step 1 to prepare is added to the single layer sheet of step 3 a
Ti3C218h is stirred in MXene colloidal solution, obtains mixed solution；
C, mixed solution is depressurized and is filtered, obtain film；Film is impregnated to 2 days in methyl alcohol to remove dimethyl therein
Sulfoxide applies pressure to film after taking-up and is kept for 2 days at room temperature, and methanol volatilizees completely, and it is multiple to obtain MXene- Kevlar fento
Close film.
Stereoscan photograph such as Fig. 4 of the section for the MXene- Kevlar fento laminated film that the present embodiment step 3 obtains
It is shown, from fig. 4, it can be seen that nanofiber content is more than the film prepared in embodiment 1, and it is distributed in the interlayer of MXene.
MXene- Kevlar fento laminated film manufactured in the present embodiment with a thickness of 13 μm, the MXene- Kevlar fento
The electromagnet shield effect figure in X-band of laminated film is as shown in figure 5, from fig. 5, it can be seen that the electromagnetic shielding performance of film is excellent
It is good, it can achieve 28dB, 18000dB cm can achieve by unit of account quality electromagnet shield effect SSE/t2g-1。
The tensile strength of MXene- Kevlar fento laminated film manufactured in the present embodiment can achieve 50MPa.
Claims (8)
1. a kind of preparation method of MXene- carbonization Kevlar fento laminated film, it is characterised in that this method according to the following steps into
Row:
One, the preparation of aramid nano-fiber: Kafra fiber, potassium hydroxide are added in anhydrous dimethyl sulphoxide, are stirred molten
Solution, obtains aramid nano-fiber solution；
Two, single layer sheet Ti3C2The preparation of MXene powder:
LiF is added in the hydrochloric acid solution that concentration is 6~12mol/L and is stirred evenly；Then Ti is added dropwise thereto3AlC2, 45
24~36h is reacted at~60 DEG C；Being washed with water after completion of the reaction to the pH value of supernatant is 5.5~6.5, is then added to deionized water
In, it is ultrasonically treated 30~45min under protection of argon gas；After being centrifugated again, upper layer suspension is freeze-dried, single-layer sheet is obtained
Shape Ti3C2MXene powder；
Three, prepared by MXene- Kevlar fento laminated film:
A, by single layer sheet Ti3C2MXene powder is added in dimethyl sulfoxide, and ultrasonic disperse is uniform, obtains single layer sheet
Ti3C2MXene colloidal solution；Wherein single layer sheet Ti3C2The concentration of MXene is 0.1~0.6mg/mL；
B, by single layer sheet Ti3C2MXene colloidal solution is added to 12~18h of stirring in aramid nano-fiber solution, is mixed
Close solution；The wherein quality of the aramid nano-fiber in aramid nano-fiber solution and single layer sheet Ti3C2MXene colloidal solution
In Ti3C2Mass ratio be 1:(10~0.5)；
C, mixed solution is depressurized and is filtered, obtain film；Film is impregnated in methyl alcohol to remove dimethyl sulfoxide therein, is taken
Pressure is applied to film after out and is kept at room temperature to methanol volatilizing, obtains MXene- Kevlar fento laminated film.
2. a kind of preparation method of MXene- carbonization Kevlar fento laminated film according to claim 1, feature exist
Kafra fiber is chopped strand in step 1.
3. a kind of preparation method of MXene- carbonization Kevlar fento laminated film according to claim 1 or 2, feature
It is in step 1 that the mass ratio of Kafra fiber and potassium hydroxide is 1:(1.5~4).
4. a kind of preparation method of MXene- carbonization Kevlar fento laminated film according to claim 1 or 2, feature
The ratio for being the volume of the quality and anhydrous dimethyl sulphoxide of Kafra fiber in step 1 is 1g:(500~1000) mL.
5. a kind of preparation method of MXene- carbonization Kevlar fento laminated film according to claim 1 or 2, feature
It is that the temperature stirred in step 1 is 20~25 DEG C, mixing time is 7~10 days.
6. a kind of preparation method of MXene- carbonization Kevlar fento laminated film according to claim 1 or 2, feature
The ratio for being the volume for the hydrochloric acid solution that the quality Yu concentration of LiF in step 2 are 6~12mol/L is 1g:(10~30) mL.
7. a kind of preparation method of MXene- carbonization Kevlar fento laminated film according to claim 1 or 2, feature
It is Ti in step 23AlC2Mass ratio with LiF is 1:(1~2).
8. a kind of preparation method of MXene- carbonization Kevlar fento laminated film according to claim 1 or 2, feature
It is in step 3 c that soaking time is 1.5~2.5 days.
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