CN106750277B - A kind of MXene- polyaniline composite material and preparation method thereof - Google Patents
A kind of MXene- polyaniline composite material and preparation method thereof Download PDFInfo
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G73/0266—Polyanilines or derivatives thereof
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Abstract
A kind of MXene- polyaniline composite material and preparation method thereof, the present invention relates to a kind of preparation methods of MXene composite material.The present invention is to solve the technical problems of the absorbing property difference of existing two-dimentional transition metal carbide Mxene.MXene- polyaniline composite material of the invention by stratiform two-dimentional transition metal carbide and be coated on the polyaniline shell on two-dimentional transition metal carbide surface and form.Preparation method: aniline being added to the water after stirring, aniline/water dispersion liquid is obtained, then adjusting pH value is 1.5~2, obtains the HCI solution of aniline；The HCI solution of amine is added to low temperature in the aqueous dispersions of two-dimentional transition metal carbide to mix, obtains MXene/ aniline mixed liquor；Ammonium persulfate solution is added drop-wise in MXene/ aniline mixed liquor again, low temperature reaction, then washs, dry, obtains MXene- polyaniline composite material.It can be used for inhaling wave field.
Description
Technical field
The present invention relates to a kind of preparation methods of MXene composite material.
Background technique
2011 Univ Drexel, the U.S. (Drexel University) Yury Gogotsi professor and Michel
W.Barsoum professor et al. cooperation has found a kind of New Two Dimensional transition metal carbide or carbonitride, since its is unique
The layer assembling structure of similar graphene (graphene), is named as MXene.Its chemical general formula can use Mn+1XnTzIt indicates, wherein M
Refer to that magnesium-yttrium-transition metal, X refer to that C or/and N, n are generally 1~3, TzRefer to surface group (such as OH-、F-Deng).It has the high ratio of graphene
It is the characteristics of surface area, high conductivity, flexibly adjustable but also with component, the advantages such as minimum nanometer thickness is controllable, in energy storage, inhale
The fields such as attached, sensor, conductive filler show huge potentiality.Nowadays, MXene is also less in the application for inhaling wave field,
Due to its excellent electrical property, dielectric loss can occur when electromagnetic wave passes through.However, the absorbing property of pure MXene is unsatisfactory.
Summary of the invention
The present invention is to solve existing two-dimentional transition metal carbide or the technologies of carbonitride MXene absorbing property difference
Problem, and a kind of MXene- polyaniline composite material is provided and preparation method thereof.
MXene- polyaniline composite material of the invention is the two-dimentional transition metal carbide by stratiform and is coated on two dimension
The polyaniline shell on transition metal carbide surface forms, wherein the two-dimentional quality of transition metal carbide and the quality of polyaniline
The ratio between be 1:(0.5~2.5).
In MXene- polyaniline composite material of the invention, polyaniline uniform adsorption is on the surface MXene, thus in MXene
Surface forms one layer of clad, works as electricity so that composite material reaches impedance matching by the electrical property that polyaniline adjusts MXene
When magnetic wave passes through, loss will be generated, so that electromagnetic wave signal weakens.Simultaneously because MXene multilayer performance and polyaniline-coated layer
Presence, enable electromagnetic wave roundtrip wherein, expand electromagnetic wave attenuation path, further enhance the suction of material
Wave performance.
The preparation method of above-mentioned MXene- polyaniline composite material, sequentially includes the following steps:
One, two-dimentional transition metal carbide (MXene), aniline and ammonium persulfate [(NH are weighed4)2S2O8], wherein two-dimentional mistake
The ratio for crossing the quality of metal carbides and the volume of aniline is 1g:(0.3~3) mL, the quality of ammonium persulfate and the volume of aniline
Ratio be (2.5~2.75) g:1ml；
Two, aniline is added to the water, aniline/water dispersion liquid is obtained after stirring, then adjust aniline/water dispersion liquid with hydrochloric acid
PH value be 1.5~2, obtain the HCI solution of aniline；
Three, the HCI solution of aniline is added in the aqueous dispersions of two-dimentional transition metal carbide, at 0~5 DEG C
It is stirred 6~18h, obtains MXene/ aniline mixed liquor；
Four, it dissolves ammonium persulfate into water, is 1.5~2 with salt acid for adjusting pH value, ammonium persulfate solution is obtained, by the mistake
Ammonium sulfate is added drop-wise in MXene/ aniline mixed liquor, is stirred to react 6~18h under conditions of 0~5 DEG C, after completion of the reaction,
With salt acid elution 3~5 times that pH is 1.5, centrifugal drying obtains MXene- polyaniline composite material.
The HCI solution of aniline is added to two-dimentional mistake by the preparation method of MXene- polyaniline composite material of the invention
It crosses in the aqueous dispersions of metal carbides, in whipping process, interlayer of the aniline monomer well into two-dimentional transition metal carbide
And it is adsorbed on surface, since the hydrochloride of aniline is positively charged, the surface of two-dimentional transition metal carbide has a large amount of OH-、
F-, keep its negatively charged, positive and negative charge attracts each other, and causes aniline monomer uniform adsorption in two-dimentional transition metal carbide table
Face recycles ammonium persulfate that aniline monomer is polymerize, and forms the polyaniline shell for being coated on two-dimentional transition metal carbide surface
Layer.Since polyaniline (PANI) is a kind of conduction high polymer, there is excellent electrical property.The polyaniline in MXene surface recombination
Afterwards, polyaniline will improve the electrical property of MXene, and the impedance of MXene/PANI compound can be made to reach one good
Match, dielectric loss will be occurred when electromagnetic wave passes through this material, at the same MXene interlayer it is also possible that electromagnetic wave in material
In roundtrip, and then increase electromagnetic wave decay path, so that material generates excellent absorbing property.
MXene- polyaniline composite material prepared by the present invention can be used for inhaling wave field.
Detailed description of the invention
Fig. 1 is the Ti for testing 1 preparation3C2Stereoscan photograph；
Fig. 2 is the stereoscan photograph for testing the MXene- polyaniline composite material of 1 preparation；
Specific embodiment
Specific embodiment 1: the MXene- polyaniline composite material of present embodiment is the two-dimentional transition metal by stratiform
Carbide and the polyaniline shell composition for being coated on two-dimentional transition metal carbide surface, wherein two-dimentional transition metal carbide or
The quality of carbonitride and the mass ratio of polyaniline are 1:(0.5~2.5).
Specific embodiment 2: the preparation method of MXene- polyaniline composite material described in specific embodiment one, is pressed
Following steps carry out:
One, two-dimentional transition metal carbide (MXene), aniline and ammonium persulfate [(NH are weighed4)2S2O8], wherein two-dimentional mistake
The ratio for crossing the quality of metal carbides and the volume of aniline is 1g:(0.3~3) mL, the quality of ammonium persulfate and the volume of aniline
Ratio be (2.5~2.75) g:1ml；
Two, aniline is added to the water, aniline/water dispersion liquid is obtained after stirring, then adjust aniline/water dispersion liquid with hydrochloric acid
PH value be 1.5~2, obtain the HCI solution of aniline；
Three, the HCI solution of aniline is added in the aqueous dispersions of two-dimentional transition metal carbide, at 0~5 DEG C
It is stirred 6~18h, obtains MXene/ aniline mixed liquor；
Four, it dissolves ammonium persulfate into water, is 1.5~2 with salt acid for adjusting pH value, ammonium persulfate solution is obtained, by the mistake
Ammonium sulfate is added drop-wise in MXene/ aniline mixed liquor, is stirred to react 6~18h under conditions of 0~5 DEG C, after completion of the reaction,
With salt acid elution 3~5 times that pH is 1.5, centrifugal drying obtains MXene- polyaniline composite material.
Specific embodiment 3: present embodiment two dimension mistake described in step 1 unlike specific embodiment two
Crossing metal carbides is Ti3C2；It is other to be identical with embodiment two.
Specific embodiment 4: present embodiment two dimension mistake described in step 1 unlike specific embodiment three
Crossing metal carbides is Ti3C2Preparation method sequentially include the following steps:
(1) concentrated hydrochloric acid and lithium fluoride that concentration is 6mol/L~12mol/L are fully mixed to uniformly in plastic containers,
Obtain milky mixed liquor；Wherein the ratio of the quality of the volume and lithium fluoride of concentrated hydrochloric acid is 10ml:(0.5~1.5) g；
(2) under agitation, by Ti3AlC2Be added in mixed liquor, the reaction process acutely and heat release, wherein
Ti3AlC2Mass ratio with lithium fluoride is 1:(1~1.5)；After adding, it is stirred to react 24~60h at 40~60 DEG C, reacts
After be washed to pH value be 5~6, obtain Ti3C2Slurries.
It is other to be the same as the specific implementation mode 3.
Specific embodiment 5: unlike one of present embodiment and specific embodiment two to four described in step 2
Hydrochloric acid concentration be 2mol/L；It is other identical as one of specific embodiment two to four.
Specific embodiment 6: being stirred in step 3 unlike one of present embodiment and specific embodiment two to five
Mixing temperature when mixing is 3 DEG C, incorporation time 12h；It is other identical as one of specific embodiment two to four.
Specific embodiment 7: being adjusted in step 4 unlike one of present embodiment and specific embodiment two to six
The concentration of hydrochloric acid used in pH value is 2mol/L；It is other identical as one of specific embodiment two to six.
Specific embodiment 8: being stirred in step 4 unlike one of present embodiment and specific embodiment two to six
The temperature of reaction is 3 DEG C, reaction time 12h；It is other identical as one of specific embodiment two to six.
With following verification experimental verification beneficial effects of the present invention:
Test 1: the preparation method of the MXene- polyaniline composite material of this test sequentially includes the following steps:
One, two-dimentional transition metal carbide Ti is prepared3C2, process sequentially includes the following steps:
(1) concentrated hydrochloric acid and 1.2g lithium fluoride that 10mL concentration is 10mol/L are fully mixed to uniformly in plastic containers,
Obtain milky mixed liquor；
(2) under agitation, by 1g Ti3AlC2Be added in mixed liquor, the reaction process acutely and heat release, add it
Afterwards, 48h is stirred to react at 50 DEG C, being washed to pH value after reaction is 5.5, obtains Ti3C2Slurries；
Two, MXene- polyaniline composite material is prepared, process sequentially includes the following steps:
(1) it weighs and contains 0.5gTi3C2Ti3C2Slurries, 0.5mL aniline and 1.25g ammonium persulfate [(NH4)2S2O8]；
(2) aniline is added in 32.5mL water, aniline/water dispersion liquid is obtained after stirring, then adjusted with 2mol/L hydrochloric acid
The pH value of aniline/water dispersion liquid is 1.5, obtains the HCI solution of aniline；
(3) HCI solution of aniline is added to Ti3C2In slurries, 12h is stirred at 1 DEG C, obtains Ti3C2/ aniline is mixed
Close liquid；
(4) it dissolves ammonium persulfate into 32.5mL water, is 1.5 with the salt acid for adjusting pH value of 2mol/L, obtains ammonium persulfate
The ammonium persulfate solution is added drop-wise to Ti by solution3C2/ aniline mixed liquor is stirred to react 12h, end of reaction under conditions of 1 DEG C
Afterwards, with salt acid elution 5 times that pH is 1.5, centrifugal drying obtains Ti3C2Polyaniline composite material.
The Ti of this test3C2After slurries drying, Ti is obtained3C2, stereoscan photograph as shown in Figure 1, it can be seen that
Ti3C2For layer structure.
The Ti that this test will be prepared in step 13C2After slurries are dry, Ti is obtained3C2Stereoscan photograph such as Fig. 1 institute
Show, as can be seen from Figure 1 Ti3C2For layer structure.The Ti that this test is prepared through step 23C2The scanning of polyaniline composite material
Electromicroscopic photograph is as shown in Fig. 2, figure it is seen that Ti3C2Surface occurs pattern and apparent variation occurs, and illustrates polyaniline success
It is combined to Ti3C2Surface, but its layer structure is still high-visible.
Ti prepared by this test3C2Polyaniline composite material is uniformly mixed with paraffin in mass ratio 1: 1 at 80 DEG C, is made
Annulus tests out the complex dielectric permittivity and complex permeability constant of sample using vector network analyzer, calculates it is found that when material is thick
Degree is 1.6mm, and at 17.2GHz, reflection loss reaches -45.26dB.When the reflection loss of material is -10dB, microwave absorption
Reach 90%, that is, thinks that material possesses good absorbing property, when reflection loss is -20dB, microwave absorption reaches 99%, when
When reflection loss is -40dB, microwave absorption has reached 99.99%.The Ti of this test preparation is proved after tested3C2Polyaniline is compound
Material wave-absorbing effect is good.
Test 2: the preparation method of the MXene- polyaniline composite material of this test sequentially includes the following steps:
One, two-dimentional transition metal carbide Ti is prepared3C2, process sequentially includes the following steps:
(1) concentrated hydrochloric acid and 1.5g lithium fluoride that 10mL concentration is 10mol/L are fully mixed to uniformly in plastic containers,
Obtain milky mixed liquor；
(2) under agitation, by 1.5Ti3AlC2Be added in mixed liquor, the reaction process acutely and heat release, add it
Afterwards, 50h is stirred to react at 60 DEG C, being washed to pH value after reaction is 5.5, obtains Ti3C2Slurries；
Two, MXene- polyaniline composite material is prepared, process sequentially includes the following steps:
(1) it weighs and contains 0.5gTi3C2Ti3C2Slurries, 1mL aniline and 2.5g ammonium persulfate [(NH4)2S2O8]；
(2) aniline is added in 32.5mL water, aniline/water dispersion liquid is obtained after stirring, then adjusted with 2mol/L hydrochloric acid
The pH value of aniline/water dispersion liquid is 1.5, obtains the HCI solution of aniline；
(3) HCI solution of aniline is added to Ti3C2In slurries, 12h is stirred at 3 DEG C, obtains Ti3C2/ aniline is mixed
Close liquid；
(4) it dissolves ammonium persulfate into 32.5mL water, is 1.5 with the salt acid for adjusting pH value of 2mol/L, obtains ammonium persulfate
The ammonium persulfate solution is added drop-wise to Ti by solution3C2/ aniline mixed liquor is stirred to react 18h, end of reaction under conditions of 3 DEG C
Afterwards, with salt acid elution 5 times that pH is 1.5, centrifugal drying obtains Ti3C2Polyaniline composite material.
Ti prepared by this test3C2Polyaniline composite material is uniformly mixed with paraffin in mass ratio 1: 1 at 80 DEG C, is made
Annulus tests out the complex dielectric permittivity and complex permeability constant of sample using vector network analyzer, calculates it is found that when material is thick
Degree is 1.4mm, and at 17.2GHz, reflection loss reaches -43.04dB, has good wave-absorbing effect.
Claims (7)
1. a kind of MXene- polyaniline composite material, it is characterised in that the composite material is carbonized by the two-dimentional transition metal of stratiform
Object and the polyaniline shell composition for being coated on two-dimentional transition metal carbide surface, wherein the quality of two-dimentional transition metal carbide
Mass ratio with polyaniline is 1:(0.5 ~ 2.5)；Wherein two-dimentional transition metal carbide is Ti3C2；MXene- polyaniline is compound
The preparation method of material sequentially includes the following steps:
One, two-dimentional transition metal carbide, aniline and ammonium persulfate are weighed, wherein the quality and benzene of two-dimentional transition metal carbide
The ratio of the volume of amine is 1g:(0.3 ~ 3) mL, the ratio of the volume of the quality and aniline of ammonium persulfate is (2.5 ~ 2.75) g:1ml；
Two, aniline is added to the water, aniline/water dispersion liquid is obtained after stirring, then adjust the pH of aniline/water dispersion liquid with hydrochloric acid
Value is 1.5 ~ 2, obtains the HCI solution of aniline；
Three, the HCI solution of aniline is added in the aqueous dispersions of two-dimentional transition metal carbide, is stirred at 0 ~ 5 DEG C mixed
6 ~ 18h is closed, MXene/ aniline mixed liquor is obtained；
Four, it dissolves ammonium persulfate into water, is 1.5 ~ 2 with salt acid for adjusting pH value, ammonium persulfate solution is obtained, by the ammonium persulfate
Solution is added drop-wise in MXene/ aniline mixed liquor, is stirred to react 6 ~ 18h under conditions of 0 ~ 5 DEG C, after completion of the reaction, is with pH
1.5 salt acid elution 3 ~ 5 times, centrifugal drying obtain MXene- polyaniline composite material.
2. the method for preparing a kind of MXene- polyaniline composite material described in claim 1, it is characterised in that this method press with
Lower step carries out:
One, two-dimentional transition metal carbide, aniline and ammonium persulfate are weighed, wherein the quality and benzene of two-dimentional transition metal carbide
The ratio of the volume of amine is 1g:(0.3 ~ 3) mL, the ratio of the volume of the quality and aniline of ammonium persulfate is (2.5 ~ 2.75) g:1ml；Institute
The two-dimentional transition metal carbide stated is Ti3C2；
Two, aniline is added to the water, aniline/water dispersion liquid is obtained after stirring, then adjust the pH of aniline/water dispersion liquid with hydrochloric acid
Value is 1.5 ~ 2, obtains the HCI solution of aniline；
Three, the HCI solution of aniline is added in the aqueous dispersions of two-dimentional transition metal carbide, is stirred at 0 ~ 5 DEG C mixed
6 ~ 18h is closed, MXene/ aniline mixed liquor is obtained；
Four, it dissolves ammonium persulfate into water, is 1.5 ~ 2 with salt acid for adjusting pH value, ammonium persulfate solution is obtained, by the ammonium persulfate
Solution is added drop-wise in MXene/ aniline mixed liquor, is stirred to react 6 ~ 18h under conditions of 0 ~ 5 DEG C, after completion of the reaction, is with pH
1.5 salt acid elution 3 ~ 5 times, centrifugal drying obtain MXene- polyaniline composite material.
3. a kind of preparation method of MXene- polyaniline composite material according to claim 2, it is characterised in that described
Two-dimentional transition metal carbide is Ti3C2Preparation method sequentially include the following steps:
(1) concentrated hydrochloric acid and lithium fluoride that concentration is 6mol/L ~ 12mol/L are fully mixed to uniformly in plastic containers, are obtained
Milky mixed liquor；Wherein the ratio of the quality of the volume and lithium fluoride of concentrated hydrochloric acid is 10ml:(0.5 ~ 1.5) g；
(2) under agitation, by Ti3AlC2Be added in mixed liquor, the reaction process acutely and heat release, wherein Ti3AlC2With
The mass ratio of lithium fluoride is 1:(1 ~ 1.5)；After adding, it is stirred to react 24 ~ 60h at 40 ~ 60 DEG C, is washed to after reaction
PH value is 5 ~ 6, obtains Ti3C2Slurries.
4. a kind of preparation method of MXene- polyaniline composite material according to claim 2 or 3, it is characterised in that step
The concentration of hydrochloric acid described in two is 2mol/L.
5. a kind of preparation method of MXene- polyaniline composite material according to claim 2 or 3, it is characterised in that step
Temperature in three when being stirred is 3 DEG C, incorporation time 12h.
6. a kind of preparation method of MXene- polyaniline composite material according to claim 2 or 3, it is characterised in that step
The concentration that hydrochloric acid used in pH value is adjusted in four is 2mol/L.
7. a kind of preparation method of MXene- polyaniline composite material according to claim 2 or 3, it is characterised in that step
The temperature being stirred to react in four is 3 DEG C, reaction time 12h.
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| CN112175478B (en) * | 2020-09-18 | 2022-03-15 | 上海船舶工艺研究所(中国船舶工业集团公司第十一研究所) | Trititanium dicarbonide-polypyrrole modified anticorrosive coating and preparation method thereof |
| CN112552801A (en) * | 2020-12-25 | 2021-03-26 | 南京大学 | Ti-containing alloy3C2TX(MXene)/polyaniline water-based anticorrosive paint and preparation method thereof |
| CN113426428B (en) * | 2021-06-28 | 2022-04-29 | 武汉大学 | Polyaniline-sulfur nitrogen MXene/sodium alginate composite gel adsorbent and preparation method and application thereof |
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