CN110330677A - A kind of MXene/ polypyrrole nanotube composite film and preparation method thereof - Google Patents
A kind of MXene/ polypyrrole nanotube composite film and preparation method thereof Download PDFInfo
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- CN110330677A CN110330677A CN201910550044.4A CN201910550044A CN110330677A CN 110330677 A CN110330677 A CN 110330677A CN 201910550044 A CN201910550044 A CN 201910550044A CN 110330677 A CN110330677 A CN 110330677A
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- C08G73/0605—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0611—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring, e.g. polypyrroles
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Abstract
The present invention provides a kind of MXene/ polypyrrole nanotube composite film and preparation method thereof, the preparation method, the following steps are included: after MXene dispersion liquid and polypyrrole nanotube dispersion liquid are mixed, stirring a period of time, then, vacuum filter, vacuum drying, obtains MXene/ polypyrrole nanotube composite film.The preparation method of MXene/ polypyrrole nanotube composite film of the invention is by mixing MXene dispersion liquid into polypyrrole nanotube dispersion liquid, then, MXene/ polypyrrole nanotube composite film is made using vacuum drying method, its preparation process is simple, without complex device, it can fast filming, effectively reduce production cost, application easy to spread, and the use of preparation method of the invention without chemical solvents such as organic solvents, it is environmentally friendly, in addition, the made MXene/ polypyrrole nanotube composite film of present invention photothermal conversion efficiency with higher and flexibility, its photothermal conversion efficiency is up to 87%.
Description
Technical field
The present invention relates to new material technology field, in particular to a kind of MXene/ polypyrrole nanotube composite film and its system
Preparation Method.
Background technique
Polypyrrole can be made by pyrrole monomer by chemical oxidization method or electrochemical method, and chemical oxidation method is molten
Oxidant is utilized in agent system, causes polymerization such as trivalent iron salt, the chemical structure of polypyrrole decides that he has excellent conduction
Performance, synthesis technology is simple, has many advantages, such as that air stability is good, nontoxic, is widely used to electrochemical field and biology
Material Field.But the preparation of existing polypyrrole composite film need to usually use organic dyestuff and organic solvent, it is caused to prepare
Journey is complex, higher cost, is unfavorable for promoting, and has larger pollution to environment.
Therefore, it is low to develop a kind of preparation cost, simple and quick can form a film, is suitble to promote and apply, it is environmentally friendly, there is height
The polypyrrole nanotube composite film of effect photothermal conversion efficiency has a very important significance.
Summary of the invention
In view of this, the present invention is directed to propose a kind of preparation method of MXene/ polypyrrole nanotube composite film, with solution
Certainly existing polypyrrole nanotube composite film preparation process is complicated, preparation cost is high, has the problem of larger pollution to environment.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:
A kind of preparation method of MXene/ polypyrrole nanotube composite film, comprising the following steps:
After MXene dispersion liquid and polypyrrole nanotube dispersion liquid are mixed, stirring a period of time, then, vacuum filter, very
Sky is dry, obtains MXene/ polypyrrole nanotube composite film.
Optionally, the concentration of the MXene dispersion liquid is 1-3mg/mL.
Optionally, the concentration of the polypyrrole nanotube dispersion liquid is 1-3mg/mL.
Optionally, the volume ratio of the MXene dispersion liquid and the polypyrrole nanotube dispersion liquid is 1: 3~3: 1.
Optionally, the mixing time of the stirring is 10-30min.
Optionally, the filter membrane of the vacuum filter is one of polyvinylidene fluoride film and polycarbonate membrane.
Optionally, the vacuum drying drying temperature is 50-60 DEG C, drying time 0.5-1h.
The second object of the present invention is to provide a kind of using MXene/ polypyrrole nanotube made from above-mentioned preparation method
Laminated film.
Compared with the existing technology, the preparation method of MXene/ polypyrrole nanotube composite film of the present invention have with
Lower advantage:
The preparation method of MXene/ polypyrrole nanotube composite film of the invention is by polypyrrole nanotube dispersion liquid
Then MXene/ polypyrrole nanotube composite film, system is made using vacuum drying method in middle mixing MXene dispersion liquid
Standby process is simple, is not necessarily to complex device, can fast filming, effectively reduce production cost, application easy to spread, and of the invention
Use of the preparation method without chemical solvents such as organic solvents, it is environmentally friendly, in addition, the made MXene/ polypyrrole of the present invention is received
Mitron laminated film photothermal conversion efficiency with higher and flexibility, photothermal conversion efficiency is up to 87%.
Specific embodiment
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the present invention can phase
Mutually combination.
MXene is a kind of metal carbides with two-dimensional layered structure and metal nitride new material, with graphene
Potato chips similar, that shape photo piece stacks, with unique two-dimensional layered structure, high-specific surface area and good hydrophilicity
And high conduction performance, the present invention is based on this, MXene is applied to the preparation of polypyrrole nanotube composite film, to provide one kind
Preparation process is simple, preparation cost is low, environmentally friendly, and products made thereby has efficient photothermal conversion efficiency and higher flexibility
The preparation method of MXene/ polypyrrole nanotube composite film.
Below in conjunction with embodiment, the present invention will be described in detail.
Embodiment 1
A kind of preparation method of MXene/ polypyrrole nanotube composite film, comprising the following steps:
The polypyrrole nanotube dispersion liquid that 10mL concentration is 1mg/mL is added to the MXene that 10mL concentration is 1mg/mL and is divided
After being mixed in dispersion liquid, magnetic agitation 30min, then, vacuum filter, and it is dried in vacuo 0.5h at 50 DEG C, it is poly- to obtain MXene/
Pyrroles's nanotube composite film,
Wherein, concentration is that the MXene dispersion liquid of 1mg/mL is prepared especially by following method:
It is sufficiently stirred in plastic beaker after hydrochloric acid and 3.2g lithium fluoride that 40mL concentration is 9mol/L are mixed, then,
2g titanium aluminum carbide is added, and after being stirred for 24 hours under conditions of 35 DEG C, reaction product is separated, light green liquid is obtained, then,
Deionized water is added into light green liquid to stir and evenly mix, then 60min is centrifuged with the revolving speed of 3500rpm, is uniformly peeled off
MXene supernatant liquor, as MXene solution；
MXene solution is filtered, is dried, obtains MXene solid matter；
It takes 10mg MXene solid matter to be scattered in 10mL deionized water, obtains the MXene solution that concentration is 1mg/mL.
Concentration is that the polypyrrole nanotube dispersion liquid of 1mg/mL is prepared especially by following method:
The ammonium persulfate of 1mmol is added to the methyl orange aqueous solution that 20mL concentration is 5mmol/L under stirring conditions
In, then, 3mmol pyrrole monomer is introduced, stirs 2min, then be not stirred to react at room temperature for 24 hours, then, be washed with deionized water
Suction filtration is washed to colourless, then at 80 DEG C dry 6h to get polypyrrole nanotube；
It disperses 10mg polypyrrole nanotube in 10mL deionized water, obtains the polypyrrole nanotube that concentration is 1mg/mL
Dispersion liquid.
In addition, the filter membrane in vacuum filtration process is polycarbonate membrane.
Pass through η=vHe/qsolarMeasure the photothermal conversion effect of the MXene/ polypyrrole nanotube composite film of the present embodiment
Rate, time of measuring are 1 hour, every the quality of 5min record water reduction in measurement process, wherein η is photothermal conversion efficiency；v
For water evaporation rate, unit kg/m2；HeFor the vaporization enthalpy of water, vaporization enthalpy depends on temperature, unit kJ/kg；qsolarFor light
Solar power density after stablizing according to 1 hour, unit kJ/m2。
The photothermal conversion efficiency of the calculation shows that, the MXene/ polypyrrole nanotube composite film of the present embodiment is
81.8%.
The flexibility of the MXene/ polypyrrole nanotube composite film of the present embodiment is tested.
After tested it is found that by 10 folded bents, the MXene/ polypyrrole nanotube composite film of the present embodiment is remained to
It keeps intact, can't occur to rupture or damages, illustrate it with excellent flexibility.
Embodiment 2
A kind of preparation method of MXene/ polypyrrole nanotube composite film, comprising the following steps:
The polypyrrole nanotube dispersion liquid that 10mL concentration is 2mg/mL is added to the MXene that 10mL concentration is 1mg/mL and is divided
After being mixed in dispersion liquid, magnetic agitation 30min, then, vacuum filter, and it is dried in vacuo 1h at 55 DEG C, obtain the poly- pyrrole of MXene/
Nanotube composite film is coughed up,
Wherein, concentration is the specific preparation method of the MXene dispersion liquid of 1mg/mL with embodiment 1.
Concentration is that the polypyrrole nanotube dispersion liquid of 2mg/mL is prepared especially by following method:
The ammonium persulfate of 1mmol is added to the methyl orange aqueous solution that 20mL concentration is 5mmol/L under stirring conditions
In, then, 3mmol pyrrole monomer is introduced, stirs 2min, then be not stirred to react at room temperature for 24 hours, then, be washed with deionized water
Suction filtration is washed to colourless, then at 80 DEG C dry 6h to get polypyrrole nanotube；
It disperses 20mg polypyrrole nanotube in 10mL deionized water, obtains the polypyrrole nanotube that concentration is 2mg/mL
Dispersion liquid.
In addition, the filter membrane in vacuum filtration process is polyvinylidene fluoride film.
Pass through η=vHe/qsolarMeasure the photothermal conversion effect of the MXene/ polypyrrole nanotube composite film of the present embodiment
Rate, time of measuring are 1 hour, every the quality of 5min record water reduction in measurement process, wherein η is photothermal conversion efficiency；v
For water evaporation rate, unit kg/m2；HeFor the vaporization enthalpy of water, vaporization enthalpy depends on temperature, unit kJ/kg；qsolarFor light
Solar power density after stablizing according to 1 hour, unit kJ/m2。
The photothermal conversion efficiency of the calculation shows that, the MXene/ polypyrrole nanotube composite film of the present embodiment is
84.3%.
The flexibility of the MXene/ polypyrrole nanotube composite film of the present embodiment is tested.
After tested it is found that by 15 folded bents, the MXene/ polypyrrole nanotube composite film of the present embodiment is remained to
It keeps intact, can't occur to rupture or damages, illustrate it with excellent flexibility.
Embodiment 3
A kind of preparation method of MXene/ polypyrrole nanotube composite film, comprising the following steps:
The polypyrrole nanotube dispersion liquid that 10mL concentration is 3mg/mL is added to the MXene that 10mL concentration is 1mg/mL and is divided
After being mixed in dispersion liquid, magnetic agitation 30min, then, vacuum filter, and it is dried in vacuo 0.8h at 58 DEG C, it is poly- to obtain MXene/
Pyrroles's nanotube composite film,
Wherein, concentration is the specific preparation method of the MXene dispersion liquid of 1mg/mL with embodiment 1.
Concentration is that the polypyrrole nanotube dispersion liquid of 3mg/mL is prepared especially by following method:
The ammonium persulfate of 1mmol is added to the methyl orange aqueous solution that 20mL concentration is 5mmol/L under stirring conditions
In, then, 3mmol pyrrole monomer is introduced, stirs 2min, then be not stirred to react at room temperature for 24 hours, then, be washed with deionized water
Suction filtration is washed to colourless, then at 80 DEG C dry 6h to get polypyrrole nanotube；
It disperses 30mg polypyrrole nanotube in 10mL deionized water, obtains the polypyrrole nanotube that concentration is 3mg/mL
Dispersion liquid.
In addition, the filter membrane in vacuum filtration process is polycarbonate membrane.
Pass through η=vHe/qsolarMeasure the photothermal conversion effect of the MXene/ polypyrrole nanotube composite film of the present embodiment
Rate, time of measuring are 1 hour, every the quality of 5min record water reduction in measurement process, wherein η is photothermal conversion efficiency；v
For water evaporation rate, unit kg/m2；HeFor the vaporization enthalpy of water, vaporization enthalpy depends on temperature, unit kJ/kg；qsolarFor light
Solar power density after stablizing according to 1 hour, unit kJ/m2。
The photothermal conversion efficiency of the calculation shows that, the MXene/ polypyrrole nanotube composite film of the present embodiment is
85.6%.
The flexibility of the MXene/ polypyrrole nanotube composite film of the present embodiment is tested.
After tested it is found that by 18 folded bents, the MXene/ polypyrrole nanotube composite film of the present embodiment is remained to
It keeps intact, can't occur to rupture or damages, illustrate it with excellent flexibility.
Embodiment 4
A kind of preparation method of MXene/ polypyrrole nanotube composite film, comprising the following steps:
The polypyrrole nanotube dispersion liquid that 10mL concentration is 1mg/mL is added to the MXene that 10mL concentration is 2mg/mL and is divided
After being mixed in dispersion liquid, magnetic agitation 30min, then, vacuum filter, and it is dried in vacuo 1h at 56 DEG C, obtain the poly- pyrrole of MXene/
Nanotube composite film is coughed up,
Wherein, concentration is that the MXene dispersion liquid of 2mg/mL is prepared especially by following method:
It is sufficiently stirred in plastic beaker after hydrochloric acid and 3.2g lithium fluoride that 40mL concentration is 9mol/L are mixed, then,
2g titanium aluminum carbide is added, and after being stirred for 24 hours under conditions of 35 DEG C, reaction product is separated, light green liquid is obtained, then,
Deionized water is added into light green liquid to stir and evenly mix, then 60min is centrifuged with the revolving speed of 3500rpm, is uniformly peeled off
MXene supernatant liquor, as MXene solution；
MXene solution is filtered, is dried, obtains MXene solid matter；
It takes 20mg MXene solid matter to be scattered in 10mL deionized water, obtains the MXene solution that concentration is 2mg/mL.
Concentration is the specific preparation method of the polypyrrole nanotube dispersion liquid of 1mg/mL with embodiment 1.
In addition, the filter membrane in vacuum filtration process is polyvinylidene fluoride film.
Pass through η=vHe/qsolarMeasure the photothermal conversion effect of the MXene/ polypyrrole nanotube composite film of the present embodiment
Rate, time of measuring are 1 hour, every the quality of 5min record water reduction in measurement process, wherein η is photothermal conversion efficiency；v
For water evaporation rate, unit kg/m2；HeFor the vaporization enthalpy of water, vaporization enthalpy depends on temperature, unit kJ/kg；qsolarFor light
Solar power density after stablizing according to 1 hour, unit kJ/m2。
The photothermal conversion efficiency of the calculation shows that, the MXene/ polypyrrole nanotube composite film of the present embodiment is
86.1%.
The flexibility of the MXene/ polypyrrole nanotube composite film of the present embodiment is tested.
After tested it is found that by 20 folded bents, the MXene/ polypyrrole nanotube composite film of the present embodiment is remained to
It keeps intact, can't occur to rupture or damages, illustrate it with excellent flexibility.
Embodiment 5
A kind of preparation method of MXene/ polypyrrole nanotube composite film, comprising the following steps:
The polypyrrole nanotube dispersion liquid that 10mL concentration is 2mg/mL is added to the MXene that 10mL concentration is 2mg/mL and is divided
After being mixed in dispersion liquid, magnetic agitation 30min, then, vacuum filter, and it is dried in vacuo 1h at 60 DEG C, obtain the poly- pyrrole of MXene/
Nanotube composite film is coughed up,
Wherein, concentration is the specific preparation method of the MXene dispersion liquid of 2mg/mL with embodiment 4.
Concentration is the specific preparation method of the polypyrrole nanotube dispersion liquid of 2mg/mL with embodiment 2.
In addition, the filter membrane in vacuum filtration process is polycarbonate membrane.
Pass through η=vHe/qsolarMeasure the photothermal conversion effect of the MXene/ polypyrrole nanotube composite film of the present embodiment
Rate, time of measuring are 1 hour, every the quality of 5min record water reduction in measurement process, wherein η is photothermal conversion efficiency；v
For water evaporation rate, unit kg/m2；HeFor the vaporization enthalpy of water, vaporization enthalpy depends on temperature, unit kJ/kg；qsolarFor light
Solar power density after stablizing according to 1 hour, unit kJ/m2。
The calculation shows that, the photothermal conversion efficiency of the MXene/ polypyrrole nanotube composite film of the present embodiment are 87%.
The flexibility of the MXene/ polypyrrole nanotube composite film of the present embodiment is tested.
After tested it is found that by 25 folded bents, the MXene/ polypyrrole nanotube composite film of the present embodiment is remained to
It keeps intact, can't occur to rupture or damages, illustrate it with excellent flexibility.
Embodiment 6
A kind of preparation method of MXene/ polypyrrole nanotube composite film, comprising the following steps:
The polypyrrole nanotube dispersion liquid that 10mL concentration is 1mg/mL is added to the MXene that 10mL concentration is 3mg/mL and is divided
After being mixed in dispersion liquid, magnetic agitation 30min, then, vacuum filter, and it is dried in vacuo 0.8h at 58 DEG C, it is poly- to obtain MXene/
Pyrroles's nanotube composite film,
Wherein, concentration is that the MXene dispersion liquid of 3mg/mL is prepared especially by following method:
It is sufficiently stirred in plastic beaker after hydrochloric acid and 3.2g lithium fluoride that 40mL concentration is 9mol/L are mixed, then,
2g titanium aluminum carbide is added, and after being stirred for 24 hours under conditions of 35 DEG C, reaction product is separated, light green liquid is obtained, then,
Deionized water is added into light green liquid to stir and evenly mix, then 60min is centrifuged with the revolving speed of 3500rpm, is uniformly peeled off
MXene supernatant liquor, as MXene solution；
MXene solution is filtered, is dried, obtains MXene solid matter；
It takes 30mg MXene solid matter to be scattered in 10mL deionized water, obtains the MXene solution that concentration is 3mg/mL.
Concentration is the specific preparation method of the polypyrrole nanotube dispersion liquid of 1mg/mL with embodiment 1.
In addition, the filter membrane in vacuum filtration process is polyvinylidene fluoride film.
Pass through η=vHe/qsolarMeasure the photothermal conversion effect of the MXene/ polypyrrole nanotube composite film of the present embodiment
Rate, time of measuring are 1 hour, every the quality of 5min record water reduction in measurement process, wherein η is photothermal conversion efficiency；v
For water evaporation rate, unit kg/m2；HeFor the vaporization enthalpy of water, vaporization enthalpy depends on temperature, unit kJ/kg；qsolarFor light
Solar power density after stablizing according to 1 hour, unit kJ/m2。
The photothermal conversion efficiency of the calculation shows that, the MXene/ polypyrrole nanotube composite film of the present embodiment is
84.7%.
The flexibility of the MXene/ polypyrrole nanotube composite film of the present embodiment is tested.
After tested it is found that by 30 folded bents, the MXene/ polypyrrole nanotube composite film of the present embodiment is remained to
It keeps intact, can't occur to rupture or damages, illustrate it with excellent flexibility.
The above is merely preferred embodiments of the present invention, be not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of preparation method of MXene/ polypyrrole nanotube composite film, which comprises the following steps:
After MXene dispersion liquid and polypyrrole nanotube dispersion liquid are mixed, stirring a period of time, then, vacuum filter, vacuum is done
It is dry, obtain MXene/ polypyrrole nanotube composite film.
2. the preparation method of MXene/ polypyrrole nanotube composite film according to claim 1, which is characterized in that described
The concentration of MXene dispersion liquid is 1-3mg/mL.
3. the preparation method of MXene/ polypyrrole nanotube composite film according to claim 1, which is characterized in that described
The concentration of polypyrrole nanotube dispersion liquid is 1-3mg/mL.
4. the preparation method of MXene/ polypyrrole nanotube composite film according to claim 1, which is characterized in that described
The volume ratio of MXene dispersion liquid and the polypyrrole nanotube dispersion liquid is 1: 3~3: 1.
5. the preparation method of MXene/ polypyrrole nanotube composite film according to claim 1, which is characterized in that described
The mixing time of stirring is 10-30min.
6. the preparation method of MXene/ polypyrrole nanotube composite film according to claim 1, which is characterized in that described
The filter membrane of vacuum filter is one of polyvinylidene fluoride film and polycarbonate membrane.
7. the preparation method of MXene/ polypyrrole nanotube composite film according to claim 1, which is characterized in that described
Vacuum drying drying temperature is 50-60 DEG C, drying time 0.5-1h.
8. a kind of MXene/ polypyrrole nanotube composite film, which is characterized in that the MXene/ polypyrrole nanotube THIN COMPOSITE
Film is made by the preparation method of the described in any item MXene/ polypyrrole nanotube composite films of claim 1 to 7.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106128799A (en) * | 2016-07-15 | 2016-11-16 | 武汉工程大学 | A kind of preparation method based on Graphene/polypyrrole nanotube composite film ultracapacitor |
| JP2018527275A (en) * | 2015-07-03 | 2018-09-20 | 河海大学 | Method for preparing sulfonated two-dimensional titanium carbide nanosheets |
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2019
- 2019-06-24 CN CN201910550044.4A patent/CN110330677A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2018527275A (en) * | 2015-07-03 | 2018-09-20 | 河海大学 | Method for preparing sulfonated two-dimensional titanium carbide nanosheets |
| CN106128799A (en) * | 2016-07-15 | 2016-11-16 | 武汉工程大学 | A kind of preparation method based on Graphene/polypyrrole nanotube composite film ultracapacitor |
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| Title |
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| 刘晓辉等: "MXene/聚吡咯复合材料的制备及其超电性能研究", 《电子元件与材料》 * |
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Application publication date: 20191015 |
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