CN109336083A - A kind of method of High Internal Phase Emulsion template controllable preparation foamy carbon/carbon nano tube compound material - Google Patents
A kind of method of High Internal Phase Emulsion template controllable preparation foamy carbon/carbon nano tube compound material Download PDFInfo
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- CN109336083A CN109336083A CN201811194113.4A CN201811194113A CN109336083A CN 109336083 A CN109336083 A CN 109336083A CN 201811194113 A CN201811194113 A CN 201811194113A CN 109336083 A CN109336083 A CN 109336083A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000000839 emulsion Substances 0.000 title claims abstract description 42
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 28
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 28
- 239000000463 material Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 21
- -1 carbon nano tube compound Chemical class 0.000 title claims abstract description 20
- 239000002131 composite material Substances 0.000 claims abstract description 29
- 229920000767 polyaniline Polymers 0.000 claims abstract description 16
- 239000006260 foam Substances 0.000 claims abstract description 15
- 239000000178 monomer Substances 0.000 claims abstract description 11
- 229920000642 polymer Polymers 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000003999 initiator Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 4
- 238000000605 extraction Methods 0.000 claims abstract description 4
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- 238000013019 agitation Methods 0.000 claims abstract description 3
- 239000012043 crude product Substances 0.000 claims abstract 2
- 239000004094 surface-active agent Substances 0.000 claims abstract 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 11
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 6
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 239000011148 porous material Substances 0.000 abstract description 10
- 238000003763 carbonization Methods 0.000 abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 4
- 230000033228 biological regulation Effects 0.000 abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000002861 polymer material Substances 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 description 18
- 238000002474 experimental method Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- 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
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- 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
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F112/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F112/34—Monomers containing two or more unsaturated aliphatic radicals
- C08F112/36—Divinylbenzene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention belongs to field of polymer material preparing technology, and in particular to a kind of method of High Internal Phase Emulsion template controllable preparation foamy carbon/carbon nano tube compound material.-- surfactant, monomer and initiator are dissolved in oil-based solvent and obtain oily phase, the water phase for being dispersed with PANI-CNT is slowly dropped in oily phase under mechanical agitation, water-in-oil type High Internal Phase Emulsion is obtained, polymerization reaction is then carried out, obtains solid block crude product.Interior phase is removed with dehydrated alcohol extraction, obtains porous polymer composite material precursor after dry；Carbonization obtains foam carbon composite under nitrogen protection.A series of foamy carbon/carbon nano tube compound materials with Different Pore Structures are made in the content of PANI-CNT in covering amount and High Internal Phase Emulsion of the present invention by changing carbon nano tube surface polyaniline, realize the regulation to foam carbon composite pore structure.
Description
Technical field
The invention belongs to field of polymer material preparing technology, and in particular to a kind of High Internal Phase Emulsion template controllable preparation
Foamy carbon/carbon nano tube compound material method.
Background technique
Supercapacitor is a kind of new energy between battery and traditional capacitor, and it is a kind of have quickly fill
The energy storage device of electric energy power.Various electrode materials applied to supercapacitor include carbon material, conducting polymer, metal oxidation
Object and its composite material, especially carbon material are considered as most having prospect and application most because of its good physical and chemical properties
One of wide electrode material.
High Internal Phase Emulsion refers to the lotion that interior phase or dispersed phase volume fraction are greater than or equal to 74%.High Internal Phase Emulsion template
Method is to prepare one of high porosity, effective way of multistage pore polymer, and be able to achieve the Effective Regulation to pore structure.Phase in height
There is the porous material of emulsion template method preparation simple preparation method, aperture size and distribution can controllably, between hole be mutually communicated
Advantage.Using the method for polymer carbonization, the preparation of multi-stage porous carbon composite material is realized, pore structure is constructed, and by changing
Become conditional parameter, realizes regulating and controlling to multi-stage porous carbon composite material pore structure.
Carbon nanotube has good electric conductivity, has low effect series electrical when making it as electrode material for super capacitor
Resistance and good power characteristic, therefore its application just concern by numerous researchers as electrode material.The present invention passes through
Change the content of the carbon nanotube PANI-CNT of polyaniline-coated in High Internal Phase Emulsion template, realizes compound to the foamy carbon of preparation
The Effective Regulation of material pore structure；Polyaniline-coated can improve its dispersibility in aqueous solution on the surface of carbon nanotube
Can, after the polymer composite carbonization prepared by High Internal Phase Emulsion template, the wetting of foam carbon composite obtained
Property increase, so as to generate good combination interface between electrolyte solution, improve the property of foam carbon composite
Energy；Nitrogen atom doping induction produces fake capacitance effect in PANI-CNT simultaneously, thus uses in water phase and be dispersed with PANI-CNT
High Internal Phase Emulsion template prepare foamy carbon/carbon nano tube compound material with good chemical property.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of High Internal Phase Emulsion template controllable preparation bubble
Foam carbon/carbon nano tube compound material method.By adjusting the content of PANI-CNT in High Internal Phase Emulsion template, realize to preparation
Foam carbon composite pore structure optimization, while polyaniline-coated can improve it in aqueous solution on the surface of carbon nanotube
In dispersion performance.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of method of High Internal Phase Emulsion template controllable preparation foamy carbon/carbon nano tube compound material, the specific steps are as follows:
(1) by a certain amount of monomer, initiator (molar ratio with monomer is 1:100) and 80 fully dissolved of span in oil-based solvent
In be made into oily phase；
(2) water phase for being dispersed with PANI-CNT is slowly added into the oily phase that step (1) obtains under mechanical agitation, is dripped
Add finish after continue stir 1h obtain water-in-oil type High Internal Phase Emulsion；
(3) polymerization reaction is carried out at 70 DEG C after sealing the High Internal Phase Emulsion that step (2) obtains, and is obtained solid block and is slightly produced
Object removes interior phase with dehydrated alcohol extraction, porous polymer composite material is obtained after vacuum drying；
(4) composite material obtained with a certain amount of potassium hydroxide solution mixing step (3), it is dry after under the conditions of 700 DEG C carbon
Change obtains foam carbon composite.
Monomer as described in step (1) is divinylbenzene.
Oil-based solvent as described in step (1) is toluene.
Initiator as described in step (1) is azodiisobutyronitrile.
Volume fraction of the span 80 as described in step (1) in oily phase is 5%-15%.
In step (1), the volume ratio of the monomer and oil-based solvent is 1:2-2:1.
The volume fraction of phase is 75%-95% in High Internal Phase Emulsion described in step (2).
The mass ratio of PANI/CNT is 0:1-5:1 in PANI-CNT water phase described in step (2).
PANI-CNT mass fraction in PANI-CNT water phase described in step (2) is 0%-10%.
The mass ratio of potassium hydroxide described in step (4) and step (3) composite material is 1:2-2:1.
The beneficial effects of the present invention are:
(1) a kind of method that the present invention develops High Internal Phase Emulsion template controllable preparation foamy carbon/carbon nano tube compound material.
By adjusting the content of PANI-CNT in High Internal Phase Emulsion template, realize to the effective of the foam carbon composite pore structure of preparation
Regulation, while nitrogen atom doping can induce generation fake capacitance effect in PANI-CNT, thus optimize chemical property, thus to carbon
The performance of composite material and application are of great significance.
(2) carbon nanotube has good electric conductivity and power characteristic, and polyaniline-coated can be on the surface of carbon nanotube
Improve its dispersion performance in aqueous solution, after the polymer composite carbonization prepared by High Internal Phase Emulsion template, system
The wetability of the foam carbon composite obtained increases, so as to generate good combination circle between electrolyte solution
The performance of foam carbon composite is improved in face.
Detailed description of the invention
The electron microscope for the foam carbon composite that Fig. 1 is embodiment 1-7, prepared by comparative example 1；Wherein, a figure is embodiment 1；
B figure is embodiment 2, and c figure is embodiment 3, and d figure is embodiment 4；E figure is embodiment 5；F figure is embodiment 6；G figure is embodiment
7；H figure is comparative example 1；
The nitrogen adsorption desorption curve graph for the foam carbon composite that Fig. 2 is embodiment 1-7, prepared by comparative example 1；
Fig. 3 is the constant current charge-discharge curve graph and cyclic voltammetry curve of foam carbon composite prepared by embodiment 2,5,6,7
Figure；Wherein, a figure is constant current charge-discharge curve graph；B figure is cyclic voltammetry curve figure.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be further described, but the present invention is not limited only to these embodiments.
Embodiment 1
Span 80, divinylbenzene and azodiisobutyronitrile are dissolved in toluene first and obtain oily phase, span 80 is in oily phase
In volume fraction be 10%, the volume ratio of monomer and oil-based solvent is 1:1, initiator: monomer=1:10(molar ratio)；In machinery
Aqueous solution of the 1wt% PANI-CNT(PANI/CNT mass ratio for 3:1) will be dispersed under stirring condition to be slowly dropped in oily phase,
Continue stirring 1h after being added dropwise and obtains the water-in-oil type High Internal Phase Emulsion that internal phase volume score is 80%；After sealing at 70 DEG C
Polymerization reaction is carried out, reaction obtained solid block product after 24 hours；Interior phase is removed with dehydrated alcohol extraction, after vacuum drying
To porous polymer composite material；It is mixed again with the potassium hydroxide for being 1:1 with composite material mass ratio, in 700 DEG C of items after drying
Carbonization obtains foam carbon composite under part.
Embodiment 2: specific experiment step is same as Example 1, and the aqueous solution of the High Internal Phase Emulsion of preparation is to be dispersed with
The aqueous solution of 2wt% PANI-CNT, the mass ratio of PANI/CNT are 3:1.
Embodiment 3: specific experiment step is same as Example 1, and the aqueous solution of the High Internal Phase Emulsion of preparation is to be dispersed with
The aqueous solution of 4wt% PANI-CNT, the mass ratio of PANI/CNT are 3:1.
Embodiment 4: specific experiment step is same as Example 1, and the aqueous solution of the High Internal Phase Emulsion of preparation is to be dispersed with
The aqueous solution of 8wt% PANI-CNT, the mass ratio of PANI/CNT are 3:1.
Embodiment 5: specific experiment step is same as Example 1, and the aqueous solution of the High Internal Phase Emulsion of preparation is to be dispersed with
The aqueous solution of 2wt% PANI-CNT, the mass ratio of PANI/CNT are 2:1.
Embodiment 6: specific experiment step is same as Example 1, and the aqueous solution of the High Internal Phase Emulsion of preparation is to be dispersed with
The aqueous solution of 2wt% PANI-CNT, the mass ratio of PANI/CNT are 1:1.
Embodiment 7: specific experiment step is same as Example 1, and the aqueous solution of the High Internal Phase Emulsion of preparation is to be dispersed with
The aqueous solution of 2wt% PANI-CNT, the mass ratio of PANI/CNT are 0:1.
Comparative example 1: specific experiment step is same as Example 1, and the aqueous solution of the High Internal Phase Emulsion of preparation is to be dispersed with
The aqueous solution of 0wt% PANI-CNT, the mass ratio of PANI/CNT are 0:1.
Foamy carbon/carbon nano tube compound material the data prepared under 1 different condition of table
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with repair
Decorations, are all covered by the present invention.
Claims (10)
1. a kind of method of High Internal Phase Emulsion template controllable preparation foamy carbon/carbon nano tube compound material, which is characterized in that packet
Include following steps:
(1) a certain amount of monomer, initiator and surfactant span 80 are dissolved completely in oil-based solvent and are made into oily phase；
(2) water phase for being dispersed with the carbon nanotube PANI-CNT for being coated with polyaniline is slowly added into step under agitation
(1) in the oily phase obtained, continue stirring 1h after being added dropwise and obtain water-in-oil type High Internal Phase Emulsion；
(3) 24 h of polymerization reaction is carried out at 70 DEG C after the High Internal Phase Emulsion sealing obtained step (2), obtains solid block
Crude product removes interior phase with dehydrated alcohol extraction, porous polymer composite material is obtained after vacuum drying；
(4) composite material obtained with a certain amount of potassium hydroxide solution mixing step (3), it is dry after under the conditions of 700 DEG C carbon
Change 2 h and obtains foam carbon composite.
2. a kind of High Internal Phase Emulsion template controllable preparation foamy carbon/carbon nano tube compound material according to claim 1
Method, it is characterised in that: monomer as described in step (1) be divinylbenzene.
3. a kind of High Internal Phase Emulsion template controllable preparation foamy carbon/carbon nano tube compound material according to claim 1
Method, it is characterised in that: oil-based solvent as described in step (1) be toluene.
4. a kind of High Internal Phase Emulsion template controllable preparation foamy carbon/carbon nano tube compound material according to claim 1
Method, it is characterised in that: initiator as described in step (1) is azodiisobutyronitrile, is 1:100 with the molar ratio of monomer.
5. a kind of High Internal Phase Emulsion template controllable preparation foamy carbon/carbon nano tube compound material according to claim 1
Method, it is characterised in that: volume fraction of the span 80 as described in step (1) in oily phase be 5%-15%.
6. a kind of High Internal Phase Emulsion template controllable preparation foamy carbon/carbon nano tube compound material according to claim 1
Method, it is characterised in that: in step (1), the volume ratio of the monomer and oil-based solvent is 1:2-2:1.
7. a kind of High Internal Phase Emulsion template controllable preparation foamy carbon/carbon nano tube compound material according to claim 1
Method, it is characterised in that: in High Internal Phase Emulsion described in step (2) volume fraction of phase be 75%-95%.
8. a kind of High Internal Phase Emulsion template controllable preparation foamy carbon/carbon nano tube compound material according to claim 1
Method, it is characterised in that: in PANI-CNT described in step (2) mass ratio of PANI and CNT be 0:1-5:1.
9. a kind of High Internal Phase Emulsion template controllable preparation foamy carbon/carbon nano tube compound material according to claim 1
Method, it is characterised in that: in PANI-CNT water phase described in step (2) PANI-CNT mass fraction be 0 %-10 %.
10. a kind of High Internal Phase Emulsion template controllable preparation foamy carbon/carbon nano tube compound material according to claim 1
Method, it is characterised in that: the mass ratio of potassium hydroxide described in step (4) and step (3) composite material is 1:2-2:1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811194113.4A CN109336083B (en) | 2018-10-15 | 2018-10-15 | Method for controllably preparing foam carbon/carbon nanotube composite material by high internal phase emulsion template method |
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| CN201811194113.4A CN109336083B (en) | 2018-10-15 | 2018-10-15 | Method for controllably preparing foam carbon/carbon nanotube composite material by high internal phase emulsion template method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110228808A (en) * | 2019-05-30 | 2019-09-13 | 福州大学 | A kind of High Internal Phase Emulsion template of the interior phase preparing porous carbon materials-foreign minister's collaboration |
| CN114684803A (en) * | 2022-03-31 | 2022-07-01 | 福州大学 | Method for preparing porous carbon composite material with nickel/cobalt microparticles loaded on surface by using high internal phase emulsion template |
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| CN114684803A (en) * | 2022-03-31 | 2022-07-01 | 福州大学 | Method for preparing porous carbon composite material with nickel/cobalt microparticles loaded on surface by using high internal phase emulsion template |
| CN114684803B (en) * | 2022-03-31 | 2023-11-28 | 福州大学 | Method for preparing porous carbon composite material with nickel/cobalt microparticles loaded on surface by using high internal phase emulsion template |
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