CN106700297A - Preparation method of carboxylated carbon nanotube and PS (polystyrene) composite material - Google Patents
Preparation method of carboxylated carbon nanotube and PS (polystyrene) composite material Download PDFInfo
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- CN106700297A CN106700297A CN201510799991.9A CN201510799991A CN106700297A CN 106700297 A CN106700297 A CN 106700297A CN 201510799991 A CN201510799991 A CN 201510799991A CN 106700297 A CN106700297 A CN 106700297A
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Abstract
The invention relates to a preparation method of a carboxylated carbon nanotube and PS (polystyrene) composite material. The preparation method comprises the following three experiment steps of (1) stirring a certain amount of carboxylated multi-walled carbon nanotube (with carboxyl content of 0-8wt%, length of 0.5 to 2mu m, and purity more than 95wt%), 0.1ml of surfactant triton X-100 and 5ml of tetrahydrofuran for 1h at the temperature of 60 DEG C, controlling the reaction temperature to 60 DEG C, and treating by ultrasonic waves for 1h; (2) adding a certain amount of PS into a mixed solution, mechanically stirring to completely dissolve, treating by ultrasonic waves for 0.5h, and completely and uniformly dispersing the carbon nanotube; (3) pouring the mixed solution into a special container (with flange gasket diameter of 5.5cm and height of 2mm), and putting a flange gasket into water to form a film after 20min, so as to obtain a sample. The preparation method has the advantages that the technology is simple, the experiment cycle is short, the cost is low, and the like; a PS and multi-walled carbon nanotube composite material film with excellent property is prepared.
Description
Technical field
The present invention relates to a kind of carboxylic carbon nano-tube and the preparation side of the composite of polystyrene
Method, belongs to functionalization field of material technology.
Background technology
CNT (CNTs) is by certain spiral by single or multiple lift graphite flake around central shaft
Angle curling forms seamless nanoscale pipe, is with sp2 hydridization between the carbon atom of carbon nano tube surface
Mode is present, and carbon pipe two ends are regarded as being formed by hemispheric fullerene sealing cap, this uniqueness
Structure causes CNT to have many excellent performances, such as big draw ratio and specific surface area,
Special electrical properties, excellent mechanical property and heat endurance, these special performances cause many
Wall carbon nano tube causes extensive concern as the obturator of composite.However, due to many wall carbon
The draw ratio and specific surface area of nanotube are larger to enable that CNT has surface very high, many walls
Van der Waals interaction between CNT is very strong so that be easily interweaved between CNT
Together, dispersiveness of the aggregate influence carbon pipe in solvent or polymeric matrix is formed, causes compound
The degradation of material.Therefore, for carbon pipe has preferably dispersiveness, system in the composite
Obtain the more excellent carbon nano tube compound material of performance, it is necessary to first CNT is modified and is repaiied
Decorations.
The surface modification of CNT：Carbon atom in CNT is mainly sp2Hydridization, can be with
Generation addition reaction, the group of some functionalization is connected on the surface of CNT, forms covalent bond
Modification；Can also utilize CNT in big π keys structure and other π keys directly occur π-
Pi accumulation, forms non-covalent bond modification.It is easy to reunite in itself due to CNT, and
It is not readily dissolved in water and other organic solvents, these factors greatly limit answering for CNT
With.So being modified using covalent bond, carbon nano tube surface is set to connect the group of some functionalization, with
This dissolubility and dispersiveness to improve CNT so that CNT is easier to be employed.
Addition reaction is carbon nano-tube modified, typically common are electrophilic addition reaction and nucleophilic addition is anti-
Should.Also by the surface of styrene-grafted to CNT, then it is polymerized, is obtained polyphenyl second
The composite of alkene-CNT.The nucleophilic addition of carbon, can use the carbanion and carbon of stabilization
Directly there is nucleophilic addition in nanotube, it is anti-that the anion produced in reaction is also used as polymerization
The initiator answered, may finally obtain the composite of polymer-carbon nanotube, CNT table
The polymer lateral chain in face can cause that the mechanical performance of composite is significantly improved.Can also be using parent
The intermediate of core addition, is subsequently adding different alkyl and halide, can so obtain multifunctional
The carbon nano tube derivative of group's modification.
As the production technology of CNT is continued to develop, the reality of carbon nano tube compound material should
With being more presented in our life.Such as New Electric Polymer, multifunctional polymeric
Thing composite, conducting metal based composites and fracture strength ceramic material high etc..Due to carbon
The finiteness and preciousness of nanotube, now, people still receive the exploitation carbon that focuses on of research
Nanotube content is less than on the advanced composite material (ACM) of mass fraction 10%.
Polystyrene is a kind of thermoplastic being most widely used in the world at present, in colourless
Bright shape.Polystyrene is polymerized generally by the free radical polymerization of styrene monomer.
Polystyrene is due to there is the glass transition temperature higher than 100 degrees Celsius, so being usually utilized to system
It is made plastic cup or disposable lunch box.Because polystyrene is in molten condition with good stream
Dynamic property, so being usually used in injection molding technique, the polystyrene for occurring in the market can typically divide
It is versatility polystyrene (GPPS), impact resistant polystyrene (HIPS) and foaming polyphenyl second
Alkene (EPS).
The present invention mainly describes the composite wood of a kind of functionalized multi-wall carbonnanotubes and polystyrene
The preparation method of material.Using the multi-walled carbon nano-tubes/PS/ tetra- of several different carboxylated contents in reaction
Hydrogen furans/surfactant mixed solution, using three elementary reactions is to dissolve, disperse in course of reaction
And text message, and solution blended process is used, with THF as organic solvent, prepare polyphenyl second
Alkene multi-wall carbon nano-tube composite material film.
The content of the invention
It is an object of the invention to provide a kind of good carboxylated content multi-walled carbon nano-tubes and polyphenyl second
The method of the superior performance of the composite of alkene.
The technical solution adopted by the present invention is to provide a kind of functionalized multi-wall carbonnanotubes and polyphenyl second
The preparation method of the composite of alkene, the method step is as follows：
1) will be with a certain amount of functionalized multi-wall carbonnanotubes (carboxyl-content 0-8wt%, length
0.5-2 μm, purity ＞ 95wt%), 0.1ml surfactant triton x-100s, the four of 5ml
Hydrogen furans, 60 ° of stirrings 1h, 60 ° of ultrasound 1h of controlling reaction temperature.
2) add a certain amount of polystyrene (PS) in above-mentioned mixed liquor kind mechanical agitation to being completely dissolved
Afterwards, ultrasonic 0.5h is completely dispersed uniformly to CNT.
3) mixed liquor is poured into specific container (flange gasket diameter 5.5cm, height 2mm), 20min
Flange gasket is put into film forming in water afterwards, you can obtain sample.
The composite of a kind of carboxylic carbon nano-tube and polystyrene is prepared using solution blended process
Preparation method, material therefor is, polystyrene；Tetrahydrofuran；Functionalized multi-wall carbonnanotubes
(carboxyl-content 0-8wt%, 0.5-2 μm of length, purity ＞ 95wt%)；Surfactant Qula
Logical X-100；
Described method is solution blended process.
Described dispersion multi-walled carbon nano-tubes method is the mechanical agitation and ultrasound for controlling certain rotating speed
Wavelength-division dissipates to be used in combination.
The described functionalized multi-wall carbonnanotubes that prepare are used with the composite material of polystyrene
Surfactant Qula is logical to make that composite material film surface is rounder and more smooth, and pore structure is more obvious.
The functionalized multi-wall carbonnanotubes of described preparation and the composite of polystyrene, with one
The multi-walled carbon nano-tubes for determining carboxylated content is added in polystyrene, can effectively control compound film material
The bulk density of material, calorifics and mechanical property.
Described prepares functionalized multi-wall carbonnanotubes with the composite of polystyrene when carboxyl contains
When measuring high, the hole on surface will become big with the increase of carboxyl-content, polystyrene and many wall carbon
Connection between nanotube very well, shows CNT dispersiveness in the polymer very well.
The beneficial effects of the invention are as follows：
1) the compound of functionalized multi-wall carbonnanotubes and polystyrene is prepared using ultrasonic wave added oxidation
In materials process, consersion unit small investment is simple to operate, functionalization efficiency high and to many wall carbon
The low advantage of destructiveness of nanotube.
2) three phases are divided in experimentation to different carboxylated content multi-walled carbon nano-tubes and polyphenyl
Ethene blending reaction in THF, shortens experimental period, reduces experimental cost.
3) multi-walled carbon nano-tubes is made in THF by the way of mechanical agitation and ultrasound are carried out simultaneously
In be uniformly dispersed, the composite of the superior carbon nano-tube/poly styrene of availability.
Brief description of the drawings
Fig. 1 is different functionalized multi-wall carbonnanotubes-poly styrene composite materials prepared by embodiment 1
Scanning electron microscope analysis.
Fig. 2 is the surfactant of embodiment 1 compound to different functionalized multi-wall carbonnanotubes-polystyrene
The scanning electron microscope analysis of the scattered influence of carbon pipe in material.
Specific embodiment
The method that polystyrene carbon nano tube compound material is prepared using solution blended process, with different carboxylics
The multi-walled carbon nano-tubes of base content/PS/THF/ surfactants blending, experimentation is by machinery
Stirring and dissolving, dispersion, film forming three phases are simultaneously divided in scatter stage using ultrasonic wave added CNT
Dissipate uniform.
With reference to embodiment, the invention will be further described, so that those skilled in the art
The present invention can be better understood from and can be practiced, but illustrated embodiment is not as to of the invention
Limit.
Embodiment 1
A kind of preparation method of the composite of carboxylic carbon nano-tube and polystyrene, the method step
It is rapid as follows：
1) carboxyl-content 0,0.5,2,4,8wt% multi-walled carbon nano-tubes, 0.1ml surface-actives
Agent triton x-100, the tetrahydrofuran of 5ml, 60 ° of stirring 1h, 60 ° of controlling reaction temperature surpasses
Sound 1h.
2) disperse：After adding PS mechanical agitations to be completely dissolved, ultrasonic 0.5h is complete to CNT
It is uniformly dispersed.
3) film forming：Mixed liquor is poured into specific container (flange gasket diameter 5.5cm, height 2mm),
Flange gasket is put into film forming in water after 20min, you can obtain sample.
Claims (8)
1. the preparation method of the composite of a kind of carboxylic carbon nano-tube and polystyrene, it is characterised in that the method step is as follows,
1) will be with a certain amount of functionalized multi-wall carbonnanotubes (carboxyl-content 0-8wt%, 0.5-2 μm of length, purity ＞ 95wt%,), 0.1ml surfactant triton x-100s, the tetrahydrofuran of 5ml, 60 ° of stirrings 1h, 60 ° of ultrasound 1h of controlling reaction temperature.
2) add a certain amount of polystyrene (PS) in above-mentioned mixed liquor kind mechanical agitation to after being completely dissolved, ultrasonic 0.5h to CNT is completely dispersed uniformly.
3) mixed liquor is poured into specific container (flange gasket diameter 5.5cm, height 2mm), flange gasket is put into film forming in water after 20min, you can obtain sample.
2. the preparation method of the composite of a kind of carboxylic carbon nano-tube according to claim 1 and polystyrene, it is characterised in that material therefor is, polystyrene；Tetrahydrofuran；Several multi-walled carbon nano-tubes (carboxyl-content 0-8wt%, 0.5-2 μm of length, purity ＞ 95wt%) with different carboxylated contents；Surfactant triton x-100.
3. the preparation method of the composite of a kind of carboxylic carbon nano-tube according to claim 1 and polystyrene, it is characterised in that experimentation is broadly divided into three phases i.e.：Dissolution phase, scatter stage and text message.
4. the preparation method of the composite of a kind of carboxylic carbon nano-tube according to claim 1 and polystyrene, it is characterised in that described method is solution blended process.
5. the preparation method of the composite of a kind of carboxylic carbon nano-tube according to claim 1 and polystyrene, it is characterized in that, it is that CNT is uniformly dispersed to prevent multi-walled carbon nano-tubes from reuniting effect occurring, by the way of mechanical agitation and ultrasonic disperse are carried out simultaneously.
6. the preparation method of the composite of a kind of carboxylic carbon nano-tube according to claim 1 and polystyrene, it is characterized in that, polystyrene is modified with the multi-walled carbon nano-tubes of different carboxylated contents, with tetrahydrofuran as organic solvent, polystyrene multi-walled carbon nano-tubes composite porous material film has been prepared.
7. the preparation method of the composite of a kind of carboxylic carbon nano-tube according to claim 1 and polystyrene, it is characterised in that the composite material film surface of addition surfactant is rounder and more smooth, and pore structure is more obvious.
8. the preparation method of the composite of a kind of carboxylic carbon nano-tube according to claim 1 and polystyrene, it is characterized in that, multi-walled carbon nano-tubes with certain carboxylated content is added in polystyrene, can effectively control bulk density, calorifics and the mechanical property of composite film material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108250603A (en) * | 2018-01-19 | 2018-07-06 | 广州润锋科技有限公司 | Polystyrene carrier material that a kind of carbon nanotube conducting is modified and preparation method thereof |
| CN111807351A (en) * | 2019-04-11 | 2020-10-23 | 天津工业大学 | Method for analyzing carboxylation degree of carbon nano tube by using adsorption degree of dye |
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| CN1793216A (en) * | 2005-12-29 | 2006-06-28 | 黄德欢 | Process for preparing carbon nano pipe/polyhenylethylene nano conducting composite |
| CN101805491A (en) * | 2009-09-22 | 2010-08-18 | 龙海市奈特化工有限责任公司 | Composite material with electromagnetic shielding effect and preparation method thereof |
| KR20110008518A (en) * | 2009-07-20 | 2011-01-27 | 주식회사 엑사이엔씨 | Method for manufacturing carbon nano tube solution having polymer and method for manufacturing transparency conductivity film using the same and transparency conductivity film manufacured by the method |
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| CN1410454A (en) * | 2002-03-14 | 2003-04-16 | 四川大学 | Preparation method of polymer/carbon nano pipe composite material and its in situ mass polymerization |
| CN1793216A (en) * | 2005-12-29 | 2006-06-28 | 黄德欢 | Process for preparing carbon nano pipe/polyhenylethylene nano conducting composite |
| KR20110008518A (en) * | 2009-07-20 | 2011-01-27 | 주식회사 엑사이엔씨 | Method for manufacturing carbon nano tube solution having polymer and method for manufacturing transparency conductivity film using the same and transparency conductivity film manufacured by the method |
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| CN108250603A (en) * | 2018-01-19 | 2018-07-06 | 广州润锋科技有限公司 | Polystyrene carrier material that a kind of carbon nanotube conducting is modified and preparation method thereof |
| CN111807351A (en) * | 2019-04-11 | 2020-10-23 | 天津工业大学 | Method for analyzing carboxylation degree of carbon nano tube by using adsorption degree of dye |
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