CN106243637A - The PET antistatic film that a kind of Activated Carbon Nanotubes is modified - Google Patents
The PET antistatic film that a kind of Activated Carbon Nanotubes is modified Download PDFInfo
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- CN106243637A CN106243637A CN201610516602.1A CN201610516602A CN106243637A CN 106243637 A CN106243637 A CN 106243637A CN 201610516602 A CN201610516602 A CN 201610516602A CN 106243637 A CN106243637 A CN 106243637A
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- carbon nanotubes
- activated carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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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
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
Abstract
The invention discloses the PET antistatic film that a kind of Activated Carbon Nanotubes is modified, be made up of the component of following weight portion: pet polymer matrix material 70～95 mass parts, Activated Carbon Nanotubes 0.01～10 mass parts, auxiliary agent 0.1～20 mass parts；Described auxiliary agent is one or more the mixing in dispersant B, coupling agent, antioxidant, lubricant, antifriction liniment；Described Activated Carbon Nanotubes is to be dissolved in solvent by dispersant A, obtains dispersant solution, is then sprayed into by dispersant solution in the CNT of high-speed stirred by high-pressure spraying method, after high-speed stirred mixing, prepares Activated Carbon Nanotubes.The PET antistatic film electric conductivity that the present invention provides is good, and antistatic persistency is strong, and service life is long.
Description
One, technical field
The present invention relates to the PET antistatic film that a kind of Activated Carbon Nanotubes is modified.
Two, background technology
Polyethylene terephthalate (PET) has many excellent performances, thus PET film and thin slice are extensively applied
In packaging material such as food, medicine, fiber, electronic components, be used as the most in large quantities tape, soft mould magnetic holder, photograph use
Egative film etc..
But PET film is produced electrostatic phenomenon by friction, often can cause viscous carriage return, pollution, poor attachment, piebaldism, matter
The lower degradation trouble of amount, accordingly, it would be desirable to carry out antistatic treatment to thin film.
PET film is carried out antistatic treatment and is commonly divided into surface processing-type and internal two kinds of methods of addition type.Surface
Addition type is the purpose reaching to eliminate electrostatic at the film surface coating material such as antistatic additive or anti-static material.Internal addition type
It is usually and in film manufacturing processes, anlistatig material is directly filled, thus reach anlistatig purpose.
Wherein, conductivity type filler is used to be possible not only to produce PET antistatic plastic thin film, and due to its antistatic behaviour base
In the electric conductivity of filler, persistency is good compared with surface-coated type PET antistatic film, and antistatic behaviour is affected by ambient humidity
Little.
In numerous conductivity type fillers, CNT has good electric conductivity, has again bigger draw ratio simultaneously, because of
And it is well suited for making conductive filler, relative to other metallic particles and graphite granule, its little consumption just can form conductive net,
And its density is more much smaller than metallic particles, it is difficult to the coagulation because of the effect of gravity.These characteristics utilizing CNT are made
Join in plastics for conducting medium, the electric conductivity of plastics can be produced strong impact.At present, CNT is at PET antistatic
Applied research in material mainly by changing structure and the content of CNT, improves CNT dispersion in PET
Property, and CNT is carried out surface process and equalize electric conductivity and other properties of PET anti-static material.
Three, summary of the invention
The invention provides the PET antistatic film that a kind of Activated Carbon Nanotubes is modified, the preprocessed modification of CNT
After, add to PET material matrix as conductive filler, prepare PET antistatic film.
The technical solution used in the present invention is:
The PET antistatic film that a kind of Activated Carbon Nanotubes is modified, it is characterised in that the modification of described Activated Carbon Nanotubes
PET antistatic film is made up of the component of following weight portion:
Pet polymer matrix material 70～95 mass parts, Activated Carbon Nanotubes 0.01～10 mass parts, auxiliary agent 0.1～20
Mass parts；
Described auxiliary agent is the mixed of one or more in dispersant B, coupling agent, antioxidant, lubricant, antifriction liniment
Close；
Described Activated Carbon Nanotubes prepares by the following method:
Dispersant A is dissolved in solvent, obtains dispersant solution, then dispersant solution is sprayed into by high-pressure spraying method
In the CNT of high-speed stirred, after high-speed stirred mixing, prepare Activated Carbon Nanotubes.Described CNT, dispersant A, molten
The mass fraction ratio of agent is 85～95:0.1～5:5～10.
Described pet polymer matrix material, Activated Carbon Nanotubes, the mass fraction of auxiliary agent be 70～95 mass parts, 0.01
～10 mass parts, 0.1～20 mass parts, preferably 70～95 mass parts, 1～10 mass parts, 0.1～20 mass parts；
Described auxiliary agent is the mixed of one or more in dispersant B, coupling agent, antioxidant, lubricant, antifriction liniment
Close；The most described auxiliary agent is mixed with dispersant B of one or more in coupling agent, antioxidant, lubricant, antifriction liniment
Close, one or more during more preferably auxiliary agent is coupling agent, antioxidant, antifriction liniment with dispersant B, lubricant mixed
Close.
Further, the most described auxiliary agent is dispersant B, coupling agent, antioxidant, lubricant and antifriction liniment, described raw material
Formula be: pet polymer matrix material, Activated Carbon Nanotubes, dispersant B, coupling agent, antioxidant, lubricant, antifriction liniment
Mass fraction be 70～90 mass parts, 1～10 mass parts, 0.1～10 mass parts, 0.01～5 mass parts, 0.01～2 mass
Part, 0.01～10 mass parts, 0.01～5 mass parts, wherein dispersant B, coupling agent, antioxidant, lubricant and antifriction liniment
Total mass fraction is 0.1～20 mass parts.
Further, in preferred steps (2), the formula of raw material is: pet polymer matrix material, Activated Carbon Nanotubes, point
Powder B, coupling agent, antioxidant, lubricant, the mass fraction of antifriction liniment be 70～90 mass parts, 1～10 mass parts, 1～10
Mass parts, 0.01～3 mass parts, 0.01～2 mass parts, 0.01～3 mass parts, 0.01～5 mass parts, wherein dispersant B, idol
Total mass fraction of connection agent, antioxidant, lubricant and antifriction liniment is 0.1～20 mass parts.
Further, in preferred steps (2), the formula of raw material is: pet polymer matrix material, Activated Carbon Nanotubes, point
Powder B, coupling agent, antioxidant, lubricant, the mass fraction of antifriction liniment are 70～90 mass parts, 3～8 mass parts, 1～8 matter
Amount part, 0.5～3 mass parts, 0.5～2 mass parts, 0.5～3 mass parts, 0.5～3 mass parts.
In described method, dispersant A and dispersant B are for distinguishing the dispersant used in different step, and A, B do not have
Chemical sense.
Described dispersant A and dispersant B each stand alone as dodecylbenzene sodium sulfonate, polyvinylpyrrolidone, polyethylene
Alcohol, xanthan gum, sodium lauryl sulphate, Triton X-100, sodium carboxymethyl cellulose, Dihexadecylphosphate, Ah
Draw primary glue, cetyl trimethylammonium bromide, alkyl phenol ethylene oxide condensation substance emulsifying agent, cetyl trimethyl sodium bromide,
One or more mixture in Kynoar.
Described solvent be water, N,N-dimethylformamide, N-Methyl pyrrolidone, n-butyl alcohol, chloroform, dehydrated alcohol, third
One or more mixture in ketone, petroleum ether, ethyl acetate, butyl acetate；
Described CNT, dispersant A, the mass fraction ratio of solvent are 85～95:0.1～5:5～10.
Described CNT is one or both the mixture in multi-walled carbon nano-tubes, SWCN, the most
Wall carbon nano tube.
Described pet polymer matrix material is particle or pulverulent material, pet polymer pulverulent material is preferably used, averagely
Particle diameter be 0.5 μm be 2-100g/10min, preferably 10-30g/ to 5mm, the preferably melt index of pet polymer matrix material
10min, the beneficially CNT dispersion in PET matrix.
Described coupling agent is one or more the mixture in titante coupling agent, silane coupling agent；Institute
Stating titante coupling agent can be isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters, isopropyl three (dioctyl phosphoric acid
Acyloxy) titanate esters, isopropyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanate esters, monoalkoxy unsaturated fatty acid
One or more mixture in titanate esters or Di(dioctylpyrophosphato) ethylene titanate；Described silane is even
Connection agent can use KH550, one or more the mixture in KH560, KH570, KH792, DL602, DL171；
Described antioxidant is preferably 1098,168,1010,1076, DLTP, one or more in MB, 164,264
Mixture.
Described lubricant is fatty acid, aliphatic amide type or ester lubricant, paraffin class lubricant, metallic soap salt profit
One or more mixing in lubrication prescription, low-molecular-weight wax, further, described lubricant preferred PE wax, montanin wax, silicone
One or more mixture in powder, stearic acid, oleic acid, calcium stearate, ethylene bis stearic acid amide, erucyl amide
Described antifriction liniment is preferably nano inorganic implant or nano plastic micropowder, and described nano inorganic implant is usual
For nano-calcium carbonate, nanometer calcium silicates, nano silicon, nanoclay etc..
The PET antistatic film of the Activated Carbon Nanotubes modification that the present invention provides can prepare by the following method: by activated carbon
Nanotube and pet polymer matrix material stirring and evenly mixing, then mix with auxiliary agent, melt extrude pelletize system through double screw extruder
Obtain PET/ carbon nanotube conducting master batch；PET/ carbon nanotube conducting master batch is prepared into by blowing, curtain coating or stretch processes
To the PET antistatic film that Activated Carbon Nanotubes is modified.Prepare what the technique of thin film was known to the skilled person.
The processing technique of described double screw extruder is screw speed 100～1000r/min, and extrusion temperature is 250-280
℃。
Double screw extruder melt extrudes pelletize, and pelletize mode has multiple, and optional water cooling bracing pelletizing, air-cooled tie rod are cut
Grain, die face are earnestly, cut under water.The method being well known to those skilled in the art.
Present invention high-pressure spraying method used when preparing Activated Carbon Nanotubes is to be filled by high-pressure spraying by dispersant solution
Putting the CNT spraying into high-speed stirred with the form of spraying, described high-pressure spray device can use high-pressure spraying machine, by height
Dispersant solution is become spray form to spray in material through high-pressure nozzle by water pump.Described high-pressure spraying machine is located in advance for CNT
Reason still belongs to the first time.High-pressure spraying method by dispersant solution be atomized, obtain a large amount of fine droplet after atomization, significantly increase solution with
The contact area of CNT, beneficially carbon nanotube particulate are coated with by auxiliary agent, strengthen its dispersibility.
In described high-pressure spraying method, spray rate is generally 10～100ml/min；
Atomized particle size is 0.1～1um.
The rotating speed of described high-speed stirred is 300～1500 turns/min.
The time of described high-speed stirred mixing is generally 1 minute～1 hour, preferably 5～40 minutes.
The present invention carries out high-speed stirred to CNT, to its surface pretreatment, simultaneously by dispersant, surface activity
The auxiliary agents such as agent are dissolved in liquid in the carbon nanotube dust being sprayed in stirring by the way of spraying so that CNT table
Face activates, and simultaneously by the material uniform wet such as dispersant, surfactant, causes to be formed between CNT and repels, significantly carry
The high dispersibility of CNT, and the bulk density of CNT can be improved, to obtain optimal dispersion effect with good simultaneously
Good processability.
The present invention innovation by CNT after pretreatment modification, as conductive filler add to PET material base
In body, prepare high efficiency dispersion PET/ carbon nanotube conducting master batch, then prepared by blowing, curtain coating or stretch processes
The PET antistatic film of different performance.Compared with traditional PET antistatic film, owing to when reaching same electric conductivity, carbon is received
The addition of mitron is well below the addition of other conductive fillers, hence in so that this antistatic film keeps to the full extent
Original performance of PET matrix resin, improves antistatic persistency and the service life of thin film.
The PET antistatic film that the present invention provides, outward appearance: uniform color, without stain, corrugationless, surface is without projection, without broken
Hole, without vestige；Excellent mechanical: hot strength: >=170MPA, elongation at break: >=120%, percent thermal shrinkage :≤5%, table
Surface resistivity (Ω): 106～109(content of carbon nanotubes=3wt.%).
Four, detailed description of the invention
With specific embodiment, technical scheme is described further below, but the protection content of the present invention is not
It is limited to this.
Embodiment 1～16
According to the form below 1 takes each raw material, is dissolved in solvent by dispersant, obtains dispersant solution, is then led to by dispersant solution
Cross high pressure spray process and spray into the CNT (diameter 1～30nm, length 1～100 μm, bulk density 0.02g/mL) of high-speed stirred
In, technological parameter is as shown in table 1, after high-speed stirred mixing, prepares Activated Carbon Nanotubes；
Table 1
The performance test results such as table 2 below of the Activated Carbon Nanotubes prepared
Table 2
Described dispersibility experiment detection by the following method: Activated Carbon Nanotubes 10mg embodiment 1～16 prepared is respectively
Add 10mL and prepare in the solvent (seeing table 1) used by this Activated Carbon Nanotubes, ultrasonic disperse 30 minutes, obtain suspension, quiet
Putting, when occurring substantially being layered, the record time is the holding time, and acquired results refers to table 2.Holding time is the longest, shows that it disperses
Property is the best.The most pretreated CNT cannot form stable suspension.
Above-mentioned test result indicate that, after pretreatment, the bulk density of CNT improve about 10 times (untreated
The bulk density of CNT is about 0.02g/mL), dispersibility is all significantly increased.
Embodiment 17～32
Activated Carbon Nanotubes and pet polymer pulverulent material prepared by embodiment 1～16 (mean diameter 100 μm～
2mm) stirring and evenly mixing, then mixes with auxiliary agent, and each raw material dosage refers to table 3 and table 4, melt extrudes through double screw extruder, draws
Stretch, cooling and dicing prepares PET/ carbon nanotube conducting master batch；The processing technique of double screw extruder is screw speed 200r/min,
Extrusion temperature is 255 DEG C.
The content of carbon nanotubes of the PET/ carbon nanotube conducting master batch prepared is as shown in table 5.
The PET/ carbon nanotube conducting master batch of preparation is prepared antistatic film through biaxial tension, according to " GB/T1410-
2006 solid insulating material specific insulations and surface resistivity test method " surface resistivity of testing film, and detect it
Physical property, result is as shown in table 5.
Table 3
Table 4
Table 5
Embodiment data show, the surface resistivity of antistatic film prepared by the present invention is preferable, in content of carbon nanotubes
In the case of about 3wt.%, surface resistivity is 106～109About Ω, antistatic property is good.And excellent mechanical,
Hot strength: >=170MPA, elongation at break: >=120%.
Claims (10)
1. the PET antistatic film that an Activated Carbon Nanotubes is modified, it is characterised in that the PET that described Activated Carbon Nanotubes is modified
Antistatic film is made up of the component of following weight portion:
Pet polymer matrix material 70～95 mass parts, Activated Carbon Nanotubes 0.01～10 mass parts, auxiliary agent 0.1～20 mass
Part；
Described auxiliary agent is one or more the mixing in dispersant B, coupling agent, antioxidant, lubricant, antifriction liniment；
Described Activated Carbon Nanotubes prepares by the following method:
Dispersant A is dissolved in solvent, obtains dispersant solution, then dispersant solution is sprayed at a high speed by high-pressure spraying method
In the CNT of stirring, after high-speed stirred mixing, prepare Activated Carbon Nanotubes.
2. the PET antistatic film that Activated Carbon Nanotubes as claimed in claim 1 is modified, it is characterised in that described carbon nanometer
Pipe, dispersant A, the mass fraction ratio of solvent are 85～95:0.1～5:5～10.
3. the PET antistatic film that Activated Carbon Nanotubes as claimed in claim 1 is modified, it is characterised in that described dispersant A
Each stand alone as with dispersant B dodecylbenzene sodium sulfonate, PET ketopyrrolidine, PET alcohol, xanthan gum, sodium lauryl sulphate,
Triton X-100, sodium carboxymethyl cellulose, Dihexadecylphosphate, arabic gum, cetyl trimethyl bromination
In ammonium, alkyl phenol ethylene oxide condensation substance emulsifying agent, cetyl trimethyl sodium bromide, Kynoar one or both with
On mixture.
4. the PET antistatic film that Activated Carbon Nanotubes as claimed in claim 1 is modified, it is characterised in that described auxiliary agent is even
One or more in connection agent, antioxidant, antifriction liniment are with dispersant B, the mixing of lubricant.
5. the PET antistatic film that Activated Carbon Nanotubes as claimed in claim 1 is modified, it is characterised in that described auxiliary agent is for dividing
Powder B, coupling agent, antioxidant, lubricant and antifriction liniment, the formula of described raw material is: pet polymer matrix material, activity
CNT, dispersant B, coupling agent, antioxidant, lubricant, the mass fraction of antifriction liniment be 70～90 mass parts, 1～10
Mass parts, 0.1～10 mass parts, 0.01～5 mass parts, 0.01～2 mass parts, 0.01～10 mass parts, 0.01～5 mass
Part, wherein total mass fraction of dispersant B, coupling agent, antioxidant, lubricant and antifriction liniment is 0.1～20 mass parts.
6. the PET antistatic film that Activated Carbon Nanotubes as claimed in claim 1 is modified, it is characterised in that described solvent is
Water, N,N-dimethylformamide, N-Methyl pyrrolidone, n-butyl alcohol, chloroform, dehydrated alcohol, acetone, petroleum ether, ethyl acetate,
One or more mixture in butyl acetate.
7. the PET antistatic film that Activated Carbon Nanotubes as claimed in claim 1 is modified, it is characterised in that described coupling agent is
One or more mixture in titante coupling agent, silane coupling agent.
8. the PET antistatic film that Activated Carbon Nanotubes as claimed in claim 1 is modified, it is characterised in that described antioxidant is
1098,168,1010,1076, one or more the mixture in DLTP, MB, 164,264.
9. the PET antistatic film that Activated Carbon Nanotubes as claimed in claim 1 is modified, it is characterised in that described lubricant is
In fatty acid, aliphatic amide type or ester lubricant, paraffin class lubricant, metallic soap salt lubricant, low-molecular-weight wax one
Kind or two or more mixing.
10. the method for claim 1, it is characterised in that in described step (2), described antifriction liniment is that nano inorganic is filled out
Fill thing or nano plastic micropowder.
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Cited By (3)
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| PL421952A1 (en) * | 2017-06-20 | 2019-01-02 | Zachodniopomorski Uniwersytet Technologiczny W Szczecinie | Method for producing a structural element and method for producing a container with the bottom |
| PL421953A1 (en) * | 2017-06-20 | 2019-01-02 | Zachodniopomorski Uniwersytet Technologiczny W Szczecinie | Method for producing a structural element, preferably a bottom and method for producing a container with the bottom |
| PL421950A1 (en) * | 2017-06-20 | 2019-01-02 | Zachodniopomorski Uniwersytet Technologiczny W Szczecinie | Method for producing a structural element and method for producing a container with the bottom |
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| PL421952A1 (en) * | 2017-06-20 | 2019-01-02 | Zachodniopomorski Uniwersytet Technologiczny W Szczecinie | Method for producing a structural element and method for producing a container with the bottom |
| PL421953A1 (en) * | 2017-06-20 | 2019-01-02 | Zachodniopomorski Uniwersytet Technologiczny W Szczecinie | Method for producing a structural element, preferably a bottom and method for producing a container with the bottom |
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Application publication date: 20161221 |