CN106147200A - The modified TPU antistatic film of a kind of Activated Carbon Nanotubes - Google Patents
The modified TPU antistatic film of a kind of Activated Carbon Nanotubes Download PDFInfo
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- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses the modified TPU antistatic film of a kind of Activated Carbon Nanotubes, be made up of the component of following weight portion: TPU polymeric 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 dispersant B, coupling agent, antioxidant, lubricant, one or more the mixing in antifriction liniment；Described Activated Carbon Nanotubes is to be dissolved in solvent by dispersant A, obtains dispersant solution, is then sprayed into dispersant solution by high-pressure spraying method in the CNT of high-speed stirred, after high-speed stirred mixing, prepares Activated Carbon Nanotubes.The TPU antistatic film electric conductivity that the present invention provides is good, and antistatic persistence is strong, and service life is long.
Description
First, technical field
The present invention relates to the modified TPU antistatic film of a kind of Activated Carbon Nanotubes.
2nd, background technology
Thermoplastic polyurethane (TPU) not only has the rubber properties such as the high intensity of cross-linked polyurethane, high abrasion, and has
The thermoplastic property of standby linear polymeric material, so that its application is expanded to plastic applications.Especially recent decades, TPU
Have become as one of macromolecular material with fastest developing speed.TPU film is a kind of important application form of TPU material, in recent years with
High-tech development and progress to have also been obtained and be increasingly widely applied.
Owing to TPU has high intensity, good, weather-proof feature wear-resisting, elastic so that TPU film be widely used in auto industry,
The fields such as footwear material, clothes laminating, ready-made clothes, chemical industry, electronics, medical treatment.Wherein, TPU antistatic film is one of them.
TPU antistatic film mainly includes that application antistatic additive is prepared TPU antistatic film, used conductivity type filler to produce
TPU antistatic plastic film, employing coating material production TPU antistatic film etc..
Wherein, conductivity type filler is used to be possible not only to produce TPU antistatic plastic film, and due to its antistatic behaviour base
In the electric conductivity of filler, persistence is good compared with surfactant type TPU antistatic film, and antistatic behaviour is by the shadow of ambient humidity
Ring 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,
It and its density is more much smaller than metallic particles, is difficult to the coagulation because of the effect of gravity.These characteristics utilizing CNT are made
Join in plastics for conducting medium, strong impact can be produced on the electric conductivity of plastics.At present, CNT is antistatic at TPU
Application study in material mainly by changing structure and the content of CNT, improves dispersion in TPU for the CNT
Property, and carry out electric conductivity and other properties that surface treatment equalizes TPU anti-static material to CNT.
3rd, content of the invention
The invention provides the modified TPU antistatic film of a kind of Activated Carbon Nanotubes, the preprocessed modification of CNT
After, add to TPU material matrix as conductive filler, prepare TPU antistatic film.
The technical solution used in the present invention is:
The modified TPU antistatic film of a kind of Activated Carbon Nanotubes, it is characterised in that the modification of described Activated Carbon Nanotubes
TPU antistatic film is made up of the component of following weight portion:
TPU polymeric 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 dispersant B, coupling agent, antioxidant, lubricant, one or more mixed in 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 TPU polymeric 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 dispersant B, coupling agent, antioxidant, lubricant, one or more mixed in antifriction liniment
Close；Preferably described auxiliary agent is mixed with dispersant B of coupling agent, antioxidant, lubricant, one or more in antifriction liniment
Close, more preferably auxiliary agent be coupling agent, antioxidant, one or more in antifriction liniment with dispersant B, lubricant mixed
Close.
Further, preferably described auxiliary agent is dispersant B, coupling agent, antioxidant, lubricant and antifriction liniment, described raw material
Formula be: TPU polymeric 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: TPU polymeric 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: TPU polymeric 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 neopelex, polyvinylpyrrolidone, polyethylene
Alcohol, xanthans, lauryl sodium sulfate, Triton X-100, sodium carboxymethylcellulose, Dihexadecylphosphate, Ah
Draw primary glue, cetyl trimethylammonium bromide, alkyl phenol ethylene oxide condensation product emulsifying agent, cetyl trimethyl sodium bromide,
One or more mixture in Kynoar.
Described solvent be water, N,N-dimethylformamide, 1-METHYLPYRROLIDONE, n-butanol, chloroform, absolute ethyl 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 multi-walled carbon nano-tubes, one or both the mixture in SWCN, preferably many
Wall carbon nano tube.
Described TPU polymeric matrix material is particle or pulverulent material, TPU polymer pulverulent material is preferably used, averagely
Particle diameter is 0.5 μm and arrives 5mm, and the melt index of preferably TPU polymeric matrix material is 2-100g/10min, preferably 10-30g/
10min, the beneficially CNT dispersion in TPU matrix.
Described coupling agent is titante coupling agent, one or more the mixture in 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 unrighted 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；
The 1098th, described antioxidant be preferably the 168th, the 1010th, the 1076th, DLTP, one or more in MB, the 164th, 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 filler or nano plastic micro mist, and described nano inorganic filler is usual
For nano-calcium carbonate, nanometer calcium silicates, nano silicon, nanoclay etc..
The modified TPU antistatic film of the Activated Carbon Nanotubes that the present invention provides can prepare by the following method: by activated carbon
Nanotube stirs and evenly mixs with TPU polymeric matrix material, then mixes with auxiliary agent, melt extrudes granulation system through double screw extruder
Obtain TPU/ carbon nanotube conducting master batch；TPU/ carbon nanotube conducting master batch is prepared into by blowing, curtain coating or stretch processes
To the modified TPU antistatic film of Activated Carbon Nanotubes.Prepare what the technique of film was known to the skilled person.
The processing technology of described double screw extruder is screw speed 100～1000r/min, and extrusion temperature is 180-250
℃。
Double screw extruder melt extrudes granulation, and granulation 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 dispersant solution by high-pressure spraying
The form with spraying of putting sprays into the CNT of high-speed stirred, and 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 dispersiveness.
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, pre-processes its surface, simultaneously by dispersant, surface-active
The auxiliary agents such as agent are dissolved in liquid in the carbon nanotube dust being sprayed in stirring by 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 dispersiveness of CNT, and can simultaneously improve the bulk density of CNT, with obtain optimal dispersion effect with good
Good processability.
The present invention innovation by CNT after pretreatment modification, as conductive filler add to TPU material base
In body, prepare high efficiency dispersion TPU/ carbon nanotube conducting master batch, then prepared by blowing, curtain coating or stretch processes
The TPU antistatic film of different performance.Compared with traditional TPU 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 TPU matrix resin, improves antistatic persistence and the service life of film.
The TPU antistatic film that the present invention provides, outward appearance: uniform color, without stain, corrugationless, surface is without projection, without breaking
Hole, without vestige；Excellent mechanical: tensile strength: >=30MPA, elongation at break: >=150%, surface resistivity (Ω): 106
～109(content of carbon nanotubes=3wt.%).
4th, 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 dispersant in solvent, obtains dispersant solution, then leads to 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 preparing
Table 2
Described dispersiveness experiment detects by the following method: the Activated Carbon Nanotubes 10mg preparing embodiment 1～16 is respectively
10mL is added to 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 longer, shows that it disperses
Property is better.Not 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), dispersiveness is all significantly increased.
Embodiment 17～32
By Activated Carbon Nanotubes and the TPU polymer pulverulent material of embodiment 1～16 preparation (average grain diameter 100 μm～
2mm) stirring and evenly mixing, then mixing with auxiliary agent, each raw material dosage refers to table 3 and table 4, melt extrudes through double screw extruder, draws
Stretch, cooling and dicing prepares TPU/ carbon nanotube conducting master batch；The processing technology of double screw extruder is screw speed 200r/min,
Extrusion temperature is 180 DEG C.
The content of carbon nanotubes of the TPU/ carbon nanotube conducting master batch preparing is as shown in table 5.
The TPU/ carbon nanotube conducting master batch of preparation is prepared antistatic film through blow moulding machine blowing, 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,
Tensile strength: >=30MPA, elongation at break: >=150%.
Claims (10)
1. the TPU antistatic film of an Activated Carbon Nanotubes modification, it is characterised in that the modified TPU of described Activated Carbon Nanotubes
Antistatic film is made up of the component of following weight portion:
TPU polymeric 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 dispersant B, coupling agent, antioxidant, lubricant, one or more the mixing in 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 TPU antistatic film of Activated Carbon Nanotubes modification as claimed in claim 1, 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 TPU antistatic film of Activated Carbon Nanotubes modification as claimed in claim 1, it is characterised in that described dispersant A
Each stand alone as with dispersant B neopelex, TPU pyrrolidones, TPU alcohol, xanthans, lauryl sodium sulfate,
Triton X-100, sodium carboxymethylcellulose, Dihexadecylphosphate, Arabic gum, cetyl trimethyl bromination
In ammonium, alkyl phenol ethylene oxide condensation product emulsifying agent, cetyl trimethyl sodium bromide, Kynoar one or both with
On mixture.
4. the TPU antistatic film of Activated Carbon Nanotubes modification as claimed in claim 1, it is characterised in that described auxiliary agent is even
Connection agent, antioxidant, one or more and dispersant B, the mixing of lubricant in antifriction liniment.
5. the TPU antistatic film of Activated Carbon Nanotubes modification as claimed in claim 1, 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: TPU polymeric 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 TPU antistatic film of Activated Carbon Nanotubes modification as claimed in claim 1, it is characterised in that described solvent is
Water, N,N-dimethylformamide, 1-METHYLPYRROLIDONE, n-butanol, chloroform, absolute ethyl alcohol, acetone, petroleum ether, ethyl acetate,
One or more mixture in butyl acetate.
7. the TPU antistatic film of Activated Carbon Nanotubes modification as claimed in claim 1, it is characterised in that described coupling agent is
One or more mixture in titante coupling agent, silane coupling agent.
8. the TPU antistatic film of Activated Carbon Nanotubes modification as claimed in claim 1, it is characterised in that described antioxidant is
1098th, the 168th, the 1010th, the 1076th, DLTP, one or more the mixture in MB, the 164th, 264.
9. the TPU antistatic film of Activated Carbon Nanotubes modification as claimed in claim 1, it is characterised in that described lubricant is
Fatty acid, aliphatic amide type or ester lubricant, paraffin class lubricant, metallic soap salt lubricant, in low-molecular-weight wax one
Plant 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 micro mist.
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| CN109852035A (en) * | 2019-01-07 | 2019-06-07 | 山东中塑泰富科技有限公司 | A kind of reflective high/low temperature film and preparation method thereof |
| CN110903633A (en) * | 2019-11-28 | 2020-03-24 | 苏州市雄林新材料科技有限公司 | High-scratch-resistance TPU (thermoplastic polyurethane) film and preparation method thereof |
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| CN109852035A (en) * | 2019-01-07 | 2019-06-07 | 山东中塑泰富科技有限公司 | A kind of reflective high/low temperature film and preparation method thereof |
| CN110903633A (en) * | 2019-11-28 | 2020-03-24 | 苏州市雄林新材料科技有限公司 | High-scratch-resistance TPU (thermoplastic polyurethane) film and preparation method thereof |
| CN110903633B (en) * | 2019-11-28 | 2024-08-23 | 苏州市雄林新材料科技有限公司 | High scratch-resistant TPU film and preparation method thereof |
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