CN109130441A - A kind of controllable method for preparing of gradient HDPE electromagnetic wave shield film with multi-layer structure - Google Patents
A kind of controllable method for preparing of gradient HDPE electromagnetic wave shield film with multi-layer structure Download PDFInfo
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- 229920001903 high density polyethylene Polymers 0.000 title claims abstract description 61
- 239000004700 high-density polyethylene Substances 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000004743 Polypropylene Substances 0.000 claims abstract description 96
- 229920001155 polypropylene Polymers 0.000 claims abstract description 93
- 239000002048 multi walled nanotube Substances 0.000 claims abstract description 31
- 229920006262 high density polyethylene film Polymers 0.000 claims abstract description 28
- 239000000835 fiber Substances 0.000 claims abstract description 26
- 238000007731 hot pressing Methods 0.000 claims abstract description 23
- -1 polypropylene Polymers 0.000 claims abstract description 16
- 150000001875 compounds Chemical class 0.000 claims abstract description 15
- 238000009987 spinning Methods 0.000 claims abstract description 13
- 238000005507 spraying Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims description 15
- 239000006185 dispersion Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 7
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 6
- 239000008096 xylene Substances 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 abstract description 11
- 238000005516 engineering process Methods 0.000 abstract description 9
- 230000004048 modification Effects 0.000 abstract description 7
- 238000012986 modification Methods 0.000 abstract description 7
- 238000002604 ultrasonography Methods 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 44
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 14
- 239000010410 layer Substances 0.000 description 13
- 239000002041 carbon nanotube Substances 0.000 description 11
- 229910021393 carbon nanotube Inorganic materials 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 208000011580 syndromic disease Diseases 0.000 description 5
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- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000005670 electromagnetic radiation Effects 0.000 description 3
- 230000002745 absorbent Effects 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229910000906 Bronze Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000010974 bronze Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
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- 229920000128 polypyrrole Polymers 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/0088—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising a plurality of shielding layers; combining different shielding material structure
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
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- Electromagnetism (AREA)
- Microelectronics & Electronic Packaging (AREA)
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- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
- Nonwoven Fabrics (AREA)
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Abstract
The invention discloses a kind of controllable method for preparing of gradient HDPE electromagnetic wave shield film with multi-layer structure: with polypropylene (PP) for raw material, melt-blown PP superfine fibre net is made by melt-spraying spinning technology；It is modified using multi-walled carbon nanotube (MWCNTs) by the method for ultrasound modification, prepare the PP conducting fibrous web of various concentration gradient；The PP conducting fibrous web of HDPE film and various concentration gradient is subjected to alternately superposition and hot pressing is compound prepares multi-gradient HDPE electromagnetic wave shield film.The present invention carries out modification to melt-blown PP superfine fibre net using multi-walled carbon nanotube and prepares PP conducting fibrous web, and the PP conducting fibrous web of different electric conductivities and HDPE film carry out to hot pressing is compound to prepare multi-gradient HDPE electromagnetic wave shield film.The electromagnetic shielding performance of film is excellent, wide suitable for range, by the number of plies of selective stacking and the various concentration gradient of PP conducting fibrous web, it can be achieved that the controllable preparation of electromagnetic wave shield film.
Description
Technical field
The present invention relates to field of material preparation, and in particular to a kind of preparation of multilayered structure gradient HDPE electromagnetic wave shield film
Method.
Background technique
With the rapid development of electronic information technology and the extensive use of wireless technology, electromagnetic radiation becomes increasingly conspicuous.
Electromagnetic radiation has become the fourth-largest pollution sources after water pollution, atmosphere pollution and noise pollution, is not only detrimental to health,
Electromagnetic interference, electromagnetism is brought the safety problems such as to divulge a secret.Currently, that there are absorptivities is low, safeguard function is single, easy for electromagnetic shielding material
Generate secondary pollution problems.Therefore, the excellent electromagnetic shielding material of developing low-cost, high shield effectiveness, wideband absorbent properties
It is particularly important.
Polypropylene (PP) and high density polyethylene (HDPE) (HDPE) are general high molecular materials, from a wealth of sources, at low cost, are easy to
Processing, is widely used in film field.Multi-walled carbon nanotube (MWCNTs) has excellent electrical property, hot property, mechanical property,
As ideal filler be widely used in preparation have superior electrical conductivity energy, thermal stability, mechanical performance composite material.It is important
, with excellent flexibility, sheared, the external forces such as ultrasound when performance it is not easily damaged.
Summary of the invention
Aiming at the problems existing in the prior art, the present invention provides a kind of gradient HDPE electromagnetic screens with multi-layer structure
The controllable method for preparing of film is covered, with polypropylene (PP) and high density polyethylene (HDPE) (HDPE) for raw material, multi-walled carbon nanotube
(MWCNTs) it is modifying agent, prepares multi-gradient HDPE electromagnetic wave shield film.The preparation process is simple, and equipment requirement is low, HDPE
Film has preferable electromagnetic shielding performance in wideband, by the various concentration gradient and superimposion that select PP conducting fibrous web
The number of plies can realize the regulation to the electromagnet shield effect of HDPE film.
In order to solve the above technical problems, the invention adopts the following technical scheme:
A kind of controllable method for preparing of multi-gradient HDPE electromagnetic wave shield film, steps are as follows:
(1) with polypropylene (PP) for raw material, PP superfine fibre net is prepared using melt-spraying spinning technology；
(2) multi-walled carbon nanotube of different quality (MWCNTs) is added separately in xylene solvent, prepares mixed solution, it will
Mixed solution is put into ultrasonic washing instrument, ultrasonic vibration 60-90 minutes in 50-75 DEG C of water-bath, obtains dispersion liquid；
(3) the PP superfine fibre net prepared in step (1) is respectively placed in the dispersion liquid of different carbon nanotube concentrations in step (2)
In, ultrasonic vibration takes out after 1-3 minutes, dries 5-10 minutes in 50-70 DEG C of baking oven, the PP for obtaining various concentration gradient is led
Electric web；
(4) the PP conducting fibrous web for the various concentration gradient that HDPE film and step (3) obtain is overlapped, the compound system of hot pressing
Standby gradient HDPE electromagnetic wave shield film with multi-layer structure.
Melt-spraying spinning technology prepares the technological parameter of PP web in the step (1) are as follows: the setting temperature of screw extruder
Degree is 175-185 DEG C of 1st area, 2 215-225 DEG C of areas, 3 225-245 DEG C of areas, 4 235-250 DEG C of areas, 5 230-240 DEG C of areas；Melt blown die
The temperature of head is 230-235 DEG C；The temperature of metering pump is 230-250 DEG C, and metering pump speed is 230-235 r/ minutes；Drawing-off heat
The wind-warm syndrome and wind pressure of wind are respectively 230-250 DEG C and 8-15 MPa；The movement speed of lace curtaining is 2.5-4.5 m/ minutes.
In the step (1) PP web with a thickness of 10-30 μm, the diameter range of fiber is 5-10 μm.
The concentration of mixed solution is 0.01-0.5 mg/mL in the step (2).
It takes out after ultrasonic vibration 1-3 minutes in the step (3), is dried 5-10 minutes in 50-70 DEG C of baking oven, it should
Step in triplicate, obtains the PP conducting fibrous web of various concentration gradient.
The resistivity of PP conducting fibrous web is less than 500 Ω in the step (3).m。
HDPE film can be prepared by hot-forming or tentering film forming in the step (4), HDPE film with a thickness of
0.05-1mm。
The compound process conditions of hot pressing in the step (4): cope plate, lower template temperature be respectively 140-160oC,
Preheating 5-10 minutes, precompressed 0.5-1 minutes, hot pressing pressure 5-7 MPa.
Prepared multi-gradient HDPE film with a thickness of 0.15-3 mm in the step (4).
The mode that polypropylene conductive web and HDPE film are superimposed in the step (4) is to replace superposition, and HDPE film
The number of plies=polypropylene conductive web number of plies+1, gradient profile include from low to high, low-high-low, three kinds of forms of high-low-high.
The beneficial effects of the present invention are: the materials such as common intrinsic conducting polymers polyaniline, polypyrrole in (1) and document
It comparing, the present invention conducts a research using commodity polymer HDPE and PP as raw material, and it is at low cost, it is easily processed into type, it is applied widely；
(2) it compared with the metal modifiers such as common nickel powder, bronze, copper powder, using MWCNTs as modifying agent, not only significantly reduces and uses
Amount mitigates the quality of screened film, and has better absorbent properties to electromagnetic wave, (passes through reflecting barrier with metal modifiers
Electromagnetic wave) it compares, it can be reduced the secondary pollution of electromagnetic radiation；(3) pass through ultrasonic wavelength-division as carrier to be meltblown PP superfine fibre net
Scattered method carries out conductive modification, is conducive to MWCNTs in the evenly dispersed of web, substantially reduces the dosage of MWCNTs, reduces
Cost；(4) when conductive modification, make PP web that appropriateness occur in a solvent at a suitable temperature and be swollen, be conducive to enhance
The binding force of MWCNTs and PP web form stable conductive network, are conducive to the electromagnet shield effect for improving HDPE film；
(5) multilayered structure HDPE electromagnetic wave shield film prepared by the present invention, it is multiple anti-inside electromagnetic wave shield film by electromagnetic wave
It penetrates and decays, improve the electromagnetic shielding performance of material.In addition, by controlling carbon nanometer in the compound number of plies and PP conducting fibrous web
The concentration gradient of pipe can realize the controllable preparation to electromagnet shield effect；(6) PP conducting fibrous web and HDPE film are handed over
For superposition, the compound preparation HDPE screened film of hot pressing, hot-forming temperature higher than HDPE fusing point and lower than PP fusing point, both protected
The combination between HDPE electromagnetic wave shield film film multilayer is demonstrate,proved, and the structure of PP conducting fibrous web will not be destroyed.In HDPE screened film
PP conducting fibrous web is introduced, the controllable preparation of HDPE electromagnetic wave shield film is not only realized, is also beneficial to mechanical property and heat is steady
The raising of qualitative energy；(7) due to the particularity of gradient film material, thermal stress, electric conductivity, mechanical performance and electromagnetic shielding effect
It can wait related to the property of gradient film material itself and composition distribution.It can be with by adjusting the composition distribution of material in the present invention
Realize the regulation to the shield effectiveness of multi-gradient HDPE shielded film, mechanical property, thermal stability.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of multi-gradient HDPE electromagnetic wave shield film prepared by embodiment 1；
Fig. 2 is the electromagnet shield effect curve of multi-gradient HDPE electromagnetic wave shield film prepared by embodiment 1.
Specific embodiment
Below with reference to the embodiment of the present invention, technical solution of the present invention is clearly and completely described.Obviously, it is retouched
The embodiment stated is only a part of the embodiment of the present invention, instead of all the embodiments.Based on implementation disclosed in this invention
Example, those of ordinary skill in the art can carry out partial modification or equivalent replacement to technical solution of the present invention, not pay
Every other embodiment obtained under the premise of creative work out, shall fall within the protection scope of the present invention.
Embodiment 1
The controllable method for preparing of the present embodiment gradient HDPE electromagnetic wave shield film with multi-layer structure, steps are as follows:
(1) with polypropylene (PP) for raw material, PP superfine fibre net is prepared using melt-spraying spinning technology.Melt-spraying spinning technological parameter
Are as follows: -5 area's temperature of 1st area of screw extruder is followed successively by 185 DEG C, 225 DEG C, 245 DEG C, 250 DEG C, 240 DEG C；The temperature of meltblown beam is
235℃；The temperature of metering pump is 240 DEG C, and metering pump speed is 235 r/ minutes；The wind-warm syndrome and wind pressure of drawing-off hot wind be respectively
250 DEG C and 15 MPa；The movement speed of lace curtaining is 4.5 m/ minute, PP web with a thickness of 10 μm, the diameter of fiber is 6
µm；
(2) multi-walled carbon nanotube of different quality (MWCNTs) is added separately in 40mL xylene solvent, preparation quality is dense
Degree is respectively 0.1mg/mL, and mixed solution is put into ultrasonic washing instrument by 0.175mg/mL and 0.25mg/mL mixed solution,
Ultrasonic vibration 60 minutes, obtains the dispersion liquid of MWCNTs in 75 DEG C of water-baths；
(3) the PP superfine fibre net prepared in step (1) is respectively placed in the carbon nano tube dispersion liquid of various concentration in step (2)
In, ultrasonic vibration takes out after 1 minute, dries 10 minutes in 50 DEG C of baking ovens, obtains PP conducting fibrous web, and repetitive operation should
Step three times, tests the resistivity of PP conducting fibrous web, and chooses resistivity less than 500 Ω.The PP conducting fibrous web of m is spare；
(4) the hot-forming HDPE film with a thickness of 0.05 mm, the PP conducting fibrous web that HDPE film and step (3) are obtained
Alternately superposition is carried out, and is superimposed according to the gradient profile that carbon nanotube concentration in PP conducting fibrous web gradually increases, hot pressing is compound
Prepare gradient HDPE electromagnetic wave shield film with multi-layer structure.Hot pressing combination process are as follows: cope plate, lower template temperature be
160 oC, preheating 10 minutes, precompressed 1 minute, 5 MPa of hot pressing pressure, prepared multi-gradient HDPE electromagnetic wave shield film
With a thickness of 0.2mm.
The structural schematic diagram of multilayered structure gradient HDPE electromagnetic wave shield film manufactured in the present embodiment is as shown in Figure 1.By scheming
As can be seen that PP conducting fibrous web and HDPE film carry out alternately superposition (PP conducting fibrous web is clipped among HDPE film), and
It is overlapped according to the sequence that the concentration of carbon nanotube in PP fibre web gradually increases.For convenience, it is indicated with x/y/z-HDPE
Multi-gradient HDPE electromagnetic wave shield film, wherein x, y, z respectively represents the PP conduction after the solution modification of different MWCNTs concentration
Web, such as: 0.1/0.175/0.25-HDPE refers to that concentration is respectively 0.1 mg/mL, 0.175 mg/mL and 0.25 mg/
PP web after the modification of mL MWCNTs solution replaces the compound prepared electromagnetic wave shield film of superposition hot pressing with HDPE film.
In order to compare, it is prepared for single layer PP conducting fibrous web under identical process conditions and the electromagnetic shielding of HDPE Film laminated is thin
Film is named as x-HDPE, such as: 0.1-HDPE refers to the PP web after modifying using 0.1 mg/mL MWCNTs solution as interlayer
With the compound HDPE electromagnetic wave shield film with class " sandwich structure " of HDPE film hot-pressing.
Fig. 2 is the shield effectiveness curve of multi-gradient HDPE electromagnetic wave shield film.As seen from the figure, single under identical frequency
The shield effectiveness of layer electromagnetic wave shield film increases with the increase of MWCNTs pipe content in PP conducting fibrous web.This is because with
MWCNTs concentration increases, and is evenly distributed in PP fibre web, forms good conductive network, concentration is bigger, and conductive network is more perfect.
For multi-layer H DPE electromagnetic wave shield film in 3-21 gigahertz frequency range, shield effectiveness is above 32 dB, reaches civilian requirement.
Compared with single layer HDPE shielded film, the shield effectiveness of multi-gradient HDPE electromagnetic wave shield film is significantly improved.This is because electric
Order of reflection of the magnetic wave inside multilayer electromagnetic wave shield film and decaying number increase, and improve the electromagnetic shielding performance of material,
Front end electromagnet shield effect is also improved simultaneously.
Embodiment 2
The controllable method for preparing of the present embodiment gradient HDPE electromagnetic wave shield film with multi-layer structure, steps are as follows:
(1) with polypropylene (PP) for raw material, PP superfine fibre net is prepared using melt-spraying spinning technology.Melt-spraying spinning technological parameter
Are as follows: -5 area's temperature of 1st area of screw extruder is followed successively by 180 DEG C, 220 DEG C, 240 DEG C, 245 DEG C, 235 DEG C；The temperature of meltblown beam is
230℃；The temperature of metering pump is 235 DEG C, and metering pump speed is 235 r/ minutes；The wind-warm syndrome and wind pressure of drawing-off hot wind be respectively
250 DEG C and 15 MPa；The movement speed of lace curtaining is 4.5 m/ minutes.PP web with a thickness of 20 μm, the diameter of fiber is 7
µm；
(2) multi-walled carbon nanotube of different quality (MWCNTs) is added separately in 40mL xylene solvent, preparation quality is dense
It is clear to be put into ultrasonic wave by degree respectively 0.05mg/mL, 0.1mg/mL, 0.15mg/mL and 0.2mg/mL mixed solution for mixed solution
It washes in instrument, ultrasonic vibration 90 minutes, obtains the dispersion liquid of MWCNTs in 75 DEG C of water-baths；
(3) the PP superfine fibre net prepared in step (1) is respectively placed in the dispersion liquid of different carbon nanotube concentrations in step (2)
In, ultrasonic vibration takes out after 3 minutes, dries 10 minutes in 50 DEG C of baking ovens, obtains PP conducting fibrous web, the repetitive operation step
Suddenly three times.The resistivity of PP conducting fibrous web is tested, and chooses resistivity less than 500 Ω.The PP conducting fibrous web of m is spare；
(4) the hot-forming HDPE film with a thickness of 0.1 mm, the different carbon nanotubes that HDPE film is obtained from step (3) are dense
The PP conducting fibrous web of degree carries out alternately superposition, and the gradient shape gradually increased according to carbon nanotube concentration in PP conducting fibrous web
Formula superposition, hot pressing is compound to prepare gradient HDPE electromagnetic wave shield film with multi-layer structure, the temperature of cope plate when hot pressing, lower template
Degree is 150oC is preheated 10 minutes, and precompressed 1 minute, 7 MPa of hot pressing pressure, prepared gradient HDPE electromagnetic shielding was thin
Film with a thickness of 0.5mm.
Embodiment 3
The controllable method for preparing of the present embodiment gradient HDPE electromagnetic wave shield film with multi-layer structure, steps are as follows:
(1) with polypropylene (PP) for raw material, PP superfine fibre net is prepared using melt-spraying spinning technology；Melt-spraying spinning technological parameter
Are as follows: -5 area's temperature of 1st area of screw extruder is followed successively by 175 DEG C, 215 DEG C, 225 DEG C, 235 DEG C, 230 DEG C；The temperature of meltblown beam is
230℃；The temperature of metering pump is 230 DEG C, and metering pump speed is 230 r/ minutes；The wind-warm syndrome and wind pressure of drawing-off hot wind be respectively
230 DEG C and 8 MPa；The movement speed of lace curtaining is 2.5 m/ minutes.PP web with a thickness of 10 μm, the diameter of fiber is 10
µm。
(2) multi-walled carbon nanotube of different quality (MWCNTs) is added separately in 40mL xylene solvent, prepares matter
Amount concentration is respectively 0.01mg/mL, and mixed solution is put into ultrasound by 0.1mg/mL, 0.25mg/mL and 0.5mg/mL mixed solution
In wave cleaning device, ultrasonic vibration 90 minutes, obtains the dispersion liquid of MWCNTs in 75 DEG C of water-baths；
(3) the PP superfine fibre net prepared in step (1) is respectively placed in the dispersion liquid of different carbon nanotube concentrations in step (2)
In, ultrasonic vibration takes out after 2 minutes, dries 10 minutes in 50 DEG C of baking ovens, obtains PP conducting fibrous web, and repetitive operation should
Step is three times.The resistivity of PP conducting fibrous web is tested, and chooses resistivity less than 500 Ω.The PP conducting fibrous web of m is spare；
(4) film of the tentering film forming HDPE with a thickness of 0.1mm, the different carbon nanometers that HDPE film is obtained from step (3)
The PP conducting fibrous web of pipe concentration carries out alternately superposition, and the ladder gradually increased according to carbon nanotube concentration in PP conducting fibrous web
The superposition of degree form, hot pressing is compound to prepare gradient HDPE electromagnetic wave shield film with multi-layer structure, wherein when hot pressing, cope plate,
The temperature of lower template is 150oC, preheating 10 minutes, precompressed 1 minute, hot pressing pressure 7 MPa, prepared gradient HDPE
Electromagnetic wave shield film with a thickness of 0.5mm.
Embodiment 4
The controllable method for preparing of the present embodiment gradient HDPE electromagnetic wave shield film with multi-layer structure, steps are as follows:
(1) with polypropylene (PP) for raw material, PP superfine fibre net is prepared using melt-spraying spinning technology.Melt-spraying spinning technological parameter
Are as follows: -5 area's temperature of 1st area of screw extruder is followed successively by 180 DEG C, 220 DEG C, 240 DEG C, 245 DEG C, 235 DEG C；The temperature of meltblown beam is
230℃；The temperature of metering pump is 235 DEG C, and metering pump speed is 235 r/ minutes；The wind-warm syndrome and wind pressure of drawing-off hot wind be respectively
250 DEG C and 15 MPa；The movement speed of lace curtaining is 4.5 m/ minutes, PP web with a thickness of 30 μm, the diameter of fiber is
10 µm；
(2) multi-walled carbon nanotube of different quality (MWCNTs) is added separately in 40mL xylene solvent, preparation quality is dense
Degree is respectively 0.01mg/mL, 0.05mg/mL, 0.1mg/mL, 0.15mg/mL and 0.2mg/mL mixed solution puts mixed solution
Enter in ultrasonic washing instrument, ultrasonic vibration 90 minutes, obtains the dispersion liquid of MWCNTs in 50 DEG C of water-baths；
(3) the PP superfine fibre net prepared in step (1) is respectively placed in the dispersion liquid of different carbon nanotube concentrations in step (2)
In, ultrasonic vibration takes out after 2 minutes, dries 7 minutes in 50 DEG C of baking ovens, obtains PP conducting fibrous web, the repetitive operation step
Suddenly three times, the resistivity of PP conducting fibrous web is tested, and chooses resistivity less than 500 Ω.The PP conducting fibrous web of m is spare.
(4) the hot-forming HDPE film with a thickness of 0.5mm, the different carbon nanometers that HDPE film is obtained from step (3)
The PP conducting fibrous web of pipe concentration carries out alternately superposition, and according to the Gradient methods of carbon nanotube concentration high-low-high in PP fibre web
Superposition, hot pressing is compound to prepare gradient HDPE electromagnetic wave shield film with multi-layer structure, wherein the temperature of cope plate, lower template
It is 140oC, preheating 10 minutes, precompressed 1 minute, 7 MPa of hot pressing pressure, prepared multi-gradient HDPE electromagnetic shielding
Film with a thickness of 3mm.
Embodiment 5
The present embodiment difference from example 1 is that: in step (2) bath temperature be 75 DEG C, the ultrasonic vibration time be 30
Minute, the concentration of mixed solution is respectively 0.04 mg/mL, 0.08 mg/mL, 0.12 mg/mL and 0.16 mg/mL.
Embodiment 6
The present embodiment difference from example 1 is that: the stacking pattern of PP conducting fibrous web is alternately folded in step (4)
Add, concentration gradient mode is low-high-low.
Basic principles and main features and advantages of the present invention of the invention have been shown and described above.The skill of the industry
Art personnel it should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (10)
1. a kind of controllable method for preparing of gradient HDPE electromagnetic wave shield film with multi-layer structure, it is characterised in that step is such as
Under:
(1) using polypropylene as raw material, polypropylene superfine fiber net is prepared using melt-spraying spinning；
(2) multi-walled carbon nanotube of certain mass is added in xylene solvent, prepares mixed solution, mixed solution is put into
In ultrasonic washing instrument, ultrasonic vibration 60-90 minutes in 50-75 DEG C of water-bath, dispersion liquid is obtained；
(3) the polypropylene superfine fiber net prepared in step (1) is placed in the dispersion liquid that step (2) obtains, ultrasonic vibration 1-3
It is taken out after minute, is dried 5-10 minutes in 50-70 DEG C of baking oven, obtain the PP conducting fibrous web of various concentration gradient；
(4) the PP conducting fibrous web for the various concentration gradient that HDPE film and step (3) obtain is overlapped, the compound system of hot pressing
Obtain gradient HDPE electromagnetic wave shield film with multi-layer structure.
2. the controllable method for preparing of multilayered structure gradient HDPE electromagnetic wave shield film according to claim 1, feature exist
In: melt-spraying spinning prepares the technological parameter of polypropylene fiber net in the step (1) are as follows: the set temperature of screw extruder is 1
175-185 DEG C of area, 2 215-225 DEG C of areas, 3 225-245 DEG C of areas, 4 235-250 DEG C of areas, 5 230-240 DEG C of areas；The temperature of meltblown beam
Degree is 230-235 DEG C；The temperature of metering pump is 230-250 DEG C, and metering pump speed is 230-235r/ minutes；The wind of drawing-off hot wind
Mild wind pressure is respectively 230-250 DEG C and 8-15MPa；The movement speed of lace curtaining is 2.5-4.5m/ minutes.
3. the controllable method for preparing of gradient HDPE electromagnetic wave shield film with multi-layer structure according to claim 1,
Be characterized in that: in the step (1) polypropylene fiber net with a thickness of 10-30 μm, the diameter range of fiber is 5-10 μm.
4. the controllable method for preparing of gradient HDPE electromagnetic wave shield film with multi-layer structure according to claim 1,
Be characterized in that: the concentration of mixed solution is 0.01-0.5 mg/mL in the step (2).
5. the controllable method for preparing of gradient HDPE electromagnetic wave shield film with multi-layer structure according to claim 1,
It is characterized in that: being taken out after ultrasonic vibration 1-3 minutes in the step (3), dried 5-10 minutes in 50-70 DEG C of baking oven, the step
Suddenly in triplicate, the polypropylene conductive web of various concentration gradient is obtained.
6. the controllable method for preparing of gradient HDPE electromagnetic wave shield film with multi-layer structure according to claim 1,
Be characterized in that: the resistivity of PP conducting fibrous web is less than 500 Ω in the step (3).m。
7. the controllable method for preparing of gradient HDPE electromagnetic wave shield film with multi-layer structure according to claim 1,
It is characterized in that: HDPE film with a thickness of 0.05-1 mm in the step (4).
8. the controllable method for preparing of gradient HDPE electromagnetic wave shield film with multi-layer structure according to claim 1,
Be characterized in that: the compound process conditions of hot pressing in the step (4): cope plate, lower template temperature be respectively 140-160oC,
Preheating 5-10 minutes, precompressed 0.5-1 minutes, hot pressing pressure 5-7 MPa.
9. the controllable method for preparing of gradient HDPE electromagnetic wave shield film with multi-layer structure according to claim 1,
It is characterized in that: the compound prepared HDPE electromagnetic wave shield film of hot pressing with a thickness of 0.15-3mm in the step (4).
10. the controllable method for preparing of gradient HDPE electromagnetic wave shield film with multi-layer structure according to claim 1,
Be characterized in that: the mode that polypropylene conductive web and HDPE film are superimposed in the step (4) is to replace superposition, and HDPE film
The number of plies=polypropylene conductive web number of plies+1, gradient profile include from low to high, low-high-low, three kinds of forms of high-low-high.
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| CN114316637A (en) * | 2021-12-28 | 2022-04-12 | 南开大学 | Controllable preparation method of gradient composite membrane |
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| CN112980034A (en) * | 2021-02-26 | 2021-06-18 | 清华大学深圳国际研究生院 | Electromagnetic shielding film and preparation method thereof |
| CN114316637A (en) * | 2021-12-28 | 2022-04-12 | 南开大学 | Controllable preparation method of gradient composite membrane |
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