CN109251411A - A kind of preparation method of high-strength magnetic shielding plastic - Google Patents
A kind of preparation method of high-strength magnetic shielding plastic Download PDFInfo
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- CN109251411A CN109251411A CN201810926409.4A CN201810926409A CN109251411A CN 109251411 A CN109251411 A CN 109251411A CN 201810926409 A CN201810926409 A CN 201810926409A CN 109251411 A CN109251411 A CN 109251411A
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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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
- C08K2201/001—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
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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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
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/04—Thermoplastic elastomer
Abstract
The invention discloses a kind of preparation method of high-strength magnetic shielding plastic, include the following steps: that (1) matrix resin selection mixing, the preparation of (2) functional stuffing, (3) raw material weigh mixing process, (4) extrusion molding.The collocation of the method for the present invention integrated artistic step is rationally, easy to promote and utilize, and plastics obtained have very strong electromagnetic shielding capability, and the service performances such as its mechanics are strong, comprehensive to use good quality, the great market competitiveness and processing benefit.
Description
Technical field
The invention belongs to high-performance composite materials technical fields, and in particular to a kind of preparation of high-strength magnetic shielding plastic
Method.
Background technique
The rapid development of modern electronic technology is provided a great convenience to people's lives, while also being brought serious
Electromagnetic pollution.It not only endangers the health of people, also to the system stability of the information security of electronic equipment and surrounding devices
It constitutes a threat to.Developing high performance electromagnetic shielding material is the effective way to solve the above problems.In recent years, it is set to adapt to electronics
The development trend of standby lightness and Highgrade integration, electromagnetic shielding material are increasingly becoming new research hotspot.
Electromagnetic radiation is ubiquitous, and after atmosphere pollution, water pollution is acknowledged as the fourth-largest pollution after noise pollution.Electromagnetism
Radiation not only results in electromagnetic interference, destroys the normal operation of electronic electric equipment, and can threaten to human health.Tool
There is the electromagnetic shielding material of good shielding to have become the hot spot studied now, various countries are in the research side of novel shielding material
It does a lot of work in face.Filled-type composite electromagnetic shield materials are concerned due to superior performance, and it is domestic in this respect
Research far lags behind foreign countries, therefore studies novel electromagnetic shielding composite material and have practical significance.Electromagnetic shielding refers to
By electromagnetic pollution source to the Electromagnetic Wave Propagation pathway disruption between specified region, to reduce or eliminate pollution sources to specified region
The adverse effect that interior sensitive equipment, device or human body generates.
Traditional electromagnetic shielding material, such as metal material, although there is good electromagnet shield effect, due to it
Own wt is big, can not adapt to the purposes high molecular material of some special occasions with mechanical property is good, weight is small, can be soft
Property the features such as, start gradually to substitute some traditional material in many fields and the material with electromagnetic shielding performance be added
Composite material is formed into high molecular material, is a kind of solution that people seek Combined Electromagnetic Shielding Materials.
Carbon fiber is light, and raw material sources are extensive, has good electric conductivity, is a kind of great potential for substituted metal
The raw material of shielding.But the binding ability presently between its high molecular material is poor, is unfavorable for the increasing of integral composite quality
By force.In this regard, people have done a large amount of experiment to improve.Such as application No. is: 201710507824.1 Chinese patent discloses one
Kind low-resistance composite electromagnetic screen plastics enhance modeling by being added to the chopped graphite fibre imparting of the special active asphaltic base of one kind
The anti-electromagnetic shielding capability of material, and the mechanical quality of material is improved to a certain extent.But it is integrated can not still be expired using quality
The increasingly increased performance requirement of sufficient people, needs further to improve.
Summary of the invention
The purpose of the present invention is being directed to existing problem, a kind of preparation method of high-strength magnetic shielding plastic is provided.
The present invention is achieved by the following technical solutions:
A kind of preparation method of high-strength magnetic shielding plastic, includes the following steps:
(1) matrix resin selection mixing:
Weigh following resins by corresponding parts by weight: 60 ~ 65 parts of acrylic resins, 15 ~ 20 parts of polyvinyl resins, 8 ~ 12 parts it is poly- to benzene
Then naphthalate resin is put into above-mentioned resin in agitator tank jointly, matrix is taken out to obtain after 2 ~ 3h of stir process
Resin is spare；
(2) prepared by functional stuffing:
A. first multi-walled carbon nanotube is put into hydrogen peroxide solution, is taken out after 1 ~ 2h of immersion treatment, it then will that treated be more
Wall carbon nano tube and nonylphenol polyoxyethylene ether, deionized water be corresponding to be carried out mixing according to weight ratio 1:6 ~ 8:90 ~ 100 and puts into
In agitator tank, then with frequency be 400 ~ 420kHz ultrasonic echography handle 40 ~ 45min after take out mixture A is spare；
B. the resulting mixture A of a will be operated to be poured on filter membrane, then using Suction filtration device in the environment of 400 ~ 420kPa
Multi-wall carbon nano-tube film is made in suction filtration, carries out followed in turn by deionized water and methanol to manufactured multi-wall carbon nano-tube film anti-
Multiple flushing, until after cleaning solution is colourless, then the vacuum that temperature is 93 ~ 96 DEG C is put into multi-wall carbon nano-tube film taking-up and is done
It is dried, is taken out after 6 ~ 8h spare in dry case；
C. it the resulting multi-wall carbon nano-tube film of b will be operated is put into irradiation box and carry out radiation treatment, taken out after 50 ~ 60min
It is spare；
D. will operation c treated that multi-wall carbon nano-tube film is immersed in the chemical aqueduct for filling electroplate liquid, then adjust electricity
The pH value of plating solution is 8.5 ~ 9.0, and the temperature heated in the chemical aqueduct of holding is 33 ~ 36 DEG C, and subsequent start-up Vltrasonic device carries out
Chemical plating filters out the multi-wall carbon nano-tube film after plating after 35 ~ 40min, and drying is standby after being rinsed one time with deionized water
With；
E. operation d treated multi-wall carbon nano-tube film is launched into modification liquid, it is laggard is stirred continuously 3 ~ 4h of processing
Row filters, and is then washed repeatedly 4 ~ 5 times with dehydrated alcohol and dilute hydrochloric acid to object is filtered, and finally places it in again dry in insulating box
Taking-up is spare to get functional stuffing after handling 18 ~ 20h；
(3) raw material weighs mixing process:
Weigh following raw materials according by corresponding parts by weight: the resulting matrix resin of 90 ~ 100 parts of steps (1), 8 ~ 12 parts of steps (2) are made
Functional stuffing, 10 ~ 15 parts of plasticized modifiers, 1 ~ 3 part of antioxidant, 1 ~ 2 part of ultraviolet absorbing agent, then by above-mentioned all raw materials
Put into jointly and carry out mixing process in kneading machine, taken out after 35 ~ 40min mixing materials are spare；
(4) extrusion molding:
Step (3) resulting mixing materials are put into double screw extruder after carrying out extrusion molding, then cooled to room temperature
Afterwards.
Further, the mass fraction of hydrogen peroxide solution described in step (2) operation a is 25 ~ 30%.
Further, radiation treatment described in step (2) operation c is the processing of He ion irradiation, controls spoke in processing
According to energy be 300 ~ 320keV, irradiation temperature control be 430 ~ 450 DEG C, injection rate be 3 ~ 5 × 1016 cm-2。
Further, step (2) operates electroplate liquid described in d by the material composition of following parts by weight: 300 ~ 320 parts of matter
Measure nickel sulfate solution, 3 ~ 5 parts of ammonium chlorides, 0.2 ~ 0.4 part of sodium citrate, 0.1 ~ 0.3 part of phytic acid that score is 35%.
Further, step (2) operates modification liquid described in e by the material composition of following parts by weight: 90 ~ 100
Hydrochloric acid solution, 4 ~ 7 part neopelexes, 3 ~ 5 part polyethylene glycol, 6 ~ 9 part aniline hydrochloride, 2 of part mass fraction for 20%
~ 4 parts of 4- toluenesulfonic acid sodium salts, 1 ~ 3 part of ammonium persulfate, 0.5 ~ 1 part of sodium pyrophosphate.
Further, temperature when drying process described in step (2) operation e in control insulating box is 70 ~ 75 DEG C.
Further, plasticized modifier described in step (3) is thermoplastic elastomer (TPE).
Further, antioxidant described in step (3) is one of antioxidant 1010, irgasfos 168.
Further, ultraviolet absorbing agent described in step (3) is Ultraviolet Absorber UV-P, ultraviolet absorbing agent
One of UV-O.
Further, it is 210 ~ 220 that the temperature that double screw extruder squeezes out is controlled when extrusion molding described in step (4)
℃。
The present invention provides a kind of composite plastics with good electromagnetic shielding performance, specifically optimize its preparation side
Method, a kind of functional stuffing ingredient of during which special preparation, hence it is evident that enhance mechanical quality, the electromagnet shield effect of material.It is made
The functional stuffing obtained is a kind of using multi-walled carbon nanotube as made of base matter modification, and carbon nanotube has good conduction
Property, but it is still bad compared to for the electromagnetic shielding capability of metal material, limit its popularization and application.In this regard, the present invention carries out
Targetedly enhancing is handled, and has first been made into multi-wall carbon nano-tube film convenient for subsequent modification, then to multi wall
Carbon nano-tube film has carried out the processing of He ion irradiation, this radiation treatment can carry out a degree of etching to carbon nanotube wall,
So that wall portion grouping is knitted and is deformed, and texturing tube wall tissue, whole surface roughness is moderately improved, is subsequent
Electroplating deposition processing is laid a good foundation, while radiation treatment also irradiates the helium bubble group for introducing small particle on multi-walled carbon nanotubes
It knits, this organizes the specific surface area and adsorption capacity that can further promote multi-walled carbon nanotube, enhances and disappears to the absorption of electromagnetic wave
It receives ability, has then carried out chemical plating, electroplating deposition metal nickel layer, is coated on multi wall carbon and receives on multi-walled carbon nanotubes
On the outer wall of mitron, this nickel layer can further enhance electromagnetic wave absorption, last to be impregnated again with modification liquid, in multi wall
The outermost layers of polymer of carbon nanotube has secured the polyaniline of one layer of 4- toluenesulfonic acid natrium doping, and polyaniline has stable lead
Electrically, its electrical property further enhances after 4- toluenesulfonic acid sodium salt doping treatment.The functional stuffing being finally made is that one kind is more
The three-decker that wall carbon nano tube is internal layer, metal nickel layer is middle layer, polyaniline is outer layer, the hollow structure energy of innermost layer
Enough play the role of multipath reflection loss, middle layer can play the absorption loss ability of metal, and outermost layer can not only play suction
Receive loss, moreover it is possible to play the role of coupling with innermost layer, shunt attenuation is played to electromagnetic wave, it furthermore can also reinforcing filler
Compatible combination strength between plastic resin matrix, and then the qualities such as mechanics for enhancing material entirety.
The present invention has the advantage that compared with prior art
The collocation of the method for the present invention integrated artistic step is rationally, easy to promote and utilize, and plastics obtained have very strong electromagnetic shielding
Ability, and the service performances such as its mechanics are strong, it is comprehensive to use good quality, the great market competitiveness and processing benefit.
Specific embodiment
Embodiment 1
A kind of preparation method of high-strength magnetic shielding plastic, includes the following steps:
(1) matrix resin selection mixing:
Following resins: 60 parts of acrylic resins, 15 parts of polyvinyl resins, 8 parts of poly terephthalic acid second are weighed by corresponding parts by weight
Then terephthalate resin is put into above-mentioned resin in agitator tank jointly, taken out after stir process 2h matrix resin is spare；
(2) prepared by functional stuffing:
A. first multi-walled carbon nanotube is put into hydrogen peroxide solution, is taken out after immersion treatment 1h, it then will treated multi wall
Carbon nanotube and nonylphenol polyoxyethylene ether, deionized water be corresponding to be carried out mixing according to weight ratio 1:6:90 and puts into agitator tank
It is interior, the ultrasonic echography for being then 400kHz with frequency processing 40min after take out mixture A is spare；
B. the resulting mixture A of a will be operated to be poured on filter membrane, then filtered in the environment of 400kPa using Suction filtration device
Multi-wall carbon nano-tube film is made, manufactured multi-wall carbon nano-tube film is rushed repeatedly followed in turn by deionized water and methanol
It washes, until after cleaning solution is colourless, then multi-wall carbon nano-tube film is taken out and is put into the vacuum oven that temperature is 93 DEG C
It is dried, is taken out after 6h spare；
C. it the resulting multi-wall carbon nano-tube film of b will be operated is put into irradiation box and carry out radiation treatment, taken out after 50min standby
With；
D. will operation c treated that multi-wall carbon nano-tube film is immersed in the chemical aqueduct for filling electroplate liquid, then adjust electricity
The pH value of plating solution is 8.5, and the temperature heated in the chemical aqueduct of holding is 33 DEG C, and subsequent start-up Vltrasonic device carries out at chemical plating
It manages, filters out the multi-wall carbon nano-tube film after plating after 35min, drying for standby after being rinsed one time with deionized water；
E. operation d treated multi-wall carbon nano-tube film is launched into modification liquid, is carried out after being stirred continuously processing 3h
It filters, is then washed repeatedly 4 times with dehydrated alcohol and dilute hydrochloric acid to object is filtered, finally place it in insulating box and be dried again
It is taken out after 18h spare to get functional stuffing；
(3) raw material weighs mixing process:
Weigh following raw materials according by corresponding parts by weight: function made from the resulting matrix resin of 90 parts of steps (1), 8 parts of steps (2) is filled out
Above-mentioned all raw materials are then put into mixing by material, 10 parts of plasticized modifiers, 1 part of antioxidant, 1 part of ultraviolet absorbing agent jointly
Mixing process is carried out in machine, taken out after 35min mixing materials are spare；
(4) extrusion molding:
Step (3) resulting mixing materials are put into double screw extruder after carrying out extrusion molding, then cooled to room temperature
Afterwards.
Further, the mass fraction of hydrogen peroxide solution described in step (2) operation a is 25%.
Further, radiation treatment described in step (2) operation c is the processing of He ion irradiation, controls spoke in processing
According to energy be 300keV, irradiation temperature control be 430 DEG C, injection rate be 3 × 1016 cm-2。
Further, step (2) operates electroplate liquid described in d by the material composition of following parts by weight: 300 parts of quality point
Nickel sulfate solution, 3 part ammonium chlorides, 0.2 part sodium citrate, 0.1 part phytic acid of the number for 35%.
Further, step (2) operates modification liquid described in e by the material composition of following parts by weight: 90 parts of matter
Measure hydrochloric acid solution, the 4 parts of neopelexes, 3 parts of polyethylene glycol, 6 parts of aniline hydrochlorides, 2 parts of 4- toluene sulphurs that score is 20%
Sour sodium, 1 part of ammonium persulfate, 0.5 part of sodium pyrophosphate.
Further, temperature when drying process described in step (2) operation e in control insulating box is 70 DEG C.
Further, plasticized modifier described in step (3) is thermoplastic elastomer (TPE).
Further, antioxidant described in step (3) is antioxidant 1010.
Further, ultraviolet absorbing agent described in step (3) is Ultraviolet Absorber UV-P.
Further, it is 210 DEG C that the temperature that double screw extruder squeezes out is controlled when extrusion molding described in step (4).
Embodiment 2
A kind of preparation method of high-strength magnetic shielding plastic, includes the following steps:
(1) matrix resin selection mixing:
Following resins: 63 parts of acrylic resins, 18 parts of polyvinyl resins, 10 parts of poly terephthalic acid second are weighed by corresponding parts by weight
Then terephthalate resin is put into above-mentioned resin in agitator tank jointly, taken out after stir process 2.5h matrix resin is spare；
(2) prepared by functional stuffing:
A. first multi-walled carbon nanotube is put into hydrogen peroxide solution, is taken out after immersion treatment 1.6h, it then will that treated be more
Wall carbon nano tube and nonylphenol polyoxyethylene ether, deionized water be corresponding to be carried out mixing according to weight ratio 1:7:95 and puts into agitator tank
It is interior, the ultrasonic echography for being then 410kHz with frequency processing 43min after take out mixture A is spare；
B. the resulting mixture A of a will be operated to be poured on filter membrane, then filtered in the environment of 410kPa using Suction filtration device
Multi-wall carbon nano-tube film is made, manufactured multi-wall carbon nano-tube film is rushed repeatedly followed in turn by deionized water and methanol
It washes, until after cleaning solution is colourless, then multi-wall carbon nano-tube film is taken out and is put into the vacuum oven that temperature is 95 DEG C
It is dried, is taken out after 7h spare；
C. it the resulting multi-wall carbon nano-tube film of b will be operated is put into irradiation box and carry out radiation treatment, taken out after 55min standby
With；
D. will operation c treated that multi-wall carbon nano-tube film is immersed in the chemical aqueduct for filling electroplate liquid, then adjust electricity
The pH value of plating solution is 8.8, and the temperature heated in the chemical aqueduct of holding is 35 DEG C, and subsequent start-up Vltrasonic device carries out at chemical plating
It manages, filters out the multi-wall carbon nano-tube film after plating after 37min, drying for standby after being rinsed one time with deionized water；
E. operation d treated multi-wall carbon nano-tube film is launched into modification liquid, it is laggard is stirred continuously processing 3.5h
Row filters, and is then washed repeatedly 4 times with dehydrated alcohol and dilute hydrochloric acid to object is filtered, and finally places it in again at dry in insulating box
Taking-up is spare to get functional stuffing after managing 19h；
(3) raw material weighs mixing process:
Following raw materials according: function made from the resulting matrix resin of 95 parts of steps (1), 10 parts of steps (2) is weighed by corresponding parts by weight
Filler, 13 parts of plasticized modifiers, 2 parts of antioxidant, 1.5 parts of ultraviolet absorbing agents, then put into above-mentioned all raw materials jointly
Mixing process is carried out in kneading machine, taken out after 38min mixing materials are spare；
(4) extrusion molding:
Step (3) resulting mixing materials are put into double screw extruder after carrying out extrusion molding, then cooled to room temperature
Afterwards.
Further, the mass fraction of hydrogen peroxide solution described in step (2) operation a is 28%.
Further, radiation treatment described in step (2) operation c is the processing of He ion irradiation, controls spoke in processing
According to energy be 310keV, irradiation temperature control be 440 DEG C, injection rate be 4 × 1016 cm-2。
Further, step (2) operates electroplate liquid described in d by the material composition of following parts by weight: 310 parts of quality point
Nickel sulfate solution, 4 part ammonium chlorides, 0.3 part sodium citrate, 0.2 part phytic acid of the number for 35%.
Further, step (2) operates modification liquid described in e by the material composition of following parts by weight: 95 parts of matter
Measure hydrochloric acid solution, the 6 parts of neopelexes, 4 parts of polyethylene glycol, 8 parts of aniline hydrochlorides, 3 parts of 4- toluene sulphurs that score is 20%
Sour sodium, 2 parts of ammonium persulfates, 0.8 part of sodium pyrophosphate.
Further, temperature when drying process described in step (2) operation e in control insulating box is 73 DEG C.
Further, plasticized modifier described in step (3) is thermoplastic elastomer (TPE).
Further, antioxidant described in step (3) is antioxidant 1010.
Further, ultraviolet absorbing agent described in step (3) is Ultraviolet Absorber UV-P.
Further, it is 215 DEG C that the temperature that double screw extruder squeezes out is controlled when extrusion molding described in step (4).
Embodiment 3
A kind of preparation method of high-strength magnetic shielding plastic, includes the following steps:
(1) matrix resin selection mixing:
Following resins: 65 parts of acrylic resins, 20 parts of polyvinyl resins, 12 parts of poly terephthalic acid second are weighed by corresponding parts by weight
Then terephthalate resin is put into above-mentioned resin in agitator tank jointly, taken out after stir process 3h matrix resin is spare；
(2) prepared by functional stuffing:
A. first multi-walled carbon nanotube is put into hydrogen peroxide solution, is taken out after immersion treatment 2h, it then will treated multi wall
Carbon nanotube and nonylphenol polyoxyethylene ether, deionized water be corresponding to be carried out mixing according to weight ratio 1:8:100 and puts into agitator tank
It is interior, the ultrasonic echography for being then 420kHz with frequency processing 45min after take out mixture A is spare；
B. the resulting mixture A of a will be operated to be poured on filter membrane, then filtered in the environment of 420kPa using Suction filtration device
Multi-wall carbon nano-tube film is made, manufactured multi-wall carbon nano-tube film is rushed repeatedly followed in turn by deionized water and methanol
It washes, until after cleaning solution is colourless, then multi-wall carbon nano-tube film is taken out and is put into the vacuum oven that temperature is 96 DEG C
It is dried, is taken out after 8h spare；
C. it the resulting multi-wall carbon nano-tube film of b will be operated is put into irradiation box and carry out radiation treatment, taken out after 60min standby
With；
D. will operation c treated that multi-wall carbon nano-tube film is immersed in the chemical aqueduct for filling electroplate liquid, then adjust electricity
The pH value of plating solution is 9.0, and the temperature heated in the chemical aqueduct of holding is 36 DEG C, and subsequent start-up Vltrasonic device carries out at chemical plating
It manages, filters out the multi-wall carbon nano-tube film after plating after 40min, drying for standby after being rinsed one time with deionized water；
E. operation d treated multi-wall carbon nano-tube film is launched into modification liquid, is carried out after being stirred continuously processing 4h
It filters, is then washed repeatedly 5 times with dehydrated alcohol and dilute hydrochloric acid to object is filtered, finally place it in insulating box and be dried again
It is taken out after 20h spare to get functional stuffing；
(3) raw material weighs mixing process:
Following raw materials according: function made from the resulting matrix resin of 100 parts of steps (1), 12 parts of steps (2) is weighed by corresponding parts by weight
Filler, 15 parts of plasticized modifiers, 3 parts of antioxidant, 2 parts of ultraviolet absorbing agents are then put into above-mentioned all raw materials mixed jointly
Mixing process is carried out in mill, taken out after 40min mixing materials are spare；
(4) extrusion molding:
Step (3) resulting mixing materials are put into double screw extruder after carrying out extrusion molding, then cooled to room temperature
Afterwards.
Further, the mass fraction of hydrogen peroxide solution described in step (2) operation a is 30%.
Further, radiation treatment described in step (2) operation c is the processing of He ion irradiation, controls spoke in processing
According to energy be 320keV, irradiation temperature control be 450 DEG C, injection rate be 5 × 1016 cm-2。
Further, step (2) operates electroplate liquid described in d by the material composition of following parts by weight: 320 parts of quality
Nickel sulfate solution, 5 part ammonium chlorides, 0.4 part sodium citrate, 0.3 part phytic acid of the score for 35%.
Further, step (2) operates modification liquid described in e by the material composition of following parts by weight: 100 parts
Hydrochloric acid solution, 7 part neopelexes, 5 part polyethylene glycol, 9 part aniline hydrochlorides, 4 part 4- toluene of the mass fraction for 20%
Sodium sulfonate, 3 parts of ammonium persulfates, 1 part of sodium pyrophosphate.
Further, temperature when drying process described in step (2) operation e in control insulating box is 75 DEG C.
Further, plasticized modifier described in step (3) is thermoplastic elastomer (TPE).
Further, antioxidant described in step (3) is irgasfos 168.
Further, ultraviolet absorbing agent described in step (3) is ultraviolet absorbing agent UV-O.
Further, it is 220 DEG C that the temperature that double screw extruder squeezes out is controlled when extrusion molding described in step (4).
Comparative example 1
This comparative example 1 compared with Example 2, in the preparation of step (2) functional stuffing, eliminates the processing of operation c, removes this
Outer method and step is all the same.
Comparative example 2
This comparative example 2 compared with Example 2, in the preparation of step (2) functional stuffing, eliminates the processing of operation d, removes this
Outer method and step is all the same.
Comparative example 3
This comparative example 3 compared with Example 2, in the preparation of step (2) functional stuffing, eliminates the processing of operation e, removes this
Outer method and step is all the same.
Comparative example 4
Compared with Example 2, in step (3), raw material weighs in mixing process this comparative example 4, with etc. mass parts it is commercially available more
Functional stuffing ingredient made from wall carbon nano tube step of replacing (2), method and step in addition to this are all the same.
Control group
Application No. is: a kind of low-resistance composite electromagnetic screen plastics disclosed in 201710507824.1.
In order to compare effect of the present invention, to above-described embodiment 2, comparative example 1, comparative example 2, comparative example 3,
The corresponding plastic components of comparative example 4, control group carry out performance detection, and specific correlation data is as shown in table 1 below:
Table 1
Note: the corresponding unified detection according to national standards of performance indexes described in upper table 1.
The overall performance of the plastics made from the method for the present invention it can be seen from upper table 1 is obviously improved, and is overcome existing
There is the problem bad for carbon nanotube service performance, provides a kind of new technical solution, the great market competitiveness.
Claims (10)
1. a kind of preparation method of high-strength magnetic shielding plastic, which comprises the steps of:
(1) matrix resin selection mixing:
Weigh following resins by corresponding parts by weight: 60 ~ 65 parts of acrylic resins, 15 ~ 20 parts of polyvinyl resins, 8 ~ 12 parts it is poly- to benzene
Then naphthalate resin is put into above-mentioned resin in agitator tank jointly, matrix is taken out to obtain after 2 ~ 3h of stir process
Resin is spare；
(2) prepared by functional stuffing:
A. first multi-walled carbon nanotube is put into hydrogen peroxide solution, is taken out after 1 ~ 2h of immersion treatment, it then will that treated be more
Wall carbon nano tube and nonylphenol polyoxyethylene ether, deionized water be corresponding to be carried out mixing according to weight ratio 1:6 ~ 8:90 ~ 100 and puts into
In agitator tank, then with frequency be 400 ~ 420kHz ultrasonic echography handle 40 ~ 45min after take out mixture A is spare；
B. the resulting mixture A of a will be operated to be poured on filter membrane, then using Suction filtration device in the environment of 400 ~ 420kPa
Multi-wall carbon nano-tube film is made in suction filtration, carries out followed in turn by deionized water and methanol to manufactured multi-wall carbon nano-tube film anti-
Multiple flushing, until after cleaning solution is colourless, then the vacuum that temperature is 93 ~ 96 DEG C is put into multi-wall carbon nano-tube film taking-up and is done
It is dried, is taken out after 6 ~ 8h spare in dry case；
C. it the resulting multi-wall carbon nano-tube film of b will be operated is put into irradiation box and carry out radiation treatment, taken out after 50 ~ 60min
It is spare；
D. will operation c treated that multi-wall carbon nano-tube film is immersed in the chemical aqueduct for filling electroplate liquid, then adjust electricity
The pH value of plating solution is 8.5 ~ 9.0, and the temperature heated in the chemical aqueduct of holding is 33 ~ 36 DEG C, and subsequent start-up Vltrasonic device carries out
Chemical plating filters out the multi-wall carbon nano-tube film after plating after 35 ~ 40min, and drying is standby after being rinsed one time with deionized water
With；
E. operation d treated multi-wall carbon nano-tube film is launched into modification liquid, it is laggard is stirred continuously 3 ~ 4h of processing
Row filters, and is then washed repeatedly 4 ~ 5 times with dehydrated alcohol and dilute hydrochloric acid to object is filtered, and finally places it in again dry in insulating box
Taking-up is spare to get functional stuffing after handling 18 ~ 20h；
(3) raw material weighs mixing process:
Weigh following raw materials according by corresponding parts by weight: the resulting matrix resin of 90 ~ 100 parts of steps (1), 8 ~ 12 parts of steps (2) are made
Functional stuffing, 10 ~ 15 parts of plasticized modifiers, 1 ~ 3 part of antioxidant, 1 ~ 2 part of ultraviolet absorbing agent, then by above-mentioned all raw materials
Put into jointly and carry out mixing process in kneading machine, taken out after 35 ~ 40min mixing materials are spare；
(4) extrusion molding:
Step (3) resulting mixing materials are put into double screw extruder after carrying out extrusion molding, then cooled to room temperature
Afterwards.
2. a kind of preparation method of high-strength magnetic shielding plastic according to claim 1, which is characterized in that step (2)
The mass fraction for operating hydrogen peroxide solution described in a is 25 ~ 30%.
3. a kind of preparation method of high-strength magnetic shielding plastic according to claim 1, which is characterized in that step (2)
Radiation treatment described in c is operated as the processing of He ion irradiation, the energy of control irradiation is 300 ~ 320keV, irradiation in processing
Temperature control be 430 ~ 450 DEG C, injection rate be 3 ~ 5 × 1016 cm-2。
4. a kind of preparation method of high-strength magnetic shielding plastic according to claim 1, which is characterized in that step (2)
Electroplate liquid described in d is operated by the material composition of following parts by weight: nickel sulfate solution that 300 ~ 320 parts of mass fractions are 35%,
3 ~ 5 parts of ammonium chlorides, 0.2 ~ 0.4 part of sodium citrate, 0.1 ~ 0.3 part of phytic acid.
5. a kind of preparation method of high-strength magnetic shielding plastic according to claim 1, which is characterized in that step (2)
Modification liquid described in e is operated by the material composition of following parts by weight: the hydrochloric acid that 90 ~ 100 parts of mass fractions are 20% is molten
Liquid, 4 ~ 7 parts of neopelexes, 3 ~ 5 parts of polyethylene glycol, 6 ~ 9 parts of aniline hydrochlorides, 2 ~ 4 parts of 4- toluenesulfonic acid sodium salts, 1 ~ 3 part
Ammonium persulfate, 0.5 ~ 1 part of sodium pyrophosphate.
6. a kind of preparation method of high-strength magnetic shielding plastic according to claim 1, which is characterized in that step (2)
Temperature when operating drying process described in e in control insulating box is 70 ~ 75 DEG C.
7. a kind of preparation method of high-strength magnetic shielding plastic according to claim 1, which is characterized in that step (3)
Described in plasticized modifier be thermoplastic elastomer (TPE).
8. a kind of preparation method of high-strength magnetic shielding plastic according to claim 1, which is characterized in that step (3)
Described in antioxidant be one of antioxidant 1010, irgasfos 168.
9. a kind of preparation method of high-strength magnetic shielding plastic according to claim 1, which is characterized in that step (3)
Described in ultraviolet absorbing agent be one of Ultraviolet Absorber UV-P, ultraviolet absorbing agent UV-O.
10. a kind of preparation method of high-strength magnetic shielding plastic according to claim 1, which is characterized in that step (4)
Described in extrusion molding when control double screw extruder squeeze out temperature be 210 ~ 220 DEG C.
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