CN106433070B - A kind of halogen-free flame retardant PC material and preparation method thereof with electromagnetic shielding characteristic - Google Patents
A kind of halogen-free flame retardant PC material and preparation method thereof with electromagnetic shielding characteristic Download PDFInfo
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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Abstract
The present invention relates to electromagnetic shielding composite material field more particularly to a kind of halogen-free flame retardant PC materials and preparation method thereof with electromagnetic shielding characteristic, and the halogen-free flame retardant PC material includes the raw material components of following mass percent：PC resin, makrolon poly organo alkyl copolymer, stainless fiber beam carbon fiber, carbon nanotube, ethylene butyl acrylate copolymer, silica acrylic acid copolymer, poly aryl phosphate ester, fire retardant, fire retarding synergist, polytetrafluoroethylene (PTFE), antioxidant 612S, antioxidant 1076, pentaerythritol stearate.The present invention first carries out pre-treatment to stainless fiber beam, then it is carrying out that granulation is blended with unclassified stores, the standby halogen-free flame retardant PC material for providing electromagnetic shielding characteristic, conductive characteristic, shield effectiveness, flame-retarding characteristic and strength and toughness are excellent, and process operation is convenient, efficient.
Description
Technical field
The present invention relates to electromagnetic shielding composite material field more particularly to a kind of halogen-free flameproofs with electromagnetic shielding characteristic
PC materials and preparation method thereof.
Background technology
The advantages such as high intensity, high tenacity, high heat resisting temperature and good electrology characteristic that makrolon has, make its
The electronics industry epoch are widely used, and with the fast development of electronics and communications industry, it is generated by electronic equipment
Some electromagnetic radiations increasingly cause the concern of society, these electromagnetic waves cause threat to the health of human body, and these
In electronic application field industry all to it is fire-retardant and it is environmentally friendly carried out strict requirements, thus develop with electromagnetic shielding characteristic
Halogen-free flame retardant PC material sense is very big.
Current existing electromagnetic shielding composite material is mainly using filler of the addition with conductive characteristic（Conductive black, gold
Belong to powder）Or fiber（Conductive carbon fibre, stainless steel fibre, metallic fiber）Etc. being modified.However conductive black, carbon fiber
There are the disadvantages such as poorly conductive, additive amount are big, shield effectiveness is low, while conductive black also has the technology difficulty for being difficult to add to deposit
；Nickel, copper, iron, silver powder belong to me tallic conductive filler, good conductivity, however since it belongs to one-dimension type conductive filler, it is moulding
It is in powdered presence substantially in material, the two dimension connection and bridging action between conductive filler become very weak, and then influence whether the phase
Shield effectiveness.
Stainless steel fibre is mainstream applications on the market due to having preferable sexual valence when processing characteristics, main at present
Melt blending is carried out in double screw extruder with plastics by directly adding stainless steel fibre, this method is it is easier that stainless steel is fine
Dimension becomes very broken under screw rod shearing effect, while larger to the abrasion of extruder gun barrel, screw rod, and practical operation gets up to integrate effect
Fruit is unsatisfactory.
East is opened to cause to exist《The preparation of SSF_ABS and GF_PA6 composite materials and performance study》In point out to first pass through cable cladding
Technique prepares stainless steel fibre filling ABS masterbatch, is added to be blended in ABS composite material by master batch later and takes out grain, this method has
Effect avoids being in direct contact for stainless steel fibre and screw rod, reduces the friction damage to screw machine gun barrel, however master batch exists
After being blended with the melting of ABS shearing, the draw ratio of stainless steel fibre inevitably declines, and then influences conductive and shielding effect
Fruit.
Chinese patent CN101812239B discloses a kind of preparation method of particle-filled conductive thermoplastic polymer, and carbon is received
Mitron, stainless steel fibre are respectively adopted special preparation process and are molded into master batch, later directly by conductive agglomerate and conducting base
Injection molding product after resin physical blending.It is found in practical operation since the proportion of conductive agglomerate is larger, especially stainless steel
Conductive agglomerate prepared by fiber, larger difference of specific gravity between these master batches and conducting base resin so that it is difficult to be thoroughly mixed
Uniformly, and the region of hopper blanking is layered it is easy to appear conductive agglomerate and conducting base resin and blanking is unstable phenomenon,
And then it is very big to cause the conductive characteristic of injection molding product to fluctuate.
Invention content
In order to overcome shortcoming and defect existing in the prior art, the purpose of the present invention is to provide one kind having electromagnetic screen
The halogen-free flame retardant PC material of characteristic is covered, conductive characteristic, shield effectiveness, flame-retarding characteristic and strength and toughness are excellent.
The purpose of the present invention is to provide a kind of preparation method of the halogen-free flame retardant PC material with electromagnetic shielding characteristic,
Have the characteristics that easy processing operates, is efficient.
The purpose of the invention is achieved by the following technical solution：
A kind of halogen-free flame retardant PC material with electromagnetic shielding characteristic, includes the raw material components of following mass percent：
PC resin 45-60%
Makrolon-poly organo alkyl copolymer 5-15%
Stainless fiber beam 5-10%
Carbon fiber 5-10%
Carbon nanotube 5-10%
Ethylene butyl acrylate copolymer 3-6%
Silica acrylic acid copolymer 2-6%
Poly aryl phosphate ester 8-12%
Fire retardant 0.08-0.1%
Fire retarding synergist 0.5-1%
Polytetrafluoroethylene (PTFE) 0.1-0.4%
Antioxidant 612S 0.2-0.4%
Antioxidant 1076 0.1-0.2%
Pentaerythritol stearate 0.2-0.4%,
The total amount of above-mentioned raw materials is 100%, wherein the PC resin is bisphenol A polycarbonate, in 300 DEG C/1.2kg items
Under part, melt index 10-30g/10min.
Wherein, in the makrolon-poly organo alkyl copolymer Organosiloxane block copolymer content in 10-
20wt% can effectively improve the percussion of material.The makrolon-poly organo alkyl copolymer hereinafter referred to as PC-
PDMS。
Wherein, the fire retardant is the combination of one or both of perfluoro butyl sulfosalt, diphenyl sulfone sulfonate.
Wherein, the fire retarding synergist is the organosilicon auxiliary agent containing phenyl functional group, and the presence of phenyl can greatly reinforce
The compatibility of fire retardant and PC molecules, improves the compatibility of fire retardant and makrolon material, and organosilicon primarily serves fire-retardant fire
The effect of flame diffusion.Preferably, fire retarding synergist is the one or more of FCA-107, FCA-117 of DOW CORNING.
Wherein, the silica acrylic acid copolymer is the graft copolymer of organosilicon and acrylic resin.Acrylic resin is made
Enhance its compatibility with makrolon for the shell of core-shell copolymerized object, the flexibility that silicon strand has can be mentioned needed for material
Toughness.
A kind of preparation method of the halogen-free flame retardant PC material with electromagnetic shielding characteristic, includes the following steps：
a）The pre-treatment of stainless fiber beam：Fiber-treating liquid is put into fiber treatment slot, then by stainless steel fibre
Dimension beam is placed in solution tank, is taken out after immersion treatment 25-35min, is then cleaned 3 times with deionized water, then by stainless steel fibre
Beam is tieed up in 90-110 DEG C of drying, then it is 0.5-1.5wt%'s that stainless fiber beam, which is put into 3- aminopropyl triethoxysilane contents,
1-2h is impregnated in ethanol solution, a solution is stirred every 25-35min, finally by stainless fiber beam taking-up and in 90-110
DEG C drying；
The present invention handles stainless fiber beam using fiber-treating liquid, eliminates the impurity on its surface, and directly use silicon
The coating infiltration of alkane coupling agent carries out surface modification, greatly improves the compatibility with plastics.
b）Extruding pelletization：By above-mentioned formula ratio by PC resin, makrolon-poly organo alkyl copolymer, ethylene propylene
Olefin(e) acid acrylate copolymer, poly aryl phosphate ester, fire retardant, fire retarding synergist, polytetrafluoroethylene (PTFE), resists silica acrylic acid copolymer
Oxygen agent 612S, antioxidant 1076, pentaerythritol stearate are added by main feeding after mixing；Carbon nanotube, carbon fiber by
Side feeding is added；Using infiltrated with molten metal method, distraction step a）Treated, and stainless fiber beam passes through enhancing thermoplastic composite material
Material infiltration mold is added, and the halogen-free flame retardant PC material with electromagnetic shielding characteristic is prepared in pelletizing later.
The present invention using existing roving glass fiber filling enhancing thermoplastic composite mold, directly utilization by plastics with it is stainless
Steel fiber bundle is blended together, and utmostly remains the draw ratio and conductive characteristic of stainless steel fibre, while reducing processing journey
Sequence.Carbon fiber, carbon nanotube are introduced, can suitably reduce the dosage of stainless fiber beam, the cost for reducing material while drops
Its low proportion, enhances the strength of materials；The present invention is compounded using halogen-free flame retardants aryl phosphate ester and Sulfonates, and is added
Fire retarding synergist, which is promoted, improves material flame-retarding characteristic；Also improve material using makrolon-poly organo alkyl copolymer
Toughness and surface effect.
Wherein, the step a）In stainless fiber beam filament diameter be 12-15 μm, preferably 13 μm.
Wherein, the step a）In fiber-treating liquid mixed by following components：2000 parts of deionized water, permanganic acid
60-120 parts of potassium, the 400-800 parts of concentrated sulfuric acids.
Wherein, the additive amount of the stainless fiber beam by the pressure roller rotating speed of the engine speed of extruder and dragger come
It adjusts, the engine speed is 300-480r/min, and dragger pressure roller rotating speed is 60-100r/min.To stainless fiber beam
Filling content can realize online adjusting control, improve the overall mechanical properties of material.
Wherein, the step b）In, the specific process parameter of double screw extruder is：One area's temperature be 220-240 DEG C, two
Area's temperature is 235-250 DEG C, and three area's temperature are 245-255 DEG C, and four area's temperature are 250-260 DEG C, and five area's temperature are 260-265
DEG C, six area's temperature are 260-265 DEG C, and seven area's temperature are 260-265 DEG C, and eight area's temperature are 255-260 DEG C, and nine area's temperature are 255-
260 DEG C, ten area's temperature are 255-260 DEG C, screw speed 300-480r/min.
The beneficial effects of the present invention are：
1, present invention introduces carbon fiber, carbon nanotubes, can reduce the dosage of stainless fiber beam, reduce the raw material of material
The proportion that stainless steel fibre is reduced while cost enhances the intensity of halogen-free flame retardant PC material of the present invention；
2, the present invention is compounded by aryl phosphate ester and halogen-free flame retardants, and it is fire-retardant to improve material to add fire retarding synergist
Characteristic
3, the present invention improves the tough of halogen-free flame retardant PC material of the present invention using makrolon-poly organo alkyl copolymer
Property and surface effect；
4, the present invention is by the reasonable compounding to various raw materials, and the conductive features of obtained material are excellent, sheet resistance
Rate ＜ 103, shield effectiveness is strong, reaches as high as 69dB, and flame-retarding characteristic reaches V0, intensity and good-toughness.
Another advantageous effect of the present invention：
1, the present invention handles stainless fiber beam using fiber-treating liquid, eliminates the impurity on its surface, and directly use
Silane coupling agent coating infiltration carries out surface modification, greatly improves the compatibility with plastics；
2, by the improvement to processing step, online adjusting control can be realized to the filling content of stainless fiber beam, changed
It has been apt to the overall mechanical properties of material.
3, of the invention using existing roving glass fiber filling enhancing thermoplastic composite mold, directly using by plastics and not
Rust steel fiber bundle is blended together, and utmostly remains the draw ratio and conductive characteristic of stainless steel fibre, while being reduced and being added
Engineering sequence.
4, preparation method of the invention is simply ripe, and production efficiency is high, is conducive to popularity application.
Specific implementation mode
For the ease of the understanding of those skilled in the art, with reference to embodiment, the present invention is further illustrated, real
The content that the mode of applying refers to not is limitation of the invention.
Embodiment 1
A kind of halogen-free flame retardant PC material with electromagnetic shielding characteristic, includes the raw material components of following mass percent：
PC resin 45.42%
PC-PDMS 15.00%
Stainless fiber beam 5.00%
Carbon fiber 10.00%
Carbon nanotube 10.00%
Ethylene butyl acrylate copolymer 3.00%
Silica acrylic acid copolymer 2.00%
Poly aryl phosphate ester 8.00%
Perfluoro butyl sulfosalt 0.08%
Organic silicon flame-retardant synergist 0.70%
Polytetrafluoroethylene (PTFE) 0.30%
Antioxidant 612S 0.20%
Antioxidant 1076 0.10%
Pentaerythritol stearate 0.20%.
A kind of preparation method of halogen-free flame retardant PC material with electromagnetic shielding characteristic of the present embodiment, it includes following system
Standby step：
a）The pre-treatment of stainless fiber beam：Fiber-treating liquid is put into fiber treatment slot, it then will be continuous stainless
Steel fiber bundle is placed in solution tank, immersion treatment 30min, is put into sink and is cleaned 3 times with deionized water later, has cleaned taking-up
It is placed in 90 DEG C of baking ovens and dries.Stainless fiber beam is put into the silane coupling agent of 0.5wt% later（Three ethoxy of 3- aminopropyls
Base silane）In ethanol solution, 1h is impregnated, a solution is stirred every 30min, fibre bundle taking-up is placed in 90 DEG C of bakings after processing
It is dried in case.
The step a）In fiber-treating liquid mixed by following components：Deionized water 2000ml, potassium permanganate
60g, the concentrated sulfuric acid 400ml that mass concentration is 98%.
b）Extruding pelletization：By above-mentioned formula ratio by PC resin, makrolon-poly organo alkyl copolymer（PC-PDMS）,
Ethylene butyl acrylate copolymer, silica acrylic acid copolymer, poly aryl phosphate ester, perfluoro butyl sulfosalt, organic silicon flame-retardant
Synergist, polytetrafluoroethylene (PTFE), antioxidant 612S, antioxidant 1076, pentaerythritol stearate are uniformly mixed through high-speed mixer
It is added afterwards by main feeding；Carbon nanotube, carbon fiber are added by side feeding；Using infiltrated with molten metal method, traction stainless fiber beam is logical
Enhancing thermoplastic composite infiltration mold is crossed, under the premise of standing screw rotating speed, adjusting pressure roller rotating speed makes stainless fiber beam
Content control 5%, after prepared special with electromagnetic shielding through double screw extruder extruding pelletization, the pelleter pelletizing of use
The halogen-free flame retardant PC material of property.
The specific process parameter of double screw extruder is：One area's temperature is 230 DEG C, and two area's temperature are 240 DEG C, three area's temperature
It it is 250 DEG C, four area's temperature are 260 DEG C, and five area's temperature are 265 DEG C, and six area's temperature are 265 DEG C, and seven area's temperature are 265 DEG C, 8th area
Temperature is 260 DEG C, and nine area's temperature are 260 DEG C, and ten area's temperature are 260 DEG C, screw speed 450r/min, and the pressure roller of dragger turns
Speed is 72r/min.
Embodiment 2
A kind of halogen-free flame retardant PC material with electromagnetic shielding characteristic, includes the raw material components of following mass percent：
PC resin 49.42%
PC-PDMS 8.00%
Stainless fiber beam 6.50%
Carbon fiber 8.50%
Carbon nanotube 8.50%
Ethylene butyl acrylate copolymer 4.50%
Silica acrylic acid copolymer 3.00%
Poly aryl phosphate ester 9.50%
Perfluoro butyl sulfosalt 0.08%
Organic silicon flame-retardant synergist 1.00%
Polytetrafluoroethylene (PTFE) 0.20%
Antioxidant 612S 0.20%
Antioxidant 1076 0.20%
Pentaerythritol stearate 0.40%.
A kind of preparation method of halogen-free flame retardant PC material with electromagnetic shielding characteristic of the present embodiment, it includes following system
Standby step：
a）The pre-treatment of stainless fiber beam：Fiber-treating liquid is put into fiber treatment slot, it then will be continuous stainless
Steel fiber bundle is placed in solution tank, immersion treatment 25min, is put into sink and is cleaned 3 times with deionized water later, has cleaned taking-up
It is placed in 100 DEG C of baking ovens and dries.Stainless fiber beam is put into the silane coupling agent of 1wt% later（3- aminopropyl-triethoxies
Silane）In ethanol solution, 2h is impregnated, a solution is stirred every 25min, is placed in stainless fiber beam taking-up after processing
It is dried in 100 DEG C of baking ovens.
The step a）In fiber-treating liquid mixed by following components：Deionized water 2000ml, potassium permanganate
120g, the 800ml concentrated sulfuric acid.
b）Extruding pelletization：By formula ratio by PC resin, makrolon-poly organo alkyl copolymer（PC-PDMS）, ethylene
Butyl acrylate copolymer, silica acrylic acid copolymer, poly aryl phosphate ester, 0.08% perfluoro butyl sulfosalt, organosilicon resistance
Synergist is fired, polytetrafluoroethylene (PTFE), antioxidant 612S, 0.1% antioxidant 1076, pentaerythritol stearate are through high-speed mixer
It is added after mixing by main feeding；Carbon nanotube, carbon fiber are added by side feeding；Using infiltrated with molten metal method, stainless steel is drawn
Fibre bundle infiltrates mold by enhancing thermoplastic composite, and governing speed makes the content of stainless fiber beam control 6.5%,
After through double screw extruder extruding pelletization, the pelleter pelletizing of use prepare the halogen-free flameproof with electromagnetic shielding characteristic
PC materials.
The specific process parameter of double screw extruder is：One area's temperature is 220 DEG C, and two area's temperature are 235 DEG C, three area's temperature
It it is 245 DEG C, four area's temperature are 255 DEG C, and five area's temperature are 260 DEG C, and six area's temperature are 260 DEG C, and seven area's temperature are 260 DEG C, 8th area
Temperature is 255 DEG C, and nine area's temperature are 255 DEG C, and ten area's temperature are 255 DEG C, screw speed 420r/min, and the pressure roller of dragger turns
Speed is 80r/min.
Embodiment 3
A kind of halogen-free flame retardant PC material with electromagnetic shielding characteristic, includes the raw material components of following mass percent：
PC resin 52.20%
PC-PDMS 10.00%
Stainless fiber beam 7.00%
Carbon fiber 7.00%
Carbon nanotube 5.00%
Ethylene butyl acrylate copolymer 4.00%
Silica acrylic acid copolymer 3.00%
Poly aryl phosphate ester 10.00%
Perfluoro butyl sulfosalt 0.10%
Organic silicon flame-retardant synergist 0.60%
Polytetrafluoroethylene (PTFE) 0.30%
Antioxidant 612S 0.40%
Antioxidant 1076 0.10%
Pentaerythritol stearate 0.30%
A kind of preparation method of halogen-free flame retardant PC material with electromagnetic shielding characteristic of the present embodiment, it includes following system
Standby step：
a）The pre-treatment of stainless fiber beam：Fiber-treating liquid is put into fiber treatment slot, it then will be continuous stainless
Steel fiber bundle is placed in solution tank, immersion treatment 30min, is put into sink and is cleaned 3 times with deionized water later, has cleaned taking-up
It is placed in 105 DEG C of baking ovens and dries.Stainless fiber beam is put into the silane coupling agent of 1.5wt% later（Three ethoxy of 3- aminopropyls
Base silane）In ethanol solution, 1.5h is impregnated, a solution is stirred every 25min, stainless fiber beam is taken out into juxtaposition after processing
It is dried in 100 DEG C of baking ovens.
The step a）In fiber-treating liquid mixed by following components：Deionized water 2000ml, potassium permanganate
100g, the 600ml concentrated sulfuric acid.
b）Extruding pelletization：By formula ratio by PC resin, makrolon-poly organo alkyl copolymer（PC-PDMS）, ethylene
Butyl acrylate copolymer, silica acrylic acid copolymer, poly aryl phosphate ester, perfluoro butyl sulfosalt, organic silicon flame-retardant synergistic
Agent, polytetrafluoroethylene (PTFE), antioxidant 612S, antioxidant 1076, pentaerythritol stearate through high-speed mixer after mixing by
Main feeding is added；Carbon nanotube, carbon fiber are added by side feeding；Using infiltrated with molten metal method, traction stainless fiber beam passes through increasing
Heat-flash plastic composites infiltrate mold, and governing speed makes the content of stainless fiber beam control 7%, after squeezed through twin-screw
Go out machine extruding pelletization, the halogen-free flame retardant PC material with electromagnetic shielding characteristic is prepared in the pelleter pelletizing of use.
The specific process parameter of double screw extruder is：One area's temperature is 240 DEG C, and two area's temperature are 250 DEG C, three area's temperature
It it is 255 DEG C, four area's temperature are 250 DEG C, and five area's temperature are 265 DEG C, and six area's temperature are 265 DEG C, and seven area's temperature are 265 DEG C, 8th area
Temperature is 260 DEG C, and nine area's temperature are 260 DEG C, and ten area's temperature are 255 DEG C, screw speed 400r/min, and the pressure roller of dragger turns
Speed is 86r/min.
Embodiment 4
A kind of halogen-free flame retardant PC material with electromagnetic shielding characteristic, includes the raw material components of following mass percent：
PC resin 54.50%
PC-PDMS 7.50%
Stainless fiber beam 8.50%
Carbon fiber 8.50%
Carbon nanotube 5.00%
Ethylene butyl acrylate copolymer 2.50%
Silica acrylic acid copolymer 4.00%
Poly aryl phosphate ester 8.00%
Perfluoro butyl sulfosalt 0.10%
Organic silicon flame-retardant synergist 0.60%
Polytetrafluoroethylene (PTFE) 0.20%
Antioxidant 612S 0.20%
Antioxidant 1076 0.20%
Pentaerythritol stearate 0.20%.
A kind of preparation method of halogen-free flame retardant PC material with electromagnetic shielding characteristic of the present embodiment, it includes following system
Standby step：
a）The pre-treatment of stainless fiber beam：Fiber-treating liquid is put into fiber treatment slot, it then will be continuous stainless
Steel fiber bundle is placed in solution tank, immersion treatment 25min, is put into sink and is cleaned 3 times with deionized water later, has cleaned taking-up
It is placed in 95 DEG C of baking ovens and dries.Stainless fiber beam is put into the silane coupling agent of 1.5wt% later（Three ethoxy of 3- aminopropyls
Base silane）In ethanol solution, 1h is impregnated, a solution is stirred every 25min, fibre bundle taking-up is placed in 110 DEG C after processing
It is dried in baking oven.
The step a）In fiber-treating liquid mixed by following components：Deionized water 2000ml, potassium permanganate
80g, the 700ml concentrated sulfuric acid.
b）Extruding pelletization：By formula ratio by PC resin, makrolon-poly organo alkyl copolymer（PC-PDMS）, ethylene
Butyl acrylate copolymer, silica acrylic acid copolymer, poly aryl phosphate ester, perfluoro butyl sulfosalt, organic silicon flame-retardant synergistic
Agent, polytetrafluoroethylene (PTFE), antioxidant 612S, antioxidant 1076, pentaerythritol stearate through high-speed mixer after mixing by
Main feeding is added；Carbon nanotube, carbon fiber are added by side feeding；Using infiltrated with molten metal method, traction stainless fiber beam passes through increasing
Heat-flash plastic composites infiltrate mold, and governing speed makes the content of stainless fiber beam control 8.5%, after through twin-screw
The halogen-free flame retardant PC material with electromagnetic shielding characteristic is prepared in extruder extruding pelletization, the pelleter pelletizing of use.
The specific process parameter of double screw extruder is：One area's temperature is 220 DEG C, and two area's temperature are 235 DEG C, three area's temperature
It it is 245 DEG C, four area's temperature are 255 DEG C, and five area's temperature are 260 DEG C, and six area's temperature are 260 DEG C, and seven area's temperature are 260 DEG C, 8th area
Temperature is 255 DEG C, and nine area's temperature are 255 DEG C, and ten area's temperature are 255 DEG C, screw speed 360r/min, and the pressure roller of dragger turns
Speed is 86r/min.
Embodiment 5
A kind of halogen-free flame retardant PC material with electromagnetic shielding characteristic, includes the raw material components of following mass percent：
PC resin 57.50%
PC-PDMS 5.00%
Stainless fiber beam 9.00%
Carbon fiber 5.00%
Carbon nanotube 5.00%
Ethylene butyl acrylate copolymer 2.00%
Silica acrylic acid copolymer 3.00%
Poly aryl phosphate ester 12.00%
Perfluoro butyl sulfosalt 0.10%
Organic silicon flame-retardant synergist 0.70%
Polytetrafluoroethylene (PTFE) 0.20%
Antioxidant 612S 0.20%
Antioxidant 1076 0.10%
Pentaerythritol stearate 0.20%.
A kind of preparation method of halogen-free flame retardant PC material with electromagnetic shielding characteristic of the present embodiment, it includes following system
Standby step：
a）The pre-treatment of stainless fiber beam：Fiber-treating liquid is put into fiber treatment slot, it then will be continuous stainless
Steel fiber bundle is placed in solution tank, immersion treatment 25min, is put into sink and is cleaned 3 times with deionized water later, has cleaned taking-up
It is placed in 100 DEG C of baking ovens and dries.Stainless fiber beam is put into the silane coupling agent of 1wt% later（3- aminopropyl-triethoxies
Silane）In ethanol solution, 2h is impregnated, a solution is stirred every 25min, fibre bundle taking-up is placed in 100 DEG C of bakings after processing
It is dried in case.
The step a）In fiber-treating liquid mixed by following components：Deionized water 2000ml, potassium permanganate
110g, the 500ml concentrated sulfuric acid.
b）Extruding pelletization：By formula ratio by PC resin, makrolon-poly organo alkyl copolymer（PC-PDMS）, ethylene
Butyl acrylate copolymer, silica acrylic acid copolymer, poly aryl phosphate ester, 0.08% perfluoro butyl sulfosalt, organosilicon resistance
Synergist is fired, polytetrafluoroethylene (PTFE), antioxidant 612S, 0.1% antioxidant 1076, pentaerythritol stearate are through high-speed mixer
It is added after mixing by main feeding；Carbon nanotube, carbon fiber are added by side feeding；Using infiltrated with molten metal method, stainless steel is drawn
Fibre bundle infiltrates mold by enhancing thermoplastic composite, and governing speed makes the content of stainless fiber beam control 9%, it
By double screw extruder extruding pelletization, the halogen-free flame retardant PC with electromagnetic shielding characteristic is prepared in the pelleter pelletizing of use
Material.
The specific process parameter of double screw extruder is：One area's temperature is 220 DEG C, and two area's temperature are 235 DEG C, three area's temperature
It it is 245 DEG C, four area's temperature are 255 DEG C, and five area's temperature are 260 DEG C, and six area's temperature are 260 DEG C, and seven area's temperature are 260 DEG C, 8th area
Temperature is 255 DEG C, and nine area's temperature are 255 DEG C, and ten area's temperature are 255 DEG C, screw speed 340r/min, and the pressure roller of dragger turns
Speed is 95r/min.
The performance detection data of the electromagnetic shielding PC materials of halogen-free flameproof made from 1 ~ embodiment of the embodiment of the present invention 5 is shown in
Table 1.
The performance detection data of the electromagnetic shielding PC materials of halogen-free flameproof made from 1 ~ embodiment of the embodiment of the present invention 5 is shown in
Table 1.
It can be seen from the above results that the mechanical property of the electromagnetic shielding PC materials of the present invention is good, conductive characteristic, screen
It is excellent to cover efficiency, flame-retarding characteristic and strength and toughness.
It can be seen from the above results that the mechanical property of the electromagnetic shielding PC materials of the present invention is good, conductive characteristic, screen
It is excellent to cover efficiency, flame-retarding characteristic and strength and toughness.
Above-described embodiment is the preferable implementation of the present invention, and in addition to this, the present invention can be realized with other manner,
Any obvious replacement is not departed under the premise of present inventive concept within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of the halogen-free flame retardant PC material with electromagnetic shielding characteristic, it is characterised in that：It is described that there is electromagnetism
The halogen-free flame retardant PC material of shielding character, includes the raw material components of following mass percent：
The total amount of above-mentioned raw materials is 100%, wherein the PC resin is under 300 DEG C/1.2kg test conditions, and melt index is
The bisphenol A polycarbonate of 10-30g/10min；
The preparation method of the halogen-free flame retardant PC material with electromagnetic shielding characteristic, includes the following steps：
A) pre-treatment of stainless fiber beam：Fiber-treating liquid is put into fiber treatment slot, then by stainless fiber beam
It is placed in solution tank, takes out after immersion treatment 25-35min, then cleaned 2-3 times with deionized water, then by stainless steel fibre
Beam is in 90-110 DEG C of drying；It is 0.5-1.5wt%'s that stainless fiber beam, which is put into 3- aminopropyl triethoxysilane contents, again
1-2h is impregnated in ethanol solution, a solution is stirred every 25-35min, finally by stainless fiber beam taking-up and in 90-110
DEG C drying；
B) extruding pelletization：It is by formula ratio that PC resin, makrolon-poly organo alkyl copolymer, ethylene butyl acrylate is total
Polymers, poly aryl phosphate ester, fire retardant, fire retarding synergist, polytetrafluoroethylene (PTFE), antioxidant 612S, resists silica acrylic acid copolymer
Oxygen agent 1076 and pentaerythritol stearate are added by main feeding after mixing；Carbon nanotube and carbon fiber are added by side feeding
Enter；Using infiltrated with molten metal method, distraction step a) treated stainless fiber beams are prepared by infiltrating mold, later pelletizing
Halogen-free flame retardant PC material with electromagnetic shielding characteristic.
2. a kind of preparation method of halogen-free flame retardant PC material with electromagnetic shielding characteristic according to claim 1, special
Sign is：The filament diameter of stainless fiber beam in the step a) is 10-15 μm.
3. a kind of preparation method of halogen-free flame retardant PC material with electromagnetic shielding characteristic according to claim 1, special
Sign is：Fiber-treating liquid in the step a) is mixed by following components：60-120 parts of potassium permanganate, concentrated sulfuric acid 400-
800 parts and 2000 parts of deionized water.
4. a kind of preparation method of halogen-free flame retardant PC material with electromagnetic shielding characteristic according to claim 1, special
Sign is：The additive amount of the stainless fiber beam is adjusted by the pressure roller rotating speed of the engine speed of extruder and dragger,
Engine speed is 300-480r/min, and dragger pressure roller rotating speed is 60-100r/min.
5. a kind of preparation method of halogen-free flame retardant PC material with electromagnetic shielding characteristic according to claim 1, special
Sign is：In the step b), the specific process parameter of double screw extruder is：One area's temperature is 220-240 DEG C, two area's temperature
It it is 235-250 DEG C, three area's temperature are 245-255 DEG C, and four area's temperature are 250-260 DEG C, and five area's temperature are 260-265 DEG C, 6th area
Temperature is 260-265 DEG C, and seven area's temperature are 260-265 DEG C, and eight area's temperature are 255-260 DEG C, and nine area's temperature are 255-260 DEG C,
Ten area's temperature are 255-260 DEG C, screw speed 300-480r/min.
6. a kind of halogen-free flame retardant PC material with electromagnetic shielding characteristic, it is characterised in that：By claim 1-5 any one institute
The preparation method for stating the halogen-free flame retardant PC material with electromagnetic shielding characteristic is made.
7. a kind of halogen-free flame retardant PC material with electromagnetic shielding characteristic according to claim 6, it is characterised in that：It is described
The content of polysiloxane block is in 10-20wt% in makrolon-poly organo alkyl copolymer.
8. a kind of halogen-free flame retardant PC material with electromagnetic shielding characteristic according to claim 6, it is characterised in that：It is described
Fire retardant is the combination of one or both of perfluoro butyl sulfosalt, diphenyl sulfone sulfonate.
9. a kind of halogen-free flame retardant PC material with electromagnetic shielding characteristic according to claim 6, it is characterised in that：It is described
Fire retarding synergist is the organosilicon auxiliary agent containing phenyl functional group.
10. a kind of halogen-free flame retardant PC material with electromagnetic shielding characteristic according to claim 6, it is characterised in that：Institute
State the graft copolymer that silica acrylic acid copolymer is organosilicon and acrylic resin.
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| CN108276755A (en) * | 2018-03-02 | 2018-07-13 | 合肥思博特软件开发有限公司 | A kind of composite material and preparation method for electromagnetic shielding |
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