CN104371229B - High wellability high intensity continuous carbon fibre strengthens polyvinylidene fluoride composite material and preparation method - Google Patents
High wellability high intensity continuous carbon fibre strengthens polyvinylidene fluoride composite material and preparation method Download PDFInfo
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- CN104371229B CN104371229B CN201410620345.7A CN201410620345A CN104371229B CN 104371229 B CN104371229 B CN 104371229B CN 201410620345 A CN201410620345 A CN 201410620345A CN 104371229 B CN104371229 B CN 104371229B
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
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- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The present invention relates to high wellability high intensity continuous carbon fibre and strengthen polyvinylidene fluoride composite material and preparation method thereof, joining in high mixer by 60 90 parts of PVDF resins, 0.1 0.7 parts of antioxidant, 0.1 0.6 parts of lubricants, the material mixed joins in double screw extruder；Use the impregnating equipment of the continuous lod PVDF resin being connected to extruder head, the melt that extruder is extruded is squeezed in maceration tank at the melt inlet of impregnating equipment；Continuous carbon fibre first enters into the surface treatment chamber in impregnating equipment at the fiber entry of impregnating equipment, carries out surface process, subsequently in the maceration tank of impregnating equipment, fully infiltrates with gained PVDF melt；Involved from the sizing mouth die of impregnating equipment by traction machine, and obtain composite products by pelleter pelletizing.Compared with prior art, it is low that continuous carbon fibre of the present invention strengthens PVDF composite density, and intensity is high, and excellent in mechanical performance has energy-conserving and environment-protective, low cost and other advantages.
Description
Technical field
The invention belongs to macromolecular material recovery technology field, be specifically related to a kind of high wellability high intensity continuous carbon
Fiber reinforcement polyvinylidene fluoride composite material and preparation method thereof.
Background technology
Kynoar (PVDF) have in fluoroplastics obdurability, low-friction coefficient, corrosion resistance strong,
Resistance to ag(e)ing, weatherability, the features such as radiation-resistant property is good, therefore it is widely used in coating, petrochemical industry sets
The standby field such as pipeline, functional membrane.But PVDF self-strength is low, limits it and at some, product strength is wanted
Ask the application in higher field.
Continuous lod polyvinylidene fluoride composite material is with continuous fiber, such as glass fibre, carbon fiber, virtue
Synthetic fibre fibers etc. are inorganic or organic fiber is as reinforcing material, with polyvinylidene fluoride resin as matrix, pass through special process
The advanced composite material (ACM) manufactured；Compared with the polyvinylidene fluoride composite material of chopped fiber or long fiber reinforcement, fine continuously
Dimension strengthen polyvinylidene fluoride composite material mechanical property had qualitative leap, have lightweight, specific strength is high, ratio
The excellent properties such as modulus height, good corrosion resistance, are particularly suitable for automobile, aircraft, protection and other are to mechanical property
Energy requirement is higher, need to alleviate the purposes of weight, is one of material with fastest developing speed in current composite markets.
Carbon fiber is that a kind of to have very high intensity and the high-temperature fibre of modulus, density low, the characteristic of these excellences
Impart carbon fibre composite and there is the highest mechanical property, be that other glass fibre etc. strengthen composite institute nothing
Method analogy, therefore it is widely used in Aero-Space, auto industry, track traffic, new forms of energy, physical culture use
The new high-tech industry fields such as product.And the composite property using continuous carbon fibre to strengthen increases with other continuous fibers
Strong composite is compared, and has higher mechanical property, the most lightweight, has the widest application.
But key problem in technology prepared by continuous carbon fibre enhancing PVDF composite is dispersion and the dipping of fiber.
The quality of fiber dispersion effect, resin can complete wetting in the middle of fiber and fiber is straight with the compatibility of resin
Connect the quality that decide final products performance.And the retrieval of existing patented technology is found do not have continuous carbon fibre to increase
The relevant report of strong PVDF composite.
Summary of the invention
Defect that the purpose of the present invention is contemplated to overcome above-mentioned prior art to exist and a kind of energy-conserving and environment-protective are provided
High wellability high intensity continuous carbon fibre strengthens polyvinylidene fluoride composite material and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions: a kind of high wellability high intensity continuous carbon fibre
Strengthen polyvinylidene fluoride composite material, it is characterised in that comprise the component of following weight portion:
Fiber strength agent, its content is to be 1-3% relative to the weight/mass percentage composition of continuous carbon fibre.
Described continuous carbon fibre is polyacrylonitrile-based carbon fibre or asphalt base carbon fiber.
Described Fiber strength agent is the one in silane coupler, titanate coupling agent, aluminate coupling agent
Or more than one.
Described antioxidant is four (β-(3,5-di-tert-butyl-hydroxy phenyl) propionate) (antioxygen
Agent 1010), 3,5-di-t-butyl-4-hydroxy benzenes propionyl-hexamethylene diamine (antioxidant 1098), tricresyl phosphate-(2,4-bis-uncle
Butyl benzene phenolic ester) one or more in (irgasfos 168).
Described lubricant is stearic acid, calcium stearate, zinc stearate, ethylene bis stearamide (EBS), mustard
Acid amide in one or more.
A kind of high wellability high intensity continuous carbon fibre strengthens the preparation method of polyvinylidene fluoride composite material, its feature
Being, the method comprises the following steps:
(1) 60-90 part PVDF resin, 0.1-0.7 part antioxidant, 0.1-0.6 part lubricant are joined high mixed
In machine, stop after mixed at high speed 3-5min under room temperature, then the material mixed is joined double screw extruder
In；
(2) impregnating equipment of the continuous lod PVDF resin being connected to extruder head is used, by extruder
The melt of extrusion is squeezed in maceration tank at the melt inlet of impregnating equipment；
(3) continuous carbon fibre first enters into the surface treatment chamber in impregnating equipment at the fiber entry of impregnating equipment,
Fiber strength agent in surface treatment chamber carries out surface process, the carbon that then surface is handled well to continuous carbon fibre
Fiber proceeds immediately in the maceration tank of impregnating equipment, in maceration tank carbon fiber carry out disperseing and with step (2)
Gained PVDF melt fully infiltrates；
(4) carbon fiber after step (3) gained is fully impregnated with PVDF resin is set from dipping by traction machine
Standby sizing mouth die involves, and obtains composite products by pelleter pelletizing.
The screw diameter of described double screw extruder is 50mm, and draw ratio is 44:1, and extruder temperature is
160-210 DEG C, the maceration tank temperature of impregnating equipment is set in 220 DEG C；
In described composite products, carbon fiber content is existed by the sizing mouth die size of regulation impregnating equipment
2-5mm and the rotating speed of extruder and rate of feeding control between 10-40%；Turned by regulation pelleter cutting knife
Speed, makes the particle length of the continuous carbon fibre reinforced polypropylene compound material product finally prepared control
8-12mm, size controlling is at 1-5mm.
Compared with prior art, present invention achieves the surface process of fiber, fiber dispersion and be combined with resin infiltration
An impregnating equipment is continuously finished, simplifies production technology；Carbon fiber and PVDF in the composite obtained
Not only there is good wellability, and carbon fiber is processed by surface conditioning agent with PVDF before infiltration, make
Both have had good interfacial bonding property；The continuous carbon fibre prepared strengthens PVDF Compound Material Engineering
Can be excellent, density is low simultaneously, and composite can be widely used in Aero-Space, automobile, machinery, electronics electricity
Device, the product component such as household electrical appliances.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated.
In following example, bending property testing standard is ASTM D790, unnotched impact strength testing standard
For ASTM D256.
Embodiment 1
Weigh 60 parts of PVDF resins, 0.3 part of antioxidant 1010,0.1 part of irgasfos 168,0.1 part of lubricant
EBS is room temperature mixing 5min in high mixer, is then added to double screw extruder extrusion, and gained melt is from dipping
The melt inlet port of equipment is squeezed in the maceration tank of impregnating equipment；
Continuous carbon fibre (toray company, trade mark T300) is introduced at the fiber entry of impregnating equipment,
Enter the surface treatment chamber of impregnating equipment, control surface conditioning agent silane coupler KH560 relative to carbon fiber
Weight content is 1%, and the carbon fiber after then surface treated agent being processed is incorporated in the maceration tank of impregnating equipment,
Realize the dispersion of carbon fiber and be combined with PVDF resin；By selecting the size (2mm) of sizing mouth die,
Adjusting the engine speed 13-14HZ of extruder, rate of feeding, at 9-10HZ, controls continuous carbon fibre content simultaneously
About 40%；The rotating speed of regulation pelleter, makes the continuous carbon fibre prepared strengthen PVDF composite
Length at about 10mm, particle diameter is at about 3mm；
Double screw extruder is directly 50mm, screw slenderness ratio 44:1, and dual-screw-stem machine each district temperature is: 1st district
160 DEG C, 2 170 DEG C of districts, 3 170 DEG C of districts, 4 180 DEG C of districts, 5 180 DEG C of districts, 6 190 DEG C of districts, 7 190 DEG C of districts,
8 200 DEG C of districts, 9 210 DEG C of districts, maceration tank 220 DEG C.
Embodiment 2
Weigh 80 parts of PVDF resins, 1098,0.2 part of irgasfos 168 of 0.5 part of antioxidant, 0.3 part of lubricant
Calcium stearate is room temperature mixing 3min in high mixer, is then added to double screw extruder extrusion, by melt from leaching
The melt inlet port of stain equipment is squeezed in the maceration tank of impregnating equipment；
Continuous carbon fibre (toray company, trade mark T300J) is introduced at the fiber entry of impregnating equipment,
Enter the surface treatment chamber of impregnating equipment, control the different stearoyl metatitanic acid of surface conditioning agent titanate coupling agent isopropyl three
Ester is 2% relative to the weight content of carbon fiber, and the carbon fiber after then surface treated agent being processed is incorporated into leaching
In the maceration tank of stain equipment, it is achieved the dispersion of carbon fiber is also combined with PVDF fat；By selecting sizing mouth
The size (4mm) of mould, adjusts the engine speed 13-14HZ of extruder simultaneously, and rate of feeding is in 9-10HZ, control
Continuous carbon fibre content processed is about 20%；The rotating speed of regulation pelleter, makes the continuous carbon fibre prepared increase
The length of strong PVDF composite is at about 10mm, and particle diameter is at about 3mm；
Double screw extruder is directly 50mm, screw slenderness ratio 44:1, and dual-screw-stem machine each district temperature is: 1st district
160 DEG C, 2 170 DEG C of districts, 3 170 DEG C of districts, 4 180 DEG C of districts, 5 180 DEG C of districts, 6 190 DEG C of districts, 7 190 DEG C of districts,
8 200 DEG C of districts, 9 210 DEG C of districts, maceration tank 220 DEG C.
Embodiment 3
Weigh 90 parts of PVDF resins, 1098,0.1 part of irgasfos 168 of 0.3 part of antioxidant, 0.6 part of lubricant
Stearic acid is room temperature mixing 5min in high mixer, is then added to double screw extruder extrusion, by melt from dipping
The melt inlet port of equipment is squeezed in the maceration tank of impregnating equipment；
Continuous carbon fibre (toray company, trade mark T700S) is introduced at the fiber entry of impregnating equipment,
Enter the surface treatment chamber of impregnating equipment, control surface conditioning agent aluminate coupling agent distearyl acyl-oxygen isopropyl aluminic acid
Ester is 3% relative to the weight content of carbon fiber, and the carbon fiber after then surface treated agent being processed is incorporated into leaching
In the maceration tank of stain equipment, it is achieved the dispersion of carbon fiber is also combined with PVDF resin；Shaped by selection
The size (5mm) of mouth die, adjusts the engine speed 15-16HZ of extruder simultaneously, rate of feeding at 11-12HZ,
Control continuous carbon fibre content about 5%；The rotating speed of regulation pelleter, makes the continuous carbon fibre prepared increase
The length of strong PVDF composite is at about 10mm, and particle diameter is at about 3mm；
Double screw extruder is directly 50mm, screw slenderness ratio 44:1, and dual-screw-stem machine each district temperature is: 1st district
160 DEG C, 2 170 DEG C of districts, 3 170 DEG C of districts, 4 180 DEG C of districts, 5 180 DEG C of districts, 6 190 DEG C of districts, 7 190 DEG C of districts,
8 200 DEG C of districts, 9 210 DEG C of districts, maceration tank 220 DEG C.
Embodiment 4
Weigh 70 parts of PVDF resins, 0.3 part of antioxidant 1010,0.1 part of irgasfos 168,0.6 part of lubricant
Zinc stearate is room temperature mixing 5min in high mixer, is then added to double screw extruder extrusion, by melt from leaching
The melt inlet port of stain equipment is squeezed in the maceration tank of impregnating equipment；
Continuous carbon fibre (toray company, trade mark T800H) is introduced at the fiber entry of impregnating equipment,
Enter the surface treatment chamber of impregnating equipment, control surface conditioning agent aluminate coupling agent distearyl acyl-oxygen isopropyl aluminic acid
Ester is 2% relative to the weight content of carbon fiber, and the carbon fiber after then surface treated agent being processed is incorporated into leaching
In the maceration tank of stain equipment, it is achieved the dispersion of carbon fiber is also combined with PVDF resin；Shaped by selection
The size (3mm) of mouth die, adjusts the engine speed 13-14HZ of extruder simultaneously, rate of feeding at 8-9HZ,
Control continuous carbon fibre content about 30%；The rotating speed of regulation pelleter, makes the continuous carbon fibre prepared
The length of enhancing PVDF composite is at about 10mm, and particle diameter is at about 3mm；
Double screw extruder is directly 50mm, screw slenderness ratio 44:1, and dual-screw-stem machine each district temperature is: 1st district
160 DEG C, 2 170 DEG C of districts, 3 170 DEG C of districts, 4 180 DEG C of districts, 5 180 DEG C of districts, 6 190 DEG C of districts, 7 190 DEG C of districts,
8 200 DEG C of districts, 9 210 DEG C of districts, maceration tank 220 DEG C.
Comparative example
Weigh 100 parts of PVDF resins, 1098,0.2 part of irgasfos 168 of 0.5 part of antioxidant, 0.3 part of lubricant
Erucyl amide is room temperature mixing 3min in high mixer, is then added to double screw extruder and extrudes, cooling and dicing,
Obtaining length at about 4mm, particle diameter is at about 3mm；
Double screw extruder is directly 50mm, screw slenderness ratio 44:1, and dual-screw-stem machine each district temperature is: 1st district
160 DEG C, 2 170 DEG C of districts, 3 170 DEG C of districts, 4 180 DEG C of districts, 5 180 DEG C of districts, 6 190 DEG C of districts, 7 190 DEG C of districts,
8 200 DEG C of districts, 9 210 DEG C of districts, maceration tank 220 DEG C.
Each embodiment mechanical experimental results is as shown in table 1 below:
Table 1 mechanical experimental results
From upper table knowable to mechanical experimental results analysis, use the PVDF composite wood that continuous carbon fibre strengthens
Material intensity is high, excellent in mechanical performance, meets the occasion to performance requirement is higher and uses.
The above-mentioned description to embodiment is to be understood that and apply this for ease of those skilled in the art
Invention.Embodiment obviously easily can be made various amendment by person skilled in the art, and this explanation
General Principle be applied in other embodiments without through performing creative labour.Therefore, the invention is not restricted to this
In embodiment, those skilled in the art are according to the announcement of the present invention, the improvement made without departing from scope
All should be within protection scope of the present invention with amendment.
Claims (7)
1. one kind high wellability high intensity continuous carbon fibre strengthens polyvinylidene fluoride composite material, it is characterised in that
Comprise the component of following weight portion:
Fiber strength agent, its content is to be 1-3% relative to the weight/mass percentage composition of continuous carbon fibre；
Described continuous carbon fibre is polyacrylonitrile-based carbon fibre or asphalt base carbon fiber；
Above-mentioned composite is made by following steps:
(1) 60-90 part PVDF resin, 0.1-0.7 part antioxidant, 0.1-0.6 part lubricant are joined high mixed
In machine, stop after mixed at high speed 3-5min under room temperature, then the material mixed is joined double screw extruder
In；
(2) impregnating equipment of the continuous lod PVDF resin being connected to extruder head is used, by extruder
The melt of extrusion is squeezed in maceration tank at the melt inlet of impregnating equipment；
(3) continuous carbon fibre first enters into the surface treatment chamber in impregnating equipment at the fiber entry of impregnating equipment,
Fiber strength agent in surface treatment chamber carries out surface process, the carbon that then surface is handled well to continuous carbon fibre
Fiber proceeds immediately in the maceration tank of impregnating equipment, in maceration tank carbon fiber carry out disperseing and with step (2)
Gained PVDF melt fully infiltrates；
(4) carbon fiber after step (3) gained is fully impregnated with PVDF resin is set from dipping by traction machine
Standby sizing mouth die involves, and obtains composite products by pelleter pelletizing.
High wellability high intensity continuous carbon fibre the most according to claim 1 strengthens Kynoar composite wood
Material, it is characterised in that described Fiber strength agent is silane coupler, titanate coupling agent, Aluminate idol
Connection agent in one or more.
High wellability high intensity continuous carbon fibre the most according to claim 1 strengthens Kynoar composite wood
Material, it is characterised in that described antioxidant is four (β-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid Ji Wusi
Alcohol ester) (antioxidant 1010), 3,5-di-t-butyl-4-hydroxy benzenes propionyl-hexamethylene diamine (antioxidant 1098), phosphoric acid
One or more in three-(2,4-di-tert-butyl phenolic ester) (irgasfos 168).
High wellability high intensity continuous carbon fibre the most according to claim 1 strengthens Kynoar composite wood
Material, it is characterised in that described lubricant is stearic acid, calcium stearate, zinc stearate, ethylene bis stearamide
(EBS), one or more in erucyl amide.
5. a high wellability high intensity continuous carbon fibre as claimed in claim 1 enhancing Kynoar is combined
The preparation method of material, it is characterised in that the method comprises the following steps:
(1) 60-90 part PVDF resin, 0.1-0.7 part antioxidant, 0.1-0.6 part lubricant are joined high mixed
In machine, stop after mixed at high speed 3-5min under room temperature, then the material mixed is joined double screw extruder
In；
(2) impregnating equipment of the continuous lod PVDF resin being connected to extruder head is used, by extruder
The melt of extrusion is squeezed in maceration tank at the melt inlet of impregnating equipment；
(3) continuous carbon fibre first enters into the surface treatment chamber in impregnating equipment at the fiber entry of impregnating equipment,
Fiber strength agent in surface treatment chamber carries out surface process, the carbon that then surface is handled well to continuous carbon fibre
Fiber proceeds immediately in the maceration tank of impregnating equipment, in maceration tank carbon fiber carry out disperseing and with step (2)
Gained PVDF melt fully infiltrates；
(4) carbon fiber after step (3) gained is fully impregnated with PVDF resin is set from dipping by traction machine
Standby sizing mouth die involves, and obtains composite products by pelleter pelletizing.
High wellability high intensity continuous carbon fibre the most according to claim 5 strengthens Kynoar composite wood
The preparation method of material, it is characterised in that the screw diameter of described double screw extruder is 50mm, and draw ratio is
44:1, extruder temperature is 160-210 DEG C, and the maceration tank temperature of impregnating equipment is set in 220 DEG C.
High wellability high intensity continuous carbon fibre the most according to claim 5 strengthens Kynoar composite wood
The preparation method of material, it is characterised in that in described composite products, carbon fiber content is by regulation impregnating equipment
Sizing mouth die size control between 10-40% at 2-5mm and the rotating speed of extruder and rate of feeding；Pass through
Regulation pelleter cutter rotating velocity, makes the continuous carbon fibre finally prepared strengthen polyvinylidene fluoride composite material product
Particle length control at 8-12mm, size controlling is at 1-5mm.
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| CN104723576A (en) * | 2015-03-10 | 2015-06-24 | 北京化工大学 | Forming device and forming method of continuous fiber reinforced thermoplastic resin preimpregnation sheet material |
| CN105295264B (en) * | 2015-12-02 | 2017-08-08 | 上海三爱富新材料股份有限公司 | The preparation method of Kynoar powder composite material and composite porous |
| CN106046633A (en) * | 2016-06-29 | 2016-10-26 | 青岛海之源智能技术有限公司 | High-strength polyvinylidene fluoride composite material master batch |
| CN110054909A (en) * | 2019-04-18 | 2019-07-26 | 佛山市仁享精密五金塑料制品有限公司 | Carbon fibre plastic composite |
| CN112736188B (en) * | 2020-12-21 | 2022-12-09 | 西安交通大学 | Electric auxiliary preparation device and method for piezoelectric functional fiber |
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