CN104371229A - High-wettability and high-strength continuous carbon fiber reinforced polyvinylidene fluoride (PVDF) composite material and preparation method thereof - Google Patents
High-wettability and high-strength continuous carbon fiber reinforced polyvinylidene fluoride (PVDF) composite material and preparation method thereof Download PDFInfo
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- 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
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Abstract
The invention relates to a high-wettability and high-strength continuous carbon fiber reinforced polyvinylidene fluoride (PVDF) composite material and a preparation method thereof. The preparation method comprises the following steps of adding 60-90 parts of PVDF resin, 0.1-0.5 part of antioxidant and 0.1-0.6 part of lubricating agent into a high-speed mixer, and then, adding the mixed material into a double-screw extruder; extruding a melt extruded from the extruder into a dipping tank from a melt inlet of dipping equipment, wherein the dipping equipment for continuous carbon fiber reinforced PVDF resin is connected to an extrusion head; enabling continuous carbon fiber to enter a surface treatment chamber of the dipping equipment from a fiber inlet of the dipping equipment to be subjected to surface treatment; then, enabling the continuous carbon fiber to enter the dipping tank of the dipping equipment to sufficiently wet the obtained PVDF melt; and dragging the continuous carbon fiber from a shaping mold of the dipping equipment through a dragger, and pelletizing through a pelletizer to obtain a composite material product. Compared with the prior art, the high-wettability and high-strength continuous carbon fiber reinforced PVDF composite material disclosed by the invention is low in density, high in strength and excellent in mechanical property and has the advantages of energy saving, environment friendliness, low cost and the like.
Description
Technical field
The invention belongs to macromolecular material recovery technology field, be specifically related to a kind of high wetting property high strength continuous carbon fibre and strengthen polyvinylidene fluoride composite material and preparation method thereof.
Background technology
Polyvinylidene difluoride (PVDF) (PVDF) has in fluoroplastics that most obdurability, low-friction coefficient, erosion resistance are strong, ageing resistance, weather, the features such as radiation-resistant property is good, are therefore widely used in the fields such as coating, petrochemical equipment pipeline, functional membrane.But PVDF self-strength is low, limit it in some application to the higher field of product strength requirement.
Continuous lod polyvinylidene fluoride composite material is with continuous fibre, and as inorganic in glass fibre, carbon fiber, aramid fiber etc. or organic fibre, as strongthener, take polyvinylidene fluoride resin as matrix, the advanced composite material manufactured by special process; Compared with the polyvinylidene fluoride composite material of staple fibre or long fiber reinforcement, the polyvinylidene fluoride composite material mechanical property of continuous lod has had qualitative leap, there is lightweight, the excellent properties such as specific tenacity is high, specific modulus is high, good corrosion resistance, being particularly suitable for automobile, aircraft, protection and other purposes that is higher to mechanical property requirements, that need weight reduction, is one of material with fastest developing speed in current composite markets.
Carbon fiber is that a kind of high-temperature fibre, density with very high strength and modulus is low, the characteristic of these excellences imparts carbon-fibre composite and has very high mechanical property, be the reinforced composites such as other glass fibre incomparable, be therefore widely used in the new high-tech industry fields such as aerospace, automotive industry, track traffic, new forms of energy, sports goods.And the composite property adopting continuous carbon fibre to strengthen is compared with other continuous fiber reinforced composite materials, there is higher mechanical property, simultaneously lightweight, there is very wide Application Areas.
But key problem in technology prepared by continuous carbon fibre enhancing PVDF matrix material is dispersion and the dipping of fiber.The quality of fiber dispersion effect, resin can in the middle of complete wetting to fiber and the consistency of fiber and resin directly decide the quality of the finished product performance.And existing patented technology retrieval is found to do not have continuous carbon fibre to strengthen the relevant report of PVDF matrix material.
Summary of the invention
Object of the present invention is exactly provide a kind of high wetting property high strength continuous carbon fibre of energy-conserving and environment-protective to strengthen polyvinylidene fluoride composite material and preparation method thereof to overcome defect that above-mentioned prior art exists.
Object of the present invention can be achieved through the following technical solutions: a kind of high wetting property high strength continuous carbon fibre strengthens polyvinylidene fluoride composite material, it is characterized in that, comprises the component of following weight part:
Fiber strength agent, its content is be 1-3% relative to the mass percentage of continuous carbon fibre.
Described continuous carbon fibre is PAN-based carbon fiber or asphalt base carbon fiber.
Described Fiber strength agent is one or more in silane coupling agent, titanate coupling agent, aluminate coupling agent.
Described oxidation inhibitor is four (β-(3,5-di-tert-butyl-hydroxy phenyl) propionate) (antioxidant 1010), 3, one or more in 5-di-t-butyl-4-hydroxybenzene propionyl-hexanediamine (oxidation inhibitor 1098), tricresyl phosphate-(2,4-DTBP ester) (irgasfos 168).
Described lubricant is one or more in stearic acid, calcium stearate, Zinic stearas, ethylene bis stearamide (EBS), erucicamide.
High wetting property high strength continuous carbon fibre strengthens a preparation method for polyvinylidene fluoride composite material, and it is characterized in that, the method comprises the following steps:
(1) 60-90 part PVDF resin, 0.1-0.5 part oxidation inhibitor, 0.1-0.6 part lubricant are joined in high mixer, stop after high-speed mixing 3-5min under normal temperature, then the material mixed is joined in twin screw extruder;
(2) adopt the impregnating equipment being connected to the continuous lod PVDF resin of extruder head, the melt extruded by forcing machine is squeezed in steeping vat from the melt inlet of impregnating equipment;
(3) continuous carbon fibre first enters into the surface treatment chamber of impregnating equipment from the fiber entry of impregnating equipment, Fiber strength agent in surface treatment chamber carries out surface treatment to continuous carbon fibre, then and then the carbon fiber that surface treatment is good enters in the steeping vat of impregnating equipment, and in steeping vat, carbon fiber carries out disperseing and fully infiltrates with step (2) gained PVDF melt;
(4) step (3) gained is fully infiltrated the carbon fiber after having PVDF resin and is involved by the sizing mouth mould of tractor from impregnating equipment, and obtains composite products by dicing machine pelletizing.
The screw diameter of described twin screw extruder is 50mm, and length-to-diameter ratio is 44: 1, and extruder temperature is 160-210 DEG C, and the steeping vat temperature of impregnating equipment is set in 220 DEG C;
In described composite products, carbon fiber content controls by regulating the sizing mouth mould size of impregnating equipment between 10-40% at the rotating speed of 2-5mm and forcing machine and rate of feeding; By regulating dicing machine cutter rotating velocity, make the particle length of the continuous carbon fibre reinforced polypropylene compound material product finally prepared control at 8-12mm, size controlling is at 1-5mm.
Compared with prior art, present invention achieves the surface treatment of fiber, fiber dispersion and infiltrate to be compounded in an impregnating equipment with resin and complete continuously, simplify production technique; In the matrix material obtained, carbon fiber and PVDF not only have good wetting property, and carbon fiber and PVDF before infiltration by surface treatment agent process, make both have good interfacial bonding property; It is excellent that the continuous carbon fibre prepared strengthens PVDF composite materials property, and density is low simultaneously, and matrix material can be widely used in aerospace, automobile, machinery, electronic apparatus, the product components such as household electrical appliances.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
In following examples, bending property testing standard is ASTM D790, and unnotched impact strength testing standard is ASTM D256.
Embodiment 1
Take 60 parts of PVDF resins, 0.3 part of antioxidant 1010,0.1 part of irgasfos 168,0.1 part of Lubricate EBS normal temperature mixing 5min in high mixer, then join twin screw extruder to extrude, gained melt is squeezed into the steeping vat of impregnating equipment from the melt admission port of impregnating equipment;
By continuous carbon fibre (toray company, trade mark T300) introduce from the fiber entry of impregnating equipment, enter the surface treatment chamber of impregnating equipment, control surface treatment agent silane coupling agent KH560 is 1% relative to the weight content of carbon fiber, then the carbon fiber after surface treatment agent process is incorporated in the steeping vat of impregnating equipment, realizes the dispersion of carbon fiber and carry out compound with PVDF resin; By selecting the size (2mm) of sizing mouth mould, adjust the engine speed 13-14HZ of forcing machine, rate of feeding, at 9-10HZ, controls continuous carbon fibre content about 40% simultaneously; Regulate the rotating speed of dicing machine, make the continuous carbon fibre prepared strengthen the length of PVDF matrix material at about 10mm, particle diameter is at about 3mm;
Twin screw extruder be directly 50mm, screw slenderness ratio 44: 1, dual-screw-stem machine each district temperature is: 1 160 DEG C, district, 2 170 DEG C, districts, 3 170 DEG C, districts, 4 180 DEG C, districts, 5 180 DEG C, districts, 6 190 DEG C, districts, 7 190 DEG C, districts, 8 200 DEG C, districts, 9 210 DEG C, districts, steeping vat 220 DEG C.
Embodiment 2
Take 80 parts of PVDF resins, 0.5 part of oxidation inhibitor, 1098,0.2 part of irgasfos 168,0.3 part of lubricant stearic acid calcium normal temperature mixing 3min in high mixer, then join twin screw extruder to extrude, melt is squeezed into the steeping vat of impregnating equipment from the melt admission port of impregnating equipment;
By continuous carbon fibre (toray company, trade mark T300J) introduce from the fiber entry of impregnating equipment, enter the surface treatment chamber of impregnating equipment, the different stearoyl titanic acid ester of control surface treatment agent titanate coupling agent sec.-propyl three is 2% relative to the weight content of carbon fiber, then the carbon fiber after surface treatment agent process is incorporated in the steeping vat of impregnating equipment, realizes the dispersion of carbon fiber and carry out compound with PVDF fat; By selecting the size (4mm) of sizing mouth mould, adjust the engine speed 13-14HZ of forcing machine, rate of feeding, at 9-10HZ, controls continuous carbon fibre content about 20% simultaneously; Regulate the rotating speed of dicing machine, make the continuous carbon fibre prepared strengthen the length of PVDF matrix material at about 10mm, particle diameter is at about 3mm;
Twin screw extruder be directly 50mm, screw slenderness ratio 44: 1, dual-screw-stem machine each district temperature is: 1 160 DEG C, district, 2 170 DEG C, districts, 3 170 DEG C, districts, 4 180 DEG C, districts, 5 180 DEG C, districts, 6 190 DEG C, districts, 7 190 DEG C, districts, 8 200 DEG C, districts, 9 210 DEG C, districts, steeping vat 220 DEG C.
Embodiment 3
Take 90 parts of PVDF resins, 0.3 part of oxidation inhibitor, 1098,0.1 part of irgasfos 168,0.6 part of lubricant stearic acid normal temperature mixing 5min in high mixer, then join twin screw extruder to extrude, melt is squeezed into the steeping vat of impregnating equipment from the melt admission port of impregnating equipment;
By continuous carbon fibre (toray company, trade mark T700S) introduce from the fiber entry of impregnating equipment, enter the surface treatment chamber of impregnating equipment, control surface treatment agent aluminate coupling agent distearyl acyl-oxygen sec.-propyl Aluminate is 3% relative to the weight content of carbon fiber, then the carbon fiber after surface treatment agent process is incorporated in the steeping vat of impregnating equipment, realizes the dispersion of carbon fiber and carry out compound with PVDF resin; By selecting the size (5mm) of sizing mouth mould, adjust the engine speed 15-16HZ of forcing machine, rate of feeding, at 11-12HZ, controls continuous carbon fibre content about 5% simultaneously; Regulate the rotating speed of dicing machine, make the continuous carbon fibre prepared strengthen the length of PVDF matrix material at about 10mm, particle diameter is at about 3mm;
Twin screw extruder be directly 50mm, screw slenderness ratio 44: 1, dual-screw-stem machine each district temperature is: 1 160 DEG C, district, 2 170 DEG C, districts, 3 170 DEG C, districts, 4 180 DEG C, districts, 5 180 DEG C, districts, 6 190 DEG C, districts, 7 190 DEG C, districts, 8 200 DEG C, districts, 9 210 DEG C, districts, steeping vat 220 DEG C.
Embodiment 4
Take 70 parts of PVDF resins, 0.3 part of antioxidant 1010,0.1 part of irgasfos 168,0.6 part of lubricant stearic acid zinc normal temperature mixing 5min in high mixer, then join twin screw extruder to extrude, melt is squeezed into the steeping vat of impregnating equipment from the melt admission port of impregnating equipment;
By continuous carbon fibre (toray company, trade mark T800H) introduce from the fiber entry of impregnating equipment, enter the surface treatment chamber of impregnating equipment, control surface treatment agent aluminate coupling agent distearyl acyl-oxygen sec.-propyl Aluminate is 2% relative to the weight content of carbon fiber, then the carbon fiber after surface treatment agent process is incorporated in the steeping vat of impregnating equipment, realizes the dispersion of carbon fiber and carry out compound with PVDF resin; By selecting the size (3mm) of sizing mouth mould, adjust the engine speed 13-14HZ of forcing machine, rate of feeding, at 8-9HZ, controls continuous carbon fibre content about 30% simultaneously; Regulate the rotating speed of dicing machine, make the continuous carbon fibre prepared strengthen the length of PVDF matrix material at about 10mm, particle diameter is at about 3mm;
Twin screw extruder be directly 50mm, screw slenderness ratio 44: 1, dual-screw-stem machine each district temperature is: 1 160 DEG C, district, 2 170 DEG C, districts, 3 170 DEG C, districts, 4 180 DEG C, districts, 5 180 DEG C, districts, 6 190 DEG C, districts, 7 190 DEG C, districts, 8 200 DEG C, districts, 9 210 DEG C, districts, steeping vat 220 DEG C.
Comparative example
Take 100 parts of PVDF resins, 0.5 part of oxidation inhibitor, 1098,0.2 part of irgasfos 168,0.3 part of lubricant erucicamide normal temperature mixing 3min in high mixer, then join twin screw extruder to extrude, cooling and dicing, obtain length at about 4mm, particle diameter is at about 3mm;
Twin screw extruder be directly 50mm, screw slenderness ratio 44: 1, dual-screw-stem machine each district temperature is: 1 160 DEG C, district, 2 170 DEG C, districts, 3 170 DEG C, districts, 4 180 DEG C, districts, 5 180 DEG C, districts, 6 190 DEG C, districts, 7 190 DEG C, districts, 8 200 DEG C, districts, 9 210 DEG C, districts, steeping vat 220 DEG C.
Each embodiment mechanical experimental results is as shown in table 1 below:
Table 1 mechanical experimental results
From upper table, mechanical experimental results is analyzed, and the PVDF composite material strength adopting continuous carbon fibre to strengthen is high, excellent in mechanical performance, meets the occasion higher to performance requriements and uses.
Above-mentioned is can understand and apply the invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to embodiment, and this General Principle illustrated is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to embodiment here, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (8)
1. high wetting property high strength continuous carbon fibre strengthens a polyvinylidene fluoride composite material, it is characterized in that, comprises the component of following weight part:
Fiber strength agent, its content is be 1-3% relative to the mass percentage of continuous carbon fibre.
2. high wetting property high strength continuous carbon fibre according to claim 1 strengthens polyvinylidene fluoride composite material, and it is characterized in that, described continuous carbon fibre is PAN-based carbon fiber or asphalt base carbon fiber.
3. high wetting property high strength continuous carbon fibre according to claim 1 strengthens polyvinylidene fluoride composite material, it is characterized in that, described Fiber strength agent is one or more in silane coupling agent, titanate coupling agent, aluminate coupling agent.
4. high wetting property high strength continuous carbon fibre according to claim 1 strengthens polyvinylidene fluoride composite material, it is characterized in that, described oxidation inhibitor is four (β-(3,5-di-tert-butyl-hydroxy phenyl) propionate) (antioxidant 1010), 3, one or more in 5-di-t-butyl-4-hydroxybenzene propionyl-hexanediamine (oxidation inhibitor 1098), tricresyl phosphate-(2,4-DTBP ester) (irgasfos 168).
5. high wetting property high strength continuous carbon fibre according to claim 1 strengthens polyvinylidene fluoride composite material, it is characterized in that, described lubricant is one or more in stearic acid, calcium stearate, Zinic stearas, ethylene bis stearamide (EBS), erucicamide.
6. high wetting property high strength continuous carbon fibre as claimed in claim 1 strengthens a preparation method for polyvinylidene fluoride composite material, and it is characterized in that, the method comprises the following steps:
(1) 60-90 part PVDF resin, 0.1-0.5 part oxidation inhibitor, 0.1-0.6 part lubricant are joined in high mixer, stop after high-speed mixing 3-5min under normal temperature, then the material mixed is joined in twin screw extruder;
(2) adopt the impregnating equipment being connected to the continuous lod PVDF resin of extruder head, the melt extruded by forcing machine is squeezed in steeping vat from the melt inlet of impregnating equipment;
(3) continuous carbon fibre first enters into the surface treatment chamber of impregnating equipment from the fiber entry of impregnating equipment, Fiber strength agent in surface treatment chamber carries out surface treatment to continuous carbon fibre, then and then the carbon fiber that surface treatment is good enters in the steeping vat of impregnating equipment, and in steeping vat, carbon fiber carries out disperseing and fully infiltrates with step (2) gained PVDF melt;
(4) step (3) gained is fully infiltrated the carbon fiber after having PVDF resin and is involved by the sizing mouth mould of tractor from impregnating equipment, and obtains composite products by dicing machine pelletizing.
7. high wetting property high strength continuous carbon fibre according to claim 6 strengthens polyvinylidene fluoride composite material, it is characterized in that, the screw diameter of described twin screw extruder is 50mm, length-to-diameter ratio is 44: 1, extruder temperature is 160-210 DEG C, and the steeping vat temperature of impregnating equipment is set in 220 DEG C.
8. high wetting property high strength continuous carbon fibre according to claim 6 strengthens polyvinylidene fluoride composite material, it is characterized in that, in described composite products, carbon fiber content controls by regulating the sizing mouth mould size of impregnating equipment between 10-40% at the rotating speed of 2-5mm and forcing machine and rate of feeding; By regulating dicing machine cutter rotating velocity, make the particle length of the continuous carbon fibre reinforced polypropylene compound material product finally prepared 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 |
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| 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 |
| CN112736188A (en) * | 2020-12-21 | 2021-04-30 | 西安交通大学 | Electric auxiliary preparation device and method for piezoelectric functional fiber |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
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| CN112736188A (en) * | 2020-12-21 | 2021-04-30 | 西安交通大学 | Electric auxiliary preparation device and method for piezoelectric functional fiber |
| 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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