WO2021050078A1 - Méthode de formation d'un composite, et composite et appareil associés - Google Patents

Méthode de formation d'un composite, et composite et appareil associés Download PDF

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Publication number
WO2021050078A1
WO2021050078A1 PCT/US2019/050931 US2019050931W WO2021050078A1 WO 2021050078 A1 WO2021050078 A1 WO 2021050078A1 US 2019050931 W US2019050931 W US 2019050931W WO 2021050078 A1 WO2021050078 A1 WO 2021050078A1
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Prior art keywords
reinforced thermoplastic
thermoplastic composite
fiber
cooling zone
roller module
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PCT/US2019/050931
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English (en)
Inventor
Sungkyun Sohn
Erin DIKEMAN
Keith KLINEDINST
Roeland Leonardus Hubertus Maria VERLAEK
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Sabic Global Technologies B.V.
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Priority to PCT/US2019/050931 priority Critical patent/WO2021050078A1/fr
Publication of WO2021050078A1 publication Critical patent/WO2021050078A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/28—Shaping operations therefor
    • B29C70/40—Shaping or impregnating by compression not applied
    • B29C70/50—Shaping or impregnating by compression not applied for producing articles of indefinite length, e.g. prepregs, sheet moulding compounds [SMC] or cross moulding compounds [XMC]
    • B29C70/504—Shaping or impregnating by compression not applied for producing articles of indefinite length, e.g. prepregs, sheet moulding compounds [SMC] or cross moulding compounds [XMC] using rollers or pressure bands
    • B29C70/506—Shaping or impregnating by compression not applied for producing articles of indefinite length, e.g. prepregs, sheet moulding compounds [SMC] or cross moulding compounds [XMC] using rollers or pressure bands and impregnating by melting a solid material, e.g. sheet, powder, fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/32—Component parts, details or accessories; Auxiliary operations
    • B29C43/44—Compression means for making articles of indefinite length
    • B29C43/48—Endless belts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/32—Component parts, details or accessories; Auxiliary operations
    • B29C43/52—Heating or cooling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B30—PRESSES
    • B30B—PRESSES IN GENERAL
    • B30B15/00—Details of, or accessories for, presses; Auxiliary measures in connection with pressing
    • B30B15/34—Heating or cooling presses or parts thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B30—PRESSES
    • B30B—PRESSES IN GENERAL
    • B30B5/00—Presses characterised by the use of pressing means other than those mentioned in the preceding groups
    • B30B5/04—Presses characterised by the use of pressing means other than those mentioned in the preceding groups wherein the pressing means is in the form of an endless band
    • B30B5/06—Presses characterised by the use of pressing means other than those mentioned in the preceding groups wherein the pressing means is in the form of an endless band co-operating with another endless band
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/42—Block-or graft-polymers containing polysiloxane sequences
    • C08G77/445—Block-or graft-polymers containing polysiloxane sequences containing polyester sequences
    • C08G77/448—Block-or graft-polymers containing polysiloxane sequences containing polyester sequences containing polycarbonate sequences
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
    • C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08L79/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/32—Component parts, details or accessories; Auxiliary operations
    • B29C43/44—Compression means for making articles of indefinite length
    • B29C43/48—Endless belts
    • B29C2043/483—Endless belts cooperating with a second endless belt, i.e. double band presses

Definitions

  • Fiber-reinforced thermoplastics are increasingly used in the fabrication of interior parts for vehicles including aircraft, ships, and trains.
  • U.S. Patent Application Publication No. US 2012/0065283 A1 of Adjei et al. describes a nonwoven fabric prepared from reinforcing fibers, polyimide fibers, and polymeric binder fibers. Multiple layers of the nonwoven fabric are consolidated under elevated temperature and pressure to form a composite sheet that is optionally combined with a decorative film to form the vehicular interior part.
  • Such parts exhibit advantageous properties including low weight, high flame retardancy, and low smoke generation.
  • Consolidation of the nonwoven fabric layers is typically conducted on an isobaric (constant pressure) double belt press, in which the upper and lower belts provide a constant pressure on the processed substrate.
  • an isochoric (constant volume) double-belt press in which the upper and lower belts provide a constant volume for the processed substrate, would have advantages including ease of operation, flexibility in product width (an isobaric process requires a product whose width exactly matches that of the belt), ease of process start-up and shut-down (for example, an isobaric process cannot tolerate a sudden substrate thickness change, as that could break the isobaric seal).
  • One embodiment is a method of forming a consolidated fiber-reinforced thermoplastic composite, the method comprising: in a double belt press, heating an unconsolidated fiber-reinforced thermoplastic composite in a volume-controlled heating area comprising a fixed roller module and characterized by an initial belt separation, h 1 , and a final belt separation, h2, wherein a ratio of h1 to h2 is 5:1 to 10:1, and wherein the heating forms a consolidated fiber-reinforced thermoplastic composite; and cooling the consolidated fiber- reinforced thermoplastic composite in an isochoric cooling area, wherein the isochoric cooling area comprises a first cooling zone comprising a circulating roller module, and a second cooling zone comprising a fixed roller module, wherein the second cooling zone is downstream of the first cooling zone.
  • Another embodiment is a composite prepared by the method in any of its variations.
  • Another embodiment is an apparatus for forming a consolidated fiber-reinforced thermoplastic composite, the apparatus comprising: a double belt press comprising, a volume- controlled heating area comprising a fixed roller module and characterized by an initial belt separation, h1, and a final belt separation, h2, wherein a ratio of h1 to h2 is 5:1 to 10:1; and an isochoric cooling area comprising a first isochoric cooling zone comprising a circulating roller module, and a second isochoric cooling zone comprising a fixed roller module, wherein the second isochoric cooling zone is downstream of the first isochoric cooling zone.
  • Figure 1 is a schematic illustration of a melt spinning apparatus.
  • Figure 2 is a schematic illustration of a papermaking apparatus.
  • Figure 3 is a schematic illustration of a prior art isochoric consolidation apparatus.
  • Figure 4 is a schematic illustration of a consolidation apparatus according to the invention.
  • the present inventors have determined that generation of “flash,” generation of “tail,” and generation of wavy patterns on the surface of the consolidated composite are reduced or eliminated by heating an unconsolidated fiber-reinforced thermoplastic composite in a volume-controlled double-belt press with a heating area and a cooling area.
  • the heating area has an initial belt separation substantially greater than the final belt separation
  • the cooling area includes a first cooling zone with a circulating roller module and a second cooling zone with a fixed roller module.
  • the heating zone belt separation feature and the cooling zone roller module features are both required to solve the technical problems.
  • One embodiment is a method of forming a consolidated fiber-reinforced thermoplastic composite, the method comprising: in a double belt press, heating an unconsolidated fiber-reinforced thermoplastic composite in a volume-controlled heating area comprising a fixed roller module and characterized by an initial belt separation, h 1 , and a final belt separation, h2, wherein a ratio of h1 to h2 is 5:1 to 10:1, and wherein the heating forms a consolidated fiber-reinforced thermoplastic composite; and cooling the consolidated fiber- reinforced thermoplastic composite in an isochoric cooling area, wherein the isochoric cooling area comprises a first cooling zone comprising a circulating roller module, and a second cooling zone comprising a fixed roller module, wherein the second cooling zone is downstream of the first cooling zone.
  • the method is conducted in an isochoric double-belt press, in which, at any given distance along the machine direction, the belt separation (and therefore the volume) is constant as a function of operation time. However, in the heating area, the belt separation decreases as a function of distance along the machine direction. For this reason, the belt separation in the heating area is described as “volume-controlled” rather than “constant volume,” even though the heating area is part of the isochoric (constant volume) double-belt press. [0014] The method comprises heating an unconsolidated fiber-reinforced thermoplastic composite in a volume-controlled heating area.
  • the heating area is characterized by an initial belt separation, h1, and a final belt separation, h2, and the ratio of h1 to h2 is in the range of 5:1 to 10:1. In some embodiments, the ratio of h1 to h2 is in the range 6:1 to 9:1.
  • the initial belt separation, h 1 is measured in the heating area at the first distance along the machine direction at which the volume of the substrate is controlled by both belts.
  • the final belt separation, h2 is measured in the heating area at the last distance along the machine direction at which the volume of the substrate is controlled by both belts. See Figure 4, described in detailed below, for an illustration of positions at which h 1 and h 2 are determined.
  • the unconsolidated fiber-reinforced thermoplastic composite comprises reinforcing fibers, and matrix-component-precursor fibers; and the heating the unconsolidated fiber-reinforced thermoplastic composite comprises exposing the unconsolidated fiber-reinforced thermoplastic composite to a temperature effective to at least partially melt the matrix-component-precursor fibers but not the reinforcing fibers.
  • those fibers can comprise a matrix component characterized by a matrix-component glass transition temperature
  • the heating the unconsolidated fiber-reinforced thermoplastic composite can comprise exposing the unconsolidated fiber-reinforced thermoplastic composite to a temperature greater than the matrix-component glass transition temperature.
  • the substrate exits the heating zone it is designated a consolidated fiber- reinforced thermoplastic composite. It then proceeds into a cooling area.
  • the cooling area is isochoric, which in this context means that the belt separation is constant along the length of the cooling area.
  • the cooling area comprises a first cooling zone comprising a circulating roller module.
  • a circulating roller module includes a closed loop of closely spaced rollers, a portion of the loop being in contact with one of the two belts of the double-belt press. See Figure 4, where circulating roller modules 570 are in contact with belts 310. The closely spaced rollers of the circulating roller modules 570 rotate individually, and the closed loop of closely spaced rollers rotates so that the rollers in contact with the belts 310 are moving in the opposite direction as the belt (i.e., in Figure 4, the upper loop of closely spaced rollers is rotating clockwise, and the lower loop of closely spaced rollers is rotating counterclockwise). Compared to a fixed roller module, a circulating roller module provides more even pressure on the substrate. A circulating roller circulates at essentially the same linear speed as the belts.
  • the isochoric cooling area is characterized by a constant belt separation, h3, and the ratio of h1 to h3 is 5:1 to 10:1, or 6:1 to 9:1.
  • the ratio of h1 to h3 corresponds to the overall substrate compression ratio of the process.
  • the consolidated fiber-reinforced thermoplastic composite comprises reinforcing fibers, and a matrix comprising a matrix thermoplastic composition; and the cooling the consolidated fiber-reinforced thermoplastic composite comprises exposing the consolidated fiber-reinforced thermoplastic composite to a temperature effective to at least partially solidify the matrix thermoplastic composition.
  • that composition can be characterized by a matrix thermoplastic composition glass transition temperature, and the cooling the consolidated fiber-reinforced thermoplastic composite can comprise exposing the unconsolidated fiber-reinforced thermoplastic composite to a temperature less than the matrix thermoplastic composition glass transition temperature.
  • the consolidated fiber-reinforced thermoplastic composite comprises, based on the total weight of the composite, 25 to 55 weight percent of reinforcing fibers, 35 to 65 weight percent of a polyimide, and 5 to 20 weight percent of a block polyestercarbonate-polysiloxane.
  • the reinforcing fibers comprise glass fibers;
  • the polyimide comprises a polyetherimide;
  • the block polyestercarbonate-polysiloxane comprises a polyester block comprising resorcinol ester units having the structure , a polycarbonate block comprising carbonate units having the structure , wherein at least 60 percent of the total number of R 1 groups are aromatic divalent groups, and a polysiloxane block comprising dimethylsiloxane units; wherein the block polyestercarbonate- polysiloxane comprises, based on total moles of carbonate and ester units, 70 to 90 mole percent of resorcinol ester units, 5 to 15 mole percent of carbonate units wherein R 1 is 1,3-phenylene, and 5 to 15 mole percent of carbonate units wherein R 1 is 2,2-bis(1,4-phenylene)propane, and further comprises, based on the weight of the block polyestercarbonate-polysiloxane, 0.2 to 4 weight
  • the consolidated fiber-reinforced thermoplastic composite comprises, based on the total weight of the composite, 25 to 55 weight percent of reinforcing fibers, 35 to 65 weight percent of a polyimide, and 5 to 20 weight percent of a block polyestercarbonate-polysiloxane.
  • the reinforcing fibers comprise glass fibers;
  • the polyimide comprises a polyetherimide;
  • the block polyestercarbonate-polysiloxane comprises a polyester block comprising resorcinol ester units having the structure , a polycarbonate block comprising carbonate units having the structure wherein at least 60 percent of the total number of R 1 groups are aromatic divalent groups, and a polysiloxane block comprising dimethylsiloxane units; wherein the block polyestercarbonate- polysiloxane comprises, based on total moles of carbonate and ester units, 70 to 90 mole percent of resorcinol ester units, 5 to 15 mole percent of carbonate units wherein R 1 is 1,3-phenylene, and 5 to 15 mole percent of carbonate units wherein R 1 is 2,2-bis(1,4-phenylene)propane, and further comprises, based on the weight of the block polyestercarbonate-polysiloxane, 0.2 to 4 weight percent di
  • Another embodiment is an apparatus for forming a consolidated fiber-reinforced thermoplastic composite, the apparatus comprising: a double belt press comprising, a volume- controlled heating area comprising a fixed roller module and characterized by an initial belt separation, h1, and a final belt separation, h2, wherein a ratio of h1 to h2 is 5:1 to 10:1; and an isochoric cooling area comprising a first isochoric cooling zone comprising a circulating roller module, and a second isochoric cooling zone comprising a fixed roller module, wherein the second isochoric cooling zone is downstream of the first isochoric cooling zone.
  • the invention includes at least the following aspects.
  • a method of forming a consolidated fiber-reinforced thermoplastic composite comprising: in a double belt press, heating an unconsolidated fiber- reinforced thermoplastic composite in a volume-controlled heating area comprising a fixed roller module and characterized by an initial belt separation, h 1 , and a final belt separation, h 2 , wherein a ratio of h1 to h2 is 5:1 to 10:1, and wherein the heating forms a consolidated fiber-reinforced thermoplastic composite; and cooling the consolidated fiber-reinforced thermoplastic composite in an isochoric cooling area, wherein the isochoric cooling area comprises a first cooling zone comprising a circulating roller module, and a second cooling zone comprising a fixed roller module, wherein the second cooling zone is downstream of the first cooling zone.
  • Aspect 2 The method of aspect 1, wherein the unconsolidated fiber-reinforced thermoplastic composite comprises reinforcing fibers, and matrix-component-precursor fibers; and the heating the unconsolidated fiber-reinforced thermoplastic composite comprises exposing the unconsolidated fiber-reinforced thermoplastic composite to a temperature effective to at least partially melt the matrix-component-precursor fibers but not the reinforcing fibers.
  • Aspect 3 The method of aspect 1 or 2, wherein the consolidated fiber-reinforced thermoplastic composite comprises reinforcing fibers, and a matrix comprising a matrix thermoplastic composition; and the cooling the consolidated fiber-reinforced thermoplastic composite comprises exposing the consolidated fiber-reinforced thermoplastic composite to a temperature effective to at least partially solidify the matrix thermoplastic composition.
  • Aspect 4 The method of any one of aspects 1-3, wherein the first cooling zone is characterized by a constant belt separation, h 3 , and wherein a ratio of h 1 to h 3 is 5:1 to 10:1.
  • Aspect 5 The method of any one of aspects 1-4, wherein the consolidated fiber- reinforced thermoplastic composite comprises, based on the total weight of the composite, 25 to 55 weight percent of reinforcing fibers, 35 to 65 weight percent of a polyimide, and 5 to 20 weight percent of a block polyestercarbonate-polysiloxane.
  • Aspect 6 The method of aspect 5, wherein the reinforcing fibers comprise glass fibers; the polyimide comprises a polyetherimide; and the block polyestercarbonate-polysiloxane comprises a polyester block comprising resorcinol ester units having the structure , a polycarbonate block comprising carbonate units having the structure wherein at least 60 percent of the total number of R 1 groups are aromatic divalent groups, and a polysiloxane block comprising dimethylsiloxane units; wherein the block polyestercarbonate- polysiloxane comprises, based on total moles of carbonate and ester units, 70 to 90 mole percent of resorcinol ester units, 5 to 15 mole percent of carbonate units wherein R 1 is 1,3-phenylene, and 5 to 15 mole percent of carbonate units wherein R 1 is 2,2-bis(1,4-phenylene)propane, and further comprises, based on the weight of the block polyestercarbonate-polysiloxane, 0.2
  • Aspect 7 A composite prepared by the method of any one of aspects 1-6.
  • Aspect 8 A composite prepared by the method of aspect 5.
  • Aspect 9 A composite prepared by the method of aspect 6.
  • Aspect 10 An apparatus for forming a consolidated fiber-reinforced thermoplastic composite, the apparatus comprising: a double belt press comprising, a volume- controlled heating area comprising a fixed roller module and characterized by an initial belt separation, h 1 , and a final belt separation, h 2 , wherein a ratio of h 1 to h 2 is 5:1 to 10:1; and an isochoric cooling area comprising a first isochoric cooling zone comprising a circulating roller module, and a second isochoric cooling zone comprising a fixed roller module, wherein the second isochoric cooling zone is downstream of the first isochoric cooling zone.
  • melt spinning apparatus 1 comprises extruder 5, in which dried pellets are converted to a melt, melt pump 10, which conveys the melt to spin pack 15, where it is filtered, then to spinneret 20, where multiple fibers are formed from the filtered melt.
  • melt spinning apparatus 1 comprises extruder 5, in which dried pellets are converted to a melt, melt pump 10, which conveys the melt to spin pack 15, where it is filtered, then to spinneret 20, where multiple fibers are formed from the filtered melt.
  • the fibers are immediately conveyed to quench section 30, where they are air-cooled and solidified.
  • the cooled fibers then enter spin finish section 40, where a spin finish can be applied to the surface of the fibers.
  • the fibers then traverse a sequence of godet pairs comprising first godets 50, second godets 60, and third godets 70, where the fibers are drawn (stretched).
  • the fibers then enter winder section 80, where contact roller 90 facilitates formation of wound fiber 100 around one of two winding cores 110.
  • the melt pump was operated at 10 centimeter 3 /revolution. Extruder and melt pump temperatures were 280 to 330 °C. A 144-hole, single-position spinneret was used. Spinneret holes (nozzles) were circular with a diameter of 0.8 millimeters.
  • the length-to-diameter ratio of each spinneret was 4:1.
  • a 325 U.S. mesh (44 micrometer opening) screen filter was used in the spinpack for filtration of the composition melt. After fibers exited the nozzles, they were solidified by quenching with air at ambient temperature (about 23 °C). Individual filaments were combined to form multi-filament threads, then a spin finish (an acrylamide copolymer in an oil-in-water emulsion, obtained as LUROL TM PS-11744 from Goulston) was applied to the multi-filament threads before they contacted the first godet. The draw down ratio was 280 to 550.
  • Draw down ratio which is unitless, is defined as the ratio of speed (in meters/minute) at which the melt exits the spinneret nozzles to the speed (in meters/minute) of the fiber at the first godet.
  • the apparent shear rate was 170 to 1700 second -1 .
  • Apparent shear rate (in units of second -1 ) is defined according to the equation wherein Q is the melt throughput per spinneret nozzle (in grams/second), R is the nozzle radius (in centimeters), and r is the polymer melt density (in grams/centimeter 3 ).
  • the mechanical draw ratio was 0.95 to 1.2.
  • Nonwoven Fabric A mixture of polyetherimide fibers (50 weight percent), PEC-Si fibers (10 weight percent), and chopped glass fibers (40 weight percent) was used to prepare a nonwoven fabric via a wet-laid papermaking) process.
  • Figure 2 is a schematic illustration of a papermaking apparatus 200, which includes mixing tank 210, run tank 220, headbox 230, wire former 240, dryer 250, and winder 260.
  • a fiber dispersion was prepared by dispersing 200 kilograms total of the three ingredient fibers in 200 kilograms of an aqueous solution containing a viscosity modifying agent.
  • the viscosity modifying agent was a poly(acrylamide-co-diallyldimethylammonium chloride) solution, 10 weight percent in water, and it was used in an amount effective to provide the aqueous solution with a viscosity of 50 to 200 centipoise.
  • the fiber dispersion was fed onto the wire mesh of a paper-making machine to form an aqueous suspension layer, and aqueous solution was drained to form a fiber layer. The fiber layer was transferred to a water washing section where viscosity modifier was washed from the fiber layer.
  • the washed fiber layer was then transferred to a tunnel dryer, and finally to a winding section.
  • Water was essentially eliminated from the mat by the sequence of gravity drainage through holes in the wire mesh, squeezing through several pairs of nip rollers, and heating in an ambient-pressure tunnel dryer, where the temperature was set to 280-300 °C and the drier residence time was 120-180 seconds. ⁇ In this temperature range, the PEC-Si fibers melted and the polyetherimide fibers at least partially melted. Both types of fibers flowed, losing their fiber shape. If the tunnel dryer temperature is less than 280 °C, web tearing occurs.
  • binder activation because the binder fibers melt, and the melted PEC-Si copolymer flows within the web to bind together the network of glass and polyetherimide fibers. This gives the network enough mechanical integrity to prevent it from falling apart in subsequent processing and handling.
  • a 165 gram/meter 2 nonwoven fabric web was produced at a speed of 5 meters/minute.
  • FIG. 3 is a schematic illustration of a prior art isochoric double-belt press consolidation apparatus, 300, in which circulation of belts 310 is controlled by drums 320.
  • the heating area 325 includes heaters 330 and fixed roller modules 350.
  • the substrate proceeds to a cooling area 335 including cooler 340, and fixed roller module 350.
  • the substrate 360 exits as a consolidated fiber-reinforced thermoplastic composite.
  • Rectangular pieces 30.5 centimeters wide and 35.6 centimeters long (12 by 14 inches) were cut from the nonwoven roll. A total of eight layers of nonwoven were stacked together (collectively, “the substrate”) in preparation for consolidation to make a 1,320 gram/meter 2 composite.
  • FIG. 4 is a schematic illustration of the double-belt press 500, in which circulation of belts 310 is controlled by drums 320.
  • Substrate 560 enters heating area 325 (as an unconsolidated fiber-reinforced thermoplastic composite) at a belt separation, h 1 , and exits heating area 325 at a belt separation, h2, wherein the ratio of h1 to h2 is 5:1 to 10:1 (h1 and h2 are not shown to scale in Figure 4).
  • the heating area 325 includes heaters 330 and fixed roller modules 350. From the heating area 325, the substrate proceeds to a cooling area 335 including coolers 340, and at least one circulating roller module 570, followed by at least one fixed roller module 350.
  • the substrate 560 exits as a consolidated fiber-reinforced thermoplastic composite.
  • Table 3 summarizes process variations and properties of the resulting consolidated fiber-reinforced thermoplastic composite.
  • varying belt gap settings are presented as a function of zone, where zones are labeled Z1-Z5.
  • Z1, Z2, and Z3 correspond to the three sections of heating area 325, each section having its own heaters 330 and fixed roller module 350; and Z4 and Z5 correspond to the two sections of cooling area 335, each section having its own cooler 340, the first section having circulating roller module 570, and the second section having a fixed roller module 350.
  • there are no gap values for the Z5 inlet and Z5 outlet because the apparatus did not include a Z5 section.
  • each section had a machine direction length of 1.0 meter, and sections were separated by a machine direction distance of 0.1 meter.
  • Table 3 “h1/h2” is the ratio of the heating area initial belt separation, h1, to the heating area final belt separation, h 2 ; and “h 1 /h 3 ” is the ratio of the heating area initial belt separation, h 1 , to the cooling area constant belt separation, h3.
  • “Z4 CR?” refers to whether there is a circulating roller module in Zone 4; “yes” means that a circulating roller module is present in Zone 4; “no” means that a fixed roller module is present in Zone 4.
  • a “Consolidation” rating of “Bad” means that the consolidated fiber-reinforced thermoplastic composite exhibits visually observable fibers on its surface and/or exhibits visually observable polymer-derived fibers in cross-section; a rating of “Good” means that neither of these defects was observed.
  • “Flash?” refers to whether there is any flash present, where flash is defined as visually observable thermoplastic matrix material extending beyond the side (transverse direction) edges of the consolidated fiber-containing composite; “yes” means that flash is present, and “no” means that flash is absent.
  • Tail (cm) refers to the length of the tail, defined as the length in centimeters of any thermoplastic matrix material extending beyond the trailing machine-direction edge of the consolidated fiber- containing composite.
  • Surface appearance refers to the visual appearance of the top surface of the consolidated composite; “No wavy patterns” and “Wavy patterns” indicate the absence and presence, respectively, of visually observable wavy patterns on the surface. Flexural modulus values, expressed in megapascals (MPa) and were determined in the machine and transverse directions according to ISO 178:2010 at 23 °C using test articles cut from the consolidated composite and having dimensions 15.24 centimeters (6 inches) long by 2.54 centimeters (1 inch) wide by 1.2 millimeters thick.
  • Example 1 illustrates that only the Example 1 consolidated composite, prepared in a process with an h1/h2 value in the range 5:1 to 10:1, as well as a circulating roller module in the first cooling zone, exhibited good consolidation, no wavy patterns, no flash, and no tail.
  • Comparative Example 1 illustrates that wavy patterns resulted from a process including an hi/h2 value in the range 5:1 to 10:1, but lacking a circulating roller module (i.e., having a fixed roller module) in the first cooling zone.
  • Comparative Example 4 illustrates that wavy patterns and a 7.62 centimeter long tail resulted from a process having a circulating roller module in the first cooling zone, but having an hi/ha value below 5.

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Abstract

Une méthode de formation d'un composite thermoplastique renforcé par des fibres consolidé est mise en œuvre dans une presse à double bande et comprend le chauffage d'un composite thermoplastique renforcé par des fibres non consolidé dans une zone de chauffage à volume contrôlé pour former un composite thermoplastique renforcé par des fibres consolidé, et le refroidissement du composite thermoplastique renforcé par des fibres consolidé dans une zone de refroidissement à volume constant. La zone de chauffage à volume contrôlé comprend un module de rouleau fixe et est caractérisée par une séparation de bande initiale, h1, et une séparation de bande finale, h2, le rapport de h1 à h2 étant de 5 : 1 à 10 : 1. La zone de refroidissement à volume constant comprend une première zone de refroidissement avec un module de rouleau de circulation, et une seconde zone de refroidissement avec un module de rouleau fixe. L'invention concerne également un composite thermoplastique renforcé par des fibres consolidé préparé par la méthode, et un appareil pour la mise en œuvre de la méthode.
PCT/US2019/050931 2019-09-13 2019-09-13 Méthode de formation d'un composite, et composite et appareil associés WO2021050078A1 (fr)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2040801A (en) * 1978-12-04 1980-09-03 Ppg Industries Inc Process for laminating thermoplastic resin reinforced with fiber glass
US4956140A (en) * 1985-12-09 1990-09-11 Aluminum Company Of America Alcoa Laboratories Methods of and apparatus for producing biaxially oriented polymer product
US20120065283A1 (en) 2010-09-14 2012-03-15 Sabic Innovative Plastics Ip B.V. Reinforced thermoplastic articles, compositions for the manufacture of the articles, methods of manufacture, and articles formed therefrom

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2040801A (en) * 1978-12-04 1980-09-03 Ppg Industries Inc Process for laminating thermoplastic resin reinforced with fiber glass
US4956140A (en) * 1985-12-09 1990-09-11 Aluminum Company Of America Alcoa Laboratories Methods of and apparatus for producing biaxially oriented polymer product
US20120065283A1 (en) 2010-09-14 2012-03-15 Sabic Innovative Plastics Ip B.V. Reinforced thermoplastic articles, compositions for the manufacture of the articles, methods of manufacture, and articles formed therefrom

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