ES2624694T3 - Material de moldeo, preimpregnado, material compuesto reforzado con fibras y proceso para la producción de un material de base de moldeo reforzado con fibras - Google Patents

Material de moldeo, preimpregnado, material compuesto reforzado con fibras y proceso para la producción de un material de base de moldeo reforzado con fibras Download PDF

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ES2624694T3
ES2624694T3 ES08711788.3T ES08711788T ES2624694T3 ES 2624694 T3 ES2624694 T3 ES 2624694T3 ES 08711788 T ES08711788 T ES 08711788T ES 2624694 T3 ES2624694 T3 ES 2624694T3
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poly
fiber reinforced
molecular weight
molding
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Masato Honma
Shiro Honda
Shunsuke Horiuchi
Koji Yamauchi
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Toray Industries Inc
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Toray Industries Inc
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Priority claimed from JP2007072399A external-priority patent/JP5250986B2/ja
Priority claimed from JP2007074251A external-priority patent/JP5245266B2/ja
Priority claimed from JP2007074253A external-priority patent/JP5597908B2/ja
Priority claimed from JP2007074254A external-priority patent/JP5292711B2/ja
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    • C—CHEMISTRY; METALLURGY
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
    • 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
    • B29B15/00—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00
    • B29B15/08—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00 of reinforcements or fillers
    • B29B15/10—Coating or impregnating independently of the moulding or shaping step
    • B29B15/12—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length
    • 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
    • B29B11/00—Making preforms
    • B29B11/14—Making preforms characterised by structure or composition
    • B29B11/16—Making preforms characterised by structure or composition comprising fillers or reinforcement
    • 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
    • B29B15/00—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00
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    • B29B15/10—Coating or impregnating independently of the moulding or shaping step
    • B29B15/12—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length
    • B29B15/122—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length with a matrix in liquid form, e.g. as melt, solution or latex
    • B29B15/125—Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length with a matrix in liquid form, e.g. as melt, solution or latex by dipping
    • 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
    • B29B7/00—Mixing; Kneading
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/88—Adding charges, i.e. additives
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    • 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
    • B29B7/00—Mixing; Kneading
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/88—Adding charges, i.e. additives
    • B29B7/90—Fillers or reinforcements, e.g. fibres
    • 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
    • B29B9/00—Making granules
    • B29B9/12—Making granules characterised by structure or composition
    • B29B9/14—Making granules characterised by structure or composition fibre-reinforced
    • 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
    • B29C70/06—Fibrous reinforcements only
    • B29C70/08—Fibrous reinforcements only comprising combinations of different forms of fibrous reinforcements incorporated in matrix material, forming one or more layers, and with or without non-reinforced layers
    • B29C70/086—Fibrous reinforcements only comprising combinations of different forms of fibrous reinforcements incorporated in matrix material, forming one or more layers, and with or without non-reinforced layers and with one or more layers of pure plastics material, e.g. foam layers
    • 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
    • B29C70/06—Fibrous reinforcements only
    • B29C70/10—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres
    • B29C70/16—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of substantial or continuous length
    • B29C70/20—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of substantial or continuous length oriented in a single direction, e.g. roofing or other parallel fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • 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
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    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
    • C08J5/241—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using inorganic fibres
    • C08J5/243—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using inorganic fibres using carbon fibres
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08L81/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen or carbon only; Compositions of polysulfones; Compositions of derivatives of such polymers
    • C08L81/04—Polysulfides
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
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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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    • B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
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    • B29K2081/00—Use of polymers having sulfur, with or without nitrogen, oxygen or carbon only, in the main chain, as moulding material
    • B29K2081/04—Polysulfides, e.g. PPS, i.e. polyphenylene sulfide or derivatives thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
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    • C08J2381/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
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    • Y10T428/249921—Web or sheet containing structurally defined element or component
    • Y10T428/249924—Noninterengaged fiber-containing paper-free web or sheet which is not of specified porosity
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T428/2922—Nonlinear [e.g., crimped, coiled, etc.]
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Abstract

Un material de moldeo que comprende: (i) del 1 al 50 % en peso de un haz de fibras de refuerzo continuas (A); (ii) del 0,1 al 10 % en peso de un prepolímero de poli(sulfuro de arileno) (B) que comprende al menos el 50 % en peso de poli(sulfuro de arileno) cíclico y que tiene un peso molecular promedio en peso inferior a 10.000, o un poli(sulfuro de arileno) (B') que tiene un peso molecular promedio en peso de 10.000 o superior, estando el grado de dispersión representado por el peso molecular promedio en peso/peso molecular promedio en número de 2,5 o menor y obtenido calentando un prepolímero de poli(sulfuro de arileno) que comprende al menos el 50 % en peso de un poli(sulfuro de arileno) cíclico representado por la fórmula (a):**Fórmula** en la que Ar representa un grupo arileno y m es 2 a 50 y que tiene un peso molecular promedio en peso inferior a 10.000 y (iii) del 40 al 98,9 % en peso de resina termoplástica (C), en donde el componente (C) se adhiere a un material compuesto del componente (A) y de los componentes (B) o (B') y en el que: cuando (B) está presente, el peso molecular de la resina termoplástica (C) es 10.000 o superior y cuando (B') está presente y (C) es una resina de poli(sulfuro de fenileno), entonces (C) no es un componente (B').

Description

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Tabla 1
Ej. 1
Ej. 2 Ej. 3 Ej. comp. 1 Ej. 2
Composición
% en peso
Componente (A) fibra de carbono
% en peso 20 20 20 20 20
Componente (B) PAS
% en peso 5 5 5 - 30
Componente (C) resina termoplástica
Tipo PPS Nylon PBT PPS PPS
% en peso
75 75 75 80 50
(Condiciones de procesamiento)
Temperatura del recubridor Kiss
°C 230 230 230 - 230
Temperatura del cojinete
°C 230 230 230 - 230
Temperatura de extrusión
°C 320 280 260 320 320
Temperatura del moldeo por inyección
°C 350 300 280 - 350
Temperatura del molde
°C 140 90 80 - 140
(Propiedades de los productos moldeados)
Longitud media ponderada al número de fibras
mm 0,65 0,55 0,60 - 0,60
Longitud media ponderada al peso de la fibra
mm 1,10 1,00 1,05 - 0,95
Densidad
- 1,43 1,24 1,40 - 1,42
Módulo de flexión
Gpa 16 14 14 - 13
Resistencia a la flexión
Mpa 270 250 240 - 130
Impacto Izod
Jm 70 100 80 - 30
Evaluación del aspecto
○○ ○○ ○○ - ○
Los Ejemplos y Ejemplos Comparativos mostrados en la Tabla 1 demuestran lo siguiente. Los materiales de moldeo obtenidos en los Ejemplos 1 a 3 comprenden cantidades adecuadas de prepolímeros de poli(sulfuro de fenileno) (B) impregnados en el haz de fibras de refuerzo (A). Así, la manejabilidad de los materiales de moldeo, las propiedades dinámicas de los productos moldeados resultantes y su calidad de aspecto son aparentemente superiores a los de los Ejemplos Comparativos.
(Ejemplo 4)
El prepolímero de poli(sulfuro de fenileno) preparado en el Ejemplo de referencia 1 se funde en un baño de fusión en caliente a 240 °C y se alimenta a un recubridor Kiss utilizando una bomba de engranajes. El rodillo calentado a 230 °C se recubre con el prepolímero de poli(sulfuro de fenileno) del recubridor Kiss para formar una película.
Se dejó que la fibra de carbono Torayca® T700S-24K (Toray Industries, Inc.) pasara a través del rollo en contacto con la misma para adherir una cantidad dada de prepolímero de poli(sulfuro de fenileno) por unidad de longitud del haz de fibras de carbono.
La fibra de carbono a la que se ha adherido el prepolímero de poli(sulfuro de fenileno) se alimentó en el horno calentado a 350 °C, se dejó pasar a través de 10 rodillos (ϕ: 50 mm) dispuestos alternativamente por encima y por debajo de una línea que gira libremente con la ayuda de cojinetes y se dejó pasar a través de 10 barras de rodillos (ϕ: 200 mm) que se disponen en un estado de zigzag en el horno para permitir que el prepolímero de poli(sulfuro de fenileno) se impregne completamente en el haz de fibras de carbono para convertirlo en un polímero de poli(sulfuro de arileno) de alto peso molecular. Posteriormente, la hebra de fibra de carbono extraída del horno se enfrió mediante pulverización con aire y luego se enrolló mediante una bobinadora de tambor.
A partir del haz de fibras de carbono bobinado, se cortaron 10 hebras de 10 mm, las hebras se sometieron a reflujo en un extractor Soxhlet usando 1-cloronaftaleno a 210 °C durante 6 horas para separar la fibra de carbono del poli(sulfuro de arileno) y se determinó el peso molecular del poli(sulfuro de arileno) extraído. El peso molecular promedio en peso (Mw) del PPS obtenido fue de 26.800, el peso molecular promedio en número (Mn) del mismo fue de 14.100 y el grado de dispersión (Mw/Mn) fue de 1,90. Posteriormente, se midió la disminución del peso en el poli(sulfuro de arileno) extraído, △ Wr, y se encontró que era de 0,09 %.
Posteriormente, se fundió Ultem 1000R (resina PEI, temperatura de deflexión de carga: 200 °C, resina no cristalina, GE Plastics Japan Ltd.) a 360 °C usando un extrusor monoaxial y la masa fundida se extruyó en un cabezal de extrusión transversal montado en el extremo del extrusor. Simultáneamente, los hilos del haz de fibras de refuerzo continuas (A) y poli(sulfuro de arileno) (B’) se alimentaron continuamente en el cabezal de extrusión transversal para revestir el material compuesto del componente (A) y el componente (B') con el componente fundido (C). En este
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(4) Preparación de una placa laminada de materiales compuestos reforzados con fibras
Los preimpregnados unidireccionales preparados en (1) se laminaron hasta un grosor de 2 ± 0,4 mm y 3 ± 0,4 mm alineando la orientación de las fibras para cortar las piezas de ensayo usadas para la prueba de flexión definida por 5 JIS K 7074-1988 y en la prueba de cizallamiento entre capas definida por JIS K 7078-1991 y se obtuvo una placa laminada mediante calentamiento y presurización usando un molde de prensa a 350 °C y 3 MPa durante 30 minutos.
(5) Ensayo de resistencia a la flexión
10 Las piezas de ensayo se cortaron de la placa laminada preparada en (4) a los tamaños definidos por JIS K 70741988 designando el lado largo en una dirección del eje de la fibra y se llevó a cabo la prueba de resistencia a la flexión de tres puntos para determinar la resistencia a la flexión a 0 °C.
(6) Ensayo de resistencia al cizallamiento entre capas
15 Las piezas de ensayo se cortaron de la placa laminada preparada en (4) a los tamaños definidos por JIS K 70781991 designando el lado largo en una dirección del eje de la fibra y se llevó a cabo el ensayo de resistencia al cizallamiento entre capas para determinar la resistencia al cizallamiento entre capas.
20 Como se muestra en la Tabla 3, los preimpregnados obtenidos en los Ejemplos 6 a 8 son excelentes en términos de propiedades de impregnación. Los materiales compuestos reforzados con fibras preparados con el uso de los preimpregnados obtenidos en los Ejemplos 6 a 8 son excelentes en términos de resistencia y módulo de elasticidad, y particularmente en la resistencia al cizallamiento entre capas.
25 El preimpregnado del Ejemplo comparativo 5 preparado usando el prepolímero de poli(sulfuro de fenileno) 2 que tiene un contenido de poli(sulfuro de fenileno) cíclico fuera del intervalo descrito anteriormente, sin embargo, no presente problemas en términos de propiedades de impregnación, aunque la resistencia a la flexión y los módulos elásticos de cizalladura entre capas del material compuesto reforzado con fibras son bajos, como se muestra en la Tabla 3. En el caso del Ejemplo comparativo 6 usando un polímero de poli(sulfuro de fenileno) en lugar del
30 prepolímero de poli(sulfuro de fenileno), las propiedades de impregnación del preimpregnado son insuficientes, independientemente de las condiciones de alta temperatura y alta presión para la producción de preimpregnado. La resistencia a la flexión es también baja y la resistencia al cizallamiento de la capa intermedia es muy baja. En el caso del ejemplo comparativo 7 con un contenido de fibras reducido en peso usando el polímero de poli(sulfuro de fenileno), las propiedades de impregnación del preimpregnado se mejoran en comparación con las del Ejemplo
35 comparativo 6, aunque la resistencia a la flexión del material compuesto reforzado con fibras es muy baja y la resistencia al cizallamiento entre capas es también muy baja.
Tabla 3
Ej. 6
Ej. 7 Ej. 8 Ej. comp. 5 Ej. comp. 6 Ej. comp. 7
Prepolímero de poli(sulfuro de fenileno) 1 sintetizado en el Ej. de referencia 3
100 100 70 - - -
Prepolímero de poli(sulfuro de fenileno) 2 sintetizado en el Ej. de referencia 4
- - 30 100 - -
Poli(sulfuro de fenileno) sintetizado en el Ej. de referencia 2
- - - - 100 100
Relación entre el compuesto cíclico en el poli(sulfuro de fenileno) en peso (%)
90 90 75 40 0 0
Peso molecular promedio en peso del poli(sulfuro de fenileno)
900 900 1300 1500 20000 20000
Condiciones para la producción del preimpregnado
Temperatura de fusión de la resina (°C)
230 230 230 230 300 300
Temperatura de formación de la película (°C)
200 200 200 200 300 300
Temperatura de impregnación de la fibra (°C)
230 230 230 230 300 300
Presión del rodillo de impregnación de la fibra (MPa)
0,2 0,2 0,2 0,2 0,5 0,5
Propiedades del preimpregnado: contenido de fibra en peso (% en peso)
64 76 64 64 64 35
Propiedades del preimpregnado
Propiedades de impregnación
○ ○ ○ ○ × ∆
37
imagen35
imagen36
imagen37

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  1. imagen1
    imagen2
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CN102660118B (zh) 2015-04-29
TWI417179B (zh) 2013-12-01
KR101449232B1 (ko) 2014-10-08
EP3156439A3 (en) 2017-05-31
TW200906583A (en) 2009-02-16
US20100068518A1 (en) 2010-03-18
EP2138530A4 (en) 2013-10-30
CN101679654A (zh) 2010-03-24
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EP3156439A2 (en) 2017-04-19
CN101679654B (zh) 2012-07-18
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US7824770B2 (en) 2010-11-02
KR101438248B1 (ko) 2014-09-04
TW201406826A (zh) 2014-02-16
KR20090125828A (ko) 2009-12-07
EP3156439B1 (en) 2019-08-21
KR20130008651A (ko) 2013-01-22
EP2138530A1 (en) 2009-12-30
CN102660118A (zh) 2012-09-12

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