KR102009811B1 - Composite material preform board and method for preparing the same - Google Patents
Composite material preform board and method for preparing the same Download PDFInfo
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- KR102009811B1 KR102009811B1 KR1020150059561A KR20150059561A KR102009811B1 KR 102009811 B1 KR102009811 B1 KR 102009811B1 KR 1020150059561 A KR1020150059561 A KR 1020150059561A KR 20150059561 A KR20150059561 A KR 20150059561A KR 102009811 B1 KR102009811 B1 KR 102009811B1
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- preformed board
- composite preformed
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
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- 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
- B29C43/02—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles
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Abstract
First fibrous particles; Second fibrous particles; And a binder for binding the first fibrous particles and the second fibrous particles, wherein the first fibrous particles and the second fibrous particles are bound by the binder to form an irregular network structure including pores. The first fibrous particles are inorganic fibers or organic fibers, the second fibrous particles include a first thermoplastic resin, the binder includes a second thermoplastic resin, and the melting point of the first thermoplastic resin is the second. A composite preformed board is provided that is above the melting point of the thermoplastic resin and press molded to have an expansion ratio of 200 to 600% by volume relative to the initial volume upon standing at 140 ° C to 240 ° C for 0.5 to 10 minutes.
Description
It relates to a composite preformed board and a method of manufacturing the same.
Conventional thermoplastic composite materials are composed of reinforcing fibers such as glass fibers and carbon fibers exhibiting high rigidity and thermoplastic resins constituting a matrix. Since the thermoplastic composite material exhibits high mechanical properties compared to general thermoplastic materials, it is widely used as a vehicle and building material. In the conventional thermoplastic composite manufacturing method, the reinforcing fibers are mainly mixed with the thermoplastic resin, and then extruded to produce a final product through a mold press process. However, it is difficult to expect a uniform dispersion of the reinforcing fiber when manufacturing the product through extrusion, and it is difficult to manufacture a preformed board having a pore structure unless a foaming agent is used separately. Or, by using a dry needle punching process to prepare a reinforcing fiber sheet first, and to produce a composite material by impregnating the reinforcing fiber sheet in a resin. However, in this case, the agglomeration phenomenon of the reinforcing fiber occurs during the needle punching process, and the final composite material is difficult to have uniform mechanical properties, and the reinforcing fiber is fixed by needle punching when foaming for the manufacture of the preformed board. It has a low porosity structure.
One embodiment of the present invention provides a composite preformed board having excellent moldability while realizing uniform and excellent mechanical strength and light weight.
Another embodiment of the present invention provides a method of manufacturing the composite preformed board.
In one embodiment of the invention,
First fibrous particles; Second fibrous particles; And a binder for binding the first fibrous particles and the second fibrous particles,
The first fibrous particles and the second fibrous particles are bound by the binder to form an irregular network structure including pores,
The first fibrous particles are inorganic fibers or organic fibers,
The second fibrous particles include a first thermoplastic resin,
The binder includes a second thermoplastic resin,
The melting point of the first thermoplastic resin is higher than the melting point of the second thermoplastic resin,
Press-molded to have an expansion ratio of 200 to 600% by volume relative to the initial volume when left at 140 ° C to 240 ° C for 0.5 to 10 minutes.
Provides composite preformed boards.
In another embodiment of the invention,
Dispersing the reinforcing fibers and the bicomponent polymer fibers in an aqueous acid solution to prepare a slurry solution;
Forming a web from the slurry solution by a wet papermaking process; And
Heat treating and drying the formed web to prepare a composite sheet; And
Laminating at least two sheets of the composite sheet and then pressing molding the composite sheet to prepare a composite preformed board.
The reinforcing fibers are inorganic fibers or organic fibers,
The bicomponent polymer fiber includes a core part and a sheath part,
The core portion includes a first thermoplastic resin, the sheath portion includes a second thermoplastic resin,
The melting point of the first thermoplastic resin is higher than the melting point of the second thermoplastic resin.
Provided is a method of making a composite preformed board.
The composite preformed board is low in density while having high mechanical strength such as tensile, bending and impact strength uniformly, and has excellent sound absorbing and insulating performance and formability.
1 is a schematic diagram of a composite preformed board according to an embodiment of the present invention.
FIG. 2 illustrates that the composite preformed board is manufactured by applying heat and pressure to the reinforcing fibers and the bicomponent polymer by the method of manufacturing the composite preformed board.
3 is a view schematically showing a method of manufacturing a composite preformed board according to another embodiment of the present invention.
Figure 4 is a SEM photograph of the interior of the composite preformed board of Example 1 and Example 2.
FIG. 5 is an enlarged SEM photograph of a cross section of glass fibers in the cut surface of the composite preformed boards of Examples 1 and 2. FIG.
Hereinafter, embodiments of the present invention will be described in detail. However, this is presented as an example, by which the present invention is not limited and the present invention is defined only by the scope of the claims to be described later.
In one embodiment of the invention, the first fibrous particles; Second fibrous particles; And a binder for binding the first fibrous particles and the second fibrous particles, wherein the first fibrous particles and the second fibrous particles are bound by the binder to form an irregular network structure including pores. The first fibrous particles are inorganic fibers or organic fibers, the second fibrous particles include a first thermoplastic resin, the binder includes a second thermoplastic resin, and the melting point of the first thermoplastic resin is the second. Provided is a composite preformed board that is above the melting point of the thermoplastic resin and press molded to have an expansion ratio of from about 200 to about 600 volume percent relative to the initial volume upon standing at about 140 ° to about 240 ° C. for about 0.5 to about 10 minutes.
The first fibrous particles and the second fibrous particles are present in a state in which some or all of them are coated by the binder component. That is, the first fibrous particles and the second fibrous particles form a coating part formed of the binder on the surface of each particle.
The coating part of each of the first fibrous particles and the second fibrous particles may be fused to irregularly bind the first fibrous particles and the second fibrous particles. The first fibrous particles and the second fibrous particles bound in this way can form an irregular network structure including pores.
The composite preformed board is formed including a pore structure. Typically, the composite material produced by mixing and extruding raw materials is difficult to form a pore structure, while the composite preformed board forms a pore structure as manufactured by the method of manufacturing a composite preformed board described below. . Specifically, the composite preformed board may have a porosity of about 5 to about 80 volume percent, specifically, about 20 to about 60 volume percent.
1 is a schematic diagram of a composite preformed
The composite preformed board is press molded, manufactured to a predetermined level, and then expanded by a further molding process.
The composite preformed board may then be inflated and then implemented into a final product by mold molding. As such, when the final product is manufactured by expanding and molding the process through the steps of the composite preform board, the binder is more evenly distributed during the manufacture of the composite preform board. That is, the heat is transferred to the center of the composite preformed board so that the melt distribution of the binder can be evenly formed. As such, when the binder is evenly dispersed and then the composite preform board is expanded and molded again, the properties of the final product thus obtained can be obtained very evenly as a whole. On the contrary, if the mold is molded directly without passing through the composite preformed board, the binder may not be evenly distributed, thereby partially deteriorating physical properties in the molded final product.
The composite preformed board may be usefully applied as an intermediate material manufactured in such a compressed state, and the degree of compression may be prepared by press molding, as described above, from about 140 ° C to about 240 ° C, from about 0.5 minutes to about 10 minutes. May be at a level having an expansion ratio of about 200 to about 600 volume percent, specifically about 400 to about 600 volume percent, relative to the initial volume when left unattended.
Specifically, the composite preformed board may have a density of about 0.2 g / cm 3 to about 1.6 g / cm 3 . Since the density of the composite preformed board is manufactured so as to be within the above range, it is possible to implement better strength in a product realized by further molding. If the density of the composite preformed board is less than about 0.2 g / cm 3 , the heat transfer distribution (degree of melting) of the surface-center at the time of preheating the composite preformed board to produce the final product may cause deterioration of physical properties. When the density of the composite preformed board exceeds about 1.6 g / cm 3 , it means that it is formed by press molding at high pressure, and glass fiber may be broken during high pressure press molding operation, which may cause deterioration of physical properties. have.
The composite preformed board manufactured by compression as described above may have excellent dispersibility of fiber particles and may have excellent mechanical properties evenly throughout the composite preformed board. For example, the composite preformed board shows even better impact strength results even when the impact strength properties are evaluated at various points. Specifically, in the impact strength obtained by performing a dropping impact test according to ASTM D3763 on the composite preformed board, the difference between the maximum value and the minimum value of the impact strength obtained in one composite preformed board is about 0.2 J / It may be less than or equal to mm. In other words, this means that the composite preformed board may have a difference in impact strength according to ASTM D3763 measured at any two points in the composite preformed board up to about 0.2 J / mm or less.
Since the composite preformed board is a material that can realize high mechanical strength such as tensile strength, flexural strength, and impact strength and low weight due to low density, it can be usefully applied to the use of automobile and building materials requiring such characteristics. In addition, the composite preformed board can satisfy the excellent sound absorbing and insulating performance requirements required for such automotive and building materials.
In addition, the composite preformed board may be manufactured in a compressed state as described above, and thereafter, may be molded by expanding by an additional molding process such as lofting. In the composite preformed board, the binder binds the elastic fibrous particles, and when the temperature rises, the second thermoplastic resin of the binder softens or melts, resulting in relaxation of the binding force of the fibrous particles. While the composite preform board expands.
In the composite preformed board, the first fibrous particles and the second fibrous particles (conveniently, 'fibrous particles') are formulated by blending an appropriate content ratio of the second fibrous particles to an appropriate content of the first fibrous particles exhibiting excellent mechanical properties. By being entangled with each other, the proportion of the stressed fiber becomes higher, thereby contributing to the expansion. In addition, the presence of the second fibrous particles of the thermoplastic resin also contributes to the expansion expansion.
As such, the composite preformed board can exert excellent expandability in the further molding process and can be molded in various thicknesses during molding.
In order to maximize this expandability, a separate expanding agent may be added. As described above, since the composite preformed board is excellent in expandability, the composite preformed board can be molded by inflating to a predetermined level during molding in the future without including an expanding agent. Thus, the composite preform board may include an inflator for a particular purpose, but the composite preform board may not include an inflator.
The composite preformed board may be manufactured according to the method of manufacturing the composite preformed board, which will be described later, wherein the composite preformed board is prepared by dispersing the first fibrous particles and the second fibrous particles well.
As such, when the first fibrous particles and the second fibrous particles are well dispersed in the resin, the bonding force between the fiber and the resin is increased to improve the strength of the composite preformed board.
The composite preformed board obtains the effect of strength improvement by improving the dispersion of the fibrous particles based on the correlation between the dispersibility and the strength thus found.
As an example of a method of confirming that the dispersibility of the fibrous particles included in the composite preform board is improved, there is a method of evaluating the cross section of the composite preform board with a color difference meter. The better the dispersibility of the fibrous particles, the less the agglomerate, the more uniform the white color becomes. On the contrary, when the dispersibility of the fibrous particles is poor, the fibrous particles aggregate and overlap each other, so that these parts are darker. It will show color. This difference can be evaluated using a color difference meter. Even after the composite preformed board is expanded by applying heat, the dispersibility of the fibrous particles may be similarly evaluated using a color difference meter.
As an indirect method of confirming that the dispersibility of the fibrous particles included in the composite preformed board is improved, there is a method of comparing the strength. The improved dispersibility of the fibrous particles leads to the improvement of the strength of the composite preformed board, and thus other conditions such as the type and content of the first fibrous particles, the second fibrous particles, and the binder included in the composite preformed board. In order to ensure that only the dispersibility of the fibrous particles is changed, for example, the strength can be compared after the production by different manufacturing methods.
As the composite preformed board has excellent dispersibility of the first fibrous particles and the second fibrous particles, more excellent mechanical strength can be realized as described above, and thus the weight can be reduced.
The composite preformed board may also impart unidirectional orientation of the first fibrous particles and the second fibrous particles. The composite preformed board is first made of a composite sheet in which the first fibrous particles and the second fibrous particles are bound by the binder to form an irregular network structure including pores, and then laminated several composite sheets. The sheet may be manufactured by press molding, and when the fibrous particles are unidirectionally oriented in the composite sheet, the composite sheet has high mechanical properties along the direction in which the oriented is provided. The composite preformed board obtained by laminating such composite sheets and then press molding can withstand a large force in a specific direction.
The composite preformed board comprises two types of reinforcing fibers, first fibrous particles and second fibrous particles. The composite preformed board may include both the first fibrous particles and the second fibrous particles together, and may be designed such that predetermined characteristics are excellently expressed by controlling their type and content ratio.
For example, while using a material having a high tensile modulus such as glass fiber as the first fibrous particles, using thermoplastic fibers made of a thermoplastic resin as the second fibrous particles, the elasticity of the thermoplastic resin is further improved while further improving the strength. Can be given. Since the thermoplastic resin constituting the second fibrous particles uses a thermoplastic resin having a relatively high melting point, an additional strength improvement can be expected as compared with the case where only the first fibrous particles are present. In addition, since the thermoplastic fiber is superior in elasticity to the first fibrous particles, the impact energy can be effectively attenuated against the impact from the outside.
In addition, since the melting point of the first thermoplastic resin included in the binder is relatively low, the composite preformed board has low temperature moldability.
In one embodiment, the weight ratio of the sum of the content of the first fibrous particles to the content of the second fibrous particles and the binder in the composite preformed board is about 20:80 to about 60:40, specifically, about 30:70 to about 50 : Can be 50. As the content of the first fibrous particles increases, the strength tends to be excellent, but above a certain level, the degree of improvement may be lowered. The content range is a content range suitable for effectively securing the strength improving effect of increasing the content of the first fibrous particles and at the same time obtaining the effect from the second fibrous particles.
The second fibrous particles and the binder are attributable to the bicomponent polymer fibers according to the method for producing a composite preformed board described below. Therefore, in the method of manufacturing a composite preformed board to be described later, it is possible to manufacture a composite preformed board having the content ratio by adjusting the content of the first fibrous particles and the bicomponent polymer fibers in the above range.
In another embodiment, the composite preformed board may include about 50 parts by weight to about 250 parts by weight of the binder relative to 100 parts by weight of the second fibrous particles. By controlling the content ratio of the second fibrous particles and the binder in the content ratio, it is possible to maintain the excellent dispersibility while imparting the binding force and elasticity appropriately.
As described above, in the method of manufacturing a composite preformed board to be described later, the content ratio of the second fibrous particles and the binder is adjusted by adjusting the content ratio of the core part and the sheath part of the bicomponent polymer fiber. Can be implemented.
The first fibrous particles may include at least one selected from the group consisting of glass fibers, aramid fibers, carbon fibers, carbon nanotubes, boron fibers, metal fibers, and combinations thereof. Examples of the metal fiber include nickel fiber, iron fiber, stainless steel fiber, copper fiber, aluminum fiber, silver fiber, gold fiber.
Specifically, the first fibrous particles may have a cross-sectional diameter of about 5 μm to about 40 μm. The 1st fibrous particle which has the thickness of the said range can ensure an orientation and a dispersibility, even if it can provide strength suitably. The composite preformed board comprising the first fibrous particles having a thickness in the above range is resistant to external impact and is dispersed in an aqueous solution when the first fibrous particles are prepared in the aqueous solution according to the manufacturing method of the composite preformed board described below. It is possible to facilitate the formation of the composite sheet by having a proper entanglement (Hydroentangle property) at.
The first fibrous particles may have a length of about 1 mm to about 50 mm. The first fibrous particles having a length in the above range can be appropriately imparted strength, can secure orientation and dispersibility, and also impart appropriate bonding strength between the fibrous particles so that the composite preformed board has excellent strength. At the same time, if the fiber is too long, it is suitable for forming a composite sheet, preventing the fiber from being entangled and aggregated.
The first thermoplastic resin capable of forming the second fibrous particles may be, for example, polyester, polypropylene (PP), polyethylene (PE), acrylic butadiene styrene (ABS), polycarbonate (PC), nylon (Nylon). ), Polyvinyl chloride (PVC), polystyrene (PS), polyurethane (PU), polymethylmethacrylate (PMMA), polylactic acid (PLA), polytetrafluoroethylene and combinations thereof It may include at least one. The first thermoplastic resin capable of forming the second fibrous particles may be, for example, polypropylene or polyester.
The second thermoplastic resin capable of forming the binder is polyester, polyethylene, polypropylene, polyethylene (PE), acrylic butadiene styrene (ABS), polycarbonate (PC), nylon (Nylon), polyvinyl chloride (PVC) ), Polystyrene (PS), polyurethane (PU), polymethyl methacrylate (PMMA), polylactic acid (PLA), Teflon (polytetrafluoroethylene) and combinations thereof. .
As described above, when the first thermoplastic resin and the second thermoplastic resin are selected as in the above example, the melting point of the first thermoplastic resin must satisfy a condition higher than the melting point of the second thermoplastic resin.
Further, the first thermoplastic resin and the second thermoplastic resin can be selected so that the materials of the core part and the sheath part of the bicomponent polymer fibers used in the method for producing a composite preformed board described below satisfy the above conditions.
Specifically, the melting point of the first thermoplastic resin may be about 160 ° C or more. More specifically, the melting point of the first thermoplastic resin may be about 200 ℃ to about 400 ℃. By having a 1st thermoplastic resin have melting | fusing point of the said range, fibrous form can be maintained even after a binder melt | dissolves at the time of low temperature shaping | molding. If the melting point of the first thermoplastic resin is less than 160 ° C., the thermoforming temperature must be lowered too much to maintain the fibrous shape, or the composite preformed board including the same may cause thermal stability to deteriorate later, resulting in deformation of the dimension or polymer degradation. There is. In addition, it may be difficult to control the molding temperature because the temperature difference with the second thermoplastic resin can be reduced too much.
For example, the first thermoplastic resin may be polyester such as polyethylene terephthalate, polypropylene, or the like.
Specifically, the melting point of the second thermoplastic resin may be less than about 200 ℃. The binder serves to bind the first fibrous particles and the second fibrous particles, and when the second thermoplastic resin forming the binder has a melting point lower than that of the first thermoplastic resin, a material having a relatively low melting point is selected. Since it can be melted at a low temperature, low temperature moldability can be ensured. As the binder, for example, low melting point polyester, polypropylene, polyethylene, or the like can be used. Since low melting polyesters melt between about 100 ° C. and about 140 ° C., lower than ordinary polyesters, and polypropylene melts at about 160 ° C., low melting polyesters, specifically, depending on the molding temperature to be applied, Low melting point polyethylene terephthalate, polypropylene, polyethylene, etc. can be selected suitably.
In another embodiment, the specific gravity of the first thermoplastic resin is greater than about 1. According to the method of manufacturing a composite preformed board to be described later, the two-component polymer fibers are dispersed in an acid aqueous solution, it is easy to improve the dispersibility and form a network structure only by using a material having a specific gravity higher than 1 which is the specific gravity of water. Therefore, the core portion of the bicomponent polymer fiber may be a thermoplastic resin having a specific gravity higher than 1 such as polyester.
The second fibrous particles may have a cross-sectional diameter of about 5 μm to about 30 μm. The second fibrous particles having a thickness in the above range can secure the orientation and dispersibility while providing strength appropriately. The composite preformed board comprising the second fibrous particles having a thickness in the above range has excellent strength characteristics, and when the first fibrous particles are dispersed in an aqueous solution during preparation according to the method for preparing the composite preformed board described below, It is possible to facilitate the formation of the composite sheet by having a proper entanglement (Hydroentangle property) within.
The second fibrous particles may have a length of about 1 mm to about 50 mm. The second fibrous particles having a length in the above range can be appropriately imparted strength, can secure orientation and dispersibility, and also impart appropriate bonding strength between the fibrous particles so that the composite preformed board has excellent strength. At the same time, if the fiber is too long, the fiber is entangled to form a rope phase, which prevents the dispersibility from deteriorating and is suitable for forming the composite sheet.
When the composite preformed board is expanded by an additional molding process, the porosity increases as the pores included are increased.
In another embodiment, the composite preformed board can be expanded by a further molding process so that the porosity at about 200 to about 600 volume percent expansion can be from about 50 to about 90 volume percent.
The composite preformed board forms open pores while forming a network structure. The composite preformed board may have a porosity in the range when inflated, thereby realizing weight reduction while maintaining strength, and having excellent sound absorbing and insulating performance.
Sound waves coming through the open pores of the expanded composite preformed board is attenuated by the vibrations of the fibers of the second fibrous particles, so that the sound absorbing and insulating material can be applied. The higher the porosity of the expanded composite preformed board, the higher the content of the second fibrous particles, and the longer the passage of sound waves, the better the energy attenuation effect. The length of the passage of sound waves is, for example, even if they have the same porosity, the length of the material itself is large, or when the connectivity of the pores is good. The expanded composite preformed board has a certain degree of porosity, while controlling the content of the second fibrous particles, and also by controlling the length of the passage of the sound wave is useful as a material having improved sound absorbing and insulating performance Can be applied. In particular, since the second fibrous particles are softer than the hard first fibrous particles, the second fibrous particles have a high sound energy attenuation effect, and thus act effectively on the sound absorbing and insulating performance.
The composite preformed board may have a density of about 0.2 g / cm 3 to about 1.6 g / cm 3 , and the light weight may be realized when inflated, as described above. Specifically, the density of the composite preformed board may be about 0.1 g / cm 3. To about 1.6 g / cm 3 .
The composite preformed board may be manufactured in a form suitable for the intended use, for example, may be made of a composite sheet.
The composite preformed board may be manufactured to have a weight suitable for the application to be applied, and may, for example, have a weight of about 600 g / m 2 to about 3000 g / m 2 .
In another embodiment, the composite preform board can have a thickness of about 0.5 mm to about 10 mm.
In another embodiment of the invention,
Dispersing the reinforcing fibers and the bicomponent polymer fibers in an aqueous acid solution to prepare a slurry solution;
Forming a web from the slurry solution by a wet papermaking process; And
Heat treating and drying the formed web to prepare a composite sheet; And
Stacking at least two sheets of the composite sheet and then pressing molding the composite sheet to prepare a composite preformed board;
It provides a method for producing a composite preformed board comprising a.
The composite preformed board described above may be manufactured by the method of manufacturing the composite preformed board.
FIG. 2 shows that the
The reinforcing
The
The melting point of the first thermoplastic resin is higher than the melting point of the second thermoplastic resin.
Detailed description of the first thermoplastic resin and the second thermoplastic resin is as described above.
In the heat treatment and drying step, the second thermoplastic resin of the sheath portion is melted to bind the reinforcing fibers and the bicomponent polymer fibers by heat fusion, thereby forming an irregular mesh structure including pores.
The second thermoplastic resin of the sheath part is present in the state in which the core part is coated and then transferred to the reinforcing fiber while being melted in the heat treatment and drying step to coat some or all of the reinforcing fiber, and the bicomponent fiber is solidified in the molten state It acts as a binder for binding the core portion and the reinforcing fiber.
As such, since the sheath portion acts as a binder, the method of manufacturing the composite preformed board may not additionally use a separate binder.
The thermoplastic resin forming the sheath portion of the bicomponent polymer fiber has a relatively low melting point, which is advantageous in that low temperature molding is possible.
The porosity of the composite preformed board during expansion, the degree of coating transferred to the reinforcing fibers, and the like can be controlled by changing the core and sheath portions of the bicomponent polymer fibers.
For example, the bicomponent polymer fiber may have a weight of about 50 parts by weight to about 250 parts by weight based on 100 parts by weight of the core part.
Although the composite preformed board is manufactured by dispersing bicomponent polymer fibers made of chemically hydrophobic thermoplastic resin in an aqueous acid solution, the bicomponent polymer fibers are composed of a core part and a sheath part, By increasing specific gravity, dispersibility can be excellent. As described above, when the specific gravity of the core part of the bicomponent polymer fiber is greater than 1, the dispersion degree can be effectively improved during the stirring process in the aqueous solution.
The reinforcing fibers and the bicomponent polymer fibers can further improve the dispersibility in the aqueous acid solution by using the surface-treated sheath portion, and as a result, can produce a composite preformed board with better dispersibility. have.
Surface treatment of the sheath portion of the reinforcing fibers and the bicomponent polymer fibers may introduce functional groups such as a fluoro group, a hydroxy group, a carboxyl group, an alkyl group, or may be coated with a coating agent. For example, in the production of reinforcing fibers and bicomponent fiber polymer fibers, the reinforcing fibers may interact with the surface or the surface of the sheath portion of the bicomponent fiber polymer fibers by a dipping process to introduce a surface treatment agent and a fiber which may introduce the functional group. Can be prepared by reaction.
Specifically, by the silane treatment of the reinforcing fibers or bicomponent polymer fibers with a surface treatment agent or coating agent that can be used in the production of the reinforcing fibers and the bicomponent polymer fibers to improve the bond strength between the fibers, or carbonization (carbonization) to improve heat resistance Or hydrolysis to improve hydrophilicity, or oxidation to improve aqueous dispersibility.
Examples of the surface treatment agent include fluorine waxes (for example, PFAO), hydrocarbon waxes, and silicone polymers.
The coating agent is capable of imparting properties such as hydrophilicity / hydrophobicity, water repellency, flame retardancy, nonflammability, heat resistance, acid resistance, alkali resistance, durability, and stain resistance. Specifically, a water repellent such as a fluorine wax (for example, PFAO), a hydrocarbon wax, and a silicone polymer compatibilizer may be used as the coating agent.
Depending on the desired physical properties of the composite preformed board to be produced, it is possible to adjust the content ratio of the reinforcing fibers and the bicomponent polymer fibers.
For example, the weight ratio of the reinforcing fibers and the bicomponent polymer fibers may be about 20:80 to about 60:40, specifically, about 30:70 to about 50:50.
Specifically, in the method of manufacturing the composite preformed board, the total amount of the reinforcing fibers and the bicomponent polymer fibers per 1 L of the acid aqueous solution may be mixed in an amount of about 0.1 g to about 10 g. By controlling the total amount of fibers of the reinforcing fibers and the bicomponent polymer fibers in the content of the above range, to maintain a good dispersibility to produce a composite sheet of uniform thickness, and laminated a plurality of composite sheets as a board of uniform thickness It can be produced, it is possible to secure the physical properties due to excellent dispersibility.
The pH of the aqueous acid solution may be about 1 to about 4. By adjusting the pH of the aqueous acid solution to the above range, the charge on the surface of the glass fiber while preventing the glass fiber constituent silica (SiO 2 ), alumina (Al 2 O 3 ), boron (B 2 O 5 ) chemically decomposed to the strong acid May occur to further improve dispersibility.
The method of manufacturing the composite preformed board may further include stirring the slurry solution. Dispersibility may be further improved by further performing the step of stirring the slurry solution.
In the method of manufacturing the composite preformed board, the heat treatment and drying of the formed web may be performed at about 100 to about 180 ° C. The temperature range is defined based on the temperature at which the sheath portion of the bicomponent fiber begins to soften or melt. When the temperature is lower than 100 ° C, it is difficult to dry moisture, and softening of the bicomponent polymer fibers (sheath portion) is not sufficiently generated, so that moisture remains after drying in the shape of the composite sheet, or the composite sheet is hard to have a fixed property. . On the contrary, when the temperature is higher than 180 ° C., the sheath portion of the bicomponent polymer fiber is completely melted, so that it is difficult to uniformly transition from the bicomponent fiber to the reinforcing fiber. In addition, there is a fear that alteration of the sheath polymer of the bicomponent polymer fibers occurs at or above the melting temperature.
By appropriately arranging the core cross-sectional diameter of the bicomponent polymer fiber, and heat-treating and drying at an appropriate heat treatment temperature, the core of the bicomponent polymer fiber can be prepared to be included in a composite preformed board made of fibrous particles without melting.
During the wet papermaking process, the fibers are evenly mixed in the aqueous solution of the slurry, followed by a mesh moving along the conveyor belt to form a wet-entangled web. By providing, the composite sheet manufactured can be made to have orientation. Thus, the composite preformed board obtained by laminating the composite sheet provided with the orientation can be further strengthened in one direction by providing the fiber component with the orientation in one direction.
For example, as the content of the second fibrous particles increases, it may be disadvantageous in terms of dimensional stability, and orientation may be imparted to reinforce it.
As such, the composite preformed board may be manufactured so as to be selectively oriented according to the intended use.
For example, when the fiber is transferred from the head box to the conveyor belt and forms a composite sheet, the fiber is inclined relative to the planar conveyor belt by inclining the portion where the composite sheet is formed (inclined web formation). The process can be designed to lie down in the machine direction. Directionality can be given separately in the machine direction (MD) direction and the cross direction (CD) direction, it is easier to give the direction in the MD direction than the CD direction.
The slurry solution may further include an additive such as a crosslinking agent or an additional binder.
The crosslinking agent serves to strengthen the chemical bonding strength between the reinforcing fibers and the bicomponent polymer fibers, and for example, a silane compound, a maleic acid compound, or the like can be used.
The content of the crosslinking agent may be about 0 to about 5 parts by weight relative to 100 parts by weight of the total fibers (sum of reinforced fibers and bicomponent polymer fibers).
The additional binder may be a water-soluble polymer such as starch, casein, polyvinyl alcohol (PVA), carboxymethyl cellulose (CMC); Emulsions such as polyethylene, polypropylene and polyamide; Cement, calcium sulfate type clay, sodium silicate, alumina silicate, an inorganic compound of calcium silicate, etc. can be used.
The content of the additional binder may be about 0 to about 5 parts by weight relative to 100 parts by weight of the total fibers (sum of the reinforced fibers and the bicomponent polymer fibers).
The composite sheet formed through the web from the slurry solution has a low thickness variation in the composite sheet if the dispersibility of the fibrous particles is good. The better the dispersibility of the fibrous particles, the less the agglomeration of the fibrous particles, and conversely, when the dispersibility of the fibrous particles is poor, the fibrous particles are agglomerated. When the fibrous particles aggregate, the thickness of the composite sheet corresponding to the portion increases. Therefore, the composite sheet having excellent dispersibility of fibrous particles has a constant thickness. That is, the thickness variation in the composite sheet having excellent dispersibility of the fibrous particles becomes low.
In one embodiment, the composite sheet may have a thickness variation of about 2 mm or less in the composite sheet.
In another embodiment, the composite sheet may have a thickness variation of about 0.3 mm or less in the composite sheet.
The 'thickness variation in the composite sheet' means a difference between the maximum thickness and the minimum thickness of one composite sheet.
The composite preformed board is formed by compressing at least two or more sheets of composite sheets, and in particular, it is possible to determine how many sheets to stack according to the desired weight per unit area of the final product. For example, if the weight per unit area of the target product of the composite sheet is 1200g / m 2 , approximately two to twelve sheets are laminated, then heat press molding by applying heat and pressure can be prepared a composite preformed board. .
The hot press molding may be performed at a temperature at which the sheath portion of the bicomponent fiber can be melted while the core portion is not melted. In this temperature range, the interface between the composite sheets may be fused while the sheath is melted.
In detail, the hot press molding may be performed by applying a pressure of about 1 to about 30 bar at a temperature of about 100 to about 180 ° C. to produce a composite preform board by laminating the composite sheet.
The hot press molding may be performed so that the composite preform board can be continuously manufactured by double belt press molding.
According to another embodiment the composite preformed board can be prepared as follows. First, after blending the reinforcing fibers and the bicomponent polymer fibers, the blended fibers are stirred in an aqueous solution containing an additive, and then transferred to a head box capable of forming a web. The slurry in the head box passes through the vacuum intake system to form a wet web, which is made into a composite sheet in sheet form while passing through the dryer. The weight of the composite sheet is to be about 50g to about 600g per square meter to facilitate later thermoforming. The drying temperature is set to about 100 ° C. to about 180 ° C. depending on the sheath part material so that the sheath part of the bicomponent polymer fibers can act as a binder. The manufactured mat-shaped composite material is cut out and laminated according to the use, and then manufactured by using a thermocompression press to prepare a composite preformed board having a thickness of about 0.5 mm to about 10 mm.
When forming a composite preformed board, the temperature can be formed at a lower temperature than the bicomponent polymer fiber composed of a polypropylene sheath when using a bicomponent fiber composed of a low melting polyester sheath. The composite preformed board manufactured as described above may be manufactured into a desired molded article through an additional molding process. For example, an additional sheet of material suitable for the application to be applied to the upper and lower portions of the composite preform board may be further laminated and laminated, and further heated to expand the composite preform board and then molding By molding, a molded article having a final desired shape can be produced. Specifically, the outer layer of the PET chemical nonwoven fabric, spun bonding nonwoven fabric, hot air bonding nonwoven fabric and the like further laminated on the upper and lower portions of the composite preformed board as an additional sheet, and the laminated composite sheet is heated in an infrared oven to preheat the composite After inflating the molding board, it is transferred to a press at room temperature, and then pressurized to produce a vehicle undercover.
3 is a view schematically showing a method for manufacturing a composite preformed board according to the embodiment.
Hereinafter, examples and comparative examples of the present invention are described. Such following examples are only examples of the present invention, and the present invention is not limited to the following examples.
( Example )
Example One
The bicomponent polymer fiber has a polyester core portion and a low melting polyester sheath portion having a weight ratio of 50:50, and has a length of 5 mm and a thickness of 4 deniers (about 20 μm cross-sectional diameter) for securing aqueous dispersion. Was prepared. Glass fibers were prepared by cutting 13 mm long glass fibers with a cross-sectional diameter of 13 μm coated to be suitable for aqueous dispersion. 40 parts by weight of the glass fiber and 60 parts by weight of the bicomponent polymer fiber were combined, and the mixture was stirred for 1 hour in an aqueous solution adjusted to
Example 2
Instead of using the glass fiber used in Example 1, the composite sheet was prepared in the same manner as in Example 1, except that the glass fiber with a special silane coating on the surface was used to improve the bonding strength with the polyester resin, Subsequently, the composite preformed board was molded in the same manner as in Example 1, which was then expanded again by preheating at 200 ° C. for 2 minutes in an IR oven, transferred to a press at room temperature, and then pressurized to an average of 2.0. The final mold molded product formed to mm thickness was completed.
Example 3
A composite sheet was prepared in the same manner as in Example 2, except that 10 parts by weight of glass fibers with a special silane coating on the surface used in Example 2 and 90 parts by weight of the bicomponent polymer fibers were prepared. After molding the composite preformed board in the same manner as in Example 2, it was again expanded in an IR oven by preheating at 200 ° C. for 2 minutes, transferred to a press at room temperature, and then pressed under pressure to average 2.0 mm thick. The final mold molded product formed into a finished product was completed.
Example 4
A composite sheet was prepared in the same manner as in Example 2, except that 90 parts by weight of the glass fiber treated with silane coating and 10 parts by weight of the bicomponent polymer fiber were specially coated on the surface used in Example 2. After molding the composite preformed board in the same manner as in Example 2, it was again expanded in an IR oven by preheating at 200 ° C. for 2 minutes, transferred to a press at room temperature, and then pressed under pressure to average 2.0 mm thick. The final mold molded product formed into a finished product was completed.
Example 5
The bicomponent polymer fiber has a polyester core portion and a low melting polyester sheath portion having a weight ratio of 50:50, and has a length of 5 mm and a thickness of 4 deniers (about 20 μm cross-sectional diameter) for securing aqueous dispersion. Was prepared. Glass fibers were prepared by cutting 13 mm long glass fibers with a cross-sectional diameter of 13 μm coated to be suitable for aqueous dispersion. 40 parts by weight of the glass fiber and 60 parts by weight of the bicomponent polymer fiber were combined, and the mixture was stirred for 1 hour in an aqueous solution adjusted to
Example 6
A composite sheet was prepared in the same manner as in Example 5, except that instead of the glass fiber used in Example 5, the glass fiber coated with the silane coating was used on the surface used in Example 2, and then Example 5 After molding the composite preformed board in the same way as in the above, it was again expanded by preheating for 2 minutes at 200 ° C. in the IR oven, transferred to a press at room temperature, and then pressurized to a final thickness of 2.5 mm on average. The molded product was completed.
Example 7
A composite sheet was prepared in the same manner as in Example 6, except that 10 parts by weight of glass fibers with a special silane coating and 90 parts by weight of the bicomponent polymer fibers were blended on the surface used in Example 6. After molding the composite preformed board in the same manner as in Example 6, it was again expanded by preheating at 200 ° C. for 2 minutes in an IR oven, transferred to a press at room temperature, and pressed under pressure to average 2.5 mm thick. The final mold molded product formed into a finished product was completed.
Example 8
A composite sheet was prepared in the same manner as in Example 6, except that 90 parts by weight of glass fibers with a special silane coating and 10 parts by weight of the bicomponent polymer fibers were blended on the surface used in Example 6. After molding the composite preformed board in the same manner as in Example 6, it was again expanded by preheating at 200 ° C. for 2 minutes in an IR oven, transferred to a press at room temperature, and pressed under pressure to average 2.5 mm thick. The final mold molded product formed into a finished product was completed.
Comparative example One
The glass fiber was prepared by cutting a 13 μm glass fiber 13 μm coated so as to be suitable for aqueous dispersion. 40 parts by weight of the glass fiber and 5 parts in length and 60 parts by weight of polypropylene fiber having a thickness of 4 denier (about 20 μm cross-sectional diameter) were mixed and stirred for 1 hour in an aqueous solution adjusted to
Comparative example 2
A composite sheet was prepared in the same manner as in Comparative Example 1, except that instead of the glass fiber used in Comparative Example 1, the surface used in Example 2 used a silane-coated glass fiber with a special silane coating, and then After molding the composite preformed board in the same manner as in Comparative Example 1, it was again expanded in a IR oven by preheating at 200 ° C. for 2 minutes, transferred to a press at room temperature, and applied under pressure to average 2.0 mm. The final mold molded product formed to a thickness was completed.
Comparative example 3
40 parts by weight of glass fiber used in Comparative Example 1 and 60 parts by weight of polypropylene fiber were mixed, and the composite sheet was prepared at 600 g / m 2 using a dry needle punching process, followed by laminating two composite sheets to 170 ° C. and 1 bar. The mold was molded by a hot press process at to obtain a final mold-formed product formed on average 2.0 mm thick.
Comparative example 4
The glass fiber was prepared by cutting a 13 μm glass fiber 13 μm coated so as to be suitable for aqueous dispersion. 40 parts by weight of the glass fiber and 5 parts in length and 60 parts by weight of polypropylene fiber having a thickness of 4 denier (about 20 μm cross-sectional diameter) were mixed and stirred for 1 hour in an aqueous solution adjusted to
Comparative example 5
A composite sheet was prepared in the same manner as in Comparative Example 4, except that instead of the glass fiber used in Comparative Example 4, the surface used in Example 2 used a silane-coated glass fiber with a special silane coating, and then After molding the composite preformed board in the same manner as in Comparative Example 4, it was again expanded in a IR oven by preheating at 200 ° C. for 2 minutes, transferred to a press at room temperature, and applied under pressure to average 2.5 mm. The final mold molded product formed to a thickness was completed.
Comparative example 6
40 parts by weight of glass fiber and 60 parts by weight of polypropylene fiber used in Comparative Example 4 were combined, and the composite sheet was prepared at 600 g / m 2 using a dry needle punching process, followed by laminating two composite sheets to 170 ° C. and 1 bar. The mold was molded by a hot press process at to obtain a final mold-formed product formed to an average thickness of 2.5 mm.
evaluation
Experimental Example One
The mechanical properties of tensile strength, tensile modulus, flexural strength and flexural modulus were compared for the final mold-formed products prepared in Examples 1-8 and Comparative Examples 1-8. Tensile strength and flexural strength were measured after leaving the final mold-formed product prepared in Example 1-4 and Comparative Example 1-4, respectively, at room temperature for 24 hours.
Tensile strength and tensile modulus were measured according to ASTM D638 for samples where the final molded article had a thickness of 2 mm, and flexural strength and flexural modulus were determined according to ASTM D790 for samples where the final molded article had 2.5 mm thickness. Measured by. The results are shown in Table 1 and Table 2.
Although the content of the glass fiber of Example 4 is higher than the content of the glass fiber of Example 2, it was confirmed that the tensile strength of Example 2 is the highest. Tensile modulus should be higher as the content increases due to the higher tensile modulus value of the glass fiber itself, but Example 2 is higher than Example 4. From this, an increase in the content of the glass fiber contributes to the strength improvement, but since the above does not bring any more strength improvement over a certain content, the optimum content that brings the maximum mechanical properties may be the level of the glass fiber content of Example 2 It can be seen.
Experimental Example 2
Samples of the composite preformed boards prepared in Example 1 and Comparative Example 1 and samples of the final mold molded product of Comparative Example 3 were prepared. Impact strength was measured at five randomly selected points in each sample.
The impact strength evaluation method is an evaluation on the impact energy absorbing ability, in which a composite preformed board (Example 1 and Comparative Example 1) or a final molded article (Comparative Example 3) of each sample is left at room temperature for 24 hours before falling. Shock test was conducted. Dropping impact test was measured based on ASTM D3763 at room temperature.
The results are shown in Table 3.
[Total NTT (J / mm)]
Example 1 shows the impact strength results for any five points evenly, whereas Comparative Example 1 shows a difference in the impact strength results for any five points. From this, it can be seen that Example 1 has excellent dispersion of the fibrous particles and excellent physical properties of the composite preformed board as a whole, while Comparative Example 1 shows excellent impact strength at the point where the fibrous particles are aggregated, The impact strength is expected to drop at the point where the density is expected to be lower.
Experimental Example 3
The composite preformed boards prepared in Example 1 and Comparative Example 1 and the final mold-formed product of Comparative Example 3 were left inflated for 2 minutes at a temperature of 200 ° C., and then the thickness of the expanded composite preformed boards was measured. The results are shown in Table 4.
After preheating of Example 1 it can be seen that the expansion rate is higher than Comparative Example 1. This means that after thermoforming, the highly elastic polyester fibers constituting the material exhibit additional spring-back effects after preheating. By improving the expandability, it has been confirmed that when molding through a mold press, it is possible to manufacture a product having a relatively thick molding thickness.
4 is a SEM photograph inside the plate of Comparative Example 1 (left photograph) and Example 1 (right photograph). In Example 1, while the core portion of the bicomponent polymer fibers together with the glass fibers retained the fibrous particles, in Comparative Example 1 it can be seen that the propylene fibrous phase did not maintain the form of the fibers. In Example 1, since the core part of the bicomponent polymer fiber retained the fibrous shape, it was confirmed that the content of the fibrous particles in the material was higher than that of Comparative Example 1 even after thermoforming.
5 is an enlarged SEM photograph of the cross section of the glass fiber at the fracture surface (after the tensile test) of the plate of Example 1 (left photograph) and Example 2 (right photograph).
In Example 2, glass fiber surface-treated with a silane-based compound was used to improve the chemical affinity with the polymer to improve the binding force, and as shown in FIG. 4, the chemical bond between the glass fiber and the polymer was improved after molding. It was. Example 2 can confirm that the resin (resin material of the sheath portion of the bicomponent polymer fiber) is cluttered on the surface of the reinforcing fiber (glass fiber) after fracture, compared to Example 1, which is a reinforcing fiber (glass fiber) and resin Is because they are chemically bound. As such, when the reinforcing fibers and the resin are chemically bonded, the phenomenon in which defects occur while the reinforcing fibers are separated (pulled out) from the resin when broken can be minimized. As a result, the tensile strength can be improved as compared with the case of the first embodiment.
Although the preferred embodiments of the present invention have been described in detail above, the scope of the present invention is not limited thereto, and various modifications and improvements of those skilled in the art using the basic concepts of the present invention defined in the following claims are also provided. It belongs to the scope of the invention.
1: first fibrous particles
2: second fibrous particles
3: binder
4: reinforced fiber
5: two-component polymer fiber
5a: core part
5b: sheath
10, 20: composite preformed board
Claims (28)
The first fibrous particles and the second fibrous particles are bound by the binder to form an irregular network structure including pores,
The first fibrous particles are glass fibers,
The second fibrous particles include a first thermoplastic resin, the first thermoplastic resin is a polyester resin, and the specific gravity of the first thermoplastic resin is greater than 1,
The binder includes a second thermoplastic resin,
The melting point of the first thermoplastic resin is higher than the melting point of the second thermoplastic resin,
The weight ratio of the sum of the content of the first fibrous particles to the content of the second fibrous particles and the binder is 30:70 to 50:50,
Press-molded to have an expansion ratio of 200 to 600% by volume relative to the initial volume when left at 140 ° C to 240 ° C for 0.5 to 10 minutes,
Density is 0.2 g / cm 3 to 1.6 g / cm 3 ,
The composite preformed board has a porosity of 20 to 60% by volume, and a porosity of 50 to 90% by volume upon expansion of 200 to 600% by volume.
Composite preformed board.
The first fibrous particles and the second fibrous particles are partially or entirely coated on the surface of each particle by the binder to form a coating part, and the coating parts formed on the respective surfaces are fused and bound to each other.
Composite preformed board.
The composite preformed board has a difference in impact strength of 0.2 J / mm or less according to ASTM D3763 measured at any two points within the composite preformed board.
Composite preformed board.
The binder has a weight of 50 parts by weight to 250 parts by weight with respect to 100 parts by weight of the second fibrous particles.
Composite preformed board.
The first fibrous particles and the second fibrous particles have a unidirectional orientation.
Composite preformed board.
The first fibrous particles have a cross-sectional diameter of 5 μm to 40 μm
Composite preformed board.
The first fibrous particles are 1 mm to 50 mm in length
Composite preformed board.
Melting | fusing point of the said 1st thermoplastic resin is 160 degreeC or more
Composite preformed board.
Melting point of the second thermoplastic resin is less than 200 ℃
Composite preformed board.
The second fibrous particles have a cross-sectional diameter of 5 μm to 30 μm
Composite preformed board.
The second fibrous particles are 1 mm to 50 mm in length
Composite preformed board.
The composite preformed board has a weight of 600 g / m 2 to 3000 g / m 2
Composite preformed board.
The composite preformed board has a thickness of 0.5 mm to 10 mm
Composite preformed board.
Forming a web from the slurry solution by a wet papermaking process; And
Heat treating and drying the formed web to prepare a composite sheet; And
Laminating at least two sheets of the composite sheet and then pressing molding the composite sheet to prepare a composite preformed board.
The reinforcing fibers are glass fibers,
The bicomponent polymer fiber includes a core part and a sheath part, the specific gravity of the core part of the bicomponent polymer fiber is greater than 1,
The core portion includes a first thermoplastic resin, the sheath portion includes a second thermoplastic resin,
The melting point of the first thermoplastic resin is higher than the melting point of the second thermoplastic resin,
The first thermoplastic resin is a polyester resin,
The weight ratio of the reinforcing fibers and the bicomponent polymer fibers is 30:70 to 50:50,
The composite preformed board has a density of 0.2 g / cm 3 to 1.6 g / cm 3 ,
The composite preformed board has a porosity of 20 to 60% by volume, a porosity of 50 to 90% by volume upon expansion of 200 to 600% by volume,
PH of the acid aqueous solution is 1 to 4
Method for manufacturing composite preformed board.
Mixing so that the total content of the reinforcing fibers and the bicomponent polymer fibers per 1 L of the acid aqueous solution is 0.1 g to 10 g
Method for manufacturing composite preformed board.
Heat-treating and drying the formed web is carried out at 100 to 180 ℃
Method for manufacturing composite preformed board.
The composite sheet has a thickness variation of 2 mm or less in the composite sheet.
Method for manufacturing composite preformed board.
The press molding is a laminate of the composite sheet by applying a pressure of 1 to 30bar at a temperature of 100 to 180 ℃ to prepare a composite preformed board
Method for manufacturing composite preformed board.
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| WO1994015197A1 (en) * | 1992-12-22 | 1994-07-07 | E.I. Du Pont De Nemours And Company | Method for determining quality of dispersion of glass fibers in a thermoplastic resin preform layer and a preform layer characterized thereby |
| JP2002096413A (en) * | 2000-09-21 | 2002-04-02 | Toray Ind Inc | Composite reinforced fiber base material and preform |
| JP2011102453A (en) | 2009-11-11 | 2011-05-26 | Oji Tokushushi Kk | Nonwoven fabric for reinforcing frp |
| JP2011144473A (en) * | 2010-01-14 | 2011-07-28 | Mitsubishi Plastics Inc | Carbon fiber/thermoplastic resin composite material, method for producing the same and electric field-shielding material |
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| JPH01318045A (en) * | 1988-05-10 | 1989-12-22 | E I Du Pont De Nemours & Co | Composite material composed of wet molding mixture of glass fiber and thermoplastic fiber |
| JPH0664075A (en) * | 1992-08-12 | 1994-03-08 | Sumitomo Chem Co Ltd | Sheet, manufacture therefor and manufacture for fiber reinforced composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1994015197A1 (en) * | 1992-12-22 | 1994-07-07 | E.I. Du Pont De Nemours And Company | Method for determining quality of dispersion of glass fibers in a thermoplastic resin preform layer and a preform layer characterized thereby |
| JP2002096413A (en) * | 2000-09-21 | 2002-04-02 | Toray Ind Inc | Composite reinforced fiber base material and preform |
| JP2011102453A (en) | 2009-11-11 | 2011-05-26 | Oji Tokushushi Kk | Nonwoven fabric for reinforcing frp |
| JP2011144473A (en) * | 2010-01-14 | 2011-07-28 | Mitsubishi Plastics Inc | Carbon fiber/thermoplastic resin composite material, method for producing the same and electric field-shielding material |
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