WO2022024773A1 - シートモールディングコンパウンド及び成形品の製造方法 - Google Patents

シートモールディングコンパウンド及び成形品の製造方法 Download PDF

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Publication number
WO2022024773A1
WO2022024773A1 PCT/JP2021/026545 JP2021026545W WO2022024773A1 WO 2022024773 A1 WO2022024773 A1 WO 2022024773A1 JP 2021026545 W JP2021026545 W JP 2021026545W WO 2022024773 A1 WO2022024773 A1 WO 2022024773A1
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WO
WIPO (PCT)
Prior art keywords
carbon fiber
resin
smc
molding compound
sheet molding
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2021/026545
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English (en)
French (fr)
Japanese (ja)
Inventor
泰之 村中
一迅 人見
大介 西川
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
DIC Corp
Original Assignee
DIC Corp
Dainippon Ink and Chemicals Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by DIC Corp, Dainippon Ink and Chemicals Co Ltd filed Critical DIC Corp
Priority to EP21849738.6A priority Critical patent/EP4190524A4/en
Priority to CN202180058815.3A priority patent/CN116096543A/zh
Priority to JP2022536591A priority patent/JP7193040B2/ja
Priority to US18/017,941 priority patent/US20230271349A1/en
Publication of WO2022024773A1 publication Critical patent/WO2022024773A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • 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
    • 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

Definitions

  • the present invention relates to a method for manufacturing a sheet molding compound and a molded product.
  • thermosetting resin in which thermosetting resin is reinforced with fiber reinforced plastic
  • fiber-reinforced resin composite materials made of carbon fiber as a fiber-reinforced material and reinforced with thermosetting resins such as epoxy resin and unsaturated polyester resin are attracting attention for their light weight but excellent heat resistance and mechanical strength. Its use in structural applications is expanding.
  • discontinuous fibers are used as the fiber reinforcing material, the range of application of the molded shape is wider than that of continuous fibers, the scraps can be reused, and different material member inserts can be made. Due to its wide range, sheet molding compounds (hereinafter, may be abbreviated as "SMC") are widely used.
  • SMC sheet molding compounds
  • the problem to be solved by the present invention is to provide a method for producing SMC having excellent carbon fiber impregnation property regardless of the carbon fiber content.
  • the present inventors have found that a method for producing SMC having a step of measuring the bulkiness of the carbon fiber aggregate before the impregnation step of impregnating the carbon fiber aggregate with the resin composition can solve the above-mentioned problems. Completed the invention.
  • the present invention relates to a method for producing SMC having a step of measuring the bulkiness of the carbon fiber aggregate before the impregnation step of impregnating the carbon fiber aggregate with the resin composition.
  • the SMC and its molded products obtained from the present invention are excellent in impregnation property of carbon fiber and the like, automobile parts, railroad vehicle parts, aerospace aircraft parts, ship parts, housing equipment parts, sports parts, light vehicle parts, construction It can be suitably used for exteriors and structures of civil engineering members, OA equipment and the like.
  • the method for producing SMC of the present invention includes a step of measuring the bulkiness of the carbon fiber aggregate before the impregnation step of impregnating the carbon fiber aggregate with the resin composition.
  • the carbon fiber aggregate means an aggregate formed by carbon fibers sprayed on the surface coated with the resin composition before the impregnation step.
  • the resin composition is applied to the carrier films placed on the upper and lower sides so as to have a uniform thickness (coating step), and the fiber reinforcing material is sprayed on one of the resin composition coated surfaces.
  • coating step sandwiched between the resin compositions on the carrier films installed above and below, and then the whole is passed between the impregnating rolls, and pressure is applied to impregnate the fiber reinforcing material with the resin composition (impregnation).
  • Step) a method of winding into a roll or folding into a zigzag fold, but the method for producing SMC of the present invention is sprayed because it has a step of measuring the bulkiness of the carbon fiber aggregate before the impregnation step.
  • Examples of the measurement of the bulkiness of the carbon fiber aggregate in the measurement step include a laser displacement meter, a contact roll, a heating method, etc., but a laser displacement meter is used because it is non-contact and the device can be miniaturized. The method of doing is preferable.
  • a laser displacement meter is installed on the production line to measure the bulkiness of the carbon fiber aggregate in the width direction of SMC before the impregnation process. If the difference in bulkiness in the width direction (initial bulk height difference) is large, this bulkiness By modifying the SMC, it is possible to efficiently obtain an SMC having a uniform impregnation property and a uniform thickness in the width direction of the SMC.
  • the modified bulk height difference (modified bulk height difference) is preferably adjusted to less than 3.5 mm because the impregnation property and the uniformity of the SMC thickness are further improved.
  • the bulkiness can be corrected by, for example, a metal or plastic comb, a rotary roller, or the like.
  • FIG. 1 describes the SMC manufacturing process and the flow of the SMC sheet 8'.
  • a thermoplastic resin film having a thickness of 10 to 50 ⁇ m drawn out by the unwinding device 19a is placed on the transfer belt 20 as a lower carrier film 12a, and the resin composition 22a is placed on the lower carrier film with a doctor blade or the like.
  • the resin coating device 21a provided is used to coat the film to a predetermined thickness.
  • the coating width of the resin composition 22a is applied so as to be located inside about 30 to 60 mm from the width of the carrier film so as not to protrude from both sides of the lower carrier film 12a.
  • a guide roll for the transfer belt is appropriately arranged inside the transfer belt 20.
  • the material of the lower carrier film 12a may be a thermoplastic resin film such as polyethylene or polyethylene terephthalate film which is usually used, or a multilayer film in which a nylon film, polypropylene, polyethylene or the like is combined may be used.
  • a polypropylene film is preferably used.
  • the resin composition 22a contains a thermosetting resin such as an epoxy resin, an unsaturated polyester resin, or a vinyl ester resin as a main component, a filler, a thickener such as a thermoplastic resin powder, a curing catalyst, and internal separation. It is a paste-like product in which a mold, a hyposhrinking agent, a colorant and the like are appropriately mixed.
  • the resin composition 22a for the carbon fiber impregnated in the resin composition 22a, for example, a plurality of bundles of strands 24 are sent to the cutting device 25 by roving 23, and the resin composition 22a is used as a cut piece 24a of carbon fiber having a size of about 1/16 to 1.5 inches.
  • a carbon fiber aggregate is obtained by spraying it so as to be evenly dispersed on the top.
  • the bulkiness of the carbon fiber aggregate is measured by the measuring device 26, and when the initial bulk height difference H 0 is 3.5 mm or more, it is preferable to adjust it to less than 3.5 mm with the comb or the like.
  • thermoplastic resin film such as a polyethylene film having a thickness of 10 to 50 ⁇ m drawn out by the unwinding device 19b is used as an upper carrier film 12b, and the same as the above-mentioned resin composition 22a is applied on the upper carrier film.
  • the resin composition 22b is coated with a resin coating device 21b provided with a doctor blade or the like to a predetermined thickness, and is arranged so as to be in contact with the cut pieces 24a of the carbon fiber. Also in this case, the coating width of the resin composition 22b is applied so as to be located inward by about 30 to 60 mm so as not to protrude from both sides of the upper carrier film 12b.
  • an SMC sheet 8'with a layer structure of the lower carrier film 12a / resin composition 22a / carbon fiber cut pieces 24a / resin composition 22b / upper carrier film 12b can be obtained.
  • the thickness of the portion excluding both carrier films 12a and 12b is preferably 2.5 to 10 mm, and this is sent to the impregnation device 13 in the subsequent step as shown in FIG. 1, and a plurality of impregnation rolls having various surface groove shapes are sent.
  • the SMC sheet 8'of 10 mm or less is made by impregnating the resin composition 22a with defoaming and smoothing the surface so that the cut pieces 24a of the carbon fiber are sufficiently wetted through the 13 rolls composed of the above. Is preferable.
  • the thickness of the SMC sheet in the present invention is a value measured by a laser displacement meter in the same manner as the bulkiness of the carbon fiber aggregate.
  • thermosetting resins such as epoxy resin, vinyl ester resin, vinyl urethane resin, unsaturated polyester resin, phenol resin, melamine resin, and furan resin, but after molding.
  • Epoxy resin, vinyl ester resin and vinyl urethane resin are more preferable from the viewpoint of mechanical properties such as strength. These resins may be used alone or in combination of two or more.
  • a diluent for example, a curing agent, a curing accelerator, a polymerization inhibitor, a filler, a low shrinkage agent, a thermoplastic resin particle, a mold release agent, a thickener, and the like. It can contain a thickener, a pigment, an antioxidant, a plasticizer, a flame retardant, an antibacterial agent, an ultraviolet stabilizer, a storage stabilizer, a reinforcing material, a photocuring agent and the like.
  • the filler includes inorganic compounds and organic compounds, which can be used to adjust physical properties such as strength, elastic modulus, impact strength, and fatigue durability of molded products.
  • examples of the inorganic compound include calcium carbonate, magnesium carbonate, barium sulfate, mica, talc, kaolin, clay, celite, asbestos, barlite, baryta, silica, silica sand, dolomite limestone, gypsum, aluminum fine powder, hollow balloon, and the like.
  • Alumina, glass powder, aluminum hydroxide, cold water stone, zirconium oxide, antimony trioxide, titanium oxide, molybdenum dioxide, iron powder and the like can be mentioned.
  • organic compound examples include natural polysaccharide powders such as cellulose and chitin, synthetic resin powders, and the like, and synthetic resin powders are composed of hard resins, soft rubbers, elastomers, polymers (copolymers), and the like.
  • Particles having a multilayer structure such as organic powder or core-shell type can be used. Specific examples thereof include particles made of butadiene rubber and / or acrylic rubber, urethane rubber, silicon rubber and the like, polyimide resin powder, fluororesin powder, phenol resin powder and the like. These fillers may be used alone or in combination of two or more.
  • release agent examples include zinc stearate, calcium stearate, paraffin wax, polyethylene wax, carnauba wax, and fluorine-based compounds. Fluorine compounds and paraffin wax are preferable. These release agents can be used alone or in combination of two or more.
  • thickener examples include metal oxides such as magnesium oxide, magnesium hydroxide, calcium oxide and calcium hydroxide, acrylic resin-based fine particles such as metal hydroxides, and the fiber-reinforced molding material of the present invention. It can be selected as appropriate depending on the handleability of. These thickeners can be used alone or in combination of two or more.
  • the resin composition is obtained by mixing and dispersing each of the above components using a mixer such as a normal mixer, an intermixer, a planetary mixer, a roll mill, a kneader, and an extruder.
  • a mixer such as a normal mixer, an intermixer, a planetary mixer, a roll mill, a kneader, and an extruder.
  • the carbon fiber for example, a fiber cut to a length of 2.5 to 50 mm is used, but since the fluidity in the mold at the time of molding, the appearance of the molded product and the mechanical properties are further improved, 5 to 5 to Fibers cut to 40 mm are more preferred.
  • carbon fiber various types such as polyacrylonitrile-based, pitch-based, rayon-based, etc. can be used, but among these, polyacrylonitrile-based one is preferable because high-strength carbon fiber can be easily obtained.
  • the number of filaments of the fiber bundle used as the carbon fiber is preferably 1,000 to 60,000 because the resin impregnation property and the mechanical properties of the molded product are further improved.
  • the carbon fiber content in the components of the SMC of the present invention is preferably in the range of 30 to 65% by mass, more preferably in the range of 35 to 60% by mass, because the mechanical properties of the obtained molded product are further improved. .. If the carbon fiber content is too low, a high-strength molded product cannot be obtained, and if the fiber reinforced material content is too high, the resin impregnation property of the carbon fiber is insufficient, causing swelling of the molded product and high strength. There is a possibility that a good molded product cannot be obtained.
  • the carbon fibers in the SMC of the present invention are impregnated in the resin in a state where the fiber directions are random.
  • the method for manufacturing a molded product of the present invention is a method for molding an SMC obtained by the above-mentioned manufacturing method, but heat compression molding is preferable as the molding method from the viewpoint of excellent productivity and design diversity. ..
  • the SMC is weighed in a predetermined amount, put into a mold heated to 110 to 180 ° C. in advance, molded by a compression molding machine, and the molding material is molded.
  • a manufacturing method is used in which a molding material is cured by maintaining a molding pressure of 1 to 30 MPa, and then the molded product is taken out to obtain a molded product.
  • molding conditions in which the molding pressure of 1 to 20 MPa is maintained in the mold at a mold temperature of 120 to 160 ° C. for 1 to 5 minutes per 1 mm of the thickness of the molded product is preferable, and productivity is preferable. More preferably, the molding conditions are such that the molding pressure of 1 to 20 MPa is maintained for 1 to 3 minutes per 1 mm of the thickness of the molded product at a mold temperature of 140 to 160 ° C.
  • the SMC of the present invention is excellent in productivity, formability, etc., and the obtained molded products are automobile members, railroad vehicle members, aerospace aircraft members, ship members, housing equipment members, sports members, light vehicle members, building civil engineering members. , Can be suitably used for a housing of an OA device or the like.
  • the dispersion roller has disks attached to both ends of the shaft, and eight round bars of ⁇ 5 mm are attached at equal intervals along the outer circumference of the disk, and the fibers after cutting are dispersed by the impact of hitting the round bars of the dispersion roller.
  • the device was used.
  • the initial bulk height is measured with a laser displacement meter, the difference in bulk height in the width direction is calculated, and immediately after that, on the line.
  • the height of the comb installed in was adjusted, and the difference in bulk height was adjusted.
  • the carbon fibers are sandwiched between films coated with the resin composition (A'-1), impregnated with the resin under the conditions shown in Table 1, and then allowed to stand at 40 ° C. for 20 hours to allow SMC. Obtained.
  • the basis weight of this SMC was 2 kg / m 2 .
  • the mass of the impregnated fiber is increased by 40% or more compared to the mass of the unimpregnated fiber 4: The mass of the fiber after impregnation is increased by 20% or more and less than 40% compared to the mass of the unimpregnated fiber 3: The mass of the fiber after impregnation is the mass of the unimpregnated fiber 10% or more and less than 20% increase compared to 2: Impregnated fiber mass increased by 3% or more and less than 10% compared to unimpregnated fiber mass 1: Impregnated fiber mass increased by less than 3% compared to unimpregnated fiber mass Or, the outflow of only the resin at the end of the SMC sheet is 30 mm or more.
  • the SMC (1) obtained above was pressure-molded at a mold temperature of 140 ° C., a pressurization time of 5 minutes, and a pressurizing condition of 10 MPa at a charge rate of 75% with respect to the projected area of a 30 cm square mold. , A molded product (1) having a plate thickness of 2 mm was obtained.
  • the cross section of the molded product (1) obtained above was observed using a digital microscope VHX-5000 (manufactured by KEYENCE CORPORATION) at a magnification of 50 times, and the impregnation property was evaluated according to the following criteria.
  • Example 2 to 4 and Comparative Examples 1 to 2 SMCs (2) to (4) and molded products (2) to (4) were obtained and evaluated in the same manner as in Example 1 except for the number of rotations of the dispersed rollers (change of thread path).
  • Comparative Examples 1 and 2 are examples of SMC obtained without going through the step of measuring the bulkiness of the carbon fiber aggregate, but it was confirmed that the impregnation property was insufficient.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Reinforced Plastic Materials (AREA)
PCT/JP2021/026545 2020-07-30 2021-07-15 シートモールディングコンパウンド及び成形品の製造方法 Ceased WO2022024773A1 (ja)

Priority Applications (4)

Application Number Priority Date Filing Date Title
EP21849738.6A EP4190524A4 (en) 2020-07-30 2021-07-15 Methods for producing sheet molding compound and molded article
CN202180058815.3A CN116096543A (zh) 2020-07-30 2021-07-15 片状模塑料和成形品的制造方法
JP2022536591A JP7193040B2 (ja) 2020-07-30 2021-07-15 シートモールディングコンパウンド及び成形品の製造方法
US18/017,941 US20230271349A1 (en) 2020-07-30 2021-07-15 Methods for producing sheet molding compound and for producing molded product

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Application Number Priority Date Filing Date Title
JP2020-129103 2020-07-30
JP2020129103 2020-07-30

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WO2022024773A1 true WO2022024773A1 (ja) 2022-02-03

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US (1) US20230271349A1 (https=)
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WO (1) WO2022024773A1 (https=)

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JP7435928B1 (ja) * 2022-08-31 2024-02-21 Dic株式会社 繊維強化複合材シート用製造装置及び繊維強化複合材シートの製造方法
WO2024048076A1 (ja) * 2022-08-31 2024-03-07 Dic株式会社 繊維強化複合材シート用製造装置及び繊維強化複合材シートの製造方法
WO2024134929A1 (ja) * 2022-12-22 2024-06-27 Dic株式会社 シートモールディングコンパウンド、及び成形品

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WO2024048076A1 (ja) * 2022-08-31 2024-03-07 Dic株式会社 繊維強化複合材シート用製造装置及び繊維強化複合材シートの製造方法
WO2024134929A1 (ja) * 2022-12-22 2024-06-27 Dic株式会社 シートモールディングコンパウンド、及び成形品

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CN116096543A (zh) 2023-05-09
JP7193040B2 (ja) 2022-12-20
US20230271349A1 (en) 2023-08-31
JPWO2022024773A1 (https=) 2022-02-03
EP4190524A4 (en) 2024-08-28

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