WO2021241380A1 - レーザー溶着用透過性樹脂組成物、キット、成形品および成形品の製造方法 - Google Patents

レーザー溶着用透過性樹脂組成物、キット、成形品および成形品の製造方法 Download PDF

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Publication number
WO2021241380A1
WO2021241380A1 PCT/JP2021/019112 JP2021019112W WO2021241380A1 WO 2021241380 A1 WO2021241380 A1 WO 2021241380A1 JP 2021019112 W JP2021019112 W JP 2021019112W WO 2021241380 A1 WO2021241380 A1 WO 2021241380A1
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Prior art keywords
resin composition
resin
light
mass
molded product
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Ceased
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PCT/JP2021/019112
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English (en)
French (fr)
Japanese (ja)
Inventor
章人 岡元
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Mitsubishi Engineering Plastics Corp
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Mitsubishi Engineering Plastics Corp
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Priority to JP2022526945A priority Critical patent/JP7705854B2/ja
Priority to CN202410851862.9A priority patent/CN118667330A/zh
Priority to CN202180038411.8A priority patent/CN115698184B/zh
Priority to EP21812851.0A priority patent/EP4159789A4/en
Priority to KR1020227035552A priority patent/KR20230015316A/ko
Publication of WO2021241380A1 publication Critical patent/WO2021241380A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/02—Organic and inorganic ingredients
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
    • C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
    • C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
    • C08G69/265—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids from at least two different diamines or at least two different dicarboxylic acids
    • 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
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
    • B29C65/14—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation
    • B29C65/16—Laser beams
    • B29C65/1603—Laser beams characterised by the type of electromagnetic radiation
    • B29C65/1612—Infrared [IR] radiation, e.g. by infrared lasers
    • B29C65/1616—Near infrared radiation [NIR], e.g. by YAG lasers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
    • B29C65/14—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation
    • B29C65/16—Laser beams
    • B29C65/1629—Laser beams characterised by the way of heating the interface
    • B29C65/1635—Laser beams characterised by the way of heating the interface at least passing through one of the parts to be joined, i.e. laser transmission welding
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
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    • B29C66/737—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the state of the material of the parts to be joined
    • B29C66/7377—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the state of the material of the parts to be joined amorphous, semi-crystalline or crystalline
    • B29C66/73775—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the state of the material of the parts to be joined amorphous, semi-crystalline or crystalline the to-be-joined area of at least one of the parts to be joined being crystalline
    • 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
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/73—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset
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Definitions

  • the present invention relates to a laser welding transparent resin composition, a kit, a molded product, and a method for producing a molded product.
  • Thermoplastic resin is easy to process and is widely used for vehicle parts, electrical / electronic equipment parts, other precision equipment parts, etc. by taking advantage of its excellent characteristics.
  • parts with complicated shapes are also manufactured with thermoplastic resin, especially crystalline thermoplastic resin, and various welding techniques are used for welding parts with hollow parts such as intake manifolds. Specifically, adhesive welding, vibration welding, ultrasonic welding, hot plate welding, injection welding, laser welding and the like are used.
  • laser welding includes a resin member having transparency (also referred to as non-absorbent or weakly absorbent) to laser light (hereinafter, may be referred to as “transmissive resin member”) and absorbability to laser light.
  • transparent resin member also referred to as non-absorbent or weakly absorbent
  • absorbability to laser light.
  • This is a method of joining the two resin members by contacting and welding the resin member having the above (hereinafter, may be referred to as “absorbent resin member”). Specifically, it is a method of irradiating a joining surface with laser light from the transmission resin member side to melt and join the absorbing resin member forming the joining surface with the energy of the laser light.
  • Laser welding does not generate abrasion powder or burrs, causes less damage to the product, and since the polyamide resin itself is a material with a relatively high laser transmittance, processing of polyamide resin products by laser welding technology is possible. It has been attracting attention recently.
  • the transmissive resin member is usually obtained by molding a light transmissive resin composition.
  • Patent Document 1 describes (A) a reinforced filler having a refractive index of (B) 23 ° C. of 1.560 to 1.600 with respect to 100 parts by mass of a polyamide resin. It is a resin composition containing 1 to 150 parts by mass, and is characterized by laser welding, wherein at least one monomer constituting at least one of the polyamide resin (A) contains an aromatic ring. Resin compositions for use are described.
  • a resin composition in which a glass fiber and a colorant are blended in a blend of polyamide MXD6 and polyamide 66 or a blend of polyamide 6I / 6T and polyamide 6 is disclosed. ..
  • An object of the present invention is to solve such a problem, and a laser welding transparent resin composition, a kit, which is excellent in physical properties such as mechanical strength and low warpage and has high light transmittance. It is an object of the present invention to provide a molded product and a method for manufacturing the molded product.
  • the polyamide resin is composed of a diamine-derived structural unit and a dicarboxylic acid-derived structural unit, and 70 mol% or more of the diamine-derived structural unit is derived from xylylenediamine and 70 is a dicarboxylic acid-derived structural unit.
  • ⁇ 5> The invention according to any one of ⁇ 1> to ⁇ 4>, wherein when the resin composition is molded into a molded product having a thickness of 60 mm ⁇ 60 mm ⁇ 1 mm, the amount of warpage of the molded product is 1 mm or less. Resin composition; The amount of warpage is the difference between the height of the highest portion and the height of the lowest portion of the test piece when the molded product is placed on a reference table.
  • ⁇ 6> Any one of ⁇ 1> to ⁇ 5>, wherein the crystalline thermoplastic resin contains a polyamide resin having a crystallization calorific value of 0 to -1 mJ / mg as measured by a differential scanning calorimeter.
  • the resin composition according to.
  • ⁇ 7> A kit comprising the resin composition according to any one of ⁇ 1> to ⁇ 6> and a light-absorbing resin composition containing a thermoplastic resin and a light-absorbing dye.
  • ⁇ 8> A molded product formed from the resin composition according to any one of ⁇ 1> to ⁇ 6> or the kit according to ⁇ 7>.
  • ⁇ 9> A molded product formed from the resin composition according to any one of ⁇ 1> to ⁇ 6>, and a light-absorbing resin composition containing a thermoplastic resin and a light-absorbing dye.
  • a method for manufacturing a molded product which comprises laser welding the molded product.
  • FIG. 1 is a schematic diagram for explaining a method of measuring the height of warpage in an embodiment.
  • the present embodiment will be described in detail.
  • the following embodiments are examples for explaining the present invention, and the present invention is not limited to the present embodiment.
  • "-" is used in the meaning which includes the numerical values described before and after it as the lower limit value and the upper limit value.
  • various physical property values and characteristic values shall be at 23 ° C. unless otherwise specified.
  • the laser welding transparent resin composition of the present embodiment (hereinafter, may be simply referred to as “resin composition of the present embodiment”) has a thickness of 0.1 to 2 ⁇ m with respect to 100 parts by mass of the crystalline thermoplastic resin. It is characterized by containing 10 to 120 parts by mass of the glass flakes of the above and a light-transmitting dye. With such a configuration, it becomes possible to provide a laser welding transparent resin composition having excellent physical properties such as mechanical strength and low warpage and having a high light transmittance. Inorganic fillers have long been blended in order to achieve mechanical strength and low warpage. However, until now, it has not been known at all that the shape of the inorganic filler affects the light transmission.
  • the resin composition of the present embodiment contains a crystalline thermoplastic resin.
  • the crystalline thermoplastic resin include polyamide resin, polyacetal resin, polyester resin (preferably polybutylene terephthalate resin), and polyamide resin and polybutylene terephthalate resin are preferable, and polyamide resin is more preferable.
  • polyamide resin is more preferable.
  • a crystalline polyamide resin it can be cured more quickly when molding a molded product.
  • the obtained resin composition tends to be excellent in oil resistance, grease resistance, lubricity, sliding property, abrasion resistance, and friction resistance.
  • a crystalline thermoplastic resin has a "crystal portion" in which molecules are regularly arranged when the temperature of the resin drops to the crystallization temperature and solidifies.
  • the crystalline thermoplastic resin occupies 30% by mass or more, more preferably 40% by mass or more, and further preferably 45% by mass or more.
  • the upper limit of the content of the crystalline thermoplastic resin in the resin composition is preferably 90% by mass or less, more preferably 80% by mass or less, and further preferably 75% by mass or less. preferable.
  • the resin composition of the present embodiment may contain only one kind of crystalline thermoplastic resin, or may contain two or more kinds of crystalline thermoplastic resin. When two or more kinds are contained, it is preferable that the total amount is within the above range.
  • the polyamide resin used in this embodiment is not particularly specified, and known polyamide resins can be used.
  • the description in paragraphs 0011 to 0013 of JP-A-2011-132550 can be referred to.
  • the polyamide resin used in the present embodiment may be an aliphatic polyamide resin or a semi-aromatic polyamide resin, and is preferably a semi-aromatic polyamide resin.
  • Examples of the aliphatic polyamide resin include polyamide 6, polyamide 11, polyamide 12, polyamide 46, polyamide 66, polyamide 610, polyamide 612, polyamide 1010, and polyamide 1012.
  • the semi-aromatic polyamide resin is composed of a diamine-derived structural unit and a dicarboxylic acid-derived structural unit, and 30 to 70 mol% of the total structural unit of the diamine-derived structural unit and the dicarboxylic acid-derived structural unit is aromatic.
  • the structural unit include a ring, and it is preferable that 40 to 60 mol% of the total structural unit of the diamine-derived structural unit and the dicarboxylic acid-derived structural unit is the structural unit containing an aromatic ring.
  • the semi-aromatic polyamide resin include terephthalic acid-based polyamide resins (polyamide 6T, polyamide 9T), xylylenediamine-based polyamide resins described later, and the like.
  • At least one of the polyamide resins used in the present embodiment is composed of a diamine-derived structural unit and a diamine-derived structural unit, and 70 mol% or more of the diamine-derived structural unit is xylylenediamine (preferably xylylenedirange). More than 30 mol% of the constituent units derived from amines are derived from (constituent units derived from m-xylylenediamine), and more than 70 mol% of the constituent units derived from dicarboxylic acid are ⁇ , ⁇ -linear fats having 4 to 20 carbon atoms.
  • Polyamide resins derived from group dicarboxylic acids are preferable.
  • the diamine-derived constituent unit of the xylylenediamine-based polyamide resin is more preferably 75 mol% or more, further preferably 80 mol% or more, still more preferably 90 mol% or more, still more preferably 95 mol% or more.
  • the constituent unit derived from the dicarboxylic acid of the xylylene diamine-based polyamide resin is more preferably 75 mol% or more, further preferably 80 mol% or more, still more preferably 90 mol% or more, still more preferably 95 mol% or more, and carbon. It is derived from ⁇ , ⁇ -linear aliphatic dicarboxylic acid having a number of 4 to 20.
  • the xylylenediamine is preferably paraxylylenediamine and / or metaxylylenediamine, more preferably containing at least metaxylylenediamine, and more preferably 30 mol% or more (preferably 40 mol% or more, more preferably) of xylylenediamine. Is 50 mol% or more, more preferably 60 mol% or more) is more preferably m-xylylenediamine.
  • the xylylenediamine is more preferably 30 to 90 mol% (preferably 60 to 90 mol%) of metaxylylenediamine and 70 to 10 mol% (preferably 40 to 10 mol%) of paraxylylenedi. It is an amine.
  • the total amount of m-xylylenediamine and paraxylylenediamine is 100 mol% or less of the raw material diamine, preferably 90 to 100 mol%.
  • Examples of diamines other than metaxylylenediamine and paraxamethylenediamine that can be used as the raw material diamine component of the xylylenediamine-based polyamide resin include tetramethylenediamine, pentamethylenediamine, 2-methylpentanediamine, hexamethylenediamine, and heptamethylene.
  • An aliphatic diamine such as diamine, octamethylenediamine, nonamethylenediamine, decamethylenediamine, dodecamethylenediamine, 2,2,4-trimethyl-hexamethylenediamine, 2,4,4-trimethylhexamethylenediamine, 1,3- Bis (aminomethyl) cyclohexane, 1,4-bis (aminomethyl) cyclohexane, 1,3-diaminocyclohexane, 1,4-diaminocyclohexane, bis (4-aminocyclohexyl) methane, 2,2-bis (4-amino) Aromatic rings such as alicyclic diamines such as cyclohexamethylene) propane, bis (aminomethyl) decalin, bis (aminomethyl) tricyclodecane, bis (4-aminophenyl) ether, paraphenylenediamine, and bis (aminomethyl) naphthalene. Examples thereof include di
  • Examples of the ⁇ , ⁇ -linear aliphatic dicarboxylic acid having 4 to 20 carbon atoms preferable to be used as the raw material dicarboxylic acid component of the xylylene diamine-based polyamide resin include succinic acid, glutaric acid, pimelic acid, suberic acid and adipic acid.
  • Adipic acid, sebacic acid, undecanedioic acid, dodecanedioic acid and other aliphatic dicarboxylic acids can be exemplified, and one kind or a mixture of two or more kinds can be used.
  • the melting point of the polyamide resin is molded. Adipic acid or sebacic acid is more preferable because it is in an appropriate range.
  • dicarboxylic acid component other than the ⁇ , ⁇ -linear aliphatic dicarboxylic acid having 4 to 20 carbon atoms examples include phthalic acid compounds such as isophthalic acid, terephthalic acid and orthophthalic acid, 1,2-naphthalenedicarboxylic acid and 1,3.
  • naphthalenedicarboxylic acids such as dicarboxylic acid, 2,6-naphthalenedicarboxylic acid, and 2,7-naphthalenedicarboxylic acid can be exemplified, and one kind or a mixture of two or more kinds can be used.
  • the constituent units derived from diamine and the constituent units derived from dicarboxylic acid are the main components, the constituent units other than these are not completely excluded, and lactams such as ⁇ -caprolactam and laurolactam, aminocaproic acid. Needless to say, it may contain a constituent unit derived from an aliphatic aminocarboxylic acid such as aminoundecanoic acid.
  • the main component means that among the constituent units constituting the xylylenediamine-based polyamide resin, the total number of the constituent units derived from diamine and the constituent units derived from dicarboxylic acid is the largest among all the constituent units.
  • the total of the diamine-derived constituent units and the dicarboxylic acid-derived constituent units in the xylylenediamine-based polyamide resin preferably occupies 90% or more of all the constituent units, and more preferably 95% or more. preferable.
  • the crystalline thermoplastic resin used in the present embodiment preferably contains a polyamide resin having a crystallization calorific value of 0 to -1 mJ / mg as measured by a differential scanning calorimeter, and is preferably 0 to -0.8 mJ / mg. It is more preferable to contain the polyamide resin which is. By using such a polyamide resin, crystallization progresses effectively, and even when water is absorbed over time, the mechanical strength tends to be less likely to be significantly reduced.
  • the amount of heat of crystallization referred to here means a value measured under the conditions described in Examples described later.
  • One embodiment of the resin composition of the present embodiment includes an embodiment that does not substantially contain a thermoplastic resin other than a polyamide resin.
  • the content of the thermoplastic resin other than the polyamide resin is preferably 5% by mass or less, more preferably 3% by mass or less, and 1% by mass of the resin composition of the present embodiment. % Or less is more preferable.
  • the description in paragraphs 0009 to 0012 of JP-A-2019-123386 can be referred to, and this content is incorporated in the present specification.
  • the description in paragraphs 0016 to 0024 of JP-A-2020-109950 can be referred to, and the contents thereof are incorporated in the present specification.
  • the resin composition of the present embodiment contains 10 to 120 parts by mass of glass flakes having a thickness of 0.1 to 2 ⁇ m with respect to 100 parts by mass of the crystalline thermoplastic resin. With such a configuration, it is possible to improve the light transmittance in addition to the mechanical strength and low warpage.
  • the thickness of the glass flakes means the average thickness.
  • the thickness of the glass flakes is preferably 0.3 ⁇ m or more, more preferably 0.4 ⁇ m or more, still more preferably 0.5 ⁇ m or more, still more preferably 0.6 ⁇ m or more.
  • the thickness of the glass flakes is preferably 1.8 ⁇ m or less, more preferably 1.6 ⁇ m or less, still more preferably 1.4 ⁇ m or less, still more preferably 1.2 ⁇ m or less, still more preferably 1.0 ⁇ m or less, and even more. It is preferably 0.8 ⁇ m or less.
  • the average thickness is measured by the following method.
  • ⁇ Measuring method of average thickness It is obtained by measuring the thickness of each of 100 or more glass flakes using a scanning electron microscope (SEM) and averaging the measured values.
  • the sample table of the scanning electron microscope is adjusted by the sample table fine movement device so that the cross section (thickness surface) of the glass flakes is perpendicular to the irradiation electron beam axis of the scanning electron microscope.
  • the number average value of the aspect ratios of the glass flakes is preferably 3 to 20.
  • the aspect ratio is also measured by the same method as the above-mentioned average thickness measuring method.
  • the glass composition of the above glass flakes is not particularly limited as various glass compositions typified by A glass, C glass, D glass, R glass, S glass, E glass and the like are applied.
  • the resin composition of the present embodiment contains 10 to 120 parts by mass of glass flakes having a thickness of 0.1 to 2 ⁇ m with respect to 100 parts by mass of the crystalline thermoplastic resin.
  • the glass flakes are preferably 20 parts by mass or more, more preferably 30 parts by mass or more, still more preferably 35 parts by mass or more, and 40 parts by mass with respect to 100 parts by mass of the crystalline thermoplastic resin. It is more preferably 45 parts by mass or more, 60 parts by mass or more, 80 parts by mass or more, and 90 parts by mass or more.
  • the glass flakes having a thickness of 0.1 to 2 ⁇ m are preferably 120 parts by mass or less, more preferably 115 parts by mass or less, and 110 parts by mass or less with respect to 100 parts by mass of the crystalline thermoplastic resin. It is more preferable to have 105 parts by mass or less.
  • the glass flakes having a thickness of 0.1 to 2 ⁇ m preferably occupy 10 to 60% by mass, more preferably 20 to 60% by mass, and 25 to 55% by mass in the resin composition of the present embodiment. You may.
  • the resin composition of the present embodiment may contain only one type of glass flakes having a thickness of 0.1 to 2 ⁇ m, or may contain two or more types of glass flakes. When two or more kinds are contained, it is preferable that the total amount is within the above range.
  • the resin composition of the present embodiment may or may not contain an inorganic filler other than the glass flakes having a thickness of 0.1 to 2 ⁇ m.
  • Examples of other inorganic fillers include fibrous, scaly, spherical, and needle-shaped inorganic fillers, and examples of the components include glass, metal oxides, metal hydroxides, carbonates, and sulfates. ..
  • An example of the embodiment of the resin composition of the present embodiment is a resin composition that does not substantially contain an inorganic filler other than glass flakes having a thickness of 0.1 to 2 ⁇ m.
  • the term "substantially free" means that the content of the inorganic filler other than the glass flakes having a thickness of 0.1 to 2 ⁇ m is 5% by mass or less of the total amount of the inorganic filler contained in the resin composition. It is preferably 1% by mass or less, and more preferably 1% by mass or less.
  • the inorganic filler in this embodiment does not include the one corresponding to the nucleating agent.
  • the resin composition of the present embodiment contains a light-transmitting dye.
  • the obtained molded product can be given a color and the appearance of the molded product can be improved.
  • the color of the transmissive resin member molded from the resin composition of the present embodiment and the absorption resin member described in detail later can be unified, and the appearance of the obtained molded product (laser welded body) can be improved. Can be done.
  • the light-transmitting dye used in the present embodiment is usually a black dye, and specifically, a niglosin skeleton, a naphthalocyanine skeleton, an aniline black skeleton, a phthalocyanine skeleton, a porphyrin skeleton, a perinone skeleton, a quoterylene skeleton, an azo skeleton, and anthraquinone.
  • a black dye specifically, a niglosin skeleton, a naphthalocyanine skeleton, an aniline black skeleton, a phthalocyanine skeleton, a porphyrin skeleton, a perinone skeleton, a quoterylene skeleton, an azo skeleton, and anthraquinone.
  • Examples thereof include dyes having a skeleton selected from a skeleton, a pyrazolone skeleton, a square acid derivative skeleton, a perylene skeleton, a
  • the light-transmitting dye is, for example, a polyamide resin, 30% by mass of glass flakes, and 0.2% by mass of a dye (a dye that seems to be a light-transmitting dye) blended so as to have a total of 100% by mass, which will be described later.
  • the light-transmitting dye may be a dye or a pigment, but a pigment is preferable.
  • e-BIND LTW-8731H and e-BIND LTW-8701H which are colorants (dyes) manufactured by Orient Chemical Industry Co., Ltd., Last Yellow 8000 and Last Red M 8315, which are colorants manufactured by Arimoto Chemical Co., Ltd. , Oil Green 5602, Macrollex Yellow 3G, a colorant manufactured by LANXESS, Macrolex Red EG, Macrolex Green 3, Spectrasense K0087 (formerly: Lumogen® BlackK8), a colorant manufactured by BASF.
  • Spectrasense K0088 (formerly: Lumogen Black K0088, Lumogen Black FK4281) and the like are exemplified.
  • the content of the light-transmitting dye in the resin composition of the present embodiment is preferably 0.001 part by mass or more, more preferably 0.01 part by mass or more, out of 100 parts by mass of the resin composition. Further, it may be 0.08 part by mass or more, 0.1 part by mass or more, 0.15 part by mass or more, and 0.2 part by mass or more.
  • the upper limit of the content of the light-transmitting dye is preferably 5.0 parts by mass or less, more preferably 3.0 parts by mass or less, and 1.0 part by mass in 100 parts by mass of the resin composition. It is more preferably 0 parts by mass or less, and may be 0.8 parts by mass or less, 0.5 parts by mass or less, 0.4 parts by mass or less, and 0.3 parts by mass or less.
  • the resin composition may contain only one kind of light-transmitting dye, or may contain two or more kinds of light-transmitting dyes. When two or more kinds are contained, it is preferable that the total amount is within the above range. Further, it is preferable that the laser welding transparent resin composition of the present embodiment substantially does not contain carbon black.
  • substantially free means, for example, 0.0001% by mass or less of the resin composition.
  • the resin composition of the present embodiment may contain a nucleating agent.
  • the nucleating agent is not particularly limited as long as it is unmelted at the time of melt processing and can become a nucleus of crystals in the cooling process, but talc and calcium carbonate are preferable, and talc is more preferable.
  • the lower limit of the number average particle size of the nucleating agent is preferably 0.1 ⁇ m or more, more preferably 1 ⁇ m or more, and even more preferably 3 ⁇ m or more.
  • the upper limit of the number average particle size of the nucleating agent is preferably 40 ⁇ m or less, more preferably 30 ⁇ m or less, further preferably 28 ⁇ m or less, further preferably 15 ⁇ m or less, and even more preferably 10 ⁇ m. The following is even more preferable.
  • the proportion of the nucleating agent in the resin composition of the present embodiment is preferably 0.01 to 1% by mass, more preferably 0.1% by mass or more, and 0.5% by mass or less. Is more preferable.
  • the resin composition of the present embodiment may contain only one kind of nucleating agent or two or more kinds of nucleating agents. When two or more kinds are contained, it is preferable that the total amount is within the above range.
  • the resin composition of the present embodiment may contain a copper compound.
  • a copper compound By using a copper compound, it is possible to achieve remarkably excellent heat aging resistance.
  • the copper compound used in the present embodiment include copper halide (for example, copper iodide, copper bromide, copper chloride) and copper acetate, such as cuprous iodide, cupric iodide, and bromide.
  • copper halide for example, copper iodide, copper bromide, copper chloride
  • copper acetate such as cuprous iodide, cupric iodide, and bromide.
  • cuprous bromide cuprous acetate and cupric acetate
  • cuprous chloride cupric chloride
  • cuprous iodide cuprous acetate and cuprous chloride. It is more preferred to be selected from copper.
  • the copper compound is preferably used in combination with an alkali metal halide described later.
  • a copper compound and an alkali metal halide When a copper compound and an alkali metal halide are combined, it is preferably a mixture of a copper compound: an alkali metal halide in a ratio of 1: 1 to 1:15 (mass ratio), and a mixture of 1: 1 to 1: 5. It is more preferably present, and even more preferably a mixture of 1: 2 to 1: 4.
  • the description in paragraphs 0046 to 0048 of Japanese Patent Application Laid-Open No. 2013-513681 can also be taken into consideration, and these contents are incorporated in the present specification.
  • the proportion of the copper compound in the resin composition of the present embodiment is preferably 0.01 to 1% by mass, more preferably 0.03% by mass or more, and preferably 0.05% by mass or more. It is more preferably 0.5% by mass or less, and more preferably 0.5% by mass or less.
  • the resin composition of the present embodiment may contain only one type of copper compound or may contain two or more types of copper compounds. When two or more kinds are contained, it is preferable that the total amount is within the above range.
  • the halogenated alkali metal used in this embodiment means a halide of the alkali metal.
  • the alkali metal potassium and sodium are preferable, and potassium is more preferable.
  • the halogen atom iodine, bromine and chlorine are preferable, and iodine is more preferable.
  • Specific examples of the alkali metal halide used in the present embodiment include potassium iodide, potassium bromide, potassium chloride and sodium chloride, with potassium iodide being preferred.
  • the proportion of the alkali metal halide in the resin composition of the present embodiment is preferably 0.01 to 1% by mass, more preferably 0.1% by mass or more, and 0.5% by mass or less. Is more preferable.
  • the resin composition of the present embodiment may contain only one kind of alkali metal halide, or may contain two or more kinds of alkali metal halides. When two or more kinds are contained, it is preferable that the total amount is within the above range.
  • the resin composition of the present embodiment preferably contains a mold release agent.
  • a mold release agent By including a mold release agent, it is possible to improve the mold release property from the mold when molding using a mold such as injection molding.
  • the release agent preferably contains at least one selected from an amide wax and a fatty acid metal salt, and more preferably contains a fatty acid metal salt.
  • the amide wax examples include carboxylic acid amide wax and bisamide wax, and carboxylic acid amide wax is preferable.
  • the carboxylic acid amide wax is obtained, for example, by a dehydration reaction between a mixture of a higher aliphatic monocarboxylic acid and a polybasic acid and a diamine compound.
  • a saturated aliphatic monocarboxylic acid having 16 or more carbon atoms and a hydroxycarboxylic acid are preferable, and examples thereof include palmitic acid, stearic acid, behenic acid, montanic acid, and 12-hydroxystearic acid. Be done.
  • the polybasic acid is a carboxylic acid having a dibasic acid or more, for example, an aliphatic dicarboxylic acid such as malonic acid, succinic acid, adipic acid, sebacic acid, pimelic acid, and azelaic acid, and aromatic acids such as phthalic acid and terephthalic acid.
  • an aliphatic dicarboxylic acid such as malonic acid, succinic acid, adipic acid, sebacic acid, pimelic acid, and azelaic acid
  • aromatic acids such as phthalic acid and terephthalic acid.
  • dicarboxylic acids and alicyclic dicarboxylic acids such as cyclohexanedicarboxylic acid and cyclohexylsuccinic acid.
  • diamine compound examples include ethylenediamine, 1,3-diaminopropane, 1,4-diaminobutane, hexamethylenediamine, m-xylylenediamine, tolylenediamine, paraxylylenediamine, phenylenediamine, isophoronediamine and the like. ..
  • the carboxylic acid amide-based wax in the present embodiment can arbitrarily adjust the softening point by changing the mixing ratio of the polybasic acid with respect to the higher aliphatic monocarboxylic acid used for its production.
  • the mixing ratio of the polybasic acid is preferably in the range of 0.18 to 1 mol with respect to 2 mol of the higher aliphatic monocarboxylic acid.
  • the amount of the diamine compound used is preferably in the range of 1.5 to 2 mol with respect to 2 mol of the higher aliphatic monocarboxylic acid, and varies depending on the amount of the polybasic acid used.
  • the bisamide wax examples include diamine compounds and fatty acid compounds such as N, N'-methylene bisstearic acid amide and N, N'-ethylene bisstearic acid amide, or N, N'-dioctadecylterephthalic acid. Examples thereof include dioctadecyl dibasic acid amides such as amides.
  • a metal salt of a long-chain fatty acid having 16 to 36 carbon atoms is preferable, and for example, a metal stearate salt such as calcium stearate, zinc stearate, aluminum stearate, sodium stearate, lithium stearate, and the like.
  • a metal stearate salt such as calcium stearate, zinc stearate, aluminum stearate, sodium stearate, lithium stearate, and the like.
  • Montanic acid metal salts such as calcium montanate, sodium montanate and the like, and montanic acid metal salts are preferable.
  • Examples of the release agent include esters of an aliphatic carboxylic acid and an alcohol, an aliphatic hydrocarbon compound having a number average molecular weight of 200 to 15,000, a polysiloxane-based silicone oil, and a ketone wax.
  • esters of an aliphatic carboxylic acid and an alcohol an aliphatic hydrocarbon compound having a number average molecular weight of 200 to 15,000
  • a polysiloxane-based silicone oil examples of the release agent.
  • the content of the release agent in the resin composition of the present embodiment is preferably 0.05% by mass or more, more preferably 0.1% by mass or more, and 0.2% by mass in the resin composition. % Or more is more preferable. By setting the value to the lower limit or higher, the releasability tends to be further improved.
  • the content of the release agent is preferably 3% by mass or less, more preferably 2% by mass or less, further preferably 1% by mass or less, and 0.8% by mass or less. It is more preferably present, and even more preferably 0.6% by mass or less.
  • the resin composition of the present embodiment may contain only one type of mold release agent, or may contain two or more types of mold release agent. When two or more kinds are contained, it is preferable that the total amount is within the above range.
  • the resin composition of the present embodiment may contain other components as long as it does not deviate from the gist of the present embodiment.
  • additives include fillers other than glass flakes having a thickness of 0.1 to 2 ⁇ m, light stabilizers, antioxidants, ultraviolet absorbers, fluorescent whitening agents, anti-dripping agents, antistatic agents, anti-fog agents, and the like.
  • antiblocking agents include antiblocking agents, fluidity improving agents, plasticizers, dispersants, antiviral agents, antibacterial agents, flame retardants and the like. Only one kind of these components may be used, or two or more kinds thereof may be used in combination.
  • the flame retardant is preferably a phosphorus-based flame retardant.
  • the phosphorus-based flame retardant examples include a phosphazene-based flame retardant, a phosphinate-based flame retardant, and a diphosphinate-based flame retardant.
  • the resin composition of the present embodiment contains a crystalline thermoplastic resin (preferably a polyamide resin), glass flakes having a thickness of 0.1 to 2 ⁇ m, and light transmission so that the total of each component is 100% by mass. The content of the sex dye, the nucleating agent, the copper compound, the alkali metal halide, the mold release agent, and other additives is adjusted.
  • the total of the crystalline thermoplastic resin, the glass flakes having a thickness of 0.1 to 2 ⁇ m, and the selectively added nucleating agent, copper compound, alkali metal halide, and mold release agent is the resin composition.
  • An embodiment that occupies 99% by mass or more of the above is exemplified.
  • the resin composition of the present embodiment has a small warp when it is made into a molded product.
  • the amount of warpage of the molded product is preferably 2 mm or less, and more preferably 1 mm or less. It is preferably 0.9 mm or less, and more preferably 0.9 mm or less.
  • the amount of warpage is the difference between the height of the highest portion and the height of the lowest portion of the test piece when the molded product is placed on a reference table. For details, follow the description of the examples described later.
  • the lower limit of the warp amount is ideally 0 mm, but it is practically 0.05 mm or more.
  • the resin composition of the present embodiment is preferably formed into an ISO tensile test piece having a thickness of 4 mm and has a high bending strength measured in accordance with ISO 178.
  • the bending strength is preferably 200 MPa or more.
  • the higher the upper limit, the better, but for example, 500 MPa or less is practical.
  • the resin composition of the present embodiment is preferably formed into an ISO tensile test piece having a thickness of 4 mm and has a high flexural modulus measured in accordance with ISO178.
  • the flexural modulus is preferably 9000 MPa or more. The higher the upper limit, the better, but for example, 20000 MPa or less is practical.
  • the method for producing the resin composition of the present embodiment is not particularly limited, but a method of using a single-screw or twin-screw extruder having equipment capable of degassing from the vent port as a kneader is preferable.
  • the above-mentioned crystalline thermoplastic resin component, glass flakes having a thickness of 0.1 to 2 ⁇ m, a light-transmitting dye, and other additives to be blended as necessary may be collectively supplied to a kneader or crystallized. Other compounding components may be sequentially supplied to the thermoplastic resin.
  • Inorganic fillers such as glass flakes having a thickness of 0.1 to 2 ⁇ m are preferably supplied from the middle of the extruder in order to prevent crushing during kneading. Further, two or more kinds of components selected from each component may be mixed and kneaded in advance.
  • the light-transmitting dye is a thermoplastic resin such as polyamide 6 and polyamide 66, and a masterbatch is prepared in advance and then kneaded with other components (thermoplastic resin or the like) to carry out the present embodiment.
  • the resin composition in the form may be adjusted.
  • the method for producing a molded product using the resin composition of the present embodiment is not particularly limited, and is a molding method generally used for thermoplastic resins, that is, molding such as injection molding, hollow molding, extrusion molding, and press molding. The method can be applied.
  • the resin composition of the present embodiment is particularly suitable for a method of molding using a mold. Further, it is suitable for a molding method of cooling by a mold.
  • the kit of the present embodiment has the resin composition of the present embodiment and a light-absorbing resin composition containing a thermoplastic resin and a light-absorbing dye.
  • the kit of this embodiment is preferably used for producing a molded product by laser welding. That is, the resin composition contained in the kit serves as a light-transmitting resin composition, and the molded product obtained by molding the light-transmitting resin composition is a transparent resin member for laser light during laser welding. Become. On the other hand, a molded product obtained by molding a light-absorbing resin composition is an absorbing resin member for laser light during laser welding.
  • the light-absorbing resin composition used in the present embodiment contains a thermoplastic resin (preferably a crystalline thermoplastic resin) and a light-absorbing dye.
  • thermoplastic resin include polyamide resin, olefin resin, vinyl resin, styrene resin, acrylic resin, polyphenylene ether resin, polyester resin, polycarbonate resin, polyacetal resin, etc., and the compatibility with the resin composition is high. From a good point of view, a polyamide resin, a polyacetal resin, and a polyester resin (preferably polybutylene terephthalate resin) are particularly preferable, and a polyamide resin is more preferable. Further, the thermoplastic resin may be one kind or two or more kinds.
  • the type of the polyamide resin used in the light-absorbing resin composition is not specified, but the xylylenediamine-based polyamide resin is preferable.
  • the light-absorbing resin composition may also contain an inorganic filler.
  • the inorganic filler include fillers capable of absorbing laser light such as glass flakes (particularly glass flakes having a thickness of 0.1 to 2 ⁇ m), glass fibers, carbon fibers, and inorganic powder coated with a material that absorbs laser.
  • the light-absorbing dye is a dye that is less likely to transmit a laser beam during laser welding than a light-transmitting dye.
  • the light-absorbing dye examples include those having a maximum absorption wavelength in the range of the laser light wavelength to be irradiated, for example, the wavelength range of 800 nm to 1100 nm.
  • 0.07 part by mass of the dye is blended with 100 parts by mass of the polyamide resin (MP10 synthesized in the examples described later), and the temperature is set at 280 ° C. of the extruder.
  • examples thereof include dyes having a light transmittance of less than 2% at a wavelength of 1060 mm measured by the method described in Examples described later using melt-kneaded pellets. The mold temperature at this time is 110 ° C.
  • the light-absorbing pigment examples include black pigments such as carbon blacks (for example, acetylene black, lamp black, thermal black, furnace black, channel black, Ketjen black, etc.), iron oxide red, and the like.
  • black pigments such as carbon blacks (for example, acetylene black, lamp black, thermal black, furnace black, channel black, Ketjen black, etc.), iron oxide red, and the like.
  • red pigments orange pigments such as molybdate orange, white pigments such as titanium oxide
  • organic pigments yellow pigments, orange pigments, red pigments, blue pigments, green pigments, etc.
  • inorganic pigments are generally preferable because they have a strong hiding power, black pigments are more preferable, and carbon black is even more preferable.
  • Two or more of these light-absorbing dyes may be used in combination.
  • the content of the light-absorbing dye is preferably 0.01 to 30 parts by mass with respect to 100 parts by mass of the thermoplastic resin.
  • the kit of the present embodiment has 80% by mass or more in common of the component excluding the light-transmitting dye in the laser-welded transparent resin composition and the component excluding the light-absorbing dye in the light-absorbing resin composition. It is preferable, 90% by mass or more are common, and 95 to 100% by mass is more preferable.
  • a molded product (transmissive resin member) formed from the laser welding transparent resin composition of the present embodiment and a molded product (absorbent resin member) formed from the light-absorbing resin composition are used. Molded products can be manufactured by laser welding. By laser welding, the transmissive resin member and the absorbent resin member can be firmly welded without using an adhesive.
  • the shape of the member is not particularly limited, but since the members are joined by laser welding and used, the shape usually has at least a surface contact point (flat surface, curved surface). In laser welding, the laser light transmitted through the transmissive resin member is absorbed by the absorbent resin member and melted, and both members are welded.
  • the thickness of the member through which the laser light is transmitted (the thickness in the laser transmission direction in the portion through which the laser light is transmitted) can be appropriately determined in consideration of the application, the composition of the resin composition, and the like, and is, for example, 5 mm. It is less than or equal to, preferably 4 mm or less.
  • the lower limit of the thickness of the member through which the laser is transmitted is, for example, 0.01 mm or more.
  • the laser light source used for laser welding can be determined according to the light absorption wavelength of the light-absorbing dye, and a laser having a wavelength in the range of 800 to 1100 nm is preferable, and for example, a semiconductor laser or a fiber laser can be used.
  • the welded portions of both are brought into mutual contact with each other.
  • the welding points of both are in surface contact, and may be a combination of planes, curved surfaces, or a plane and a curved surface.
  • the laser beam is irradiated from the transmission resin member side.
  • a lens may be used to condense the laser beam on the interface between the two. The focused beam passes through the transmissive resin member, is absorbed near the surface of the absorbent resin member, generates heat, and melts.
  • the molded product in which the transmissive resin member and the absorbent resin member are welded in this way has high welding strength.
  • the molded product in the present embodiment is intended to include not only finished products and parts but also members forming a part thereof.
  • the molded product obtained by laser welding in the present embodiment has good mechanical strength, high welding strength, and less damage to the resin due to laser light irradiation. It can be applied to electrical / electronic equipment parts, office automation (OA) equipment parts, home appliance equipment parts, mechanical mechanism parts, vehicle mechanism parts, and the like.
  • OA office automation
  • the resin composition and kit of the present embodiment are suitable for hollow parts for vehicles such as an in-vehicle camera housing.
  • Raw Material MP10 Polyamide resin composed of methylylenediamine, paraxylylenediamine (MP molar ratio: 7: 3) and sebacic acid, synthesized according to paragraph 0071 of JP-A-2018-119043.
  • the amount of heat of crystallization measured by the following method was ⁇ 0.5 mJ / mg.
  • MP6 Polyamide resin composed of metaxylylenediamine, paraxylylenediamine (molar ratio: 7: 3) and adipic acid, synthesized according to paragraph 0072 of JP-A-2018-119043.
  • the amount of heat of crystallization measured by the following method was ⁇ 0.5 mJ / mg.
  • PA66 Polyamide 66, Manufacturer: INVISTA Nylon Polymer, INVISTA U4800, The amount of heat of crystallization measured by the following method was ⁇ 0.9 mJ / mg.
  • the amount of heat of crystallization was measured using a differential scanning calorimetry device as follows. ⁇ Crystallization calorie> A test piece (60 ⁇ 60 ⁇ 1 mm thick) obtained by pelletizing the synthesized resin and molding it at a cylinder temperature of 280 ° C. was subjected to differential scanning calorimetry (DSC) at a heating rate of 10 ° C./min and 30 to 300 ° C. The amount of heat of crystallization was measured in. The cylinder temperature was 260 ° C.
  • the inorganic filler is charged into the above-mentioned twin-screw extruder from the side of the extruder using a vibrating cassette waving feeder (CE-V-1B-MP manufactured by Kubota), and melt-kneaded with resin components and the like. Then, pellets (resin composition) for forming a light transmitting member were obtained.
  • the pellet for forming a light transmitting member obtained above is dried at 120 ° C. for 4 hours, and then a test piece for a light transmitting member (60 mm ⁇ 60 mm ⁇ ) is used using an injection molding machine (NEX140III-12EG manufactured by Nissei Plastic Industry Co., Ltd.). 1.0 mm thick) was produced.
  • the pellets obtained by the above manufacturing method were dried at 120 ° C. for 4 hours, and then an ISO tensile test piece (4 mm thick) was injection-molded by an injection molding machine (NEX140III-12EG manufactured by Nissei Plastic Industry Co., Ltd.). ..
  • the cylinder temperature was 260 ° C. when MP10 was used as the polyamide resin, 280 ° C. when MP6 was used, 280 ° C. when PA66 was used, and the mold temperature was polyamide, which is the main component of the resin component.
  • the temperature was 130 ° C (MP6), 110 ° C (MP10), and 90 ° C (PA66) depending on the type of resin.
  • the test piece for the light transmitting member (60 mm ⁇ 60 mm ⁇ 1.0 mm thickness) obtained above is placed on a reference table, and the height of the highest part (Max height, unit: mm) and the lowest part of the test piece are The height (Min height, unit: mm) was measured using a three-dimensional shape measuring machine, and the difference was calculated. Specifically, as shown in FIG. 1, the height of the reference table 1 is set to 0 mm, and the highest portion 3 and the lowest portion (usually) of the height when the test piece 2 for the light transmitting member is placed. The difference between the ends of the test pieces) was measured as the warp 4.
  • VR-3200 manufactured by KEYENCE Corporation was used.
  • the light transmittance of the test piece for a light transmitting member (60 mm ⁇ 60 mm ⁇ 1.0 mm thickness) obtained above was measured at a wavelength of 1060 nm. The unit is shown in%.
  • the light transmittance was measured using LMT-F1LC-PA manufactured by Tsubosaka Electric.
  • the molded product formed from the resin composition of the present invention had a high light transmittance (Examples 1 to 6).
  • the light transmittance was low (Comparative Examples 1 to 6)
  • the molded product formed from the resin composition of the present invention can maintain high mechanical strength and can effectively suppress warpage.
  • the resin composition according to Example 1 was not blended with a light-transmitting dye, but instead was blended with 3 parts by mass of carbon black masterbatch (carbon black # 45 manufactured by Mitsubishi Chemical Co., Ltd.) as a light-absorbing dye. The same procedure was carried out to obtain pellets for forming an absorbent resin member. Using the pellet for forming a light transmitting member obtained in Example 1 and the pellet for forming an absorbent resin member, laser welding was performed according to paragraphs 0072, 0073, and FIG. 1 of JP-A-2018-168346. rice field. It was confirmed that laser welding was performed properly.

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PCT/JP2021/019112 2020-05-25 2021-05-20 レーザー溶着用透過性樹脂組成物、キット、成形品および成形品の製造方法 Ceased WO2021241380A1 (ja)

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CN202410851862.9A CN118667330A (zh) 2020-05-25 2021-05-20 激光熔敷用透射性树脂组合物、组合物组合、成型品及成型品的制造方法
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EP21812851.0A EP4159789A4 (en) 2020-05-25 2021-05-20 Permeable resin composition for laser welding, kit, molded article, and method for producing molded article
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