WO2021095649A1 - Article moulé en résine, article moulé en résine pour vitre de véhicule, et procédé pour produire un article moulé en résine - Google Patents

Article moulé en résine, article moulé en résine pour vitre de véhicule, et procédé pour produire un article moulé en résine Download PDF

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Publication number
WO2021095649A1
WO2021095649A1 PCT/JP2020/041512 JP2020041512W WO2021095649A1 WO 2021095649 A1 WO2021095649 A1 WO 2021095649A1 JP 2020041512 W JP2020041512 W JP 2020041512W WO 2021095649 A1 WO2021095649 A1 WO 2021095649A1
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WO
WIPO (PCT)
Prior art keywords
layer
resin molded
hard coat
molded article
resin
Prior art date
Application number
PCT/JP2020/041512
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English (en)
Japanese (ja)
Inventor
信行 堀川
康章 堤
Original Assignee
株式会社小糸製作所
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Publication date
Application filed by 株式会社小糸製作所 filed Critical 株式会社小糸製作所
Priority to JP2021556067A priority Critical patent/JPWO2021095649A1/ja
Publication of WO2021095649A1 publication Critical patent/WO2021095649A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/06—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/02—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/16—Layered products comprising a layer of synthetic resin specially treated, e.g. irradiated
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/18—Handling of layers or the laminate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/02—Physical, chemical or physicochemical properties
    • B32B7/022—Mechanical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B60—VEHICLES IN GENERAL
    • B60J—WINDOWS, WINDSCREENS, NON-FIXED ROOFS, DOORS, OR SIMILAR DEVICES FOR VEHICLES; REMOVABLE EXTERNAL PROTECTIVE COVERINGS SPECIALLY ADAPTED FOR VEHICLES
    • B60J1/00—Windows; Windscreens; Accessories therefor
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/046—Forming abrasion-resistant coatings; Forming surface-hardening coatings

Definitions

  • the present invention relates to a resin molded product, a resin molded product for a vehicle window, and a method for manufacturing the resin molded product.
  • the resin material has lower scratch resistance and weather resistance than the glass material, there is a problem that scratches and discoloration are likely to occur due to the friction of the wiper and the ultraviolet rays contained in the sunlight.
  • a technique has been developed in which a special hard coat is applied to the surface of the resin material to improve the scratch resistance and weather resistance of the surface of the resin material.
  • a method of applying an acrylic hard coat to a resin material a method of applying a silicone hard coat on a resin material after forming a primer layer for preventing peeling, and a method of applying a silicone hard coat to the surface of the hard coat for reinforcement.
  • Techniques such as a method of forming a hard layer with silicon dioxide (SiO2) are disclosed.
  • the method of forming a hard layer for reinforcement is particularly higher than the conventional glass material ( ⁇ Haze value after taber wear is about 2%) in the taber wear test for evaluating scratch resistance. It is known to impart scratch resistance.
  • the vacuum film forming process is a method of forming a hard layer by spraying a raw material gas containing a hard layer component on a base material in a vacuum chamber and depositing a film by a chemical reaction on the surface of the base material or the gas phase.
  • the photomodification method is a method of irradiating a base material with ultraviolet rays at atmospheric pressure while applying nitrogen flow to an already coated silicone-based hard coat to modify the surface to form a hard layer.
  • the bond chain (Si—C bond chain) of the polymer is cut, and oxygen atoms slightly present in the atmosphere, hard coat, and base material are formed. It adopts the principle that silicon atoms are recombined to form a hard layer containing silicon dioxide as a main component.
  • Patent Documents 1 to 3 a hard layer is formed by using a vacuum film forming process such as a CVD method.
  • a vacuum film forming process such as a CVD method.
  • a molecular resin laminate is introduced.
  • Patent Document 2 introduces a polymer resin laminate in which a silicon oxide layer is laminated on a crosslinked resin layer by a vacuum film forming process such as a CVD method.
  • the hard coat layer formed on at least one surface of the transparent resin substrate includes an organic polymer thin film formed by vacuum vapor deposition polymerization.
  • the optical reforming method is superior in terms of cost because it does not require a large-scale device such as a vacuum chamber.
  • the vacuum film forming process since the hard layer is laminated by spraying the raw material gas, an interface is formed between the hard layer and the hard coat layer, and the hard layer may be peeled off at the interface portion.
  • the light reforming method there is no interface between the hard layer and the hard coat layer, and peeling does not occur.
  • the photo-modifying method is also excellent in scratch resistance and weather resistance.
  • a hard layer is formed by using a light reforming method.
  • a hard coat containing a silicone-based organopolysiloxane is irradiated with ultraviolet rays having a wavelength of 200 nm or less to increase the hardness of a portion having a thickness of less than 0.6 ⁇ m from the surface to form a hard layer.
  • a hard coating agent composition containing an organopolysiloxane is applied to at least one surface of a resin substrate to form a coating film, and the coating film is subjected to heat treatment, light irradiation treatment, oxidation treatment and the like. The method of forming a hard layer is introduced.
  • Patent Document 6 a silicone-based polymer is applied to a resin module substrate to form a hard coat, and the surface of the hard coat is irradiated with ultraviolet rays having a wavelength of 360 nm or less to form a hard layer.
  • the module is introduced.
  • an object of the present invention is to provide a resin molded product having improved scratch resistance and improved weather resistance, a resin molded product for a vehicle window, and a method for manufacturing the resin molded product.
  • the present invention employs the following means.
  • a step of coating at least a part of the transparent resin base material with a hard coat layer and a step of irradiating the surface of the hard coat layer with ultraviolet light to form a modified layer having a predetermined hardness or more are provided.
  • the resin molded product the resin molded product for vehicle windows, and the method for producing the resin molded product of the present invention, by setting the thickness of the modified layer to 70 nm or more, the scratch resistance is enhanced and the weather resistance is also improved. It becomes possible.
  • FIG. 1 is a schematic view of a rear module showing an embodiment of a resin molded product for a vehicle window of the present invention, and a vehicle equipped with the rear module.
  • FIG. 2 is a schematic view showing the structure of the resin layer according to the rear module of FIG.
  • FIG. 3 is a graph showing the correlation between the integrated light intensity and the surface Young's modulus.
  • FIG. 4 is a graph showing the correlation between the surface Young's modulus and the Taber wear test result.
  • FIG. 5 is a graph showing the correlation between illuminance and Young's modulus under a constant integrated light intensity.
  • FIG. 6 is a graph showing the correlation between the illuminance and the thickness of the modified layer under a constant integrated light intensity.
  • FIG. 1 is a schematic view of a rear module showing an embodiment of a resin molded product for a vehicle window of the present invention, and a vehicle equipped with the rear module.
  • FIG. 2 is a schematic view showing the structure of the resin layer according to the rear module of
  • FIG. 7 is a list showing the results of an experiment in which the illuminance, the irradiation distance, and the irradiation time were changed under a constant integrated light intensity.
  • FIG. 8 is a table showing a conventional hard coat.
  • FIG. 9 is a table comparing conventional methods for forming a hard layer.
  • FIG. 10 is a table showing the scratch resistance and weather resistance of the hard layer formed by the conventional method for each integrated light intensity.
  • the rear module 1 includes a rear window 3 as a resin molded product for a vehicle window, a rear combination lamp (RCL) 4, a window cleaner 5, a high mount stop lamp (HMSL) 6, and a license plate. It is composed of a lamp (LPL) 7, a display 8, and the like, and is fitted into the vehicle body 2 so as to cover the rear portion of the vehicle. It is also possible to preferably adopt the spoiler 9 formed on the rear module 1.
  • the weight of the entire vehicle can be reduced, and a complicated three-dimensional shape can be freely formed to improve the design of the vehicle appearance. Further, by integrating the parts at the rear of the vehicle into a module, the man-hours for assembling the vehicle can be reduced and the cost can be reduced.
  • the surface of the base 10 made of a polycarbonate resin, the primer layer 11 made of an acrylic resin, the hard coat layer 12 made of a silicone polymer, and the hard coat layer 12 is exposed to ultraviolet light. It is composed of a resin laminate including a modified layer 13 which has been photomodified by the above and modified into a hard layer, and the modified layer 13 is formed on the outside of the vehicle interior.
  • the primer layer 11 mainly has a role of relaxing the stress between the substrate 10 and the hard coat layer 12 to improve the adhesion between the substrate 10 and the hard coat layer 12, but also has the effect of improving the weather resistance.
  • the hard coat layer 12 has a hardness for protecting the substrate 10 and has an effect of improving weather resistance.
  • the modified layer 13 has an effect of improving scratch resistance.
  • the primer layer 11 is formed by applying a primer solvent made of an acrylic resin to the surface of the substrate 10 by a dip coating method (wet method), drying at room temperature, and heating for a predetermined time to cure and dry.
  • the hard coat layer 12 is formed by applying a hard coat solvent of a silicone polymer on the primer layer 11 by a dip coat method, drying at room temperature, heating for a predetermined time, and curing and drying.
  • the modified layer 13 is formed by photomodifying with ultraviolet light.
  • a high-output, high-illuminance excimer lamp capable of irradiating ultraviolet light having a peak at a wavelength of 172 nm is adopted.
  • the vicinity of the surface of the hard coat layer 12 is photomodified and hardened, and the modified layer 13 as a hard layer is formed.
  • the ultraviolet light has high output and high illuminance.
  • the modified layer 13 can be formed thicker than when low-power, low-illuminance ultraviolet light is used.
  • the modified layer 13 preferably has a thickness of 70 nm or more. By having a thickness of 70 nm or more, it is possible to form the modified layer 13 having weather resistance while improving the scratch resistance on the surface of the modified layer 13.
  • the hardness of the modified layer which is a hard layer, is determined by the predetermined measurement conditions by the nano indenter (device: KLA G200 type nano indenter, high resolution DCM-II head (maximum load: 30 mN), Berkovich indenter, measurement mode: continuous rigidity.
  • CSM measurement method
  • indentation depth 1000 nm
  • vibration frequency 65 Hz
  • vibration amplitude 1 nm
  • the term "modified layer” as used herein refers to a portion having a Young's modulus of 5 GPa or more, which indicates an elastic modulus.
  • the scratch resistance is confirmed by a taber wear test (wear wheel CS-10F, 0.5 kg load). It can be said that the smaller the ⁇ Haze value (%) around 1000 rotations of the taber wear, the less likely it is to be scratched.
  • Super UV test (SUV test, device: Eye Super UV tester S-UV-161 (manufactured by Iwasaki Electric)), which is an accelerated weather resistance test, test method: irradiation ⁇ darkness ⁇ repeated dew condensation, illuminance at the time of irradiation : Confirm the life at 900 w / m2 (300 to 400 nm)).
  • the integrated light amount is obtained by the product of illuminance and time, but as shown in FIG. 5, when the integrated light amount is the same, there is almost no effect of illuminance on the surface Young's modulus of the modified layer. That is, the surface Young's modulus is the same regardless of whether the ultraviolet rays having a strong illuminance are irradiated for a short time or the ultraviolet rays having a weak illuminance are irradiated for a long time if the integrated light amount is finally the same.
  • the thickness of the modified layer in the depth direction becomes thicker as the illuminance becomes stronger when the integrated light amount is the same. It is considered that this is because the stronger the illuminance of the ultraviolet rays to be irradiated, the deeper the light penetrates into the hard coat layer and the reform proceeds.
  • the thickness of the modified layer was 60 nm even when the same integrated light amount was irradiated, whereas in Example 1 and Example 2, the thickness could be increased to 70 nm and 100 nm, respectively, as compared with the conventional example.
  • the surface Young's modulus of these samples was able to form a modified layer of 7.8 GPa or more, and even in the Taber wear test, the ⁇ Haze value was recorded as 1.3% even in the conventional example, which is sufficient scratch resistance. It can be seen that it has.
  • the weather resistance was improved in Examples 1 and 2 in which the modified layer was thickened. doing. It is considered that the thicker the modified layer, the gentler the slope of Young's modulus in the modified layer, and the stress applied to the film is relaxed, so that the weather resistance is improved.
  • the thickness of the modified layer As a result of the above comparative test, by setting the thickness of the modified layer to 70 nm or more, it is possible to form a modified layer having high weather resistance without impairing high scratch resistance.
  • the method for producing the car resin molded product, the car window resin molded product, and the resin molded product of the present invention is not limited to the above embodiment, and the combination and material of the resin and the constituent coating layer are appropriately changed. It is also possible to arbitrarily change the configuration of each part within a range that does not deviate from the gist of the present invention.
  • the range in which the modified layer is formed may be limited to a specific location such as a wiper sliding portion.
  • a transparent resin substrate such as an acrylic resin, a cycloolefin polymer (COP), or polyethylene terephthalate (PET) can be used for the substrate 10.
  • the antifogging layer may be formed by superimposing it on the hard coat layer 12. Further, an antifouling functional layer may be provided on the hard coat layer 12, the modified layer 13, and the antifogging layer.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Medicinal Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Laminated Bodies (AREA)
  • Coating Of Shaped Articles Made Of Macromolecular Substances (AREA)

Abstract

L'invention concerne : un article moulé en résine ayant une résistance à l'abrasion supérieure et une résistance aux intempéries améliorée ; un article moulé en résine pour une vitre de véhicule ; et un procédé de production d'un article moulé en résine.　Un module arrière 1, qui est un article moulé en résine, est constitué : d'un substrat 10 constitué d'une résine de polycarbonate ; d'une couche de primaire 11 constituée d'une résine acrylique et formée sur le substrat par application d'un solvant et en laissant sécher le solvant ; et d'une couche de revêtement dur 12 constituée d'un polymère à base de silicone et formée sur la couche de primaire par application d'un solvant et en laissant sécher le solvant. Le module arrière comprend également une couche modifiée 13 dans laquelle une couche dure est formée par irradiation et modification de la couche de revêtement dur 12 par des rayons UV. La couche modifiée 13 est modifiée avec une lumière ultraviolette à éclairement élevé de sorte que la couche modifiée 13 a une épaisseur d'au moins 70 nm, ce qui permet d'obtenir une couche dure hautement résistante aux intempéries tout en conservant une résistance élevée à l'abrasion.
PCT/JP2020/041512 2019-11-12 2020-11-06 Article moulé en résine, article moulé en résine pour vitre de véhicule, et procédé pour produire un article moulé en résine WO2021095649A1 (fr)

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JP2019-204408 2019-11-12
JP2019204408 2019-11-12

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114761229A (zh) * 2019-12-05 2022-07-15 株式会社小糸制作所 树脂成型品、车窗用树脂成型品以及树脂成型品的制造方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012014653A1 (fr) * 2010-07-27 2012-02-02 コニカミノルタホールディングス株式会社 Film barrière contre les gaz, procédé de production de film barrière contre les gaz et dispositif électronique
JP2014218103A (ja) * 2013-05-02 2014-11-20 株式会社レニアス 発熱層を有する車両用樹脂ガラスとその製造方法
JP2016030392A (ja) * 2014-07-29 2016-03-07 旭硝子株式会社 ハードコート層付き樹脂基板およびハードコート層付き樹脂基板の製造方法
WO2017195350A1 (fr) * 2016-05-13 2017-11-16 株式会社レニアス Feuille de verre de résine et son procédé de fabrication
JP2019171280A (ja) * 2018-03-28 2019-10-10 株式会社レニアス 樹脂ガラス板及びその製造方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012014653A1 (fr) * 2010-07-27 2012-02-02 コニカミノルタホールディングス株式会社 Film barrière contre les gaz, procédé de production de film barrière contre les gaz et dispositif électronique
JP2014218103A (ja) * 2013-05-02 2014-11-20 株式会社レニアス 発熱層を有する車両用樹脂ガラスとその製造方法
JP2016030392A (ja) * 2014-07-29 2016-03-07 旭硝子株式会社 ハードコート層付き樹脂基板およびハードコート層付き樹脂基板の製造方法
WO2017195350A1 (fr) * 2016-05-13 2017-11-16 株式会社レニアス Feuille de verre de résine et son procédé de fabrication
JP2019171280A (ja) * 2018-03-28 2019-10-10 株式会社レニアス 樹脂ガラス板及びその製造方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114761229A (zh) * 2019-12-05 2022-07-15 株式会社小糸制作所 树脂成型品、车窗用树脂成型品以及树脂成型品的制造方法

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