Process for the production of an effect pigment preparation, a thermoplastic resin composition comprising the effect pigment preparation and a coating material or ink comprising the effect pigment preparation
By mixing effect pigments with liquid polyα-olefins in a specific ratio at room temperature, the prepared effect pigments solved the compatibility and dispersibility problems in thermoplastic resin compositions, achieving good mixing and uniform dispersion without heating.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- TOYO ALUMINIUM KK
- Filing Date
- 2024-11-01
- Publication Date
- 2026-05-29
AI Technical Summary
Existing technologies require heating and mixing when incorporating effect pigments into thermoplastic resin compositions, and their compatibility with thermoplastic resins is insufficient, resulting in inconvenient mixing and poor dispersibility.
Effect pigments are mixed with polyalphaolefins that are liquid at a specific temperature in a specific ratio to prepare effect pigment preparations. This ensures that the mixture is mixed at room temperature and is compatible with thermoplastic resins. The resulting effect pigment preparations contain more than 99% effect pigments and 5-25% polyalphaolefins, with a kinematic viscosity of less than 4000 mm²/s.
It achieves good compatibility and uniform dispersion with thermoplastic resins without the need for heating, and is suitable for thermoplastic resin compositions and solvent-based coatings, improving mixing efficiency and dispersion effect.
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Figure CN122122252A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to effect pigment preparations used in coatings and inks for purposes such as imparting gloss and visual effects, and particularly to effect pigment preparations that do not require heating during raw material mixing, are compatible with thermoplastic resins, and can be easily incorporated into thermoplastic resins, thermoplastic resin compositions containing effect pigment preparations, and methods for manufacturing coatings or inks containing effect pigment preparations. Background Technology
[0002] In the past, effect pigments were used for the purpose of imparting visual effects such as gloss to surface coatings. Effect pigments refer to all pigments that typically have a thin, plate-like structure and provide special decorative color effects to surface coatings. Examples of effect pigments include pure metallic pigments such as aluminum, iron, or copper; mica coated with titanium dioxide; mica coated with iron oxide; mica coated with mixed oxides; and interference pigments or liquid crystal pigments such as aluminum coated with metal oxides.
[0003] In addition, in order to incorporate effect pigments into thermoplastic resin compositions as effect pigment preparations, commercially available manufacturers heat solid wax above its melting point, add effect pigments to it, and mix them to form granular or particulate effect pigment preparations.
[0004] For example, Japanese Patent Application Publication No. 2010-121092 (Patent Document 1) discloses a masterbatch formed into granules using polyethylene wax and linear low-density polyethylene resin as an effect pigment preparation. Furthermore, as disclosed in Patent Document No. WO2015 / 169502 (Patent Document 2), granules are formed by mixing metallic pigments with water-soluble resins such as polyvinylpyrrolidone and then compressing them.
[0005] Existing technical documents
[0006] Patent documents
[0007] Patent Document 1: Japanese Patent Application Publication No. 2010-121092
[0008] Patent Document 2: WO2015 / 169502 Summary of the Invention
[0009] The problem that the invention aims to solve
[0010] However, since the masterbatch described in Patent Document 1 melts the wax and resin used, heating is required during mixing. On the other hand, the granules described in Patent Document 2 use a water-soluble resin in order to manufacture without heating, which sometimes results in insufficient compatibility with the resin used in the thermoplastic resin composition.
[0011] Therefore, the present invention was made in view of the above circumstances, and its object is to provide an effect pigment preparation that does not require heating when mixing raw materials, is energy-efficient, and is compatible with thermoplastic resins.
[0012] Methods for solving problems
[0013] In order to solve the above problems, the inventors conducted repeated and in-depth research on the composition of the effect pigment preparations. As a result, they found that if the effect pigments are combined with polyα-olefins that are liquid at a specific temperature in a specific ratio, the above problems can be solved, thus completing the present invention.
[0014] That is, according to the present invention, an effect pigment preparation is provided, characterized in that it contains a total of 99% by mass or more of effect pigment and polyalphaolefin, wherein the polyalphaolefin is liquid at 25°C, and relative to the effect pigment preparation, the effect pigment is 75% by mass or more and 95% by mass or less, the polyalphaolefin is 5% by mass or more and 25% by mass or less, and the volatile organic compound is 1% by mass or less.
[0015] The effect pigments of the present invention do not require heating during raw material mixing, are compatible with thermoplastic resins, and therefore can be easily incorporated into thermoplastic resins. Furthermore, the effect pigments of the present invention exhibit extremely excellent dispersibility not only when incorporated into thermoplastic resin compositions, but also when used in solvent-based coatings.
[0016] In this invention, the kinematic viscosity of the polyα-olefin at 40°C is preferably 4000 mm⁻¹. 2 / s or less.
[0017] In this invention, the effect pigment is preferably a metal, a metal oxide, a metal hydroxide, or a mixture thereof. Furthermore, the effect pigment is preferably coated with a resin, a metal oxide, a metal hydroxide, or a mixture thereof.
[0018] Furthermore, the effect pigment preferably has a colored pigment layer on its surface. Additionally, the colored pigment layer preferably contains resin, metal oxide, metal hydroxide, or a mixture thereof.
[0019] The effect pigment preparation of the present invention does not require heating during raw material mixing and is compatible with thermoplastic resins. Therefore, it can also be used as a thermoplastic resin composition by being incorporated into thermoplastic resins.
[0020] In addition, the present invention also relates to a method for manufacturing coatings or inks containing effect pigment preparations as described above.
[0021] Invention Effects
[0022] According to the present invention, there are provided effect pigment preparations that do not require heating during raw material mixing, are compatible with thermoplastic resins, and can be easily incorporated into thermoplastic resins; thermoplastic resin compositions containing effect pigment preparations; and methods for manufacturing coatings or inks containing effect pigment preparations. Furthermore, the effect pigment preparations of the present invention not only exhibit excellent uniform dispersion during incorporation into thermoplastic resin compositions, but also exhibit excellent uniform dispersion when used in solvent-based coatings. Attached Figure Description
[0023] Figure 1 This is a photograph of the effect pigment preparation (in granular form) from Example 1.
[0024] Figure 2 It means to Figure 1 A photograph of the mixture in the effect pigment preparation of Example 1, immediately after the diluent was added.
[0025] Figure 3 It means to Figure 2 A photograph of the experimental coating after the mixture of Example 1 has been stirred.
[0026] Figure 4 This is a photograph of the effect pigment preparation (in granular form) of Comparative Example 1.
[0027] Figure 5 It means to Figure 4 A photograph of the mixture in Comparative Example 1, showing the state of the effect pigment preparation immediately after the diluent was added.
[0028] Figure 6 It means to Figure 5 A photograph of the mixture of Comparative Example 1 after stirring. Detailed Implementation
[0029] Hereinafter, with reference to the accompanying drawings, a method for manufacturing an effect pigment preparation, a thermoplastic resin composition comprising the effect pigment preparation, and a coating or ink comprising the effect pigment preparation according to one embodiment of the present invention will be described in detail. It should be noted that the present invention is not limited to the embodiments shown below, and various modifications can be made without departing from the technical concept of the present invention.
[0030] <Effect Pigment Preparations>
[0031] The effect pigment preparation of the present invention comprises an effect pigment and a poly-α-olefin (hereinafter also referred to as "PAO"), and is generally in solid form. The total amount of the effect pigment and PAO is 99% by mass or more. In addition, the effect pigment preparation is ideally free of volatile organic compounds, but since it is sometimes unavoidable to contain volatile organic compounds, it is generally preferred to be 1% by mass or less.
[0032] There are no particular limitations on the shape of the effect pigment preparation. For example, it can be made into granules, particles, small flakes, or sheets.
[0033] Effects Pigments
[0034] Effect pigments refer to all pigments that impart visual effects such as gloss. The effect pigments used in this invention are not particularly limited, and known effect pigments can be used, but pigments with glossy surfaces are preferred. The content of the effect pigment in the effect pigment preparation is preferably 75% by mass or more and 95% by mass or less, more preferably 80% by mass or more and 90% by mass or less. If the content of the effect pigment is less than 75% by mass, the content of components other than the effect pigment becomes relatively high, making it difficult to maintain a granular or similar form. Furthermore, this significantly limits the design freedom of coatings, thermoplastic resin compositions, etc., when used in such applications. On the other hand, if the content of the effect pigment exceeds 90% by mass, there is insufficient PAO, resulting in dust or an inability to maintain the shape of the effect pigment preparation.
[0035] As effect pigments with glossy properties, examples include not only metal flakes such as aluminum, titanium, copper, brass, and stainless steel, but also natural mica, synthetic mica, alumina flakes, and glass flakes. Aluminum or aluminum alloys, in particular, have high hiding power and are therefore suitable for use in this invention. Furthermore, effect pigments can be water-resistant treated with phosphorus compounds, molybdenum compounds, etc., or coated with resins, metal oxides, etc.
[0036] The shape of the effect pigment is not particularly limited, but it is preferred to be in the form of flakes, scales, discs, or elliptical discs.
[0037] There are no particular limitations on the size of the effect pigments; for example, they can be suitable for D-type volume distributions based on laser diffraction. 50 Particles ranging from 1 μm to 200 μm.
[0038] <Polyalpha-olefin>
[0039] The PAO used in this invention is liquid at 25°C. Because PAO is liquid at 25°C, it can be mixed with effect pigments without heating.
[0040] The content of PAO in the effect pigment preparation is preferably 5% by mass or more and 25% by mass or less, more preferably 10% by mass or more and 20% by mass or less. If the content of PAO is less than 5% by mass, the effect pigment preparation cannot be solidified; on the other hand, if the content of PAO exceeds 25% by mass, the effect pigment preparation may become fluid.
[0041] PAO is a homopolymer or copolymer obtained primarily by polymerizing α-olefins, wherein a portion of the backbone or side chain can be substituted with other substituents, or can be hydrogenated. As α-olefins, in addition to ethylene, propylene, 1-butene, 1-hexene, 1-octene, or longer-chain α-olefins, α-olefins with branched or cyclic structures in the carbon chain other than the terminal double bond, such as 3-methyl-1-butene and vinylcyclohexane, can also be used. Preferably, α-olefins with 4 or more carbon atoms and a straight chain, such as 1-butene, 1-hexene, and 1-octene, are preferred. Furthermore, as the catalyst used in the polymerization, any known catalyst, such as a Ziegler catalyst or a metallocene catalyst, can be used.
[0042] The kinematic viscosity of PAO at 40°C is preferably 4000 mm³ for operational purposes. 2 / s or less, preferably 3500mm 2 / s or less.
[0043] Examples of commercially available PAOs with the aforementioned viscosity include the SpectraSyn (registered trademark) series manufactured by ExxonMobil. These PAOs can be used individually or in combination. It should be noted that the kinematic viscosity at 40°C can be measured using a Canon-Fensk kinematic viscometer.
[0044] <Other Additives>
[0045] In addition to PAO, the effect pigment preparations of the present invention may also contain additives such as pigment dispersants and neutralizers as appropriate, within a range that does not impair the effects of the present invention.
[0046] <Method for manufacturing effect pigments>
[0047] The effect pigment preparation of the present invention is prepared by mixing effect pigments, PAO, and other pigments and additives as needed at room temperature to obtain a mixture, shaping the resulting mixture, and then drying it. Effect pigments are commercially available in the form of pastes containing solvents, but since the solvent is removed during drying, pastes containing the aforementioned effect pigments can also be directly mixed.
[0048] There are no particular limitations on the method of mixing effect pigments with PAO; for example, known methods such as kneading mixers can be used appropriately. There are also no particular limitations on the forming method of the mixture; known methods such as extrusion molding and injection molding can be used according to the desired shape, such as flakes, granules, pellets, or noodles. Drying also depends on the type and amount of solvent from the paste containing the effect pigments, as well as the shape and size of the formed granules, etc., and is generally carried out under reduced pressure or normal pressure at room temperature (approximately 23°C) to 200°C.
[0049] <Thermoplastic Resin Composition>
[0050] In another embodiment of the present invention, a thermoplastic resin composition can be obtained by adding and mixing the effect pigment preparation of the present invention into a thermoplastic resin. Furthermore, if the thermoplastic resin composition is molded, a molded article with the desired gloss can be produced.
[0051] The thermoplastic resin used in the thermoplastic resin composition of the present invention is not particularly limited as long as it is a known thermoplastic resin, for example, at least one resin selected from polyethylene, ABS, polycarbonate and the like can be used.
[0052] The amount of thermoplastic resin in the thermoplastic resin composition is not particularly limited. For example, when using the thermoplastic resin composition to manufacture molded articles based on injection molding or the like, the amount of effect pigment is preferably 0.01 parts by weight or more and 30 parts by weight or less relative to 100 parts by weight of the thermoplastic resin. If the amount of thermoplastic resin is less than 0.01 parts by weight, the coloring strength is weak, and the desired design may not be achieved. On the other hand, if the amount of thermoplastic resin exceeds 30 parts by weight, there is a tendency for a significant decrease in the mechanical strength of the molded article.
[0053] Alternatively, in this invention, the effect pigment preparation itself can be used as a masterbatch (a solid additive for plastics). However, when a specified thermoplastic resin and a pre-mixed thermoplastic resin composition are used as the masterbatch according to the application, the amount of the effect pigment preparation is preferably 20 parts by mass or more relative to 100 parts by mass of the thermoplastic resin. If the amount of the effect pigment preparation is less than 20 parts by mass, the tinting strength is weak, and the desired design may not be obtained.
[0054] <Inks and Coatings>
[0055] In another embodiment of this invention, the effect pigment preparations of this invention can also be used in coatings or inks. In this case, the coatings or inks are not particularly limited in terms of components other than the effect pigment preparations or their manufacturing methods, and known raw materials and manufacturing methods can be used.
[0056] [Example]
[0057] The present invention will be further described in detail below with reference to specific embodiments, but the present invention is not limited to these embodiments.
[0058] <Preparation of Effect Pigment Preparations>
[0059] [Example 1]
[0060] Add 500g of a paste containing aluminum flake pigment as an effect pigment (trade name: "7680NS", solids content 65% by mass, mineral oil content 35% by mass, average particle size 11μm, manufactured by Toyo Aluminum Co., Ltd.), and SpectraSyn (registered trademark) Elite 65 (kinematic viscosity 600 mmHg at 40°C) as a PAO to a twin-screw kneading mixer. 2 35.0 g (manufactured by Exxon Mobil) was mixed for 5 minutes. The resulting mixture was granulated using an extruder (Multi Granulator MG-55-2, manufactured by DALTON Corporation). The resulting granules were then transferred to an inert oven (IPHH-201, manufactured by ESPEC Corporation) heated to 120°C and dried under a nitrogen atmosphere for 2 hours to obtain the effect pigment preparation of Example 1.
[0061] The effect pigment content in the effect pigment preparation is 90.3% by mass. It should be noted that the residual heating components in the obtained effect pigment preparation were determined according to JISK 5906, and the result was 99.9% by mass. That is, the residual solvent component in the effect pigment preparation is 0.1% by mass.
[0062] [Example 2]
[0063] Add 500g of a paste containing aluminum flake pigment as an effect pigment (trade name: "5620NS", solids content 71% by mass, mineral oil content 29% by mass, average particle size 18μm, manufactured by Toyo Aluminum Co., Ltd.), and SpectraSyn (registered trademark) Elite 65 (kinematic viscosity 600 mmHg at 40°C) as a PAO to a twin-screw kneading mixer. 2 20.0 g of the mixture (manufactured by Exxon Mobil) was mixed for 5 minutes. The resulting mixture was granulated using an extruder (Multi Granulator MG-55-2, manufactured by DALTON Corporation). The resulting granules were then transferred to an inert oven (IPHH-201, manufactured by ESPEC Corporation) heated to 120°C and dried under a nitrogen atmosphere for 2 hours to obtain the effect pigment preparation of Example 2.
[0064] The effect pigment content in the effect pigment preparation is 94.7% by mass. It should be noted that the residual heating components in the obtained effect pigment preparation were determined according to JISK 5906, and the result was 100.0% by mass. That is, the residual solvent component in the effect pigment preparation is 0.0% by mass.
[0065] [Example 3]
[0066] Add 500g of a paste containing colored aluminum flake pigment as an effect pigment (trade name: "EMR-D46BLA", solids content 55% by mass, 2-propanol content 45% by mass, average particle size 18μm, manufactured by Toyo Aluminum Co., Ltd.), and SpectraSyn (registered trademark) Elite 65 (kinematic viscosity 600 mmHg at 40°C) as a PAO to a twin-screw kneading mixer. 2 80.0 g (manufactured by Exxon Mobil) was mixed for 5 minutes. The resulting mixture was shaped into granules using an extruder (Multi Granulator MG-55-2, manufactured by DALTON Corporation). The resulting granules were transferred to an inert oven (IPHH-201, manufactured by ESPEC Corporation) heated to 120°C and dried under a nitrogen atmosphere for 30 minutes to obtain the effect pigment preparation of Example 3.
[0067] The effect pigment content in the effect pigment preparation is 77.5% by mass. It should be noted that the residual heating components in the obtained effect pigment preparation were determined according to JISK 5906, and the result was 100.0% by mass. That is, the residual solvent component in the effect pigment preparation is 0.0% by mass.
[0068] [Example 4]
[0069] Add 500g of a paste containing colored aluminum flake pigment as an effect pigment (trade name: "EMR-D46GRA", solids content 55% by mass, 2-propanol content 45% by mass, average particle size 18μm, manufactured by Toyo Aluminum Co., Ltd.), and SpectraSyn (registered trademark) Elite 65 (kinematic viscosity 600 mmHg at 40°C) as a PAO to a twin-screw kneading mixer. 260.0 g of the mixture (manufactured by Exxon Mobil) was mixed for 5 minutes. The resulting mixture was granulated using an extruder (Multi Granulator MG-55-2, manufactured by DALTON Corporation). The resulting granules were then transferred to an inert oven (IPHH-201, manufactured by ESPEC Corporation) heated to 120°C and dried under a nitrogen atmosphere for 30 minutes to obtain the effect pigment preparation of Example 4.
[0070] The effect pigment content in the effect pigment preparation is 82.1% by mass. It should be noted that the residual heating components in the obtained effect pigment preparation were determined according to JISK 5906, and the result was 100.0% by mass. That is, the residual solvent component in the effect pigment preparation is 0.0% by mass.
[0071] [Example 5]
[0072] Add 500g of a paste containing silica-coated aluminum flake pigment as an effect pigment (trade name: "EMR-D5660", 50% by weight solids, 50% by weight propylene glycol monomethyl ether, average particle size 10μm, manufactured by Toyo Aluminum Co., Ltd.), and SpectraSyn (registered trademark) Elite 65 (kinematic viscosity 600 mmHg at 40°C) as a PAO to a twin-screw kneading mixer. 2 40.0 g of the mixture (manufactured by Exxon Mobil) was mixed for 5 minutes. The resulting mixture was granulated using an extruder (Multi Granulator MG-55-2, manufactured by DALTON Corporation). The resulting granules were then transferred to an inert oven (IPHH-201, manufactured by ESPEC Corporation) heated to 120°C and dried under a nitrogen atmosphere for 1 hour to obtain the effect pigment preparation of Example 5.
[0073] The effect pigment content in the effect pigment preparation is 86.2% by mass. It should be noted that the residual heating components in the obtained effect pigment preparation were determined according to JISK 5906, and the result was 100.0% by mass. That is, the residual solvent component in the effect pigment preparation is 0.0% by mass.
[0074] [Example 6]
[0075] Add 500g of a paste containing colored aluminum flake pigment as an effect pigment (trade name: "EMR-D5620", 60% by weight solids, 40% by weight propylene glycol monomethyl ether, average particle size 20μm, manufactured by Toyo Aluminum Co., Ltd.), and SpectraSyn (registered trademark) Elite 300 (kinematic viscosity 3400 mmHg at 40°C) as a PAO to a twin-screw kneading mixer. 2 60.0 g of the mixture (manufactured by Exxon Mobil) was mixed for 5 minutes. The resulting mixture was shaped into granules using an extruder (Multi Granulator MG-55-2, manufactured by DALTON Corporation). The resulting granules were then transferred to an inert oven (IPHH-201, manufactured by ESPEC Corporation) heated to 120°C and dried under a nitrogen atmosphere for 30 minutes to obtain the effect pigment preparation of Example 6.
[0076] The effect pigment content in the effect pigment preparation is 83.3% by mass. It should be noted that the residual heating components in the obtained effect pigment preparation were determined according to JISK 5906, and the result was 100.0% by mass. That is, the residual solvent component in the effect pigment preparation is 0.0% by mass.
[0077] [Example 7]
[0078] Add 500g of a paste containing resin-coated aluminum flake pigment as an effect pigment (trade name: "BP-5660", solids content 50% by mass, mineral oil content 50% by mass, average particle size 10μm, manufactured by Toyo Aluminum Co., Ltd.) and SpectraSyn (registered trademark) Elite 65 (kinematic viscosity 600 mmHg at 40°C) as a PAO to a twin-screw kneading mixer. 2 50.0 g of (Exxon Mobil) was mixed for 5 minutes. The resulting mixture was granulated using an extruder (Multi Granulator MG-55-2, DALTON Corporation). The resulting granules were then transferred to an inert oven (IPHH-201, ESPEC Corporation) heated to 120°C and dried under a nitrogen atmosphere for 2 hours to obtain the effect pigment preparation of Example 7.
[0079] The effect pigment content in the effect pigment preparation is 83.3% by mass. It should be noted that the residual heating components in the obtained effect pigment preparation were determined according to JISK 5906, and the result was 99.9% by mass. That is, the residual solvent component in the effect pigment preparation is 0.1% by mass.
[0080] [Comparative Example 1]
[0081] For comparison, based on Patent Document 1, an effect pigment preparation was prepared under the following conditions. 700g of a paste containing aluminum flake pigment as an effect pigment (trade name: "5620NS", solid content 71% by mass, mineral oil content 29% by mass, average particle size 18μm, manufactured by Toyo Aluminum Co., Ltd.), 192g of polyethylene wax as PAO (trade name: "SANWAX 161-P", melting point 103°C, melt viscosity 4300 mPa·s, manufactured by Sanyo Chemical Co., Ltd.), and 22g of linear low-density polyethylene resin (trade name: "Evolue SP2510", manufactured by Prime Polymer Co., Ltd.) were added to a twin-screw kneading mixer and kneaded at a heating temperature of 160°C for 1 hour, followed by degassing to prepare a mixture. Next, the obtained mixture was pre-crushed using a crusher or the like, and cylindrical granules of the effect pigment preparation of Comparative Example 1 were obtained using a disc granulator.
[0082] The effect pigment content in the effect pigment preparation is 69.9% by mass. It should be noted that the residual heating components in the obtained effect pigment preparation were determined according to JISK 5906, and the result was 99.7% by mass. That is, the residual solvent component in the effect pigment preparation is 0.3% by mass.
[0083] [Comparative Example 2]
[0084] Add 500g of a paste containing silica-coated aluminum flake pigment as an effect pigment (trade name: "EMR-D5660", 50% by weight solids, 50% by weight propylene glycol monomethyl ether, average particle size 10μm, manufactured by Toyo Aluminum Co., Ltd.), and SpectraSyn (registered trademark) Elite 65 (kinematic viscosity 600 mmHg at 40°C) as a PAO to a twin-screw kneading mixer. 2 8.0 g (manufactured by Exxon Mobil) was mixed for 5 minutes. The resulting mixture was shaped into granules using an extruder (Multi Granulator MG-55-2, manufactured by DALTON Corporation). The resulting granules were transferred to an inert oven (IPHH-201, manufactured by ESPEC Corporation) heated to 120°C and dried under a nitrogen atmosphere for 5 hours. However, the granules could not be maintained and the product became powder. Therefore, the effect pigment preparation of Comparative Example 2 could not be obtained, and the experiment was discontinued.
[0085] [Comparative Example 3]
[0086] Add 500g of a paste containing silica-coated aluminum flake pigment as an effect pigment (trade name: "EMR-D5660", 50% by weight solids, 50% by weight propylene glycol monomethyl ether, average particle size 10μm, manufactured by Toyo Aluminum Co., Ltd.), and SpectraSyn (registered trademark) Elite 65 (kinematic viscosity 600 mmHg at 40°C) as a PAO to a twin-screw kneading mixer. 2 157.0 g (manufactured by Exxon Mobil) was mixed for 5 minutes. The resulting mixture was shaped into granules using an extruder (Multi Granulator MG-55-2, manufactured by DALTON Corporation). The resulting granules were transferred to an inert oven (IPHH-201, manufactured by ESPEC Corporation) heated to 120°C and dried under a nitrogen atmosphere for 5 hours. However, the granules adhered to each other and became too soft to maintain their granular state, thus the effect pigment preparation of Comparative Example 3 could not be obtained, and the experiment was discontinued.
[0087] [Comparative Example 4]
[0088] A paste containing aluminum flake pigment as an effect pigment (trade name: "EMR-D5660, 50% by mass solids, 50% by mass propylene glycol monomethyl ether, average particle size 10 μm, manufactured by Toyo Aluminum Corporation) was added to a twin-screw kneading mixer in the form of a paste containing aluminum flake pigment as an effect pigment. Similarly, since ethylene also shares an α-olefin, 62.5 g of an ethylene-α-olefin copolymer (trade name: "Tafmer (registered trademark) A", melting point 66°C, manufactured by Mitsui Chemicals Corporation) was added as a PAO and the mixture was kneaded for 5 minutes. The resulting mixture was then granulated using an extruder (Multi Granulator MG-55-2, manufactured by DALTON Corporation). The granulated material was transferred to an inert oven (IPHH-201, manufactured by ESPEC Corporation) heated to 120°C and dried under a nitrogen atmosphere for 5 hours. However, it could not maintain its granular state and became a powder, therefore the effect pigment preparation of Comparative Example 4 could not be obtained, and the experiment was discontinued.
[0089] The results are shown in Table 1.
[0090]
[0091] <Evaluation of Effect Pigment Preparations>
[0092] [Evaluation Experiment 1]
[0093] 100 parts by weight of transparent ABS resin (product name "CL-430", manufactured by DENKA Co., Ltd.) were mixed with 1 part by weight of the effect pigment preparations of Examples 1-6 and Comparative Example 1, which can be molded into granules, based on the solid content, and the mixture was kneaded at 230°C to obtain thermoplastic resin compositions of Examples 1-6 and Comparative Example 1. Using an injection molding machine "FE80S12ASE" (manufactured by Nissei Resin Kogyo Co., Ltd.), the obtained thermoplastic resin compositions were injection molded into plates (50mm × 80mm × 3mm) under the following conditions: barrel temperature 230°C for the nozzle section, 230°C for the front section, 225°C for the middle section, and 220°C for the rear section, and mold temperature 60°C. The molded bodies of Examples 1-6 and Comparative Example 1 were obtained. The condition of the obtained molded bodies was also evaluated by visual inspection. Specifically, a case where there are no defects such as bumps, scratches, or cracks in the molded body, and no color unevenness in terms of gloss (the uniform dispersion of the effect pigments can be confirmed) is evaluated as "0". A case where defects such as bumps, scratches, or cracks are observed in the molded body, or where color unevenness in terms of gloss (the aggregation and uneven dispersion of the effect pigments can be confirmed) is evaluated as "×".
[0094] [Evaluation Experiment 2]
[0095] At room temperature (23°C), 10g (based on solids) of each of the effect pigment preparations of Examples 1-6 and Comparative Example 1, which can be formed into granules, were measured into PP (polypropylene) cups. 20g of thinner (manufactured by NIPPON PAINT Co., Ltd., trade name: nax Admila 500 standard thinner) was added to the cup containing the effect pigment preparations, and the mixture was stirred with a spatula. 110g of CLEAR (manufactured by NIPPON PAINT Co., Ltd., nax Admila 280 correction CLEAR) was added to the stirred mixture, and the mixture was stirred at 500 rpm for 5 minutes. 110g of the above-mentioned thinner and 10g of nax multi (10:1) #20 hardener were added to the stirred mixture, and the mixture was further stirred with a spatula, thereby preparing the test coatings of Examples 1-6 and Comparative Example 1.
[0096] Next, a steel plate with an intermediate coating (a steel plate in which the substrate: iron, the electrodeposited layer: zinc treatment layer, the intermediate coating layer: crack-resistant layer, the base coating layer: base concealing layer and decorative layer, and the top coating layer: the protective layer of the base coating are sequentially coated) was prepared. On one surface of the steel plate, the test coatings of Examples 1 to 6 and Comparative Example 1 were applied using a spray gun (manufactured by ANEST IWATA, trade name: W-101-134G) with a dry film thickness of 13 to 15 μm, and dried at 80°C for 20 minutes.
[0097] The dried surfaces of the steel plates coated with the test coatings of Examples 1-6 and Comparative Example 1 were visually inspected and evaluated. Specifically, a case where the test coating could be produced and the resulting coating film was smooth and did not exhibit color unevenness in terms of gloss was evaluated as "0", while a case where the test coating could not be produced and unevenness or color unevenness in terms of gloss was observed on the coated surface of the steel plate was evaluated as "×".
[0098] Table 2 shows the mixing ratio of effect pigment (solid component) to PAO in the effect pigment preparations of Examples 1 to 6 and Comparative Example 1, as well as the test results of the above-mentioned evaluation test 1 and evaluation test 2 performed on the effect pigment preparations of each example and each comparative example.
[0099]
[0100] <Inspection>
[0101] As shown in Table 1, granular effect pigment preparations were obtained in Examples 1-7 and Comparative Example 1, while granular effect pigment preparations could not be obtained in Comparative Examples 2-4.
[0102] The detailed reasons are not yet clear, but it is believed that in the cases of Examples 1 to 7, the PAO content that binds the sheets together is appropriate, so the sheets are bonded together by the resin and the granule state can be maintained. In addition, it is believed that in the case of Comparative Example 1, by mixing PAO, which is solid at room temperature, and the sheets at high temperature, the PAO is melted, and the sheets are uniformly dispersed in the PAO. The mixture is then restored to room temperature and solidified again. The mixture is then extruded using a disc granulator, thus maintaining the granule state.
[0103] On the other hand, it is believed that in Comparative Example 2, the amount of PAO used to bind the sheets together was too small, so the sheets could not bond together and became powder. In Comparative Example 3, the amount of PAO used to bind the sheets together was too large, and since the PAO was liquid at room temperature, it had a flowability that could not maintain its shape. Furthermore, in Comparative Example 4, even though PAO was solid at room temperature, the PAO separated from the sheets even when mixed without heating. Extrusion and drying were performed in this state, so it did not become granules but rather powder.
[0104] As shown in Table 2, the effect pigment preparations of Examples 1 to 6 and the effect pigment preparation of Comparative Example 1 all showed the following results: in Evaluation Test 1, the molded body had no defects such as unevenness, scratches, or cracks, and there was no color unevenness in terms of gloss, resulting in a good molded body.
[0105] exist Figure 1A photograph of the effect pigment preparation (granular state) of Example 1 is shown. Figure 2 shown in the Figure 1 The photograph shown is of the effect pigment preparation of Example 1 immediately after the diluent has been added. Figure 3 The middle shows the Figure 2 A photograph showing the state of the mixture from Example 1 after stirring. On the other hand, in... Figure 4 A photograph is shown of the effect pigment preparation (granular state) of Comparative Example 1. Figure 5 shown in the Figure 4 The photograph shown depicts the state of the effect pigment preparation of Comparative Example 1 immediately after the diluent was added. Figure 6 The middle shows the Figure 5 A photograph of the state of the mixture of Comparative Example 1 after stirring.
[0106] Reference Figures 1-3 It is understood that the granular effect pigment preparation of Example 1 ( Figure 1 Dispersion begins immediately after the diluent is added. Figure 2 After stirring, disperse evenly in the diluent. Figure 3 ), thus obtaining the experimental coating. On the other hand, the granular effect pigment preparation of Comparative Example 1 ( Figure 4 Even with the addition of diluent, it did not disperse. Figure 5 Even with stirring, it did not disperse at all in the diluent. Figure 6 Therefore, it was impossible to obtain the experimental coating.
[0107] Thus, in evaluation experiment 2, the effect pigment preparations of Examples 1-6 were easily dispersed in the diluent ( Figures 1-3 Therefore, coatings prepared using the effect pigments of Examples 1-6 can produce a good coating film with a smooth surface and no color unevenness in terms of gloss. On the other hand, as Figures 4-6 As shown, the effect pigment preparation of Comparative Example 1 could not be dispersed at all in the diluent, resulting in the inability to obtain a coating for steel plate coating.
[0108] Therefore, when comparing the effect pigment preparations of Examples 1 to 6 with the effect pigment preparation of Comparative Example 1, the conditions for obtaining an effect pigment preparation that does not require heating during raw material mixing, is compatible with thermoplastic resins, and exhibits excellent dispersibility not only in the incorporation into thermoplastic resin compositions but also in use in solvent-based coatings are as follows: the total content of effect pigment and PAO is 99% or more by mass, PAO is liquid at 25°C, and the effect pigment in the effect pigment preparation is preferably 75% or more and 95% or less by mass, more preferably 80% or more and 90% or less by mass, and PAO is preferably 5% or more and 25% or less by mass, more preferably 10% or more and 20% or less by mass.
[0109] Furthermore, according to Table 2, the kinematic viscosity of PAO at 40°C is preferably 4000 mm³ / s. 2 / s or less, preferably 3500mm 2 / s or less.
[0110] Symbol Explanation
[0111] 1a, 1b: Preparations of effect pigments
[0112] 2a, 2b: Diluent
[0113] 3a: Mixture of effect pigment preparation and diluent
[0114] 4a, 4b: Cup
Claims
1. An effect pigment preparation, characterized in that, It contains more than 99% by mass of effect pigments and polyalphaolefins. The poly-α-olefin is liquid at 25°C, and, relative to the effect pigment preparation, The effect pigment is 75% or more and 95% or less by mass. The polyα-olefin is 5% by mass or more and 25% by mass or less. Volatile organic compounds are less than 1% by mass.
2. The effect pigment preparation according to claim 1, characterized in that, The kinematic viscosity of the polyα-olefin at 40°C is 4000 mm. 2 / s or less.
3. The effect pigment preparation according to claim 1, characterized in that, The effect pigment is a metal, a metal oxide, a metal hydroxide, or a mixture thereof.
4. The effect pigment preparation according to claim 1, characterized in that, The effect pigment is coated with resin, metal oxide, metal hydroxide, or a mixture thereof.
5. The effect pigment preparation according to claim 1, characterized in that, The effect pigment has a colored pigment layer on its surface.
6. The effect pigment preparation according to claim 5, characterized in that, The colored pigment layer contains resin, metal oxide, metal hydroxide, or a mixture thereof.
7. A thermoplastic resin composition comprising the effect pigment preparation of any one of claims 1 to 6 and the thermoplastic resin.
8. A method for manufacturing a coating or ink, wherein, The coating or ink comprises the effect pigment preparation according to any one of claims 1 to 6.