LIQUID CRYSTAL POLYESTER RESIN COMPOSITION AND MOLDED BODY

20220332923 · 2022-10-20

    Inventors

    Cpc classification

    International classification

    Abstract

    A liquid crystal polyester resin composition contains a component (P): a liquid crystal polyester resin, a component (M): a non-metallic and powdery pigment having a metallic color, and a component (F): an inorganic filler excluding the component (M).

    Claims

    1. A liquid crystal polyester resin composition, comprising: a component (P): a liquid crystal polyester resin; a component (M): a non-metallic and powdery pigment having a metallic color; and a component (F): an inorganic filler excluding the component (M).

    2. The liquid crystal polyester resin composition according to claim 1, wherein the component (M) is a component in which a plate-shaped inorganic filler particle is coated with a metal oxide.

    3. The liquid crystal polyester resin composition according to claim 2, wherein the plate-shaped inorganic filler particle in the component (M) contains mica.

    4. The liquid crystal polyester resin composition according to claim 3, wherein the plate-shaped inorganic filler particle in the component (M) contains synthetic mica.

    5. The liquid crystal polyester resin composition according to claim 1, wherein a content of the component (M) is 4 to 50 parts by mass with respect to 100 parts by mass of the component (P).

    6. The liquid crystal polyester resin composition according to claim 1, wherein the component (F) is a plate-shaped particle.

    7. The liquid crystal polyester resin composition according to claim 1, wherein a content of the component (F) is 10 to 80 parts by mass with respect to 100 parts by mass of the component (P).

    8. The liquid crystal polyester resin composition according to claim 1, wherein a median diameter (D50) of the component (M) is 5 to 100 μm.

    9. A molded body produced from the liquid crystal polyester resin composition according to claim 1.

    10. The molded body according to claim 9, wherein the molded body is ovenware.

    Description

    EXAMPLES

    [0148] In the following, the present invention will be described in more detail with reference to Examples, but the present invention is not limited to the following Examples.

    <Manufacturing Method of Liquid Crystal Polyester Resin 1>

    [0149] 994.5 g (7.2 mol) of parahydroxybenzoic acid, 446.9 g (2.4 mol) of 4,4′-dihydroxybiphenyl, 299.0 g (1.8 mol) of terephthalic acid, 99.7 g (0.6 mol) of isophthalic acid, and 1347.6 g (13.2 mol) of acetic anhydride were charged into a reactor including an agitator, a torque meter, a nitrogen gas inlet tube, a thermometer, and a reflux condenser, 0.2 g of 1-methylimidazole was added, and the inside of the reactor was sufficiently substituted with nitrogen gas.

    [0150] Thereafter, a temperature was raised from room temperature to 150° C. over 30 minutes under a nitrogen gas stream, and the temperature was maintained at the same temperature for reflux for 1 hour.

    [0151] Then, the temperature was raised from 150° C. to 320° C. over 2 hours and 50 minutes while distilling off by-product acetic acid or unreacted acetic anhydride, and a prepolymer was obtained at a point in time when the increase in torque was observed as the end of reaction.

    [0152] The obtained prepolymer was cooled to room temperature and pulverized with a coarse pulverizer. The obtained prepolymer powder was solid-phase polymerized by raising the temperature from room temperature to 250° C. over 1 hour, raising the temperature from 250° C. to 285° C. over 5 hours, and maintaining the temperature at 285° C. for 3 hours in a nitrogen gas atmosphere, so that a liquid crystal polyester resin 1 was obtained. The flow start temperature of the obtained liquid crystal polyester resin 1 was 327° C.

    Examples 1 to 9, and Comparative Examples 1 to 4

    <Manufacturing Method of Liquid Crystal Polyester Resin Composition>

    [0153] After compounding the component (M) and the component (F) with the liquid crystal polyester resin 1 (component (P)) obtained above in the compounding ratio shown in Table 1 below, a liquid crystal polyester resin composition of each example was obtained by using a twin-screw extruder (manufactured by lkegai Corp, PCM-30).

    TABLE-US-00001 TABLE 1 Example Example Example Example Example Example Example 1 2 3 4 5 6 7 component LCP-1 100 100 100 100 100 100 100 (P) component (M)-1 8.9 17.9 35.7 35.7 (M) (M)-2 35.7 (M)-3 35.7 (M)-4 35.7 component (F)-1 69.6 60.7 42.9 42.9 42.9 42.9 42.9 (F) (F)-2 (F)-3 0.02 Comparative Comparative Comparative Comparative Example Example Example Example Example Example 8 9 1 2 3 4 component 100 100 100 100 100 100 (P) component 35.7 35.7 78.6 (M) component 42.9 42.9 78.6 (F) 66.7 0.18 0.71

    [0154] In Table 1, each abbreviation has the following meaning. A numeral value in [ ] is a compounding amount (part by mass).

    [0155] LCP-1: Liquid crystal polyester resin 1 described above

    [0156] (M)-1: Titanium oxide-coated synthetic mica (manufactured by NIHON KOKEN KOGYO CO., LTD., trade name: TWINCLEPEARL SXD, median diameter (D50): 21 μm)

    [0157] (M)-2: Titanium oxide-coated synthetic mica (manufactured by NIHON KOKEN KOGYO CO., LTD., trade name: TWINCLEPEARL SX, median diameter (D50): 90 μm)

    [0158] (M)-3: Titanium oxide-coated synthetic mica (manufactured by NIHON KOKEN KOGYO CO., LTD., trade name: TWINCLEPEARL SXA, median diameter (D50): 9 μm)

    [0159] (M)-4: Titanium oxide-coated synthetic mica (manufactured by NIHON KOKEN KOGYO CO., LTD., trade name: TWINCLEPEARL BXB, median diameter (D50): 13 μm)

    [0160] (F)-1: Talc (manufactured by Nippon Talc Co., Ltd., trade name: MS-KY, median diameter (D50): 25 μm)

    [0161] (F)-2: Glass fiber (manufactured by Central Glass Co., Ltd., trade name: milled fiber EFH75-01)

    [0162] (F)-3: Carbon black (manufactured by Cabot Corporation, trade name: Black pearls 4350)

    [0163] It should be noted that the median diameters (D50) of (M)-1 to (M)-4 were measured by using, as a measurement device, a scattering type particle diameter distribution measurement device (manufactured by HORIBA, Ltd., trade name: LA-950V2) in a state in which each of (M)-1 to (M)-4 was dispersed in water under the following measurement conditions.

    [0164] [Conditions]

    [0165] Refractive index of particle: 1.59 to 0.1i (mica)

    [0166] Dispersion medium: water

    [0167] Refractive index of dispersion medium: 1.33

    <Manufacturing of Test Piece>

    [0168] The liquid crystal polyester resin composition of each example was molded at 330° C. to 350° C. by using an injection molding machine to obtain a test piece having a size of 60 mm×40 mm×2 mmt.

    [Metallic Evaluation]

    [0169] For the test pieces of Examples 1 to 9, and Comparative Examples 1 and 2, a reflectivity of 500 nm at a detection angle of 30° of light, which is incident at an incident angle of 45° and reflected from a surface of the test piece, was measured by using a variable-angle photometer (manufactured by DENSHOKU INDUSTRIES Co., Ltd., trade name: GC5000L).

    [0170] As the reflectivity is higher, the metallic brilliance is stronger, which means that the appearance is metallic.

    [0171] The results thereof are shown in Tables 2 and 3.

    TABLE-US-00002 TABLE 2 Example Example Example Example Example Example Example Example Example 1 2 3 4 5 6 7 8 9 Reflectivity 110 126 156 121 150 133 142 132 102

    TABLE-US-00003 TABLE 3 Comparative Comparative Example 1 Example 2 Reflectivity 91 193

    [0172] From the results shown in Tables 2 and 3, it can be confirmed that the liquid crystal polyester resin compositions of Examples have high reflectivity and high design property.

    [0173] In addition, it was confirmed that, among Examples, the liquid crystal polyester resin compositions of Examples 7 to 9 containing (F)-3: the carbon black had the same reflectivity as other Examples, but exhibited a more metallic color tone and had excellent design property that imitates a metallic appearance in the visual evaluation.

    [Evaluation of Effect of Suppressing Occurrence of Flow Mark]

    [0174] The appearance of the test piece of each example was visually observed and evaluated according to the following criteria.

    [0175] The results thereof are shown in Tables 4 and 5.

    [0176] A: Approaching an observation surface within 1 meter, and a flow mark is hardly seen from any angle

    [0177] B: Approaching the observation surface within 1 meter, a flow mark is not clearly seen from a vertical direction, but a flow mark can be seen well from a direction of 45 degrees

    [0178] C: Approaching the observation surface within 1 meter, and a flow mark can be seen well from any direction

    [0179] D: A flow mark can be seen well even in a case of being away from the observation surface by 1 meter or more

    TABLE-US-00004 TABLE 4 Example Example Example Example Example Example Example Example Example 1 2 3 4 5 6 7 8 9 Flow mark A A A B A A A A A

    TABLE-US-00005 TABLE 5 Comparative Comparative Comparative Comparative Example 1 Example 2 Example 3 Example 4 Flow mark A D C D

    [0180] From the results shown in Tables 4 and 5, it can be confirmed that the molded body (ovenware) produced by using the liquid crystal polyester resin compositions of Examples suppresses the occurrence of a flow mark.

    [0181] From the above, it can be confirmed that the liquid crystal polyester resin compositions of Examples to which the present invention is applied have high design property and can suppress the occurrence of a flow mark.

    [0182] Preferable examples of the present invention have been described above, but the present invention is not limited to these examples. It is possible to add, omit, replace, and make other changes to the configuration without departing from the spirit of the present invention. The present invention is not limited by the above description, but only limited by the scope of the appended claims.