Liquid-crystalline polyester resin composition, method for producing same, and molded article made thereof
A technology of polyester resin and manufacturing method, applied in the direction of coating, etc., can solve problems such as insufficient surface smoothness, failure to suppress filler floating, etc., and achieve excellent needle indentation strength, reduced warpage, and excellent surface smoothness Effect
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[0083] Hereinafter, the effects of the present invention will be described in more detail through examples. Compositional analysis and property evaluation of liquid crystalline polyesters were performed by the following methods.
[0084] (1) Composition analysis of liquid crystalline polyester resin
[0085] Composition analysis of liquid crystalline polyester resin passed 1 H-NMR spectrum ( 1 H-NMR) measurement to implement. Weigh 50 mg of liquid crystalline polyester resin into an NMR sample tube, dissolve it in a solvent (pentafluorophenol / 1,1,2,2-tetrachloroethane-d 2 =65 / 35 (weight ratio) mixed solvent) 800 μL, using the UNITY INOVA500 NMR apparatus (manufactured by Barian Corporation) at an observation frequency of 500 MHz and a temperature of 80° C. 1 H-NMR determination. The composition of the liquid crystalline polyester resin was analyzed from the peak area ratio derived from each structural unit observed around 7 to 9.5 ppm.
[0086] (2) Measurement of Melting...
reference example 1
[0091] [Reference Example 1] Synthesis of liquid crystalline polyester resin (A-1)
[0092] Add 870g (6.30 moles) of p-hydroxybenzoic acid, 327g (1.89 moles) of 4,4'-dihydroxybiphenyl, 89g (0.81 moles) of hydroquinone, and 292 g (1.76 mol) of formic acid, 157 g (0.95 mol) of isophthalic acid, and 1367 g (1.03 equivalents of the total phenolic hydroxyl group) of acetic anhydride were reacted at 145° C. for 2 hours while stirring under a nitrogen atmosphere, and then the temperature was raised to 320°C. Then, the polymerization temperature was kept at 320° C., the pressure was reduced to 1.0 mmHg (133 Pa) in 1.0 hour, and then the reaction was continued for 90 minutes, and the polycondensation was completed when the torque required for stirring reached 15 kg·cm. Next, pressurize the reaction vessel to 1.0kg / cm 2 (0.1 MPa), the polymer was discharged into strands through a die having a circular discharge port with a diameter of 10 mm, and pelletized by a cutter to obtain a liqu...
reference example 2
[0094] [Reference Example 2] Synthesis of liquid crystalline polyester resin (A-2)
[0095] 994 g (7.20 moles) of p-hydroxybenzoic acid, 181 g (0.97 moles) of 4,4'-dihydroxybiphenyl, 161 g (0.97 moles) of terephthalic acid, and polyterephthalic acid with an intrinsic viscosity of about 0.6 dl / g 159 g (0.83 moles) of ethylene glycol ester and 1,026 g (1.10 equivalents of the total phenolic hydroxyl groups) of acetic anhydride were added to a polymerization vessel, and the reaction was carried out at 145°C for 2 hours while stirring under a nitrogen atmosphere, and then the temperature was raised to 335°C over 4 hours. . Then, the polymerization temperature was kept at 335° C., nitrogen was pressurized to 0.1 MPa, and the mixture was heated and stirred for 20 minutes. Then, the pressure was reduced to 1.0 mmHg (133 Pa) in 1.0 hour, and then the reaction was continued for 90 minutes, and the polycondensation was completed when the torque required for stirring reached 12 kg·cm. ...
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