Method for manufacturing wholly aromatic liquid-crystalline polyester resin
View Patent ↗The present invention provides a method for manufacturing a wholly aromatic liquid-crystalline polyester resin comprising the steps of: 1) acylating the hydroxy group of major monomer components selected from the group consisting of aromatic hydroxycarboxylic acid, aromatic diol and aromatic dicarboxylic acid, with an acylating agent, provided that said major monomer components comprise at least one of aromatic hydroxycarboxylic acid and aromatic diol; and 2) polycondensing said major monomer components of which hydroxy group is acylated, wherein, the polycondensation reaction is carried out in the presence of a metal dihydrogen phosphate in an amount of 1-5000 ppm based on the total monomer components, and a liquid-crystalline polyester resin manufactured by the method and a composition comprising said resin.
1. A method for manufacturing a wholly aromatic liquid-crystalline polyester resin comprising the steps of:
1) acylating the hydroxy group of major monomer components selected from the group consisting of aromatic hydroxycarboxylic acid, aromatic diol and aromatic dicarboxylic acid, with an acylating agent, provided that said major monomer components comprise at least one of aromatic hydroxycarboxylic acid and aromatic diol; and
2) polycondensing said major monomer components of which hydroxy group is acylated,
wherein, the polycondensation reaction is carried out in the presence of a metal dihydrogen phosphate in an amount of 1-5000 ppm based on the total monomer components.
2. The method according to claim 1 , wherein the metal dihydrogen phosphate is added to the reaction system in the acylating step 1).
3. The method according to claim 1 , wherein the metal dihydrogen phosphate is an alkali metal dihydrogen phosphate.
4. The method according to claim 3 , wherein the alkali metal dihydrogen phosphate is potassium dihydrogen phosphate and/or sodium dihydrogen phosphate.
5. The method according to claim 1 , wherein the major monomer components comprise para-hydroxybenzoic acid and/or 6-hydroxy-2-naphthoic acid.
6. The method according to claim 1 , wherein the polycondensing step is carried out in the presence of a minor copolymerizing component selected from the group consisting of 4-hydroxyisophthalic acid, salicylic acid, 3-hydroxy-2-naphthoic acid and 2-hydroxynaphthalene-3,6-dicarboxylic acid in an amount of 1-5000 mmol % based on the total monomer components, and an alkali metal salt selected from the group consisting of sulfate, carbonate, bicarbonate, nitrate, carboxylate and haloid of an alkali metal in an amount of 10-3000 ppm based on the total monomer components.
7. The method according to claim 6 , wherein the alkali metal salt is an alkali metal sulfate.
8. A wholly aromatic liquid-crystalline polyester resin obtainable by the method according to claim 1 .
9. A wholly aromatic liquid-crystalline polyester resin composition comprising 100 parts by weight of wholly aromatic liquid-crystalline polyester resin according to claim 8 and 0.1-200 parts by weight of a filler and/or reinforcement.
10. The wholly aromatic liquid-crystalline polyester resin composition according to claim 9 , wherein the filler and/or reinforcement is at least one selected from the group consisting of glass fiber, silica-alumina fiber, alumina fiber, carbou fiber, aramid fiber, talc, mica, graphite, wollastonite, calcium carbonate, dolomite, clay, glass flake, glass beads, barium sulfate and titanium oxide.
11. The wholly aromatic liquid-crystalline polyester resin composition according to claim 10 , wherein the filler and/or reinforcement is glass fiber.