Reference

Flame-resistant polyester

Flame-resistant polyester. (Japan Ester Co., Ltd., Japan). Jpn. Kokai Tokkyo Koho JP 59187023 A2 24 Oct 1984 Showa, 7 pp. (Japanese). (Japan). CODEN: JKXXAF. CLASS: IC: C08G063-22; C08K005-51; C08L067-02. APPLICATION: JP 83-60546 6 Apr 1983. DOCUMENT TYPE: Patent CA Section: 37 (Plastics Manufacture and Processing) A polyester is prepd. from terephthalic acid (I) (or other bifunctional carboxylic acid or ester-formable deriv.) and ethylene glycol (II) (or other glycol) contg. a trifunctional P compd. (P 0.2-1.5 atom%/ester) in the 1st polycondensation stage; at [g] 3 0.3, 31 bifunctional P compd. (P 0.2-1.5 atom%) having 31 free acidic OH group is used in the final polycondensation stage. Thus, a slurry of I and II (II-I molar ratio 1.5) was continuously supplied to the reactor contg. bis(b-hydroxyethyl)terephthalate and its oligomer, and allowed to react at 255° (residence time 6 h) at atm. pressure, to give an ester of 96% conversion. To 20 kg above ester, 2 ′ 10-4 mol Sb2O3, 0.5 ′ 10-4 mol Co(AcO)2, and 2.5 ′ 10-2 mol Et diethylphosphonopropionate [3699-67-0] were added, and heated 1.5 h at 280°/0.2 mmHg to give a polymer of [g] = 0.60. To the polymer was added 2.5 ′ 10-2 mol phenylphosphonic acid [1571-33-1] and the reaction mixt. was heated 1.5 h at 280°/0.2 mmHg to give a polymer [25038-59-9] with [g] = 0.68, diethylene glycol% = 2.35, and L = 74.6, a = -1.7, b = -0.8, almost colorless.

Flame-retardant polyesters

Flame-retardant polyesters. (Japan Exlan Co., Ltd., Japan). Jpn. Kokai Tokkyo Koho JP 59091122 A2 25 May 1984 Showa, 5 pp. (Japanese). (Japan). CODEN: JKXXAF. CLASS: IC: C08G063-22; C08G063-68; C08G067-02; C08K005-53. APPLICATION: JP 82-200927 16 Nov 1982. DOCUMENT TYPE: Patent CA Section: 40 (Textiles) In the manuf. of poly(alkylene terephthalates) by melt polymn., 0.1-2.5% (as P) organophosphonic acids RPO3H2 are added once the polymer has reached intrinsic viscosity ([h]; at 20° in 1:1 PhOH/C2H2Cl4) 3 0.3, and then polycondensation is continued to obtain flame-retardant polyesters with high m.p. Thus, 30 kg 96%-esterified mixt. of terephthalic acid (I) and ethylene glycol (II) (I/II mol ratio 1:1.5) was heated in vacuo at 280° for 1.5 h in the presence of Sb2O3 and Co(OAc)2 (2 ′ 10-6 and 0.5 ′ 10-4 mol/mol I units, resp.) to give a polyester (III) of [h] 0.52. PhPO3H2 [1571-33-1] (0.81% as P) was added, and the mixt. was heated in vacuo for 2 h more to give a III melt with [h] 0.64, which formed fibers having good flame retardance and P content 0.77%, compared with 0.68, poor flame retardance, and 0.13% for III prepd. similarly but with addn. of PhPO3H2 to the initial ester mixt. (at [h] 0.10), which gave off irritating gases when melt spun.