Bischlorophthalimide → Bisphenol A

반응식

[Na].[Na].[OH:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]([C:13]2[CH:18]=[CH:17][C:16]([OH:19])=[CH:15][CH:14]=2)([CH3:12])[CH3:11])=[CH:6][CH:5]=1.[Na].[Na].C1(O)C=CC(C2C=CC(O)=CC=2)=CC=1.ClC1C(Cl)=C2C(=O)NC(=O)C2=CC=1>C1C=CC(Cl)=C(Cl)C=1>[CH3:12][C:10]([C:7]1[CH:6]=[CH:5][C:4]([OH:3])=[CH:9][CH:8]=1)([C:13]1[CH:18]=[CH:17][C:16]([OH:19])=[CH:15][CH:14]=1)[CH3:11]

참가 물질

실험 절차

Bisphenol A disodium salt (4.6981 g, 17.2562 mmol), 4,4′-biphenol disodium salt (2.6479 g, 11.5042 mmol), and o-DCB (60 mL) were combined in a reaction vessel equipped with a mechanical stirrer, short path distillation head, receiver, and inert gas inlet and exit. o-DCB was distilled from the mixture until the distillate contained less than 10 ppm of water. Approximately 20 to 30 mL of o-DCB was removed in this drying step. Then, 15.3885 g (29.0716 mmol) of the bischlorophthalimide prepared from ODA and 98% 3ClPA, 2% 4ClPA, and 0.1334 g (0.5177 mmol) of 4-chloro-N-methyl phthalimide chain stopper were added quantitatively to the reaction vessel along with 10-20 mL of additional o-DCB. O-DCB was distilled from the mixture until a solids level of 25% was reached. Hexaethylguanidium chloride phase transfer catalyst (0.7 mole %) was then added and polymerization initiated. The product polyetherimide had a weight average molecular weight (Mw) of 60,282 grams per mole and a number average molecular weight (Mn) of 24,100 grams per mole.