Stage #1: With N-benzyl-N,N,N-triethylammonium chloride; sodium hydroxide In water at 85 - 172℃; for 15 h; Stage #2: at 130 - 145℃; for 5 h;
79 g (0.63 mol) of a 32percent by weight aqueous sodium hydroxide solution and 62.4 g (0.3 mol) of bisphenol A were charged into the reactor.Stir and dissolve,The temperature rises to 85 ° C and the solution is transparent.Next, 510 g of a trimethylbenzene solvent and 4.2 g of a benzyltriethylammonium chloride catalyst were added.Warming and refluxing,The temperature rose to 172 ° C,Stirring reaction for 15 hours,Then cool down to 130 ° C,108 g (0.6 mol) of 4-chlorophthalic anhydride and 4.86 g of benzyltriethylammonium chloride catalyst were added.Heating from 140 ° C to 145 ° C,Reflow reaction for 5 hours,Then filter hot,Pumping the filtrate into the crystallization kettle,The filtrate is cooled to room temperature.Crystallized for 12 hours,filter,The precipitate is washed with ion-free water,Filtration, precipitation was obtained and washed with 250 g of ethanol.Stirring for 2 hours,filter,Get wet material 125g,After drying, 120 g of bisphenol A diether dianhydride product (yield 85percent),The product is white powder,
 Patent: CN108148029, 2018, A, . Location in patent: Paragraph 0011; 0012; 0014
[ 319-03-9 ]
[ 2444-90-8 ]
[ 38103-06-9 ]
Operation in experiment
at 180℃; for 0.25 h;
A dry 100 mL flask was charged with 1.69 g (7.3 mmol) of the disodium salt of biphenol, 2.44 g, (146 mmol) of 4-fluorophthalic anhydride, 2 mL (14 mmol) of hexaethylguanidinium chloride as a 15 weight percent solution in o-dichlorobenzene, and 44 g of dry o-dichlorobenzene. The flask was immersed in an oil bath maintained at 180° C. and the mixture was stirred magnetically. After 15 minutes, the reaction mixture was filtered hot to remove the sodium fluoride by-product. The filtrate was allowed to cool to room temperature and the product dianhydride crystallized from the solvent as a cream colored solid which was isolated by filtration (3.1 g, 90percent yield).
at 175℃; for 1 h;
A dry 25 mL flask was charged with 403 mg (1.482 mmol) of the disodium salt of bisphenol A, 500 mg (3.012 mmol) of 4-fluorophthalic anhydride, 46 mg (0.148 mmol) of 4-(N,N-dibutylamino)-N-neopentylpyridinium chloride, 8.5 g (10percent solids) of dry o-dichlorobenzene and 55 mg of o-terphenyl (internal standard). The flask was immersed in an oil bath maintained at 180° C. and the mixture was stirred magnetically. The temperature within the reaction flask was about 175° C. Samples (0.1 mL) were withdrawn periodically dissolved in 6 mL of acetic acid and approximately. 0.5 mL of methylamine (40percent aqueous soln.) and heated at 125-130° C. for 1.5 hours. These samples were analyzed for the bis N-methyl imide of bisphenol A dianhydride by liquid chromatography. By following the diether dianhydride formation in this manner it was determined that the yield of product bisphenol A dianhydride (BPADA) had reached 82percent after one hour.
A dry 100 mL flask was charged with 2.0 g (7.3 mmol) of the disodium salt of bisphenol A, 2.67 g (14.6 mmol) of 4-chlorophthalic anhydride, 4 mL (14 mmol) of hexaethylguanidinium chloride as a 15 weight percent solution in o-dichlorobenzene, 48 g of dry o-dichlorobenzene, and 100 mg of o-terphenyl (internal standard). The flask was immersed in an oil bath maintained at 180° C. and the mixture was stirred magnetically. The reaction was followed as in Example 1. The yield of biphenol dianhydride had reached 25percent after 5 hours.
bis(3-aminopropyl)-terminated poly(permethylsiloxane)[ No CAS ]
[ 108-45-2 ]
[ 38103-06-9 ]
reaction product of bis(3-aminopropyl)-terminated poly(permethylsiloxane) with 2,2-di[4-[(1,3-dioxo-1,3-dihydro-2-benzofuran-5-yl)oxy]phenyl]propane and 1,3-diaminobenzene, Mw = 39350, Mn = 18880, Mw/Mn = 2, Mpeak = 38750[ No CAS ]