Method of making a biphenol dianhydride composition, method for purification of a biphenol dianhydride composition, and poly(etherimides) derived from the biphenol dianhydride
A technology of bisphenol dianhydride and composition, applied in the field of preparing bisphenol dianhydride composition, purifying bisphenol dianhydride composition and poly(ether imide) derived from bisphenol dianhydride, can solve the problem of difficult production dianhydride and other issues
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Embodiment 1
[0060] Charge N,N'-phenyl-bisphenol bisimide (N,N'-Ph-BPoBI) (N,N'-Ph-3,3'- Mixture of BPoBI, N,N'-Ph-3,4'-BPoBI, N,N'-Ph-4,4'-BPoBI) wet cake (268 kg total mass). The reactor was stirred at 90% power and heated to 90°C under a nitrogen purge. A solution of 50% aqueous NaOH (60.80 kg, 760 mol, 8.0 equiv) was then added to bring the total reactor mass to 330 kg. The vessel was sealed and heated for three hours until the internal pressure reached 130-135 psig (180°C). The pressure was maintained at 130-135 psig for an additional 5 hours, then the set temperature was adjusted to 85-90°C. Stirring is also reduced to 60% power. The vessel was carefully depressurized to 2 psig and sampled. UPLC analysis indicated complete hydrolysis to the corresponding tetra-acid.
[0061] The wash vessel was charged with o-DCB (225 kg), stirred, and heated to 90-95°C. The aqueous solution of BPoTA.4Na was transferred to the wash vessel, stirred at 50% power for 30 minutes, and then the layer...
Embodiment 2
[0067] BPoTA was prepared as described in Example 1. The BPoTA wet cake obtained in Example 2 had a solids content in the range of 85-90%. A total of 46.58 kg of white BPoTA wet cake was isolated with an estimated dry mass of 39.60 kg. The wet cake was used directly in the ring closure step without further drying. ICP-Dig: Sodium (139ppm), Potassium (9ppm), Zinc (5ppm), Calcium (5ppm), Aluminum (2ppm), Iron (8ppm), Titanium (0ppm), Phosphorus (9ppm); IC Extract: Sulfate (75.08ppm), chlorine (<0.5ppm), phosphate (<0.5ppm), fluorine (<0.5ppm); IC-total: sulfate (288ppm), phosphate (<20ppm), chlorine (863ppm), fluorine (<20 ppm); UPLC: 3,3'-BPoTA+ isomer (97.10%) with small levels of 3,4'- and 4,4'-isomers and unknown impurity (1.80%).
[0068] BPoTA wet cake (39.60 kg dry basis, 76.98 mol) and o-DCB (180 kg) were charged into a container to make a 17 wt% mixture. Nitrogen was applied, the mixture was stirred, then the contents were heated to 180-185°C and held at this temper...
Embodiment 3
[0071] The above isolated 3,3'-BPoDA (Comparative Example 2) was backfilled (in three batches, each with 8-9 kg DA on a dry weight basis) into a Nutsche filter and filled with DI water at 85-90°C , then shut down the system and allow to soak for 30 minutes. The Nutsche filter is then pressurized to remove the water. This batch wash protocol was repeated 5-6 times. Send the filtrate into a polypropylene suitcase as previously described. The filter is pressurized to 50 psig for several hours to remove most of the water and finally the wet cake is transferred to a plastic drum. Continue this cake separation procedure until all BPoDA has been rewashed. Disc solids analysis of the filter cake indicated wt% solids in the range of 88-94%. UPLC: 3,3'-BPoDA + isomer (99.20%); ICP-Dig: sodium (114ppm), potassium (11ppm), calcium (1ppm), aluminum (1.07ppm), iron (15ppm), nickel (5ppm) , chromium (12ppm), phosphorus (9ppm); IC extracts: sulfate (9.1ppm), chlorine (3.6ppm), phosphate ...
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