Self-imageable film-forming polymers, compositions thereof, and devices and structures made therefrom
A technology of polymers and compositions, applied in the field of polymers
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment A1
[0092] Synthesis of Example A1.NBPhOAc
[0093]
[0094] Into an appropriately sized and equipped reaction vessel were charged 1750 g of dicyclopentadiene, 2147 g of p-acetoxystyrene and 64 g of phenothiazine. Stirring was started, then the reactor was purged of air and pressurized to 5 psig with nitrogen. Begin heating to 160°C and keep the reactor at 160°C for 6 hours. The reactor was then cooled to ambient temperature, the reaction mixture was removed from the reactor and distilled (110-120 mtorr, crucible temperature 113-114° C.) to obtain 1227 g of 99% pure (GC) NBPhOAc.
Embodiment A2
[0095] The synthesis of embodiment A2.NBMMPA
[0096]
[0097] Into an appropriately sized and equipped reaction vessel were charged 900 g (6.8 mol) of dicyclopentadiene and 11.2 kg (-98% pure, 54.5 mol) of syringyl acetate. Stirring was then started and flushed with nitrogen three times while stirring. The reaction was brought to 200°C over a 3 hr period while allowing the pressure to rise to 23 psig. Once at temperature, the reaction mixture was stirred at 200°C for 6 hours during which time the pressure ranged from 12-23 psi. The reaction was then allowed to cool to room temperature overnight. GC analysis showed the product mixture contained 72.6% syringyl acetate, 0.1% DCPD, 25.8% NBMMPA and 0.2% 4-NBCH 2 C 6 h 3 -2-OMe,4-OH. The total weight recovered from the reactor was about 12Kg.
[0098] The recovered material was distilled under high vacuum via a 6-inch column and distillation apparatus to remove most of the excess syringyl acetate. After removing 580.3 g...
Embodiment A3
[0100] The synthesis of embodiment A3.NBPhOH
[0101]
[0102] 100 g of NBPhOAc and 150 g of THF were charged to an appropriately sized and equipped reaction vessel and the reaction mixture was heated to 60°C with stirring under a nitrogen blanket pressurized to 5 psig. Then 263 g of a 20% aqueous sodium hydroxide solution were added dropwise over the course of 1 hour and the reaction mixture was stirred at temperature for a further 4 hours before the solution was acidified by the dropwise addition of 131 g of acetic acid. The mixture was then allowed to cool, transferred to a separatory funnel, diluted with 200 mL of ethyl acetate, and washed 5 times with 200 mL of water. The solvent was then removed by rotary evaporation. The resulting crystals were washed with 100 g of hexane and then recrystallized from 400 mL of a 1:1 toluene:hexane solution. Yield was 44.8 g (55.1%) NBPhOAc.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More