Reacción #1458420

Ecuación de reacción

toluene

methanol water

3,3′-diamino-4,4′-dihydroxybiphenyl

NMP

ODPA

→

polyimide resin

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.DISSOLUTIONwas completely dissolved
2. 2
   workup.STIRRINGAfter the resulting mixture was stirred at room temperature for 2 hours
3. 3
   workup.ADDITION3.9 g of NDA was added to the flask
4. 4
   workup.STIRRINGAfter the resulting mixture was stirred at room temperature for 16 hours
5. 5
   workup.DISTILLATIONa Dean-Stark distillation equipment
6. 6
   Temperaturathe reaction solution was refluxed at 140° C. for 3 hours
7. 7
   Otrothe reaction
8. 8
   OtroThe reaction solution thus prepared
9. 9
   Temperaturato cool to room temperature
10. 10
    Otroto obtain
11. 11
    Otroprecipitates
12. 12
    FiltraciónThe precipitates were filtered
13. 13
    Otrodried in a vacuum
14. 14
    Otrodrying oven at 40° C. for one day

Procedimiento

3,3′-diamino-4,4′-dihydroxybiphenyl (13.0 g) and 74.2 g of NMP were sequentially charged into a 1 L round-bottom flask. The mixture was stirred until it was completely dissolved. While maintaining the flask at room temperature, 14.9 g of ODPA was added slowly. After the resulting mixture was stirred at room temperature for 2 hours, 3.9 g of NDA was added to the flask. After the resulting mixture was stirred at room temperature for 16 hours, 16 g of toluene was added to the flask. Using a Dean-Stark distillation equipment, the reaction solution was refluxed at 140° C. for 3 hours to complete the reaction. The reaction solution thus prepared was allowed to cool to room temperature, and slowly poured into a 1:4 methanol-water mixture to obtain precipitates. The precipitates were filtered and dried in a vacuum drying oven at 40° C. for one day. 19.6 g of the soluble polyimide resin thus obtained in a powder form was charged into a 1 L round-bottom flask and dissolved in 100 g of N-methyl-2-pyrrolidone (NMP). The resulting solution was cooled on ice and then 2.12 g of triethylamine (TEA) was added thereto, maintaining the temperature at 0˜5° C. After stirring for 10 minutes, 2.27 g of chloromethylethylether was slowly added to the solution. After the resulting solution was stirred for 3 hours while maintaining it at a low temperature, triethylammonium chloride salt was filtered off. The filtrate was slowly poured into a 1:2 methanol-distilled water mixture with vigorous stirring to form precipitates as a fine white solid. The precipitates thus formed were collected, washed with 5 L of distilled water, and dried in a vacuum oven at 40° C. for 36 hours to prepare 21 g of a soluble polyimide as a white powder.

Fuente