Reaktion #1458419

Reaktionsgleichung

toluene

methanol water

2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane

N-methyl-2-pyrrolidone

5-norbornene-2,3-dicarboxylic anhydride

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polyimide resin

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISSOLUTIONwas completely dissolved
2. 2
   workup.STIRRINGAfter the resulting mixture was stirred at room temperature for 16 hours
3. 3
   workup.DISTILLATIONa Dean-Stark distillation equipment
4. 4
   Temperaturthe reaction solution was refluxed at 170° C. for 3 hours
5. 5
   Sonstigethe reaction
6. 6
   SonstigeThe reaction solution thus prepared
7. 7
   Temperaturto cool to room temperature
8. 8
   Sonstigeto obtain
9. 9
   Sonstigeprecipitates
10. 10
    FiltrationThe precipitates were filtered
11. 11
    Sonstigedried in a vacuum
12. 12
    Sonstigedrying oven at 40° C. for 24 hours

Vorschrift

2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane (36.63 g ) and 200 g of N-methyl-2-pyrrolidone (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 0-5° C., 39.98 g of 2,2-bis(3,4-benzenedicarboxylic anhydride) perfluoropropane and 3.28 g of 5-norbornene-2,3-dicarboxylic anhydride (NDA) were added to the mixture. After the resulting mixture was stirred at room temperature for 16 hours, 40 g of toluene was added to the flask. Using a Dean-Stark distillation equipment, the reaction solution was refluxed at 170° 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 24 hours to obtain 80 g of a soluble polyimide resin. Resin (20 g) thus obtained in 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 2.73 g of triethylamine (TEA) was added thereto, with maintaining the temperature at 0˜5° C. After stirring for 10 minutes, 2.84 g of chloromethylethylether was slowly added to the solution. After the resulting solution was stirred for 3 hours while maintaining at 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 filtered and collected, washed with distilled water, and dried in a vacuum oven at 40° C. for 36 hours to prepare 20 g of a soluble polyimide represented by the following Formula, as a white powder:

Quelle