A kind of transparent polyimide resin and preparation method thereof
The technology of polyimide resin and transparent polyimide is applied in the field of transparent polyimide resin and its preparation, which can solve the problems of low reactivity, inability to prepare flexible films, and precipitation of salts, and achieve simple reaction steps. , excellent solubility, easy preparation effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0047] In this example, 4,4'-bis(4-fluoroimide)trans-cyclohexane has the following structural formula:
[0048]
[0049] The specific preparation method is: under nitrogen protection, add 24.9165 (150.0 mmol) of 4-fluorophthalic anhydride, 8.5643 g (75.0 mmol) of 1,4-trans-cyclohexanediamine, and 75 ml of glacial acetic acid into a 150 mL reaction flask , heated to 150°C and stirred for 8 hours, a large amount of white precipitates precipitated during the reaction, filtered with a Buchner funnel, collected and washed the filter cake, and dried in a vacuum oven at 130°C to obtain 4,4'-bis(4-fluoro imide) trans-cyclohexane powder, yield 80%. Its melting point is 353°C.
[0050] The detection data are as follows: NMR: 1 H NMR (400MHz, CDCl 3 ,δ,ppm):7.84(dd,J 1 =8.4Hz,J 2 =4.4Hz,2H),7.51(dd,J 1 =7.2Hz,J 2 =1.6Hz,2H),7.38(dd,J 1 =8.4Hz,J 2 =1.6Hz, 2H), 4.39-4.22(m, 2H), 2.52-2.35(m, 4H), 1.95-1.80(m, 4H).FT-IR (powder): 1703, 1476, 1380, 1101cm -1 .
[0051] In this ...
Embodiment 2
[0057] In this example, 4,4'-bis(4-fluoroimide) mixed cyclohexane has the following structural formula:
[0058]
[0059] In the 1,4-cyclohexane structure, trans / cis=1 / 1;
[0060] The specific preparation method is: under nitrogen protection, add 16.9681 (100.0 mmol) of 4-fluorophthalic anhydride, 5.7095 g (50.0 mmol) of 1,4-mixed cyclohexanediamine, and 50 ml of glacial acetic acid into a 150 mL reaction flask, Raise the temperature to 150°C and stir for 8 hours. During the reaction, a large amount of white precipitates precipitated. Filter through a Buchner funnel, collect and wash the filter cake, and dry it in a vacuum oven at 130°C to obtain 4,4'-bis(4-fluoro imide) cyclohexane powder, yield 54%. Its melting point is 320°C. Wherein the cyclohexane structure trans / cis=1 / 1.
[0061] The detection data are as follows: NMR: 1 H NMR (400MHz, CDCl 3 ,δ,ppm):7.90-7.83(m,2H),7.53(dd,J 1 =7.2Hz,J 2 =0.8Hz,2H),7.43-7.35(m,2H),4.45-4.24(m,2H),2.70-2.55(m,4H),2.53-2.37(m,4H...
Embodiment 3
[0069] In this example, the trans / cis of 4,4'-bis(4-fluoroimide) mixed cyclohexane = 6 / 4, the preparation method is the same as above, except that the mixed 1,4 with different ratios of cis and trans - cyclohexanediamine.
[0070] In this embodiment, the polyimide resin material has the following structural formula:
[0071]
[0072] In the 1,4-cyclohexane structure, trans / cis=6 / 4;
[0073] The specific preparation method is: under the protection of nitrogen, mix 2.0512 (5.0 mmol) of 4,4'-bis (4-fluoroimide) cyclohexane, 1.5915 g (5.0 mmol) of phenolphthalein, 0.7610 g (5.5 mmol) ) of potassium carbonate, 10ml of N,N-dimethylacetamide and 15ml of xylene into a 100mL reaction flask, heated to 170°C and stirred for 5 hours, then gradually raised to 230°C for 6 hours to obtain viscous polyimide solution. Cool to 80°C, add N,N-dimethylacetamide to dilute the reaction solution, precipitate fibrous polyimide in ethanol, boil, wash and dry to obtain polyimide powder. The glass...
PUM
| Property | Measurement | Unit |
|---|---|---|
| glass transition temperature | aaaaa | aaaaa |
| melting point | aaaaa | aaaaa |
| transition temperature | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More