Flexible chain segment polyether-containing polyimide film material and method for preparing homogeneous film
The technology of polyimide membrane and flexible segment is applied in the field of preparation of polyimide membrane material and gas separation membrane, and can solve the problem of inability to meet application requirements, low polyimide gas permeability coefficient, and selectivity to be improved and other problems, to achieve the effect of excellent CO2 gas separation performance, large flux, and improved separation performance
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Embodiment 1
[0019] At 25°C, 10 mmol mPDA and two-terminal amino polyethylene glycol (molecular weight 2000) (mass ratio 15:85) were dissolved in 20 ml NMP, and then 10 mmol 6FDA was added under the condition of blowing nitrogen gas. The solution was stirred at room temperature for 12 hours to form a viscous polyamic acid solution. Add 40mmol of acetic anhydride and 40mmol of triethylamine for imidization, react at room temperature for 24 hours, raise the temperature and react at 60°C for 1 hour; then allow the polymer to settle in deionized water. The polymer was dried in a vacuum oven at 100°C for over 24 hours. Dissolve 0.7g of the obtained polymer in 10ml of NMP, pour the solution on a polyethylene plate, and dry it at 60°C to form a film. The obtained homogeneous film is then placed in a vacuum oven at 120°C for 48 hours. The resulting film thickness was ~50 μm.
[0020] Test gas separation performance:
[0021] P CO2 = 73.55 Barrer
[0022] (1Barrer=10 -10 cm 3 (STP)cm / (cm 2 ...
Embodiment 2
[0025] At 25° C., 10 mmol of mPDA and two-terminal amino polyethylene glycol (molecular weight 2000) (mass ratio 65:35) were dissolved in 20 ml of NMP, and then 10 mmol of 6FDA was added. The solution was stirred at room temperature for 12 hours to form a viscous polyamic acid solution. Add 40mmol of acetic anhydride and 40mmol of triethylamine for imidization, react at room temperature for 24 hours, raise the temperature and react at 60°C for 1 hour; then allow the polymer to settle in deionized water. The polymer was dried in a vacuum oven at 100°C for over 24 hours. Dissolve 0.7g of the obtained polymer in 10ml of NMP, pour the solution on a polyethylene plate, and dry it at 60°C to form a film. The obtained homogeneous film is then placed in a vacuum oven at 120°C for 48 hours. The resulting film thickness was ~50 μm.
[0026] Test gas separation performance:
[0027] P CO2 =9.65Barrer
[0028] (1Barrer=10 -10 cm 3 (STP)cm / (cm 2 scmHg))
[0029] alpha CO2 / CH4 =12...
Embodiment 3
[0031] At 25° C., under nitrogen gas, 10 mmol mPDA and two-terminal amino polyethylene glycol (molecular weight 600) (mass ratio 15:85) were dissolved in 50 ml DMAc, and then 10 mmol 6FDA was added. The solution was stirred at room temperature for 12 hours to form a viscous polyamic acid solution. Add 40mmol of phthalic acid and 40mmol of pyridine for imidization, react at room temperature for 12 hours, raise the temperature and react at 90°C for 5 hours; then allow the polymer to settle in methanol. The polymer was dried in a vacuum oven at 80°C for more than 24 hours. Dissolve 0.7 g of the obtained polymer in 15 g of THF, pour the solution on a polyethylene plate, and dry it at 25°C to form a film. After obtaining a homogeneous film, put the film in a vacuum oven at 80°C for 24 hours. The resulting film thickness was ~50 μm.
[0032] Test gas separation performance:
[0033] P CO2 = 4.79 Barrer
[0034] (1Barrer=10 -10 cm 3 (STP)cm / (cm 2 scmHg))
[0035] alpha CO2 / ...
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