Polyamide-polyimide coalbed methane denitrification concentration separation membrane with carboxylic acid group
A technology of polyimide and carboxylic acid groups, which is applied in the field of polyamide-polyimide coalbed methane denitrification concentration separation membrane and its preparation, can solve the problems of poor separation effect, reduce the procedure and significantly save energy effect, the effect of high economic and practical value
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[0052] The present invention also provides the preparation method of the above-mentioned polyamide-polyimide coal bed gas denitrification concentration separation membrane with carboxylic acid group, the preparation method comprises steps:
[0053] S100. The polyamide-polyimide compound is prepared by using diamine I, diamine II, dianhydride, and diacid chloride, and the diamine II is a diamine with a carboxyl group;
[0054] S200, using the polyamide-polyimide compound obtained in step S100 to prepare a casting solution;
[0055] S300, using the casting solution obtained in step S200 to prepare a hollow fiber membrane through a phase inversion method, the polyamide-polyimide coalbed gas denitrification concentration separation membrane with carboxylic acid groups.
[0056] In this way, after dissolving two diamines with different structures and polarities, dianhydride and diacid chloride are added for reaction at the same time. After the first step reaction is completed, tolu...
Embodiment 1
[0085] (1) Add 5.4g of p-phenylenediamine, 7.6g of 3,5-diaminobenzoic acid, 10.0g of triethylamine into the reactor which has been dehydrated beforehand, add 135.6g of N,N-dimethylformamide and stir Dissolve, cool to -10°C, add 4,4'-diacid chloride diphenyl ether and 14.7g and 4,4'-(hexafluoroisopropylene) diphthalic anhydride 22.2g alternately in four times, continue to react for 24h after the addition is complete After the first step of reaction is completed, add a water separator to the device, add 17.4g of toluene at the same time, heat to 150°C to continue the reaction for 4h, distill off the toluene, and precipitate the remaining solution in methanol to obtain a light yellow filamentous solid. Vacuum Dry and set aside.
[0086] (2) Weigh 20g of the polymer obtained in step (1), 2g of polyethylene glycol, 10g of isopropanol, 2g of tetrahydrofuran, 0.1g of sodium dodecylbenzenesulfonate, and add to 62.7g N,N- Dimethylformamide was heated to 50°C, stirred and dissolved to ...
Embodiment 2
[0090](1) Add 5.4g of m-phenylenediamine, 7.6g of 3,4-diaminobenzoic acid, 10.0g of triethylamine into the reactor which has been dehydrated beforehand, add 135.6g of N,N-dimethylformamide and stir Dissolve, cool to -10°C, add 4,4'-benzil chloride and 13.9g and 3,3',4,4'-benzophenone tetracarboxylic dianhydride 16.1g alternately in four times, continue to React for 24 hours. After the first step of reaction is completed, add a water separator to the device, add 17.4 g of toluene at the same time, heat to 150 ° C and continue the reaction for 4 hours, distill the toluene, and precipitate the remaining solution in methanol to obtain a light yellow filamentous solid , vacuum dried for later use.
[0091] (2) Weigh 20g of the polymer obtained in step (1), 2g of polyethylene glycol, 10g of isopropanol, 2g of tetrahydrofuran, 0.1g of sodium dodecylbenzenesulfonate, and add to 62.7g N,N- Dimethylformamide was heated to 50°C, stirred and dissolved to prepare a casting solution.
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