Polyimide (PI) composite membrane for pervaporation separation of amide/water and preparation method thereof

A technology for separation of amides and pervaporation, applied in semipermeable membrane separation, chemical instruments and methods, membrane technology, etc.

Inactive Publication Date: 2018-06-08
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Polyimide (PI) composite membrane for pervaporation separation of amide/water and preparation method thereof
  • Polyimide (PI) composite membrane for pervaporation separation of amide/water and preparation method thereof
  • Polyimide (PI) composite membrane for pervaporation separation of amide/water and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0028] 5 mmol 4,4'-diaminodiphenyl ether, 5 mmol 3,5-diaminobenzoic acid, 10 mmol 3,3',4,4'-benzophenone tetraacid dianhydride (diamine After mixing with dianhydride molar ratio of 1:1) and 27 (solute to solvent mass ratio of 15:85) ml NMP, mechanically stir at room temperature for 20 minutes, stir and react in ice bath and nitrogen atmosphere for 3 hours, after the reaction is completed, degassing Finally, a PAA solution is obtained. The composite film was prepared by dipping and pulling method, and the PAA casting solution was evenly coated to a thickness of 2 mm on Al 2 o 3 On the surface of the porous base membrane, the PAA solution was spread on the surface to form a composite membrane, and then the composite membrane was placed in an oven for programmed temperature imidization reaction (150°C for 0.5h, 200°C for 1h, 250°C for 1h, 300°C for 1h ), naturally cooled to room temperature to obtain a composite membrane with a polyimide separation layer of 30 μm.

[0029] The...

Embodiment 2

[0036] 5 mmoles of 4,4'-diaminodiphenyl ether, 5 mmoles of 3,5-diaminobenzoic acid, 10.3 mmoles of pyromellitic dianhydride (the molar ratio of diamine to dianhydride is 1:1.03) and After mixing 23 ml of NMP (mass ratio of solute to solvent: 15:85), mechanically stir at room temperature for 20 min, stir and react in ice bath and nitrogen atmosphere for 3 h, and obtain PAA solution after degassing at the end of the reaction. The composite film was prepared by dipping and pulling method, and the PAA casting solution was uniformly coated to a thickness of 2 mm on Al 2 o 3 On the surface of the porous base membrane, spread the PAA solution on the surface to form a composite membrane, and then put the composite membrane into an oven for programmed temperature imidization reaction (150°C for 0.5h, 200°C for 1h, 250°C for 1h, 300°C for 1h ), naturally cooled to room temperature to obtain a composite membrane with a polyimide separation layer of 30 μm.

[0037] The separation perfor...

Embodiment 3

[0044] With 5 mmoles of benzidine, 5 mmoles of 4,4'-diaminodiphenyl ether, 10.3 mmoles of 3,3',4,4'-benzophenone tetraacid dianhydride (the molar ratio of diamine to dianhydride is 1:1.03) and 29 ml of NMP (the mass ratio of solute to solvent is 15:85), mechanically stirred at room temperature for 20 min, stirred and reacted in ice bath and nitrogen atmosphere for 3 h, and the PAA solution was obtained after degassing at the end of the reaction. The composite film was prepared by the dipping and pulling method, and the PAA casting solution was evenly coated to the ZrO with a thickness of 2mm. 2 On the surface of the porous base membrane, spread the PAA solution on the surface to form a composite membrane, and then put the composite membrane into an oven for programmed temperature imidization reaction (150°C for 0.5h, 200°C for 1h, 250°C for 1h, 300°C for 1h ), naturally cooled to room temperature to obtain a composite membrane with a polyimide separation layer of 30 μm.

[00...

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Abstract

The invention discloses a polyimide composite membrane for pervaporation separation of amide/water and a preparation method thereof and belongs to the technical field of pervaporation separation. An inorganic porous base membrane is coated with a compact polyimide separated layer through a dipping and pulling process so that the polyimide pervaporation composite membrane is obtained. In order to prepare the polyimide pervaporation composite membrane with high separation performances, the main chain structure of a precursor polyamic acid resin of the separated layer polyimide membrane has symmetry groups with rigid chains (such as benzene rings) and the main chain structure contains the symmetry rigid chains. The membrane satisfies the requirements on the amide/water mixed pervaporation separation membrane in solvent resistance and selective separation and is suitable for the preparation of the pervaporation membranes.

Description

technical field [0001] The technology of the invention mainly relates to a polyimide composite membrane used for pervaporation separation of amide / water and a preparation method thereof, belonging to the technical field of pervaporation separation. Background technique [0002] Amide solvents, such as: dimethylformamide (DMF), dimethylacetamide (DMAc), etc., although they cannot easily donate protons, they have strong dissolving power because they can solvate cations. This kind of solvent has good thermal stability and chemical stability, and is widely used in petrochemical, organic synthesis, pesticide, medicine, synthetic leather industry and other fields. According to statistics, in recent years, my country's synthetic leather industry, acrylic fiber industry, spandex industry, dye industry and petrochemical industry have an annual demand for amide solvents of more than 200,000 tons. The used part forms a dilute solution of about 5-20wt%, which is directly discharged by ...

Claims

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Application Information

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IPC IPC(8): B01D71/64B01D69/12B01D67/00
CPCB01D67/0013B01D69/12B01D71/64
Inventor 钟璟马文中邓力徐荣张琪
Owner CHANGZHOU UNIV
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