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A kind of polyimide self-porous polymer membrane containing crown ether micropores and preparation method thereof

A microporous polymer and polyimide technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the problems of wide pore size distribution, difficult control of micropore size, unfavorable gas selectivity, etc. Achieve the effect of increasing free volume, easy synthesis, and improving sieving selectivity

Active Publication Date: 2019-11-08
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the pore size of this type of microporous polymer material is difficult to control, and the pore size distribution is wide, which is unfavorable for gas selectivity.

Method used

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  • A kind of polyimide self-porous polymer membrane containing crown ether micropores and preparation method thereof
  • A kind of polyimide self-porous polymer membrane containing crown ether micropores and preparation method thereof
  • A kind of polyimide self-porous polymer membrane containing crown ether micropores and preparation method thereof

Examples

Experimental program
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preparation example Construction

[0030] (1) Preparation of crown ether compounds; Crown ether compounds include diaminodibenzo-15-crown-5, diaminodibenzo-18-crown-6 or diaminodibenzo-21-crown-7, the following Taking the preparation of diaminodibenzo-18-crown-6 as an example to illustrate, when preparing other crown ether compounds, replace the dibenzo-18-crown-6 in the raw material with dibenzo-15-crown-5 or Dibenzo-21-crown-7 is sufficient.

[0031] Dissolve dibenzo-18-crown-6 in a mixed solvent composed of chloroform and glacial acetic acid to obtain dibenzo-18-crown-6 solution; add nitric acid and acetic anhydride mixture to dibenzo-18 -Crown-6 solution, wherein the ratio of dibenzo-18-crown-6, chloroform, glacial acetic acid, nitric acid and acetic anhydride is (0.0125~0.0153)mol:(95~115)mL:(70~80) mL: (3~4.5)mL: (13.5~15.5)mL; react at 10~25°C for 1~1.5h, raise the temperature to 40~80°C and continue to react for 5~6h, filter the yellow precipitate, recrystallize, and vacuum dry, namely Trans-dinitrodi...

Embodiment 1

[0042] (1) Preparation of diaminodibenzo-18-crown-6

[0043] Dissolve 0.0142mol of dibenzo-18-crown-6 in a mixed solvent consisting of 105mL of chloroform and 75mL of glacial acetic acid, and add 3.6mL of nitric acid and 14.25mL of acetic anhydride to dibenzo-18-crown-6 dropwise. In the solution, react at -17°C for 1.2h, raise the temperature to 50°C and continue to react for 5.5h, filter the yellow precipitate, recrystallize at 150°C, and dry in vacuum to obtain trans-dinitrodibenzo- 18-Crown-6, its yield can reach 62.9mol%; the filtrate stands still, and almost no cis product is precipitated.

[0044] Dissolve the prepared 0.0037mol of dinitrodibenzo-18-crown-6 in 100mL of ethylene glycol methyl ether to prepare a reaction solution with a concentration of 0.037mmol / mL, and add the reaction solution to the reaction kettle; Base dibenzo-18-crown-6 mass 4% Pd / C catalyst, then filled with H 2 to 0.35MPa, stir and heat up, and react at 75°C for 2.5h; filter the solution in the ...

Embodiment 2

[0055] (1) The preparation method of diaminodibenzo-18-crown-6 is the same as step (1) in Example 1.

[0056] (2) Preparation of crown ether microporous polyimide self-porous polymers

[0057] Under nitrogen protection, mix diaminodibenzo-18-crown-6 with commercial 4,4'-diaminodiphenylmethane at a molar ratio of 0.33, add N,N-dimethylacetamide, and magnetically stir Dissolved to obtain a diamine solution; according to the molar ratio of aromatic diamine to aromatic dianhydride as 1:1, add 4,4'-hexafluoroisopropylphthalic anhydride solid directly into the diamine solution to prepare Prepare a solution with a total mass fraction of aromatic diamine and aromatic dianhydride of 18wt%, and stir at room temperature for 9 hours; The ratio is 2:1, add a mixture of acetic anhydride and triethylamine, stir at 50°C for 3h; cool to room temperature, desolventize the final reaction solution, remove impurities, and vacuum dry at 90°C for 24h to obtain the Porous polyimides are microporous...

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Abstract

The invention relates to a crown ether micropore containing polyimide intrinsic microporosity polymer membrane and a preparation method thereof. The preparation method comprises the following steps of: firstly, preparing a diamine solution from aromatic diamine; adding aromatic dianhydride into the diamine solution, and stirring for 9-13 hours at the room temperature; further adding a dehydration agent and a catalyst, stirring for 3-6 hours at 40-65 DEG C, removing the solvent, and drying, so as to obtain a crown ether micropore containing polyimide intrinsic microporosity polymer; and dissolving the polymer by using an organic solvent so as to obtain a membrane casting liquid, and performing membrane casting and drying, thereby obtaining the crown ether micropore containing polyimide intrinsic microporosity polymer membrane. As crown ether micropores are introduced into the polymer membrane provided by the invention, dense accumulation of polymer chain segments can be effectively prevented by virtue of steric hindrance of a cyclic structure of crown ether, an intrinsic microporosity polymer membrane material has a relatively large free volume, and in addition ether bonds of the crown ether have very good affinity with CO2, so that the prepared crown ether micropore containing polyimide intrinsic microporosity polymer membrane is relatively high in gas permeability coefficient and good in selectivity.

Description

【Technical field】 [0001] The invention relates to the field of polymer membranes, in particular to a polyimide self-porous polymer membrane containing crown ether micropores and a preparation method thereof. 【Background technique】 [0002] Ordinary polymer membrane materials are better in processability, but have the disadvantage of high permeability and high selectivity; microporous materials such as molecular sieves and metal-organic framework materials have high permeability and selectivity, and can break through ordinary high The "Robenson" upper limit of molecular membrane materials, but it is difficult to scale up, difficult to prepare ultra-thin films, and poor flexibility. Compared with the first two materials, the microporous polymer material (PIM) has a microporous structure similar to molecular sieve materials, which can realize the sieving of molecules of different sizes, has high permeability selectivity, and also has the polymer material itself. It has the adv...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J5/18C08L79/08C08G73/10B01D61/14B01D67/00B01D71/64
CPCB01D61/147B01D67/0006B01D71/64C08G73/1071C08J5/18C08J2379/08
Inventor 伊春海吴东云杨伯伦
Owner XI AN JIAOTONG UNIV
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