Polyacid monomer and preparation method thereof, polyamide and preparation method thereof, and polyamide film

A technology of acid monomers and polyamides, applied in the field of organic synthesis, can solve problems such as selectivity reduction, achieve good solubility, increase free volume and flexibility, and improve poor solubility.

Active Publication Date: 2019-06-21
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] But usually, the permeability and selectivity of polymer membranes restrict each other, that is, the increase in permeability decreases the selectivity, which is the so-called Trade-off effect.

Method used

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  • Polyacid monomer and preparation method thereof, polyamide and preparation method thereof, and polyamide film
  • Polyacid monomer and preparation method thereof, polyamide and preparation method thereof, and polyamide film
  • Polyacid monomer and preparation method thereof, polyamide and preparation method thereof, and polyamide film

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preparation example Construction

[0039] The present invention also provides a method for preparing the polyacid monomer described in the above technical scheme, comprising the following steps:

[0040] When the multi-acid monomer has a structure shown in formula I, the preparation method of the multi-acid monomer comprises the following steps:

[0041] (1) cooling after heating the acetone solution of hydrogen iodide and the acetic acid solution of catechol to reflux to obtain a supersaturated solution, then carrying out hydrothermal treatment to the supersaturated solution to separate out spirotetraphenol; Phenol has the structure shown in formula III:

[0042]

[0043] (2) The spiro tetraphenol obtained in the step (1) and p-fluorobenzonitrile are subjected to a substitution reaction in the presence of a catalyst and an organic solvent to obtain a tetracyano spiro compound, and the catalyst includes salt of wormwood and carbonic acid One or both of cesium; the tetracyano spiro compound has a structure s...

Embodiment 1

[0100] 85g of HI aqueous solution with a mass concentration of 99% was added to 15mL of acetone to form a mixed solution; The mass concentration of catechol is 48%, and the mass concentration of acetic acid in the catechol acetic acid aqueous solution is 40%. The obtained solution was heated to reflux at 120°C for 10 hours, then cooled to room temperature to obtain a supersaturated solution, and the obtained supersaturated solution was hydrothermally crystallized to precipitate white microcrystalline compounds at 220°C and 0.3GPa under high temperature and pressure, filtered, and used ice Acetic acid and dichloromethane were alternately washed three times to obtain 18.0432 g of spiro tetraphenolic compounds.

[0101] In a 250mL three-necked flask equipped with a mechanical stirring device, add 15mmol of the prepared spirocyclic tetraphenol compound, 64mmol of p-fluorobenzonitrile, 12mL of N-methylpyrrolidone, the total solid content of the reaction system is 15%, and stir Unt...

Embodiment 2

[0108] The HI aqueous solution that 5g mass content is 99% is joined in the acetone of 10mL to form mixed solution, the mixed solution that forms joins in the 100mL acetic acid solution that contains 105mmol pyrocatechol, the mass concentration of acetic acid in the acetic acid solution is 40%, then Then add in the 100mL acetic acid solution that contains 150mmol hydroxybenzene, the mass concentration of acetic acid in the acetic acid solution is 40%. Stirring, under the protection of sufficient nitrogen, heating and reflux for 15h, then cooling to room temperature to obtain a supersaturated solution, using the hydrothermal crystallization method to precipitate white microcrystalline compounds at 240°C and 0.5GPa high temperature and high pressure, Filtrate, and alternately wash three times with glacial acetic acid and dichloromethane to obtain a spirocyclic triphenol compound.

[0109] In a 250mL three-necked flask equipped with a mechanical stirring device, add 15mmol of spi...

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Abstract

The invention provides a polyacid monomer and a preparation method thereof, polyamide and a preparation method thereof, and a polyamide film, and belongs to the technical field of organic synthesis. The polyacid monomer provided by the invention has a structure shown in a formula I or a formula II; the polyacid monomer provided by the invention has a microporous structure, a flexible group (etherbond) and a hydroxyl structure; the polyacid monomer provided by the invention is further polymerized with a diamine monomer to obtain polyamide; the polyamide film formed by the polyamide provided bythe invention simultaneously has relatively good selective permeability and permeability; and in addition, the polyamide provided by the invention has relatively good solubility.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a polyamine monomer and a preparation method thereof, a polyamide and a preparation method thereof, and a polyamide film. Background technique [0002] Most gas separation membranes (GS) are non-porous membranes, and the gas permeation process follows the "dissolution-diffusion" mechanism. Due to the aromatic ring structure on the main chain and intermolecular hydrogen bonding, aromatic polyamide has good heat resistance, mechanical strength and separation performance, and has been widely used in the field of gas separation since the 1990s. [0003] Gas separation membrane technology is a green separation technology. Compared with separation technologies such as "cryogenic separation" and "pressure swing adsorption separation", its separation process has the advantages of high separation efficiency, simple operation, low energy consumption, green and pollution-free, etc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C65/26C07C51/08C08G69/40C08J5/18C08L77/10
Inventor 周宏伟赫洪如王书丽王大明陈春海赵晓刚
Owner JILIN UNIV
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