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Preparation method of polyimide organic solvent nanofiltration membrane containing spirobiindane structure

A polyimide and organic solvent technology, which is applied in the field of preparation of polyimide organic solvent nanofiltration membranes containing spirobisindane structure, can solve the problem of strong toxicity of chemical solvents, unstable performance of polyamic acid, and difficulty in processing problems such as film, to achieve the effect of enhancing compaction resistance and long-term operation stability, simple and easy preparation method, and improving solvency

Active Publication Date: 2022-07-29
XI AN JIAOTONG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the solubility of aromatic polyimides is different due to the rigidity of the chain segment, and most of the polyimide materials with excellent performance are difficult to be processed into films due to their insoluble and infusible characteristics.
[0005] Based on the above problems, some scholars have proposed the following solutions: In the process of two-step synthesis of polyimide, the precursor polyamic acid will be obtained in the first step. Generally, polyamic acid is soluble in most aprotic polar Solvent, which is formulated into a casting solution and solidified into a film by phase inversion method, and then transformed into a polyimide film by imidization; this method has great application potential in theory, but the performance of polyamic acid is unstable and easy to hydrolyze , which is unfavorable for long-term storage; in addition, the large energy consumption (thermal imidization) or strong toxicity of chemical solvents (chemical imidization) in the imidization process greatly limits its application

Method used

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  • Preparation method of polyimide organic solvent nanofiltration membrane containing spirobiindane structure
  • Preparation method of polyimide organic solvent nanofiltration membrane containing spirobiindane structure
  • Preparation method of polyimide organic solvent nanofiltration membrane containing spirobiindane structure

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preparation example Construction

[0040] see figure 1 , a preparation method of a polyimide organic solvent nanofiltration membrane containing a spirobisindan structure according to an embodiment of the present invention includes the following steps:

[0041]S1: 4,5-dichlorophthalonitrile, 5,5',6,6'-tetrahydroxy-3,3,3',3'-tetramethyl-1,1'-spirobisindane (TTSBI) and anhydrous potassium carbonate are added to N,N-dimethylformamide, heated to 70~90℃ to react to obtain tetranitrile containing spirobisindane structure; exemplarily preferred, the reaction time is 3~ 4h;

[0042] S2: adding the tetranitrile containing the spirobisindane structure into a solvent, and heating to 80-90° C. in an alkaline environment to react to obtain the tetraacid containing the spirobisindane structure; wherein the solvent is methanol and A mixed solution of water or a mixed solution of ethanol and water; preferably, the solvent is a methanol / water or ethanol / water mixed solution with a volume ratio of 1:1; the alkaline environment ...

Embodiment 1

[0061] A preparation method of a polyimide organic solvent nanofiltration membrane containing a spirobisindan structure according to an embodiment of the present invention includes the following steps:

[0062] (1) Preparation of spirobisindane tetranitrile: 5,5',6,6'-tetrahydroxy-3,3,3',3'-tetramethyl-1,1'-spirobisindane was used Recrystallization from methanol, methanol-dichloromethane system; 4,5-dichlorophthalonitrile, 5,5',6,6'-tetrahydroxy-3,3,3',3'-tetramethyl- 1,1'-spirobisindane and anhydrous potassium carbonate were used as monomer raw materials, added to N,N-dimethylformamide, heated to 85°C in an oil bath for 3h reaction; the resulting milky white suspension was added to a large amount of pure water Stirring in medium, dilute hydrochloric acid is added dropwise to neutralize excess potassium carbonate until the system is acidic; the product is suction filtered, washed, and dried in vacuum to finally obtain a tetranitrile containing a spirobisindane structure.

[0...

Embodiment 2

[0068] A preparation method of a polyimide organic solvent nanofiltration membrane containing a spirobisindan structure according to an embodiment of the present invention includes the following steps:

[0069] (1) Preparation of spirobisindane tetranitrile: 5,5',6,6'-tetrahydroxy-3,3,3',3'-tetramethyl-1,1'-spirobisindane was used Recrystallization from methanol, methanol-dichloromethane system; 4,5-dichlorophthalonitrile, 5,5',6,6'-tetrahydroxy-3,3,3',3'-tetramethyl- 1,1'-spirobisindane and anhydrous potassium carbonate were used as monomer raw materials, added to N,N-dimethylformamide, heated to 85°C in an oil bath for 3h reaction; the resulting milky white suspension was added to a large amount of pure water Stirring in medium, dilute hydrochloric acid is added dropwise to neutralize excess potassium carbonate until the system is acidic; the product is suction filtered, washed, and dried in vacuum to finally obtain a tetranitrile containing a spirobisindane structure.

[0...

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Abstract

The invention discloses a preparation method of a polyimide organic solvent nanofiltration membrane containing a spirobiindane structure, which comprises the following steps: adding 4, 5-dichlorophthalonitrile, 5, 5 ', 6, 6'-tetrahydroxy-3, 3, 3 ', 3'-tetramethyl-1, 1 '-spirobiindane and anhydrous potassium carbonate into N, N-dimethylformamide to prepare tetranitrile containing the spirobiindane structure; tetracid containing a spirobiindane structure is prepared; dianhydride containing a spirobiindane structure is prepared and obtained; in an inert gas atmosphere, synthesizing to obtain polyamide acid; and preparing to obtain the polyimide organic solvent nanofiltration membrane containing the spirobisindane structure. The preparation method provided by the invention is simple and easy to implement, the cast membrane forms an all-form spongy pore structure in the phase inversion process due to the introduction of a rigid distortion structure, and the compaction resistance and long-term operation stability of the nanofiltration membrane can be greatly enhanced.

Description

technical field [0001] The invention belongs to the technical field of organic solvent nanofiltration, in particular to a preparation method of a polyimide organic solvent nanofiltration membrane containing a spirobisindan structure. Background technique [0002] Organic solvent nanofiltration is an emerging membrane separation and technology, which has great advantages over traditional separation processes. It can separate organic mixtures at the molecular level only by simple pressure driving. [0003] At present, the membrane separation materials used in organic solvent nanofiltration include organic polymer membrane materials and inorganic membrane materials; among them, the development of inorganic materials is limited due to the problems of high preparation cost and difficulty in controlling the pore size. It has won the favor of many scholars in this field. Among the existing commercial polymer membrane materials, polyimide is one of the most widely used separation m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D67/00B01D71/64
CPCB01D67/0002B01D67/0006B01D71/64Y02A20/131
Inventor 伊春海乔杰吴东云
Owner XI AN JIAOTONG UNIV
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