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Polyimide preparation method and application thereof

A technology of polyimide and polyamic acid, applied in the field of resin, can solve the problems of poor fluidity, insoluble and insoluble, application limitation, etc., and achieve the effect of improving solubility and solubility.

Inactive Publication Date: 2018-01-19
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally speaking, polyimide resin can be divided into two categories: thermoplastic and thermosetting. Although thermoplastic polyimide resin has good impact toughness, it has high melt viscosity and poor fluidity, which makes it difficult to combine with carbon fiber. The disadvantages of preparing carbon fiber / polyimide composite materials, although thermosetting polyimide resins have higher high temperature resistance, low melt viscosity, good fluidity, and are easy to compound with carbon fibers to prepare carbon fiber / polyimide composite materials , but there are disadvantages of poor impact toughness
[0004] Ordinary polyimide (PI) is refractory and insoluble due to its structural characteristics such as good molecular chain regularity, high rigidity, and strong interchain interaction. It is difficult to process and shape, and its application is limited.

Method used

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  • Polyimide preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Under the protection of an inert gas and at a temperature of -10°C to 10°C, dissolve the aromatic diamine monomer 3,3'-dimethyl-4,4'-diaminodiphenylmethane in a certain amount of N, In N-dimethylformamide, the solid content of the monomer is controlled to be 10%. After the diamine is completely dissolved, a certain amount of 3,3′,4,4′-benzophenone tetraacid dianhydride, diamine and The molar ratio of 3,3′,4,4′-benzophenonetetraacid dianhydride is 1:1.01, the reaction temperature is controlled at 5°C, and the reaction is carried out for 10-13 hours, and then a certain amount of chemical imidization reagent acetic anhydride / pyridine is added After continuing to stir and react for a period of time, a polyimide solution was obtained, and a polyimide solid was obtained after ethanol water precipitation, washing, and vacuum drying.

[0024] After testing, the weight average molecular weight Mw of the polyimide obtained in this embodiment is 3*10 6 , the average chain spacing...

Embodiment 2

[0026] Under the protection of an inert gas and at a temperature of 5°C to 10°C, dissolve the aromatic diamine monomer 3,3′-dimethyl-4,4′-diaminodiphenylmethane in a certain amount of N,N -In dimethylformamide, the solid content of the monomer is controlled to be 6%. After the diamine is completely dissolved, a certain amount of 3,3',4,4'-diphenylmethyl ether tetraacid dianhydride, diamine and The molar ratio of dianhydride is 1:0.99, and the reaction temperature is controlled at 5°C for 10-13 hours. Add a certain amount of chemical imidization reagent acetic anhydride / picoline, continue to stir and react for a period of time to obtain a polyimide solution, and obtain a polyimide solid after precipitation with ethanol water, washing, and vacuum drying.

[0027] After testing, the weight-average molecular weight Mw of the polyimide obtained in this embodiment is 3.5*10 6 , the average chain spacing is 0.56nm; the temperature at 10% thermal decomposition is 510°C; the glass tra...

Embodiment 3

[0029] Preparation of composite nanofiltration membrane:

[0030] 1) Take 10 g of the polyimide solid prepared in Example 1 above, dissolve it in 85 ml of polar protic solvent at room temperature, dissolve evenly, filter it with a 300-mesh steel mesh, and vacuum debubble it for later use. In a dust-free environment at 25°C and a humidity of 50-70%, the above-mentioned casting solution is coated on PET non-woven fabrics, with a wet film thickness of 250um, and phase-inverted in water or ethanol to form a film for use to obtain polyimide basement membrane.

[0031] 2) Immerse the polyimide base film prepared above in alcohol for a period of time to remove the residual moisture in the film by solvent exchange, and then immerse in a certain concentration of diamine / alcohol solvent for crosslinking for a period of time, the crosslinked The membrane is stored in an alcohol solvent to prevent the membrane pores from collapsing and is used to prepare PA / PI composite nanofiltration me...

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Abstract

The invention provides a polyimide preparation method and an application thereof. The method comprises the following steps: 1) under inert gas protection, dissolving an aromatic diamine monomer 3, 3'-dimethyl-4,4'-diaminodiphenylmethane in a polar aprotic solvent to obtain an aromatic diamine monomer solution, then adding dianhydride in batch in the solution, and reacting the materials at the temperature of -20-40 DEG C to obtain an polyamide acid solution having viscosity; and 2) adding a chemical imidization reagent in the polyamide acid solution for a reaction to obtain a polyimide solution; wherein the chemical imidization reagent comprises a dehydrating agent and a catalyst. The polyimide is taken as a base material, an interfacial polymerization method is employed for preparing an organic solvent-resistant nanofiltration membrane, and the polyimide has the advantages of good stability, good mechanical property and excellent dissolvability.

Description

technical field [0001] The invention belongs to the technical field of resins, and in particular relates to a preparation method and application of polyimide. Background technique [0002] From the invention of aromatic polyimide compounds by Dupont Company in the United States in 1955 to the present, many kinds of polyimide films and their products with various structures and properties have been developed. Because polyimide has unique advantages such as excellent mechanical properties, electrical properties, radiation resistance and heat resistance, it is more and more widely used in aerospace, electronics, automobiles, communications and other industries. Correspondingly, the research on polyimide materials and their preparation methods is also carried out in depth. [0003] In recent years, there have been a large number of research reports on the high temperature resistance and molding processability of polyimide resin matrix composites. Generally speaking, polyimide ...

Claims

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Application Information

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IPC IPC(8): C08G73/10B01D69/12B01D69/02D06M15/59D06M101/32
Inventor 侯影飞孟新迪牛青山远冰冰
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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