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

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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

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  • Polyimide preparation method and application thereof

Examples

Experimental program
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Effect test

Example Embodiment

[0022] Example 1

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

[0024] After testing, the polyimide obtained in this example has a weight-average molecular weight Mw of 3*10 6 , the averag...

Example Embodiment

[0025] Example 2

[0026] The aromatic diamine monomer 3,3'-dimethyl-4,4'-diaminodiphenylmethane is dissolved in a certain amount of N,N under the protection of inert gas and the temperature is 5℃~10℃. -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'-dianisole tetraacid dianhydride, diamine and The molar ratio of the dianhydride is 1:0.99, and the reaction is carried out for 10-13 hours under the control of the reaction temperature at 5°C. 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, washing and vacuum drying with ethanol water.

[0027] After testing, the polyimide obtained in this example has a weight-average molecular weight Mw of 3.5*10 6 , the average chain spacing is 0.56nm; the temperature when thermal d...

Example Embodiment

[0028] Example 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 wire mesh, and then debubble it in a vacuum for later use. Under the conditions of dust-free, 25°C, and humidity of 50-70%, the above-mentioned casting liquid is coated on PET non-woven fabric, the wet film thickness is 250um, and the film is phase-converted in water or ethanol to obtain polyimide. basement membrane.

[0031] 2) The polyimide-based film prepared above is immersed in alcohol for a period of time to remove residual moisture in the film by solvent exchange, and then immersed in a certain concentration of diamine / alcohol solvent for cross-linking for a period of time. The membrane was stored in an alcohol solvent to prevent the membrane pores from collapsing and was used to prepare a PA / PI composite na...

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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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