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Method for preparing polyimide film

A polyimide film and polyimide resin technology, which is applied in the field of polyimide resin preparation, can solve the problem of yellowing, affecting the light transmittance, yellowness index and haze of polyimide film, etc. problem, to achieve the effect of low yellowness index and haze, easy processing and production, and simple process flow

Active Publication Date: 2015-07-29
威海新元科盛新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These solvents are prone to yellowing at high temperatures, which in turn affects parameters such as light transmittance, yellowness index, and haze of the final polyimide film
Instead, use polar solvents with relatively low boiling points, such as N,N-dimethylformamide (DMF, boiling point: 155 oC), N,N -Dimethylacetamide (DMAc, boiling point: 166oC) often cannot complete the imidization reaction

Method used

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  • Method for preparing polyimide film
  • Method for preparing polyimide film
  • Method for preparing polyimide film

Examples

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Effect test

preparation example Construction

[0027] A kind of preparation method of polyimide film, it comprises the steps:

[0028] (1) In a high-pressure reactor equipped with mechanical stirring, thermometer, inert gas inlet and outlet, and Dean-Stark water trap, dissolve the diamine compound in N,N - Dimethylformamide (DMF) or N,N - In dimethylacetamide (DMAc) solvent;

[0029] (2) Pass inert gas into the autoclave and add dianhydride compound;

[0030] (3) After all the reactants are dissolved, add organic base catalyst and dehydrating agent, and seal the reaction kettle;

[0031](4) Heating to raise the temperature to 120~150°C, and carry out reflux dehydration for 3~10 hours. After the dehydration is completed, remove the toluene and continue to raise the temperature at a reaction temperature of 160~190°C and a reaction pressure of 0.1~1 MPa. Carry out imidization reaction, the time is 1-10 hours, obtain polyimide resin;

[0032] (5) Dissolving the polyimide resin prepared in step (4) in an organic solvent to ...

Embodiment

[0061] Example 1 A kind of preparation method of polyimide film, it comprises the steps:

[0062] 20.024 g (100 mmol) of ODA and 60 g of DMAc were added to a 1000 mL autoclave equipped with a nitrogen inlet and equipped with a thermometer, water separator, condenser and mechanical stirring. After stirring at room temperature to dissolve completely, under nitrogen protection, add 22.417 g (100 mmol) HPMDA and 18.8 g DMAc, adjust the solid content to 35% (mass percentage) with DMAc, and add 0.5 g isoquinoline With 250 g xylene, heat up to reflux, and divide the water for 4 hours. Then xylene is released from the water separator. The reaction system was airtight and continued to heat up to 165 o C. At this time, the system pressure is 0.12 MPa, continue to react for 6 h, stop the reaction, remove the pressure, cool to room temperature, slowly pour the obtained light yellow viscous solution into a large amount of ethanol to obtain a white filamentous resin, 100 o C was dried...

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Abstract

The invention discloses a method for preparing a polyimide film. The method comprises the following steps: in a high-pressure reaction kettle, dissolving a diamines compound in an N,N-dimethylformamide or N,N-dimethylacetamide solvent; pumping in an inert gas and adding a dianhydride compound; after the reactant is fully dissolved, adding an organic alkali catalyst and a dehydrating agent, and enclosing the reaction kettle; heating to be 120-150 DEG C, performing reflow dewatering, removing methylbenzene after finish of reflow dewatering, continually heating up, and conducting imidization reaction for 1-10 hours at the reaction temperature of 160-190 DEG C and the pressure of 0.1-1 MPa to obtain polyimide resin; dissolving the prepared polyimide resin in an organic solvent, and further preparing to obtain the colorless transparent polyimide film. The method has the advantages that the processing and the producing are easy, the technological process is simple, the operability is strong, the technology conditions are relatively mild, the reaction temperature is relatively low, the production security is high and good environment friendliness and high practicability are achieved.

Description

technical field [0001] The invention relates to a method for preparing an organic polymer material, in particular to a method for preparing a polyimide resin. Background technique [0002] Polyimide is a class of organic polymer materials containing imide rings in its molecular structure. Polyimide is usually prepared by polycondensation of aromatic dianhydride compounds and diamine compounds. Rigid imidization and polar molecular structure endow polyimide materials with excellent thermal stability, insulation properties, mechanical properties and environmental stability. But at the same time, in the polyimide molecular structure, the dianhydride unit acts as an electron donor, and the diamine unit serves as an electron acceptor, and a charge transfer complex (CTC) is easily formed between the two. The formation of CTC causes the polyimide film to produce significant absorption of visible light, making the traditional fully aromatic polyimide film present a dark brown or d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J5/18
Inventor 李璐王超王金青
Owner 威海新元科盛新材料有限公司
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