A kind of polyimide precursor composition, its preparation method and its manufacture polyimide substrate
A polyimide precursor and composition technology, which is applied in the field of polyimide substrates and polyimide precursor compositions, can solve the problem of low storage stability of polyimide precursor compositions and difficulty in preparing substrates , difficult to handle and other problems, to achieve the effect of excellent storage stability, excellent mechanical properties, high solid content
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[0058] The method for preparing polyimide precursor composition according to the present invention comprises:
[0059] (1) Mix and react aromatic dianhydride and aromatic diamine to prepare polyamic acid solution, the aromatic dianhydride contains 3,4,3',4'-biphenyltetracarboxylic dianhydride (BPDA) , the aromatic diamine comprises p-phenylenediamine (PPD);
[0060] (2) mixing the polyamic acid solution, tertiary amine curing agent and antioxidant to obtain a mixture; and
[0061] (3) The mixture is mixed with an aromatic carboxylic acid having at least four carboxyl groups.
[0062] step 1)
[0063] In this step, a polyamic acid solution is prepared by mixing and reacting an aromatic dianhydride containing 3,4,3',4'-biphenyltetracarboxylic dianhydride and an aromatic diamine (BPDA), the aromatic diamine comprising p-phenylenediamine (PPD).
[0064] The step (1) can be carried out at 30-90°C.
[0065] In the step (1), by reacting the reaction solvent, 3,4,3',4'-biphenyl...
Embodiment 1
[0096] Embodiment 1: the preparation of polyimide precursor composition
[0097] While purging nitrogen, 300 g of NMP was added to a 500 mL reactor with stirring device and nitrogen inlet / outlet. After setting the temperature of the reactor to 30° C., 27.19 g of PPD, 35.74 g of BPDA, 0.87 g of BTDA and 28.00 g of PMDA were added thereto, and the resulting mixture was stirred until completely dissolved and reacted. After the reaction was completed, 1.44 g of PMDA was dissolved in NMP at a concentration of 5 wt.%, which was added at intervals of 10 minutes until the viscosity of the mixture at 23° C. reached 6,000 cP. Then, 1 mole of DABCO and 10 moles of IQ were sequentially added for every 100 moles of the polyamic acid. FP-900L was added at a concentration of 1 wt% (based on the total weight of the polyamic acid), followed by stirring. Then, 4 moles of PMA were added per 100 moles of PPD. The resulting product was stirred well until the reaction was complete. NMP was then...
Embodiment 2
[0103] The same method as in Example 1 was used to prepare a polyimide precursor composition (viscosity at 23°C was 3,300cP, solid content was 20wt%, weight-average molecular weight was 22,000g / mol), the difference was that PMDA was not used As the aromatic dianhydride, the BPDA was used in an amount of 95 moles per 100 moles of PPD.
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