Polyimide composite film and preparation method thereof
A polyimide film and polyimide technology, applied in the field of polyimide composite film and its preparation, can solve the problems of low temperature resistance and high thermal expansion coefficient
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[0032] The embodiment of the present invention provides a kind of preparation method, see specifically figure 1 ,include:
[0033] S1. Provide diamine, and dissolve the diamine in a polar aprotic solvent under an inert gas atmosphere to form a solution A, wherein the diamine contains a benzoxazole structure.
[0034] The benzoxazole structure significantly contributes positively to the high temperature resistance of the polyimide film (PI film), therefore, diamines containing the bibenzoxazole structure are further preferred. The preferred diamine is 4,4'-([6,6']bi[benzoxazolyl]-2,2'-diyl)-bis-aniline, whose structural formula is:
[0035]
[0036] The polar aprotic solvent is at least one of N,N-dimethylacetamide, N,N-dimethylformamide and N-methylpyrrolidone.
[0037] Wherein, the preparation steps of 4,4'-([6,6']bi[benzoxazolyl]-2,2'-diyl)-bis-aniline specifically include:
[0038] Provide polyphosphoric acid, 3,3'-dihydroxybenzidine and p-aminobenzoic acid, add 3,3'-...
Embodiment 1
[0066] (1) Synthesis of 4,4'-([6,6']bi[benzoxazolyl]-2,2'-diyl)-bis-aniline:
[0067] in N 2 Under the protection of gas atmosphere, 150 g of polyphosphoric acid (PPA) was added to the flask equipped with mechanical stirring, and the initial temperature was set to 70°C. 10.8135g of 3,3'-dihydroxybenzidine (ie 0.05mol) and 14.3997g of p-aminobenzoic acid (ie 0.105mol) were sequentially added into the reaction flask, and a small amount of amino protecting agent and desiccant were added. Slowly raise the temperature to 110°C and keep for 2h; then slowly raise the temperature to 200°C and keep for 6h. Then the reaction solution is poured into deionized water, left to filter, and the filter cake is 10% NaHCO with mass fraction 3 The solution was adjusted to pH 7 and allowed to stand overnight. Wash and filter the filter cake with water, dry it in vacuum, collect and obtain unpurified diamine, and further use DMAC+H 2 O was recrystallized and purified to obtain purified diamine ...
Embodiment 2
[0083] (1) In this example, the synthesis method of 4,4'-([6,6']bi[benzoxazolyl]-2,2'-diyl)-bis-aniline is the same as in Example 1, wherein , the mass of DMAC is 59.2542g.
[0084] (2) The method for surface hydrophobic modification of ZnS particles in this example is the same as that in Example 1.
[0085] (3) prepare polyamic acid solution containing ZnS particles:
[0086] 0.6583 g of surface hydrophobically modified ZnS particles with a size of about 5-8 μm were uniformly dispersed into solution A to obtain suspension B.
[0087] 2.3993g (ie 0.011mol) of pyromellitic dianhydride (PMDA) was added to the suspension B, and a homogeneous polyamic acid solution was generated after in-situ polymerization for 12 hours; the viscosity of the polyamic acid solution was 10Pa·s.
[0088] Wherein, diamine and dianhydride account for 10% of the total reaction slurry (excluding ZnS particles); the amount of ZnS particles is 10% of the total mass of diamine and dianhydride.
[0089] T...
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