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Synthesis of Polyimide Siloxane

Jul 10, 2023

Polyimide siloxane was first synthesized in 1966. Then, thermoplastic polyimide siloxane was synthesized by the same method and successfully used as a high-strength adhesive and molding compound. The study of silicon containing polyimides shows that the introduction of flexible siloxane blocks into the polyimide skeleton can produce soluble copolymers with better processability, heat resistance, weather resistance and mechanical properties. Due to the preferential migration of siloxane segments to the surface of the copolymer, the copolymer has lower water absorption and higher atomic oxygen resistance. Silicon containing polyimides synthesized by other methods also have similar properties. It is precisely because silicon containing polyimides have these excellent properties that their research has been developing.

Modified raw materials and methods
The monomers used in copolymerization are aromatic dianhydride and aromatic diamine commonly used in the preparation of conventional PI, such as benzophenone tetraoxonic dianhydride CBTDA, pyromellitic dianhydride (PMDA), hexaazadianhydride (6F), chloroformyl phthalic anhydride (TMAC), diphenylamine A, 4,4 '- diamino Diphenyl ether (4,4' -0DA), 3,31- aminodiphenylsulfone (3,31-DDS), 3,3 '- diamino benzophenone (3,31-DABP), Diphenylamine methane (3,31-MDA) etc. Add the following three organic silicon components separately: silane compounds represented by silane coupling agents containing amino functional groups in CD Organosilicon oligomers with an amino terminated end Organosilicon oligomers with amino groups at both ends.

Copolymerization reaction: Under the presence of solvent, aromatic dianhydride is reacted with organic silicon components, and then diamine is added to increase the chain to obtain a certain molecular weight of silicon-containing polyamide acid. Among them, a quantitative amount of monoanhydride needs to be added to control the molecular weight and end group structure. Due to the different solubility of organic silicon components and aromatic monomers, mixed solvent systems are commonly used. The available solvents are N-methyl pyrrolidone (NMP), N, N-di N-Methylformamide (DMF), Dimethylacetamide (DMAC), tetrahydrofuran (THF), etc. The obtained silicone polyamide acid is heated, dehydrated and cyclized to obtain silicone modified polyimide.

There are two methods for imidization: one is the usual bulk heating dehydration imidization method. Generally, the solution of polysiloxane amide acid is streamed onto the substrate, and then the solvent is removed to form a film by vacuuming at 100 ° C for several hours. The film is then placed in the center of the blast furnace and thermally cycled at 100 ° C, 200 ° C, and 300 ° C for one hour, respectively; Another method is solution imidization. This method generally completes the imination reaction at a lower temperature of 150 l 70 ° C. Both of these imination methods can obtain tough, transparent, soft, and soluble films. The performance of products obtained by different imidization methods varies.

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