Surface-modified composite silica particles and polyimide film comprising same
A composite silicon dioxide and polyimide film technology, which is applied in the field of polyimide film, can solve problems such as increased haze, and achieve the goal of improving dispersibility, improving physical properties, compatibility and dispersibility Effect
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preparation example 1
[0068] Preparation Example 1: Preparation of Silica Particles
[0069] Add 300g of ethanol in a 500ml beaker, and add 7g of tetraethoxysilane (tetraethoxysilane, TEOS, Si(OC 2 h 5 ) 4 , Sigma-Aldrich), stirred at room temperature for 30 minutes. Next, slowly add 25 g of NH 4 After OH, it was stirred at the same temperature for 6 hours. After the reaction product obtained after the completion of the reaction was filtered, washed three times with ethanol (50 ml), and then dried in an oven at 40° C. under reduced pressure for 5 hours, 5 g of silica particles with an average particle diameter of 0.2 μm were prepared. (SiO 2 ).
[0070] Here, the shape and size of silica particles were observed by TEM (Transmission Electron Microscopy: transmission electron microscope, 200kV, JEM-2000EX, JEOL, Japan), and the Zeta sizer (ELS- 8000, Otsukaelectronics, Japan) measured the average particle size of the particles.
preparation example 2
[0071] Preparation Example 2: Preparation of Polysiloxane
[0072] In a three-necked flask, mix 40g of diphenylsilanediol (Diphenylsilandiol, DPSD, (C 6 h 5 ) 2 Si(OH) 2 , Sigma-Aldrich) and 40g of phenyltrimethoxysilane (PTMS, C 6 h 5 Si(OCH) 3 , Sigma-Aldrich), reacted at 80° C. for 10 hours to obtain 60 g of polysiloxane with a weight average molecular weight of 5000.
[0073] Here, the weight-average molecular weight (unit: g / mol) of polysiloxane is measured by GPC (Gel Permeation Chromatography: Gel Permeation Chromatography, ViscoTek Company) using polysiloxane standard (PS standard) as a standard. Measured.
preparation example 3
[0074] Preparation Example 3: Preparation of Surface Modified Composite Silica
[0075] After 5 g of the silica particles obtained in Preparation Example 1 were dispersed in 300 ml of ethanol, 0.5 g of the polysiloxane obtained in Preparation Example 2 and 1 ml of NH 4OH, reacted at room temperature for 12 hours, and prepared surface-modified composite silica particles with an average particle size of 0.2 μm. After the reaction, the obtained reaction product was filtered and washed three times with ethanol (50 ml).
[0076] At this time, the particle diameter of the surface-modified composite silica was measured by the same method as the method for measuring the average particle diameter of the above-mentioned silica particles.
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