High-refractive-index heat-resistant bisphenol S epoxy (methyl) acrylic ester and synthetic method for same
A technology of acrylates and synthetic methods, applied in chemical instruments and methods, non-polymer organic compound adhesives, preparation of organic compounds, etc.
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Embodiment 1
[0023] In the reaction of 25g bisphenol S and 150g epichlorohydrin in the four-necked flask that mechanical stirring paddle, thermometer, condenser tube and constant pressure funnel are housed, stir under nitrogen protection to make bisphenol S dissolve completely in epichlorohydrin, After heating up to 80°C, 1.75g of tetramethylammonium bromide was added, and etherification reaction was carried out at 80°C for 200min under the protection of nitrogen. Then 8 g of 50% NaOH aqueous solution was added dropwise, and the alkali addition time was 200 min to obtain the product 2. The second step reaction is the reaction of intermediate product 2 dissolved in 100ml of 1,4-dioxane and 7g of methacrylic acid; the temperature is raised to 60°C, and 0.357g of benzyltrimethylammonium chloride is added to inhibit the polymerization. The agent is that the addition of p-hydroxyanisole is 0.0331g, and the reaction terminal situation is monitored by infrared. When the epoxy group is 915cm -1...
Embodiment 2
[0027] In the reaction of 25g bisphenol S and 75g epichlorohydrin in the four-necked flask that mechanical stirring paddle, thermometer, condenser and constant pressure funnel are housed, stir under nitrogen protection and bisphenol S is dissolved in epichlorohydrin completely, After heating up to 100°C, 1.65g of tetraethylammonium bromide was added, and etherification reaction was carried out at 100°C for 70min under the protection of nitrogen. Then 8 g of 50% NaOH aqueous solution was added dropwise, and the alkali addition time was 200 min to obtain the product 2. The second step reaction is the reaction of intermediate product 2 dissolved in 100mL of N,N dimethylformamide and 6.1g of methacrylic acid; The polymerizing agent is hydroquinone in an amount of 0.0331 g, and the reaction end point is monitored by infrared. When the infrared characteristic peak of the epoxy group disappears, the product 3 is obtained by rotary evaporation.
[0028] The cured film was tested and ...
Embodiment 3
[0030] In the reaction of 25g bisphenol S and 150g epichlorohydrin in the four-necked flask that mechanical stirring paddle, thermometer, condenser tube and constant pressure funnel are housed, stir under nitrogen protection to make bisphenol S dissolve completely in epichlorohydrin, After heating up to 80°C, 1.75g of tetramethylammonium bromide was added, and etherification reaction was carried out at 80°C for 60min under the protection of nitrogen. Then 8 g of 50% NaOH aqueous solution was added dropwise, and the alkali addition time was 200 min to obtain the product 2. The second step reaction is the reaction of the intermediate product 2 dissolved in 100mL of 1,4-dioxane and 6.7g of acrylic acid; the temperature is raised to 60°C, and the catalyst 0.327g of benzyltrimethylammonium chloride, polymerization inhibitor The amount of p-hydroxyanisole added is 0.0301g, and the reaction end point is monitored by infrared. When the infrared characteristic peak of the epoxy group...
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