Methylsiloxane resin sealing material and preparation method thereof
The technology of methyl siloxane and dimethyl siloxane is applied in the field of methyl siloxane resin sealing material and its preparation, and can solve the problems of unsuitable sealing of ultraviolet light-emitting diodes, low transmittance and the like
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[0037] A preparation method of methylsiloxane resin sealant, which comprises the steps of:
[0038] S100 mixing corresponding mass parts of hydromethyl oligosiloxane and vinyl methyl siloxane-dimethyl siloxane copolymer; and
[0039] S200 Add platinum-1,3-divinyl-1,1,3,3-tetramethyldisiloxane, and keep stirring for 60-90 minutes at normal temperature to prepare methylsiloxane resin sealing compound.
[0040] Wherein, the preparation method of described hydromethyl oligosiloxane comprises steps:
[0041] S110 Add the corresponding mass parts of methyldiethoxysilane and dimethyldiethoxysilane into 0.1-0.2mol / L hydrochloric acid solution, and stir at 50°C-70°C for 20-24 hours;
[0042] After the S120 reaction is completed, feed nitrogen into the reaction system, raise the temperature to 90°C-110°C and stir for 12-16 hours to remove by-products, solvents and water; and
[0043] S130 Filter the crude product through a filter screen with a pore size of 0.45 μm, and dry it under a ...
Embodiment 1
[0050] Preparation of hydromethyl oligosiloxane
[0051] Add hydrochloric acid to deionized water to prepare a 0.1 mol / L hydrochloric acid solution. Then, methyldiethoxysilane and dimethyldiethoxysilane were added to the solution. The molar ratio of the reaction feed is methyldiethoxysilane: dimethyldiethoxysilane = 1: 1, solution: (methyldiethoxysilane + dimethyldiethoxysilane) = 2.5: 1. The reaction system was stirred at 60°C for 24 hours. After the reaction was completed, nitrogen gas was introduced into the reaction system, and the temperature was raised to 100° C. and stirred for 12 hours to remove by-products, solvents and water. The crude product was filtered through a filter with a pore size of 0.45 μm, and then dried under vacuum at 60° C. to obtain a dry and pure hydromethyl oligosiloxane product.
[0052] Preparation of Methylsiloxane Resin Sealing Material
[0053] Mix the hydromethyl oligosiloxane with the vinylmethylsiloxane-dimethylsiloxane copolymer. The mo...
Embodiment 2 to Embodiment 7
[0061] The specific method for preparing hydrogenated methyl oligosiloxane and methyl silicone resin sealant is shown in Example 1. The hydrogenated methyl oligosiloxane and vinyl methyl siloxane-dimethyl The different mass ratios of the siloxane copolymers are shown in Table 1, and the refractive index of the prepared sealant is shown in Table 1, wherein the refractive index is measured by an Abbe refractometer.
[0062] The composition ratio and test result of table 1 embodiment 1 to embodiment 7
[0063]
[0064]
[0065] It can be known from Table 1 that the molar ratio of hydromethyl oligosiloxane to vinyl methyl siloxane-dimethyl siloxane copolymer is 1:1.2.
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