A kind of preparation method of fluorine-containing cyanate ester resin
A technology of fluorine-containing cyanate and resin, which is applied in the field of preparation of fluorine-containing cyanate resin, can solve the problems of reducing polymer rigidity, reducing rigidity, and large steric hindrance, so as to improve high temperature resistance and flame retardancy, improve Flexibility, the effect of improving toughness
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Embodiment 1
[0028] Add 350g of methyl acrylate to 1L of 50% hydrochloric acid solution, stir and react for 5-6h, add the resulting product to chloroform for extraction, and then perform vacuum distillation to obtain methyl chloroacrylate with a yield of 91.3% .
[0029] Add 143g of 4-chloroanisole and ether solution into the reflux reaction vessel, then slowly add magnesium chips immersed in ether to it, and add 25g of magnesium chips based on the mass of the magnesium chips. During the addition, the solution boils slightly. After the addition is complete, the reaction is maintained until the solution does not boil and the reaction is kept stirring for 20-30 minutes, and then the unreacted magnesium powder is removed after filtration, and the filtrate is distilled under reduced pressure to obtain Grignard reagent with a yield of 87.6%.
Embodiment 2
[0031] A preparation method of fluorocyanate ester resin, the specific preparation process is as follows:
[0032] The first step: Weigh a certain amount of p-methoxyacetophenone and dissolve it in ethanol to obtain a 65% p-methoxyacetophenone solution, and add 1L of p-methoxyacetophenone solution to the reactor After stirring and mixing uniformly, the temperature is raised to 60-70°C, and then 100g sodium ethoxide and 510g methyl chloroacrylate prepared in Example 1 are added to the reaction vessel, reacted at a constant temperature for 15-18h, and then subjected to vacuum distillation to obtain biscarbonyl Unsaturated monomer
[0033] In the second step, add 1 kg of the dicarbonyl unsaturated monomer prepared in the first step to the dimethyl sulfoxide solution, stir to dissolve and add 0.705 kg of the Grignard reagent prepared in Example 1 to it, and stir to react at room temperature. 5- 6h, then carry out vacuum distillation to obtain unsaturated alkenyl trimethoxyphenyl ether...
Embodiment 3
[0039] A preparation method of fluorocyanate ester resin, the specific preparation process is as follows:
[0040] The first step: Weigh a certain amount of p-methoxyacetophenone and dissolve it in ethanol to obtain a 65% p-methoxyacetophenone solution, and add 1L of p-methoxyacetophenone solution to the reactor After stirring and mixing uniformly, the temperature is raised to 60-70°C, and then 100g sodium ethoxide and 510g methyl chloroacrylate prepared in Example 1 are added to the reaction vessel, reacted at a constant temperature for 15-18h, and then subjected to vacuum distillation to obtain biscarbonyl Unsaturated monomer
[0041] In the second step, add 1 kg of the dicarbonyl unsaturated monomer prepared in the first step to the dimethyl sulfoxide solution, stir to dissolve and add 0.705 kg of the Grignard reagent prepared in Example 1 to it, and stir to react at room temperature. 5- 6h, then carry out vacuum distillation to obtain unsaturated alkenyl trimethoxyphenyl ether...
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