Preparation method of octaphenol hydroxyl clathrate oligomeric silsesquioxane hybrid phenolic resin
A technology of polysilsesquioxane and octaphenol hydroxyl cage, which is applied in the field of ablation heat-resistant resin-based composite materials, can solve the problems of increasing resin thermal and mechanical properties, POSS agglomeration, affecting performance, etc., to increase thermal performance and tensile properties, improved oxidation resistance, and improved intrinsic properties
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[0043] The preparation method of octaphenol hydroxyl clathrate oligomeric silsesquioxane hybrid thermosetting phenolic resin of the present invention comprises the following steps:
[0044] (1) Dissolve 100-200 parts of phenol in 85-175 parts of formaldehyde solution according to the ratio of parts by mass, add 1-50 parts of octaphenolic hydroxyl clathrate oligomeric silsesquioxane as a reactant, and heat at 40-50°C Stir in a water bath for 10 to 30 minutes, then add 0.2 to 3 parts of barium hydroxide octahydrate to adjust the pH of the solution to 8 to 9, slowly raise the temperature to 60 to 70°C, and perform a constant temperature reaction for 1 to 3 hours; the heating rate is 0.16 to 0.33°C / min;
[0045] (2) Slowly raise the temperature of the solution obtained in step (1) from 60 to 70°C to 85 to 98°C, carry out a constant temperature reaction for 1 to 3 hours, and the heating rate is 0.16 to 0.33°C / min;
[0046] (3), add 0.3~3.5 parts of phosphoric acid solution, adjus...
Embodiment 1
[0068] According to parts by mass, dissolve 130 parts of phenol in 140 parts of formaldehyde solution, add 20 parts of octaphenolic hydroxyl clathrate oligomeric silsesquioxane, stir in a water bath at 40°C for 30 minutes, and then add 1.4 parts of barium hydroxide octahydrate to adjust the solution The pH value of the mixture is 8-9, and the temperature is slowly raised to 60° C., and the constant temperature reaction is carried out for 3 hours; the heating rate is 0.25° C. / min; the mass concentration of the formaldehyde solution is 37%.
[0069] Slowly raise the temperature of the above solution from 60°C to 95°C, carry out constant temperature reaction for 1 hour, and the heating rate is 0.25°C / min;
[0070] Add 1.6 parts of phosphoric acid solution, adjust the pH value of the above solution to 5-6, stir for 15 minutes, and dehydrate in a water bath at 95°C under vacuum for 1 hour, let stand, precipitate, filter, cool to room temperature, and take out the upper layer of pure...
Embodiment 2
[0080] According to parts by mass, dissolve 100 parts of phenol in 85 parts of formaldehyde solution, add 1 part of octaphenolic hydroxyl clathrate oligomeric silsesquioxane, stir in a water bath at 40°C for 30 minutes, and then add 0.2 parts of barium hydroxide octahydrate to adjust the solution The pH value of the mixture is 8-9, and the temperature is slowly raised to 60° C., and the constant temperature reaction is carried out for 1-3 hours; the heating rate is 0.16° C. / min; the mass concentration of the formaldehyde solution is 35%.
[0081] Slowly raise the temperature of the above solution from 60°C to 95°C, carry out constant temperature reaction for 1 hour, and the heating rate is 0.16°C / min;
[0082] Add 0.3 parts of phosphoric acid solution, adjust the pH value of the above solution to 5-6, stir for 15 minutes, and dehydrate in a water bath at 95°C under vacuum for 3 hours, let stand, precipitate, filter, cool to room temperature, and take out the upper layer of pure...
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