Preparation method of sacrificial bond enhanced organic silicon rubber
A technology of silicone rubber and sacrificial bonds, which is applied in the field of preparation of sacrificial bonds to reinforce silicone rubber, and can solve problems such as no reinforcement method
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Embodiment 1
[0027] The synthesis of embodiment 1 methylnitrophenyl cyclosiloxane (D n Ph-nitro )
[0028] 7g of methylphenylcyclosiloxane was dissolved in 50ml of acetic anhydride and placed in a 250ml round-bottomed three-neck flask. And install a thermometer and a constant pressure dropping funnel. Slowly drop 10ml of concentrated nitric acid into the flask through a constant pressure dropping funnel. During this period, the whole device was placed in an ice bath, and the reaction temperature of the system was kept below 10°C by magnetic stirring and controlling the dropping rate. The reaction lasted 4h. Afterwards, the reactant was introduced into 400ml of distilled water for precipitation. And wash 3 times with 100ml distilled water to remove residual acid. Finally about 6 g of a yellow viscous liquid (64%) was obtained.
Embodiment 2
[0029] The synthesis of embodiment 2 methylaminophenyl cyclosiloxane (D n Ph-amino )
[0030] 9.3g of methylnitrophenyl cyclosiloxane was dissolved in 50ml of absolute ethanol and placed in a 250ml single-necked flask equipped with a constant pressure dropping funnel. 14g of zinc powder and 5ml of distilled water were added thereto. The zinc powder was pretreated with 10% HCl aqueous solution, and then the zinc powder was washed 3 times with distilled water and 1 time with absolute ethanol before use. 12.36 g of acetic acid was slowly dropped through the constant pressure dropping funnel. Under magnetic stirring, the reaction temperature was controlled at about 55° C., and the reaction was carried out for 5.5 hours. After the reaction, the solid and liquid phases were separated by suction filtration. The liquid phase was concentrated under reduced pressure distillation at 50°C. The product was precipitated with 200 ml of distilled water and washed with distilled water to a...
Embodiment 3
[0031] The synthesis (DnPh-amide) of embodiment 3 methyl acetanilino cyclosiloxanes
[0032] Add 7.7g of methylaminophenyl cyclosiloxane toluene solution and 6.12g of acetic anhydride into a round-bottomed flask, and react at 50°C for 2h under nitrogen protection and magnetic stirring. Then heat to 110°C for 2h. The product solution is distilled under reduced pressure Concentrate and remove residual toluene, acetic acid and acetic anhydride in a vacuum oven at 140°C. Finally, about 7.4 g of an orange-yellow transparent solid was obtained.
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