Siloxane-acrylate copolymer/nano-silicon dioxide organic/inorganic hybrid nano-material and preparation method thereof
A nano-silica, nano-material technology, applied in the direction of dyeing low-molecular-weight organic compounds, fibrous fillers, etc., to achieve the effects of good hardness, mild reaction conditions and high product yield
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Embodiment 1
[0038] 1) Preparation of nano silica modified by silane coupling agent:
[0039] In a dry two-necked flask equipped with a reflux condenser, add 1 part of nano-silica, 200 parts of dry toluene and 1 part of 3-aminopropyltrimethoxysilane in molar ratio sequentially. Connect an argon bag to the other end of the condenser tube, vacuumize and fill with an inert gas to remove the air in the system, and react under reflux at 80°C in an oil bath for 12h. After cooling down, centrifuge, pour off the upper solvent, wash with toluene and acetone ultrasonically in order to remove the adsorbed silane coupling agent, and vacuum-dry at 45°C for 24 hours to obtain nano-silica modified by silane coupling agent.
[0040] 2) Preparation of nano silicon dioxide atom transfer radical surface initiator:
[0041] Add 1 part of nano-silica modified by silane coupling agent and 200 parts of toluene in molar ratio to the two-necked bottle treated with baking bottle, seal the vacuum and repeat the ope...
Embodiment 2
[0047] 1) Preparation of nano silica modified by silane coupling agent:
[0048] In a dry two-necked flask equipped with a reflux condenser, 1 part of nano-silica, 250 parts of dry toluene and 1.5 parts of 3-aminopropyltrimethoxysilane were sequentially added in molar ratio. A nitrogen bag was connected to the upper end of the condenser tube, vacuum-filled with an inert gas to remove the air in the system, and reflux reaction at 110° C. in an oil bath for 18 hours. Centrifuge after cooling down, pour off the upper solvent, wash with a large amount of toluene and acetone in order to remove the adsorbed silane coupling agent, and vacuum dry at 45°C for 24 hours to obtain nano-silica modified by silane coupling agent.
[0049] 2) Preparation of nano silicon dioxide atom transfer radical surface initiator:
[0050] Add 1 part of nano-silica modified by silane coupling agent and 250 parts of toluene into the baked two-necked bottle according to the molar ratio, seal the vacuum-fil...
Embodiment 3
[0054] 1) Except that the reaction temperature is 120° C., the reflux time is 24 h, and the toluene is 300 parts, the others are the same as step 1) in Example 1.
[0055] 2) Except that toluene is 300 parts, triethylamine is 5 parts, 2-bromoisobutyryl bromide is 2.5 parts, reaction temperature is 30° C. and reaction time is 30 h, the others are the same as step 2) in Example 1.
[0056] 3) Except that the methyl methacrylate is 200 parts, the toluene is 300 parts, the reaction time is 10 h, and the drying temperature is 50° C., the others are the same as step 3) in Example 1.
[0057] 4) Except that the monomer is 50 parts, the toluene is 300 parts, and the reaction time is 16 hours, the others are the same as step 4) in Example 1.
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