Method for preparing fluorine-silicon triblock copolymer by employing one-kettle process
A tri-block, polymer technology, applied in biocide-containing paints, coatings, antifouling/underwater coatings, etc., to achieve the effect of less reaction steps, high conversion rate, and avoiding the steps of catalyst removal
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Embodiment 1
[0028] Add 1 mol of macroinitiator PDMS-Br, 100 mol of toluene, 100 mol of methyl methacrylate (MMA), 0.005 mol of copper bromide, 0.02 mol of ligand PMDETA and 0.05 mol of stannous octoate into the reaction flask, and feed nitrogen For 10 minutes, heat to 60°C. Stir under the closed system, when the monomer conversion rate reaches 85%, slowly add the mixture of 100mol heptafluorobutyl methacrylate (HFBMA) and 0.05mol stannous octoate diluted with 100mol toluene to the reaction flask, feed nitrogen gas for 10 Minutes, heated to 60°C, reacted in a closed system, and when the monomer conversion rate reached 85%, stirred in the open, and the main component of the obtained product was the triblock polymer PDMS-b-PMMA-b-PHFBMA-Br.
Embodiment 2
[0030]Add 1mol of macromolecular initiator PDMS-Br, 250mol of xylene, 250mol of methyl methacrylate (MMA), 0.05mol of nickel bromide, 0.4mol of ligand TPMA and 0.5mol of glucose into the reaction flask, and feed nitrogen gas for 30 Minutes, heated to 80°C. Stir in a closed system, and when the monomer conversion rate reaches 90%, slowly add a mixture of 250 mol of heptafluorobutyl methacrylate (HFBMA) diluted with 250 mol of xylene and 0.5 mol of glucose into the reaction flask, and feed nitrogen for 30 minutes , heated to 80°C, and reacted in a closed system. When the monomer conversion rate reached 90%, it was stirred openly, and the main component of the obtained product was the triblock polymer PDMS-b-PMMA-b-PHFBMA-Br.
Embodiment 3
[0032] 1mol macroinitiator PDMS-Br, 500mol anisole, 500mol methyl methacrylate (MMA), 0.1mol iron bromide, 0.8mol ligand Me 6 Add TREN and 1mol ascorbic acid together into the reaction flask, pass through nitrogen for 60 minutes, and heat to 95°C. Stir in a closed system, and when the monomer conversion rate reaches 95%, slowly add a mixture of 500 mol of heptafluorobutyl methacrylate (HFBMA) and 1 mol of ascorbic acid diluted with 500 mol of anisole into the reaction flask, and feed nitrogen for 60 minutes , heated to 95°C, and reacted in a closed system when the monomer conversion rate reaches 95%, and stirred with the open door, the main component of the obtained product is the triblock polymer PDMS-b-PMMA-b-PHFBMA-Br.
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