Method for producing (meth)acryloyl-terminated polyisobutylene-based polymer
A technology of acryloyl-terminated polyisobutylene, which is applied in the field of manufacturing acryloyl-terminated polyisobutylene polymers, can solve the problems of undisclosed production examples of isobutylene-based polymers, and no special elaboration on the manufacturing method, and achieve excellent transparency and removal Easy, load and waste reduction effect
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Embodiment 1
[0159] Production of acryloyl-terminated polyisobutylene polymer (component P-1)
[0160] After substituting nitrogen in the container of a 500 mL separable flask, 17 g of n-hexane (dried over molecular sieves) and 209 g of butyl chloride (dried over molecular sieves) were added, and cooled to -70°C while stirring under a nitrogen atmosphere. Next, 140 mL (1.48 mol) of isobutylene, 2.00 g (8.65 mmol) of p-dicumyl chloride, and 0.201 g (1.99 mmol) of triethylamine were added. After the reaction mixture was cooled to -70°C, 0.66 mL (6.06 mmol) of titanium tetrachloride was added to start polymerization. After the polymerization starts, measure the residual isobutene concentration by gas chromatography, and add 3.65g (18.2mmol) of 2-phenoxyethyl bromide (β-bromophenetole) and titanium tetrachloride at the stage where the residual isobutene is lower than 0.5%. 3.79 mL (34.6 mmol). After stirring at -75°C for 3 hours, 265 g of a mixed solvent of 478 g of water, n-hexane and butyl...
Embodiment 2
[0164] Production of acryloyl-terminated polyisobutylene polymer (component P-2)
[0165] After replacing the container of a 500 mL separable flask with nitrogen, 17 g of n-hexane (dried over molecular sieves) and 209 g of butyl chloride (dried over molecular sieves) were added, and cooled to -70°C while stirring under a nitrogen atmosphere. Next, 140 mL (1.48 mol) of isobutylene, 2.00 g (8.65 mmol) of p-dicumyl chloride, and 0.201 g (1.99 mmol) of triethylamine were added. After the reaction mixture was cooled to -70°C, 0.76 mL (6.92 mmol) of titanium tetrachloride was added to start polymerization. After the polymerization started, the residual isobutene concentration was measured by gas chromatography, and when the residual isobutene was less than 0.5%, 3.15 ml (19.9 mmol) of 3-phenoxypropyl bromide and 2.85 ml (26.0 mmol) of titanium tetrachloride were added. After stirring at -75°C for 3 hours, 265g of a mixed solvent of 478g of water, n-hexane and butyl chloride (mixing...
Embodiment 3
[0169] Production of acryloyl-terminated polyisobutylene polymer (component P-3)
[0170] After replacing the container of a 500 mL separable flask with nitrogen, 17 g of n-hexane (dried over molecular sieves) and 209 g of butyl chloride (dried over molecular sieves) were added, and cooled to -70°C while stirring under a nitrogen atmosphere. Next, 140 mL (1.48 mol) of isobutylene, 2.00 g (8.65 mmol) of p-dicumyl chloride, and 0.201 g (1.99 mmol) of triethylamine were added. After the reaction mixture was cooled to -70°C, 0.76 mL (6.92 mmol) of titanium tetrachloride was added to start polymerization. After the polymerization started, the residual isobutene concentration was measured by gas chromatography, and when the residual isobutene was less than 0.5%, 4.56 g (19.9 mmol) of 4-phenoxybutyl bromide and 2.85 mL (26.0 mmol) of titanium tetrachloride were added. After stirring at -75°C for 3 hours, 265g of a mixed solvent of 478g of water, n-hexane and butyl chloride (mixing r...
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