Polyvinyl alcohol-thymolphthalein acetal and preparation method and application thereof
A polyvinyl alcohol shrinkage and polyvinyl alcohol technology, which is applied in the field of polyvinyl thymol phthalein and its preparation, can solve problems such as uncontrollable color development, achieve reduced hydroxyl density, good water resistance, and reduce dissolution sexual effect
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Embodiment 1
[0032] Synthesis of Polyvinyl Thymol Phthalaldehyde
[0033] Weigh 2mmol thymolphthalein and 4mmol urotropine, and mix them into a 100mL round bottom flask. Under the condition of ice bath, 0.15 mol trifluoroacetic acid (TFA) was added, the solution was stirred for 30 min and then warmed up to room temperature. Continue heating to 72°C and reflux for 24h. After the reaction stops, excess TFA is removed by a rotary evaporator. Add 30mL H 2 O, the mixed solution was heated to 60°C, stirred for 30 min and then filtered to obtain a solid. The solid was further separated by column chromatography, using petroleum ether and dichloromethane at a ratio of 1:3 (v / v) as a developer, and finally dried by rotary evaporation to obtain a light yellow powder.
[0034] Add 1g of polyvinyl alcohol (PVA-1788) into 20mL of secondary water, soak for 12 hours, stir and dissolve at 95°C. After the polyvinyl alcohol is completely dissolved, cool down to 85°C, add 1mL of thymolphthalein aldehyde e...
Embodiment 2
[0038] Synthesis of Polyvinyl Thymol Phthalaldehyde
[0039] Weigh 2mmol thymolphthalein and 6mmol urotropine, and mix them into a 100mL round bottom flask. Under ice-bath conditions, 0.20 mol of trifluoroacetic acid (TFA) was added, the solution was stirred for 30 min and then warmed to room temperature. Continue heating to 72°C and reflux for 24h. After the reaction stops, excess TFA is removed by a rotary evaporator. Add 60mL H 2 O, the mixed solution was heated to 60°C, stirred for 30 min and then filtered to obtain a solid. The solid was further separated by column chromatography, using petroleum ether and dichloromethane at a ratio of 1:3 (v / v) as a developer, and finally dried by rotary evaporation to obtain a light yellow powder.
[0040] Add 1g of polyvinyl alcohol (PVA-1788) into 20mL of secondary water, soak for 12 hours, stir and dissolve at 95°C. After the polyvinyl alcohol is completely dissolved, cool down to 85°C, add 1mL of thymolphthalein aldehyde ethanol...
Embodiment 3
[0044] Synthesis of Polyvinyl Thymol Phthalaldehyde
[0045] Weigh 2mmol thymolphthalein and 5mmol urotropine, mix them into a 100mL round bottom flask. Under ice-bath conditions, 0.20 mol of trifluoroacetic acid (TFA) was added, the solution was stirred for 30 min and then warmed to room temperature. Continue heating to 72°C and reflux for 24h. After the reaction stops, excess TFA is removed by a rotary evaporator. Add 40mL H 2 O, the mixed solution was heated to 60°C, stirred for 30 min and then filtered to obtain a solid. The solid was further separated by column chromatography, using petroleum ether and dichloromethane at a ratio of 1:3 (v / v) as a developer, and finally dried by rotary evaporation to obtain a light yellow powder.
[0046] Add 1g of polyvinyl alcohol (PVA-1788) into 20mL of secondary water, soak for 12 hours, stir and dissolve at 95°C. After the polyvinyl alcohol is completely dissolved, cool down to 85°C, add 1mL of thymolphthalein aldehyde ethanol sol...
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