A kind of preparation method of plant bisphenol glycidyl ether
A glycidyl ether and plant technology, which is applied in the field of plant bisphenol to prepare epoxy resin, can solve the problems of brittle performance and poor toughness of the cured product
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Embodiment 1
[0034] Pass nitrogen into a 1L four-neck flask equipped with a stirring, thermometer and condensing reflux device to replace the air, add 100g of plant bisphenol, 250g of epichlorohydrin, and 0.5g of tetraethylammonium bromide, stir and heat up to 50°C, and open Cycloaddition etherification reaction 2h. Keeping the temperature constant, 170 g of sodium hydroxide solution with a mass concentration of 30% was added dropwise with a constant pressure funnel for 4 hours, and kept for 2 hours after the dropwise addition to complete the initial ring-closing epoxidative dechlorination reaction. Distill under reduced pressure to recover water and excess epichlorohydrin. The temperature was raised to 60° C., and 20 g of sodium hydroxide solution with a mass concentration of 30% was added at one time to carry out a second ring-closing epoxidative dechlorination reaction for 1 hour. Centrifugal filtration to obtain crude plant bisphenol glycidyl ether; washing, liquid separation, distill...
Embodiment 2
[0036] Pass nitrogen into a 1L four-neck flask equipped with a stirring, thermometer and condensing reflux device to replace the air, add 80g of plant bisphenol, 240g of epichlorohydrin, 0.3g of tetramethylammonium bromide, and 0.3g of tetraethylammonium bromide g, stirring and raising the temperature to 75°C, the ring-opening addition etherification reaction was carried out for 1 h. Keeping the temperature constant, 100 g of sodium hydroxide solution with a mass concentration of 50% was added dropwise with a constant pressure funnel for 3 hours, and kept for 1.5 hours after the dropwise addition to complete the initial ring-closing epoxidative dechlorination reaction. Distill under reduced pressure to recover water and excess epichlorohydrin. The temperature was raised to 70° C., and 25 g of sodium hydroxide solution with a mass concentration of 20% was added at one time to carry out a second ring-closing epoxidative dechlorination reaction for 2 hours. Centrifugal filtratio...
Embodiment 3
[0038] Pass nitrogen into a 1L four-neck flask equipped with a stirring, thermometer and condensing reflux device to replace the air, add 60g of plant bisphenol, 210g of epichlorohydrin, and 0.6g of benzyltriethylammonium bromide and stir to raise the temperature to 80°C. Ring-opening addition etherification reaction 0.5h. Keeping the temperature constant, 50 g of sodium hydroxide solution with a mass concentration of 60% was added dropwise with a constant pressure funnel for 2.5 hours, and kept for 3 hours after the dropwise addition to complete the initial ring-closing epoxidation dechlorination reaction. Distill under reduced pressure to recover water and excess epichlorohydrin. The temperature was raised to 90° C., and 10 g of sodium hydroxide solution with a mass concentration of 30% was added at one time to carry out a second ring-closing epoxidative dechlorination reaction for 1 hour. Centrifugal filtration to obtain crude plant bisphenol glycidyl ether; washing, liqui...
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Abstract
Description
Claims
Application Information
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