A kind of method for synthesizing epoxy cage type silsesquioxane
A technology of silsesquioxane and epoxy group, which is applied in the field of cage-type silsesquioxane preparation, can solve the problems of difficult control of process control points, cumbersome steps in the synthesis process, and difficulty in industrialization, and achieve short reaction time, Avoid cumbersome control and the effect that the process is easy to control
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[0018] The specific steps of the preparation method of the above-mentioned epoxy cage type silsesquioxane are as follows:
[0019] Add glacial acetic acid and conc The volume ratio of acetic acid is (1.5~3):1, stir and heat up to 50~75°C, add chloroform dissolved in octavinyl cage silsesquioxane, wherein octavinyl cage silsesquioxane The concentration of oxane in chloroform is 75~109g / L, the volume ratio of chloroform to hydrogen peroxide is (1~2):1, condensed and refluxed for 2~5h, the lower layer of reaction solution is taken, passed through deionized water After washing and drying, a white powder is obtained, which is epoxy cage silsesquioxane, and the yield is 70%-95%.
[0020] The synthetic route of the present invention is as follows:
[0021]
Embodiment 1
[0023] Pour 1.8L glacial acetic acid and 0.09L concentrated sulfuric acid into the 20L reactor in turn, start stirring for 30min, make it completely mixed, pour 3.6L hydrogen peroxide, heat up to 68°C, add 6L dissolved in 450g octavinyl cage Chloroform of silsesquioxane, after refluxing for 3 hours, remove the lower layer of the reaction solution and wash it with water until it becomes neutral, then spin-evaporate the chloroform solution at 55°C to obtain a white solid, dry it in vacuum at 55°C for 1 hour, and then grind it into powder 429.59 g of epoxy cage silsesquioxane was obtained with a yield of 86.61%. Its nuclear magnetic resonance H spectrum and infrared absorption analysis characterization data are: 29Si NMR (119MHz, CDCL 3 , 300K, ppm): 2.245 ~ 2.259, 2.770 ~ 2.925, 5.897 ~ 6.151, the peak areas are 1.04, 2.21, 2.18, respectively, calculated by proportion, the number of epoxy groups is 4.79; FTIR (cm -1 , KBr): 1332.23 (vsC-O-C), 876.89 (vasC-O-C), 1235.94 (α-CH), ...
Embodiment 2
[0025] Pour 1.5L glacial acetic acid and 0.05L concentrated sulfuric acid into the 20L reactor in turn, start stirring for 40min, make it completely mixed, pour 3.4L hydrogen peroxide, raise the temperature to 62°C, add 5L chloroform and 450g octaethylene respectively Cage-type silsesquioxane, after reflux for 4 hours, remove the reaction solution from the lower layer and wash it with water to neutrality, spin-evaporate the chloroform solution at 55°C to obtain a white solid, vacuum-dry it at 55°C for 1 hour, and then grind it into powder to obtain Epoxy cage silsesquioxane 389.86g, yield 78.60%. Its nuclear magnetic resonance H spectrum and infrared absorption analysis characterization data are: 29Si NMR (119MHz, CDCL 3 , 300K, ppm): 2.248 ~ 2.267, 2.779 ~ 2.802, 5.889 ~ 6.172, the peak areas are 1.00, 1.89, 1.81, respectively, calculated by proportion, the number of epoxy groups is 4.92; FTIR (cm -1 , KBr): 1331.23 (vsC-O-C), 876.45 (vasC-O-C), 1235.91 (α-CH), 1604.08 (vC=C...
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