Preparation method for medicinal ethanol
A technology of ethanol and MCM-41, applied in the field of medicine and chemical industry
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Embodiment 1
[0018] Add 3 g of diethyl acetonyl phosphonate to 50 ml of dry dichloromethane, then add 15 g of Me 3 SiBr, after reacting for 24 h at room temperature, the excess Me was removed by rotary evaporation 3 SiBr and dichloromethane, the solid was dissolved in MeOH and stirred at room temperature for 3 h, then the MeOH was removed by rotary evaporation, and the residue was washed with a small amount of CH 2 Cl 2 After washing, weigh 1.0 g of the obtained product and add it into the prepared 3.0 g aqueous solution of MCM-41 molecular sieve, stir at room temperature for 20 h, and filter. The filter cake was washed with distilled water several times until the pH of the filtrate was about 7, and the organic-modified molecular sieve was obtained. The product was dried under vacuum at 50 °C for 10 h.
[0019] The PDMS of 20g is joined in the 25ml n-heptane, and the catalyst dibutyltin dilaurate of 0.5g cross-linking agent ethyl orthosilicate and 0.2g are added successively therein...
Embodiment 2
[0021] Dissolve 3 g of diethyl acetonyl phosphonate in 50 ml of dry dichloromethane, then add 15 g of Me 3 SiBr, after reacting for 24 h at room temperature, the excess Me was removed by rotary evaporation 3 SiBr and dichloromethane, the solid was dissolved in MeOH and stirred at room temperature for 3 h, then the MeOH was removed by rotary evaporation, and the residue was washed with a small amount of CH 2 Cl 2 After washing, weigh 1.0 g of the obtained product and add it into the prepared 3.0 g aqueous solution of MCM-41 molecular sieve, stir at room temperature for 20 h, and filter. The filter cake was washed with distilled water several times until the filtrate did not emit light under the ultraviolet lamp, and the organic-modified molecular sieve was obtained. The product was dried under vacuum at 50 °C for 10 h.
[0022] The PDMS of 20g is joined in the 25ml n-heptane, and the catalyst dibutyltin dilaurate of 0.5g cross-linking agent ethyl orthosilicate and 0.2g a...
Embodiment 3
[0024] Dissolve 3 g of diethyl acetonyl phosphonate in 50 ml of dry dichloromethane, then add 15 g of Me 3 SiBr, after reacting for 24 h at room temperature, the excess Me was removed by rotary evaporation 3 SiBr and dichloromethane, the solid was dissolved in MeOH and stirred at room temperature for 3 h, then the MeOH was removed by rotary evaporation, and the residue was washed with a small amount of CH 2 Cl 2 After washing, weigh 2.0 g of the obtained product and add it into the prepared 6.0 g aqueous solution of MCM-41 molecular sieve, stir at room temperature for 20 h, and filter. The filter cake was washed with distilled water several times until the filtrate did not emit light under the ultraviolet lamp, and the organic-modified molecular sieve was obtained. The product was dried under vacuum at 50 °C for 10 h.
[0025] The PDMS of 20g is joined in the 25ml n-heptane, and the catalyst dibutyltin dilaurate of 0.5g cross-linking agent ethyl orthosilicate and 0.2g ar...
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