Polyglycol modified trisilicate containing glucose amide group and preparation method
A technology containing glucosamide group and modified with polyethylene glycol, applied in the directions of sugar derivatives, organic chemistry, etc., can solve problems such as unreported preparation methods, and achieve the effects of cheap catalyst, promotion of spreading, and reduction of reaction flow.
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Embodiment 1
[0019] Add 1.62kg of hexamethyldisiloxane, 2.06kg of aminoethylaminopropyldimethoxymethylsilane, and 1.82g of tetramethylammonium hydroxide into the reaction kettle, heat to dissolve, and control the temperature at 100°C. After 4 hours, the temperature was raised to 130° C. to deactivate the catalyst. Evaporate aminoethylaminopropyl trisiloxane under reduced pressure, add equimolar gluconolactone, use methanol as solvent, heat to reflux, and react for 8 hours. Then add glycidyl ether of ethylene glycol methyl ether in equimolar number, and continue to react for 12 hours. The solvent methanol is evaporated to obtain the product. The minimum surface tension of its aqueous solution measured by K12 surface tension meter is 20.2mN / m, and the critical micelle concentration is 2.5×10 -4 mol / L, the minimum contact angle on the quartz surface is 5°.
Embodiment 2
[0021] Add 8.10kg of hexamethyldisiloxane, 2.34kg of aminoethylaminopropyldiethoxymethylsilane, and 168g of potassium hydroxide into the reaction kettle, heat to dissolve, and control the temperature at 120°C. After 5 hours of reaction, Add acetic acid to neutralize the catalyst to deactivate it, and then evaporate unreacted hexamethyldisiloxane. Evaporate aminoethylaminopropyl trisiloxane under reduced pressure, add equimolar gluconolactone, use methanol as solvent, heat to reflux, and react for 10 hours. Then add diethylene glycol methyl ether glycidyl ether in an equimolar amount, and continue the reaction for 12 hours. The solvent methanol is evaporated to obtain the product. The minimum surface tension of its aqueous solution measured by K12 surface tensiometer is 20.6mN / m, and the critical micelle concentration is 1.4×10 -4 mol / L, the minimum contact angle on the quartz surface is 18°.
Embodiment 3
[0023] Add 16.20kg of hexamethyldisiloxane, 2.06kg of aminoethylaminopropyldimethoxymethylsilane, and 151.8g of tetrabutylphosphonium hydroxide into the reaction kettle, heat to dissolve, control the temperature at 80°C, and react for 4 hours Afterwards, the temperature was raised to 110° C. to deactivate the catalyst, and at the same time, unreacted hexamethyldisiloxane was distilled off. Evaporate aminoethylaminopropyl trisiloxane under reduced pressure, add equimolar gluconolactone, use methanol as solvent, heat to reflux, and react for 8 hours. Then add triethylene glycol methyl ether glycidyl ether in an equimolar amount, and continue the reaction for 12 hours. The solvent methanol is evaporated to obtain the product. The minimum surface tension of its aqueous solution measured by K12 surface tension meter is 20.7mN / m, and the critical micelle concentration is 6×10 -5 mol / L, the minimum contact angle on the quartz surface is 15°.
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