Quaternary ammonium salt organic silicon gemini surfactant and preparation method thereof
A gemini surface and quaternary ammonium salt technology, which is applied in organic chemistry, chemical instruments and methods, compounds of group 4/14 elements of the periodic table, etc., can solve the problems of less reports on organosilicon gemini surfactants, and achieve excellent results Surface activity, easy control, effect of improving hydrolysis resistance
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Embodiment 1
[0032] Step 1. Mix 85g of polyethylene glycol glycidyl ether and 81g of α-hydrogen-ω-hydroxyl-polydimethylsiloxane with 100mL of acetone, then add 0.5g of tetrabutylammonium bromide and 0.5g of mass Fraction 30% sodium hydroxide solution, tetrabutylammonium bromide and sodium hydroxide solution play a catalytic role, then stir and reflux at 70°C for 5h, then wash with a mixed solvent of 30mL acetone and 30mL n-hexane for several times, rotate The solvent was removed by evaporation, and vacuum-dried to obtain a light yellow viscous liquid, which was epoxy-based polyether-modified siloxane.
[0033] Step 2, at 45°C, add 50mL of hydrochloric acid solution (0.202mol / L), 10g of C 12 h 25 NH(CH 3 ) 2 After reacting with 20mL of absolute ethanol for 1h, 21.67g of epoxy polyether modified siloxane prepared in step 1 was added dropwise, and reacted for 10h until the amine value (determined by hydrochloric acid-isopropanol titration) no longer changed. After the reaction, wash with ...
Embodiment 2
[0035] Step 1. Mix 90g of polyethylene glycol glycidyl ether and 83g of α-hydrogen-ω-hydroxyl-polydimethylsiloxane with 100mL of acetone, then add 0.5g of tetrabutylammonium bromide and 0.5g of mass A 30% fraction of sodium hydroxide, tetrabutylammonium bromide and sodium hydroxide solution acted as a catalyst, then stirred and refluxed at 60°C for 8 hours, then washed with a mixed solvent of 40mL acetone and 40mL n-hexane for several times, and evaporated by rotary evaporation Remove the solvent and dry in vacuum to obtain a light yellow viscous liquid, which is epoxy-based polyether-modified siloxane.
[0036] Step 2, at 40°C, add 55mL of hydrochloric acid solution (0.202mol / L), 7.0g of C 12 h 25 NH(CH 3 ) 2 After reacting with 20mL isopropanol for 1h, add 25g of the epoxy polyether modified siloxane prepared in step 1 dropwise, and react for 12h until the amine value (determined by hydrochloric acid-isopropanol titration) no longer changes. After the reaction, wash with...
Embodiment 3
[0038]Step 1. Mix 95g of polyethylene glycol glycidyl ether and 85g of α-hydrogen-ω-hydroxyl-polydimethylsiloxane with 100mL of acetone, then add 0.5g of tetrabutylammonium bromide and 0.5g of mass 30% fraction of sodium hydroxide, tetrabutylammonium bromide and sodium hydroxide solution play a catalytic role, then stirred and refluxed at 55°C for 6h, then washed with a mixed solvent of 35mL acetone and 35mL n-hexane for several times, and rotary evaporated Remove the solvent and dry in vacuum to obtain a light yellow viscous liquid, which is epoxy-based polyether-modified siloxane.
[0039] Step 2, at 50°C, add 60mL of hydrochloric acid solution (0.202mol / L), 8.4g of C 12 h 25 NH(CH 3 ) 2 After reacting with 20mL of distilled water for 1h, 23g of epoxy polyether modified siloxane prepared in step 1 was added dropwise, and reacted for 11h until the amine value (determined by hydrochloric acid-isopropanol titration) no longer changed. After the reaction, wash with cyclohexa...
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