Preparation method of quaternary ammonium salt type trisiloxane gemini surfactant
A technology of trisiloxane and gemini surface, which is applied in the preparation of quaternary ammonium salt type trisiloxane gemini surfactant and the field of quaternary ammonium salt type trisiloxane gemini surfactant, which can solve the limitation of research and industrial production , harsh experimental conditions, long reaction time and other problems, to achieve the effect of easy control, simple steps and simple reaction conditions
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[0042] Example 1: Quaternary ammonium salt type trisiloxane gemini surfactant MR 6 Preparation of M
[0043] (1) Synthesis of silyl group-containing tertiary amine (hydrosilylation reaction)
[0044] Add N,N-dimethylallylamine (20.6mmol) and heptamethyltrisiloxane (20.6mmol) into a 100mL three-necked flask with a magnetic stirrer, and stir and heat to 75°C under nitrogen protection. Stir for 30 min, add chloroplatinic acid in isopropanol solution (amount is 75ppm of heptamethyltrisiloxane) catalyst, heat to 100°C, and reflux for 3h. The resulting product was rotated under reduced pressure at 40°C to remove isopropanol to obtain a colorless transparent liquid.
[0045] (2)MR 6 Synthesis of M (quaternization reaction)
[0046] Take 20 mL of ethanol and place it in a 100 mL three-necked flask, add the tertiary amine containing silyl group (12 mmol) and 1,6-dibromohexane (5 mmol) obtained in step 1 above, heat up to 80° C., and react under reflux for 48 h. After the reaction is complete...
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[0049] Example 2: Quaternary ammonium salt type trisiloxane gemini surfactant MR 8 Preparation of M
[0050] (1) Synthesis of silyl group-containing tertiary amine (hydrosilylation reaction)
[0051] Add N,N-dimethylallylamine (20.8mmol) and heptamethyltrisiloxane (20mmol) into a 100mL three-necked flask with a magnetic stirrer, and stir under nitrogen protection. The temperature is raised to 60°C and stirred for 30min. , Add chloroplatinic acid in isopropanol solution (amount is 30ppm of heptamethyltrisiloxane) catalyst, heat up to 120°C, reflux for 3h. The resulting product was rotated under reduced pressure at 60°C to remove isopropanol to obtain a colorless transparent liquid.
[0052] (2)MR 8 Synthesis of M (quaternization reaction)
[0053] Put 20mL n-propanol into a 100mL three-necked flask, add the tertiary amine containing silyl group (10.5mmol) and 1,8-dibromooctane (5mmol) obtained in step 1 above, heat up to 80℃, reflux for 72h . After the reaction is completed, cool to...
Example Embodiment
[0056] Example 3: Preparation of quaternary ammonium salt type trisiloxane gemini surfactant MDM
[0057] (1) Synthesis of silyl group-containing tertiary amine (hydrosilylation reaction)
[0058] Add N,N-dimethylallylamine (26mmol) and heptamethyltrisiloxane (20mmol) into a 100mL three-necked flask with a magnetic stirrer. Under nitrogen protection, stir and heat up to 80°C and stir for 30min. Add chloroplatinic acid in isopropanol solution (the amount is 50ppm of heptamethyltrisiloxane) catalyst, heat up to 90°C, and reflux for 5h. The resulting product was rotated under reduced pressure at 70°C to remove isopropanol to obtain a colorless and transparent liquid.
[0059] (2) Synthesis of MDM (quaternization reaction)
[0060] Put 20 mL of ethyl acetate in a 100 mL three-necked flask, add the above-mentioned intermediate (14 mmol) and 1,4-bis(bromomethyl)benzene (5 mmol), raise the temperature to 100° C., and reflux for 96 h. After the reaction is completed, cool to room temperatur...
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