A kind of polysulfonic acid-based surfactant and its preparation method and application
A technology of surfactant and polysulfonic acid group, which can be used in the preparation of sulfonate, the preparation of carboxylic acid halide, chemical instruments and methods, etc., and can solve the problem of insufficient surface activity.
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[0028] Concrete, a kind of preparation method of polysulfonic acid-based surfactant, comprises the following steps:
[0029] (1) Dissolve dipentaerythritol in dimethylformamide to obtain a dipentaerythritol solution, add triethylamine, stir and heat to 50-60°C, and add perfluorovaleryl fluoride dropwise while stirring. Wherein the molar ratio of dipentaerythritol to perfluorovaleryl fluoride is 1:(3-3.2). After the dropwise addition, continue to heat up to 75-85°C, and stir for 4-6 hours. The resulting product was first washed twice with 5% HCl solution, and then washed with 5% NaHCO 3 The solution was washed once, washed with water, extracted with ether, separated by liquid separation to obtain the upper organic layer, and the solvent was distilled off under reduced pressure to obtain a light yellow solid.
[0030] (2) Dissolve the light yellow solid obtained in step 1 in dimethyl sulfoxide (DMSO) and add it to a four-necked flask. After it is completely dissolved, add abou...
Embodiment 1
[0036] Equipped with a stirrer, thermometer, dropping funnel and reflux condenser (anhydrous CaCl 2 Drying tube) In a dry 250mL four-neck flask, dissolve dipentaerythritol in dimethylformamide to obtain a dipentaerythritol solution, add triethylamine and stir to heat to 55°C, then add perfluorovaleryl fluoride dropwise while stirring. The molar ratio of dipentaerythritol to perfluorovaleryl fluoride is 1:3. After the dropwise addition was completed, the temperature was continued to rise to 80° C., and the reaction was stirred for 5 h. The resulting product was first washed twice with 5% HCl solution, and then washed with 5% NaHCO 3 The solution was washed once, washed with water, extracted with ether, separated by liquid separation to obtain the upper organic layer, and the solvent was distilled off under reduced pressure to obtain a light yellow solid. Dissolve the obtained pale yellow solid in dimethyl sulfoxide (DMSO) and add it to a four-necked flask. After it is complet...
Embodiment 2
[0039] Install a stirrer, a thermometer, a dropping funnel and a reflux condenser (an anhydrous CaCl 2 In a dry 250mL four-necked flask, dissolve bis-pentaerythritol in dimethylformamide to obtain a bis-pentaerythritol solution, add triethylamine and stir to heat to 55°C, and add perfluorovaleryl fluoride dropwise while stirring. The molar ratio of dipentaerythritol to perfluorovaleryl fluoride was 1:3. After the dropwise addition was completed, the temperature was continued to rise to 80 °C, and the reaction was stirred for 5 h. The obtained product was washed twice with 5% HCl solution, and then with 5% NaHCO 3 The solution was washed once, washed with water and then extracted with ether. The upper organic layer was obtained by liquid separation, and the solvent was distilled off under reduced pressure to obtain a pale yellow solid. The obtained pale yellow solid was dissolved in dimethyl sulfoxide (DMSO) and added to a four-necked flask. After all dissolved, about 2 g of ...
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