Synthesis method of polyoxyethylene ether alkylamine cationic surfactant
A technology of polyoxyethylene ether alkylamine and surfactant, which is applied in the field of synthesis of polyoxyethylene ether alkylamine cationic surfactants, and can solve problems such as low yield and long reaction time
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Embodiment 1
[0022] Step 1: Add 59g of ethylene glycol butyl ether and 3g of solid acid catalyst into the reaction kettle, stir at 70°C for 1 hour, then add 48g of epichlorohydrin at a rate of 2 ml / min, and control the reaction temperature at 70°C. Stirring at a rotating speed of 90r / min, the reaction time was 2h, and after the reaction was completed, the content of residual epichlorohydrin in the titrated product was determined by headspace gas chromatography, and the calculated conversion rate was 98.2%. Chlorohydroxypropyl glycol butyl ether was obtained. After the reaction was finished, excess epichlorohydrin was removed by distillation under reduced pressure, and the chlorine ion content in the product was determined by hydrolysis with alkali, and the calculated yield of chlorohydroxypropyl butyl glycol butyl ether was 98.2%.
[0023] Step 2: Add 107g of dodecyldimethyl tertiary amine and 60ml of propylene glycol into the reaction kettle, mix well and raise the temperature to 85°C, an...
Embodiment 2
[0026] Step 1: Add 159g of commercially available AEO-3 sample and 5g of solid acid catalyst into the reaction kettle, stir at 60°C for 1h, then add 48g of epichlorohydrin at a rate of 4 ml / min, raise the temperature to 60°C, and keep it warm for 4h. Prepare chlorohydroxypropyl polyoxyethylene ether. After the reaction was over, the excessive epichlorohydrin was distilled off under reduced pressure, and the chlorine ion content in the product was determined by adding alkali hydrolysis, and the calculated chlorohydroxypropyl polyoxyethylene ether yield was 97.5%.
[0027] Step 2: Add 60ml of absolute ethanol to 107g of dodecyl dimethyl tertiary amine, raise the temperature to 80°C, add the chlorohydroxypropyl polyoxyethylene ether prepared in step 1 at a speed of 7 ml / min, and complete the addition After heat preservation for 3 hours, 40% aqueous sodium hydroxide solution was added to adjust the pH to 9-10, the reaction temperature was raised to 100°C, and the reflux reaction w...
Embodiment 3
[0030] Step 1: Add 269g of commercially available AEO-9 sample and 6g of solid acid catalyst into the reaction kettle, stir at 60°C for 1h, then add 44g of epichlorohydrin at a rate of 4 ml / min, stir and keep at 60°C for 4h to obtain Chlorohydroxypropyl polyoxyethylene ether. After the reaction was over, the excessive epichlorohydrin was distilled off under reduced pressure, and the chlorine ion content in the product was determined by alkali hydrolysis, and the calculated and determined chlorohydroxypropyl polyoxyethylene ether yield was 97.6%.
[0031] Step 2: Add 98g of dodecyldimethyl tertiary amine and 60ml of ethanol into the reaction kettle, stir and raise the temperature to 70°C, and add the chlorohydroxypropyl polyoxyethylene ether prepared in step 1 at a speed of 8 ml / min After the addition, keep the reaction for 4 hours, add 30% sodium hydroxide aqueous solution to adjust the pH to 9-10, raise the reaction temperature to 100 ° C, continue to reflux and stir the reac...
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