Preparation method of antistatic agent onium salt fluoride
A technology of antistatic agent and onium salt, applied in the field of preparation of antistatic agent onium fluoride salt, can solve the problems of affecting yield, large amount of deionized water, long time consumption, etc., and achieves high production efficiency and short time consumption , the effect of simple process
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Embodiment 1
[0020] (1) Mix 33.9 g of potassium perfluorobutane sulfonate and 33.9 g of tetrabutylphosphine bromide, dissolve in 100 mL of tap water at 70°C, stir for 30 minutes, let stand to separate layers, and decant to remove The water-containing material in the upper layer is obtained as the lower liquid phase insoluble in water; (2) at a temperature of 70 °C, add the same volume of tap water as the lower liquid phase to wash the lower liquid phase once; (3) after cooling, dissolve the lower liquid phase with methanol , add 10 g of strong-acid styrene-based cation exchange resin, stir for 10 minutes, filter, then add 10 g of strong-base acrylic anion-exchange resin, stir for 10 minutes, and filter; (4) Distill methanol to obtain the product onium fluoride Salt 54.8 g (yield 98.2%).
[0021] The melting point of the product onium fluoride salt was measured to be 73.4° C. by a differential thermal scanning analyzer (DSC). The quality comparison of the product washed once with tap water...
Embodiment 2
[0024] (1) Mix 33.9 g of potassium perfluorobutane sulfonate and 33.9 g of tetrabutylphosphine bromide, dissolve in 100 mL of tap water at 75°C, stir for 28 minutes, let stand to separate layers, and decant to remove (2) At a temperature of 75 °C, add tap water of the same volume as the lower layer to wash twice; (3) After cooling, dissolve the lower liquid phase with methanol, add 10 g strong-acid styrene-based cation-exchange resin, stirred for 12 minutes, filtered, then added 10 g of strong-base acrylic-based anion-exchange resin, stirred for 12 minutes, filtered; (4) distilled methanol to obtain 54.6 g of onium fluoride salt (Yield 97.8%).
[0025] The melting point of the product onium fluoride salt was measured to be 74.1 °C by differential scanning calorimeter (DSC). The quality comparison of the product washed once with tap water and the final product is as follows:
[0026] project Potassium ion / ppm Magnesium ion / ppm Calcium ion / ppm Chloride / ppm ...
Embodiment 3
[0028] (1) Mix 1.0 kg potassium perfluorobutane sulfonate with 1.0 kg tetrabutylphosphine bromide, dissolve in 1500 mL tap water at 68°C, stir for 35 minutes, let stand to separate layers, and decant to remove (2) At 68°C, add tap water of the same volume as the lower layer to wash once; (3) After cooling, dissolve the lower liquid phase with methanol and add 300 g strong-acid styrene-based cation-exchange resin, stirred for 15 minutes, filtered, then added 300 g of strong-base acrylic-based anion-exchange resin, stirred for 15 minutes, filtered; (4) distilled off methanol to obtain 1.63 kg of onium fluoride salt (Yield 98.8%).
[0029] The melting point of the product onium fluoride salt was 74.3 °C as measured by a differential scanning calorimeter (DSC). The quality comparison of the product washed once with tap water and the final product is as follows:
[0030] project Potassium ion / ppm Magnesium ion / ppm Calcium ion / ppm Chloride / ppm Bromide / ppm Sul...
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