purification method | firstly, fresh sodium bisulfite with qualified analysis is added to the preparation kettle, and 35wt% aqueous solution is prepared with distilled water under room temperature and normal pressure conditions. The prepared sodium bisulfite solution 2857Kg (concentration 35wt%) is sent to the ethoxylation reactor. After nitrogen replacement and heating operation, ethylene oxide is added at 90 ℃ to start the reaction. The temperature is controlled at 90~100 ℃ and the pressure is 0~0.1MPag (gauge pressure). After 500Kg of ethylene oxide is added, it is cured at 90~100 ℃ for 30 minutes and discharged. The crude product (concentration 40 ~ 45wt%) synthesized in the previous step is sent to a double-effect continuous evaporation heavy crystallizer, and the method of downstream operation, continuous feeding, and intermittent discharging is used, that is, the dilute solution is advanced to a one-effect evaporator. After preliminary concentration, the concentration reaches 55 ~ 60wt%, the concentrated liquid enters a two-effect evaporator, and is further concentrated and evaporated to 72 ~ 75wt%, and then the concentrated liquid enters the continuous crystallization machine, after crystallization at a constant speed of cooling to 20~40 ℃, the crystal slurry enters the centrifuge for centrifugal separation, the solid enters the next process, and the mother liquor returns to the two-effect evaporator to continue to participate in evaporation concentration. When the ethylene glycol content in the product reaches below 0.1% wt, it is regarded as qualified. Through analysis and testing, the purity of the product is greater than 99.5wt%. A small amount of non-crystallizable residual liquid is extracted with 3 times the solvent. The extractant used is anhydrous ethanol. Sodium hydroxyethyl sulfonate products are precipitated in anhydrous ethanol. A small amount of water and organic impurities, such as ethylene glycol, Polyethylene glycol and hydroxyethyl sulfonate will enter the liquid phase ethanol, and then enter the centrifuge for centrifugal separation. Finally, the crystals will be dried at 120°C in a disc dryer, remove a small amount of residual solvent impurities and moisture from the product. The used extractant ethanol is recycled and reused. Extractant ethanol can be distilled and recovered. |