A dmf saline waste liquid recovery process
A technology for salt-containing waste liquid and process, which is applied in the fields of organic chemistry, carboxylic acid amide separation/purification, etc., to achieve the effect of reducing the cost of treatment and recovery, simplifying the treatment process, and recovering products with high purity
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Embodiment 1
[0047] Embodiment 1 (centrifugal separation)
[0048] like figure 1 As shown, a novel two-phase centrifugal separation device includes a liquid pump system, a centrifugal separator, a solid collector, and a liquid collection tank connected in sequence. During work, the DMF waste liquid is heated to 50°C in the DMF waste liquid storage tank 1, and then quantitatively transported to the centrifuge 3 by the screw pump 2, and the rotational speed of the centrifuge drum is set to 2000r·min -1 , due to the centrifugal force generated by the rotation of the rotating inner barrel, the DMF liquid and the solid waste are separated in layers, and the solid waste enters the solid collector (solid collection pool) from the bottom through the shaftless screw conveyor 4. The upper part of the liquid is operated by centrifugation, so that the liquid phase is efficiently separated from the solid and collected in the DMF receiving tank 5. The liquid phase collected by the DMF receiving tank 5...
Embodiment 2
[0049] Embodiment 2 (extraction separation)
[0050] like figure 2 As shown, an extraction and separation device circulates 0°C cooling brine in the system, and quantitatively sends the centrifuged DMF liquid (containing a small amount of inorganic salt) into the intermittent extraction tank (the temperature of the extraction tank is 80°C ), then the extractant carbon tetrachloride is injected in the extraction tank, the mass ratio of carbon tetrachloride and DMF liquid is 10:1, after carrying out extraction and separation for 30 minutes, leave standstill for 30 minutes, obtain solid and liquid layering, solid The inorganic salt is at the bottom of the extraction tank, and the extractant-DMF mixture is at the top. The solid inorganic salt is discharged from the bottom of the tank, and the obtained carbon tetrachloride and DMF mixture is transported to the rectification device through a pump.
Embodiment 3
[0051] Embodiment 3 (rectification purification)
[0052] like image 3 Shown, a kind of rectification / distillation device. Use a feeding pump to pump the mixed solution containing carbon tetrachloride and DMF from the mixture receiving tank 6' into the heating kettle 1'. After preheating to 120°C through the oil furnace 2', the mixed solution is vaporized and rises through the pipeline to enter the refining tank. Distillation column or distillation column 3' for separation; then enter the condenser 7' to cool the gas into liquid, part of it is refluxed, and part of it enters the product cooler for further cooling and is extracted as a finished product; the part that has not been cooled into liquid enters the lower condenser for cooling again , after cooling into liquid, enter the reflux tube and return to the rectification column (distillation column); at 30-80°C, discharge the light component extractant into the extractant receiving tank 5'; at 80-140°C, drain the heavy comp...
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