[0032] Example 2
[0033] Waste solvent ethanol-ethyl acetate-piperazine recovery method, the introduction steps include:
[0034] Take the waste solvent containing 55% ethanol, 39% ethyl acetate, 5% piperazine, rectification, rectification conditions: Distilor bottom temperature 112 ° C, liquid temperature in the kettle 109 ° C, kettle temperature 70 ~ 78 ° C , Control reflow ratio 6: 1; separation of ethanol, ethyl acetate and a small amount of water; tower kettle off piperazine, detects the canal, filled with nitrogen, to obtain purity ≥99.5% (wt) water absorbent piperazine .
[0035]The ethanol and ethyl acetate obtained above the above-mentioned rectification were added to the waste solvent 1.35 times the volume of water, washed, and the upper layer was obtained from the organic phase composed of ethyl acetate and water, and the lower layer was obtained from ethanol and water.
[0036] The organic phase, azeotrope rectification, and distillation of the above water was washed in: the bottom of the rectification could be 79 ° C, the liquid temperature in the kettle was 77 ° C, the ceiling temperature was 70 ° C, and the reflux ratio was 18: 1. The top of the column is given azeotropic azeoglycetic azeotropic mixture, a layered, separation; the upper layer returns to the column, continues to be azeotropic rectification; the aqueous layer returns to the extract, and ethyl acetate and ethanol are continuously separated. The tower was taking ethyl acetate, detecting the canal, and filled with nitrogen, and the purity of ≥99.0% (Wt) was obtained. EtOAc.
[0037] The aqueous phase of step 2 was washed, distilled, and the distillation of distillation was: the bottom temperature of the distillation could be 100 ° C, the liquid temperature in the kettle was 90 ° C, the top temperature of the jack was 82 ° C. Tower top ethanol and water of the water are made of 1.5m 3 / Hour flow rate film dehydration, ethanol detection can be passed, and the filled nitrogen is preserved, that is, the industrial-grade anhydrous ethanol of purity ≥99.9% (wt); wastewater and tower replacement water return to the extract tower, continue to circulate.
[0038] Examples 1 to 2 The technical indicators of water and peptipiperazine after purification are shown in Table:
[0039] Table I
[0040]
[0041]
[0042] Examples 1 to 2 The technical indicators of ethyl acetate after purification are shown in Table 2:
[0043] Table II
[0044]
[0045] Example 1 to 2 The technical indicators of industrial-grade anhydrous ethanol after purification are shown in Table 3:
[0046] Table three
[0047]
[0048]
[0049] The anti-flow device includes a reactor, and the top fixed communication of the reactor is provided with a ventilation tube 2 for distillation gas flowing out. The outer side wall of the air tube 2 is provided with a condenser groove 3, and the inside of the air pipe 2 is fixedly mounted with a heat sensor 4. The inside of the air tube 2 is connected to the drive motor 501, and the inner portion of the air pipe 2 is connected to the drive mechanism 5 and the transmission mechanism 6, the drive motor 501 and the heat sensor 4 are electrically connected, and the heat sensor 4 can control the driving motor 501 work. The drive mechanism 5 includes a rotating screw 504 fixed to the output terminal of the drive motor 501, and the side surface of the drive motor 501 is fixedly connected to the mounting rod 502, and the mounting lever 502 is fixed to the inner side wall of the air pipe 2, the drive motor 501 outer wall cover The protective cover 503, the rotary rod 504, and the driving motor 501 output terminal are provided with the base rod 505, and the inner side wall of the air pipe 2 is fixedly connected to the drive rod 506, and the outer wall of the rotary rod 504 is attached. There is a transmission shaft 10, and the drive shaft 10 is slidable with the drive rod 506.
[0050] The transmission mechanism 6 includes two sliding grooves 601, which are opened on the inside of the vent, and the end of the transmission shaft 10 fixes the sliding bump 602, the sliding bump 602 slides inside the sliding groove 601, the inside of the sliding groove 601 It is provided with a telescopic rod 603, and both ends of the telescoping rod 603 respectively couple the side wall of the sliding bump 602 and the inner side wall of the sliding groove 601, and the stretch rod 603 is provided with a spring 604, and the outer wall transfer sleeve of the drive shaft 10 is provided. Two fixed sleeves 9, the bottom of the two fixed sleeves 9 fixedly connected to the arc-shaped anti-backflow plate 7, and the edge position of the backflow plate 7 is fixedly connected to the mounting rubber 8, the anti-backflow plate 7 and the mounting rubber 8 The inclination is close to the bottom of the inner side wall of the air pipe 2, and the retractable returning back-to-return retraction plate 7 is returned by the retracting of the rubber 8 in the inner side wall of the air tube 2 is attached to the bottom of the ventilation tube 2. However, it is not returned to the reaction kettle 1, and the inclined anti-backflow plate 7 is blocked by the inner side wall of the ventilation pipe 2, ensuring that the anti-backflow plate 7 can only rotate half, avoid the current ethanol solution liquid. In the case where the liquid elut elut is low, the efficient purification process of ethanol solution is guaranteed.
[0051] When the mating between the drive mechanism and the transmission mechanism is operated by the gas, the drive motor 501 operates, the rotating rod 504 drives the drive shaft 10 and the anti-backflow plate 7 to move to the base rod 505. As the distillation ends, the drive motor 501 stops working. At this time, the compressed telescopic rod 603 and the spring 604 drive the transmission shaft 10 and the backflow plate 7, at this time, the inner side wall of the backflow plate 7 and the inner side wall of the mounting rubber 8 are Scraping on the inner side wall of the trachea 2, the residual portion of the exhaust pipe 2 is residual, the diameter side wall of the air tube 2 is raised out, and after solving the current liquid tube, some liquid will remain in The phenomenon in the liquid tube is effectively improved the efficiency of the liquid, and it is to be noted that the rotary screw 504 and the base rod 505 are free to rotate at the output of the drive motor 501 when the retransmission plate 7 is reset.
[0052] In the present invention, during the recovery of ethanol-acetate-piperazine waste solvent, the ethanol solution is involved in distillation, which is specifically that distilled the mixed ethanol solution in the reaction kettle 1, and the evaporated ethanol gas is from out. The tracheal 2 out, and the gas is liquefied into a liquid through the cooling of the condensate groove 3, at which time the ethanol solution flows out along the bottom of the inner side wall of the air pipe 2, and the heat gas triggered heat sensor 4 in the delivery pipe 2 is introduced. Work, the heat sensor 4 can drive the drive motor 501 to operate, the output of the drive motor 501 drives the rotary rod 504 to rotate, so that the transmission shaft 10 is rotated to rotate the position of the drive motor 501 until the drive shaft 10 Slide to the base rod 505, at which time the transmission shaft 10 and the base rod 505 are in the rotation state, corresponding to the position of the anti-backflow plate 7 at this time, in the air tube 2, the cooling ethanol solution is passed freely. The baffle 7 flows out, since the anti-backflow plate 7 is inclined, after the evaporation is completed, the partial reflow liquid will go back through the air tube 2, at which time the anti-backflow plate 7 in the inner side wall of the ventilator 2 blocks the reflow liquid, while At this time, the heat sensor 4 senses the temperature drop to stop the drive motor 501, and the compressed telescopic rod 603 and the spring 604 drive the drive shaft 10 and the anti-backflow plate 7 overall reset.
