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CN-121573877-B - Medicine production waste liquid separation recovery system

CN121573877BCN 121573877 BCN121573877 BCN 121573877BCN-121573877-B

Abstract

The application discloses a separation and recovery system for waste liquid in drug production, which comprises a conical settling chamber, a pulse recoil membrane assembly, a modularized membrane package, a mixing tank and a miniature vacuum pump, wherein the mixing tank is used for containing drug waste liquid or enrichment liquid, slurry in the mixing tank is discharged into the conical settling chamber, the conical settling chamber is used for separating separated slurry into large-particle impurities and suspension liquid, the suspension liquid comprises medium particles and small particles, the pulse recoil membrane assembly is used for separating the suspension liquid into enrichment liquid and solvent permeation liquid, and the modularized membrane package is used for separating the solvent permeation liquid into enrichment liquid and high-concentration solvent. The application reduces the membrane pollution rate of the pulse backflushing membrane component, realizes the stable liquid level and the dynamic concentration balance, improves the control precision of the solid content of the enriched liquid, improves the recovery purity of the waste liquid in the drug production, and reduces the energy consumption of the system operation.

Inventors

  • DING HONGWEI
  • Ding Shuangwei
  • Yuan Zhixiao
  • LUO XIAOQING

Assignees

  • 上海亿鼎技术(集团)有限公司

Dates

Publication Date
20260505
Application Date
20260127

Claims (4)

  1. 1. The utility model provides a medicine production waste liquid separation recovery system which characterized in that, including toper settling chamber, pulse recoil membrane module, modularization membrane package, blending tank and miniature vacuum pump, the blending tank is used for holding medicine waste liquid or enrichment liquid, and the thick liquid in the blending tank discharges to toper settling chamber, toper settling chamber is used for separating the separation thick liquid into large granule impurity and suspension, and the suspension contains medium granule and tiny particle, the pulse recoil membrane module is used for separating suspension into enrichment liquid and solvent permeate, the modularization membrane package is used for separating solvent permeate into enrichment liquid and high concentration solvent, and large granule impurity indicates the material of >50 mu m, and medium granule is the material of diameter 5-50 mu m, and tiny particle is the material of diameter <5 mu m; The mixing tank is provided with a waste liquid inlet, an enriched liquid inlet and a slurry outlet, the waste liquid in the drug production enters the mixing tank through the waste liquid inlet, the slurry outlet is communicated with a feed inlet of the conical settling chamber, the slurry outlet is also communicated with an inlet of a finished product tank, the finished product tank is used for containing enriched liquid with the concentration reaching the standard, and a valve is arranged at the inlet of the finished product tank; The cavity of the conical settling chamber is formed by an upper cone and a lower cone, the tip end of the lower cone faces downwards, the tip end of the upper cone faces upwards, the bottom circumferences of the upper cone and the lower cone are fixedly connected, the central axes of the upper cone and the lower cone coincide, the feed inlet of the conical settling chamber is arranged on the surface of the upper cone, a valve is arranged at the feed inlet of the conical settling chamber, the feed inlet is a tangential feed inlet so that slurry is injected into the conical settling chamber along the tangential direction of the side wall of the upper cone, the slurry forms stable spiral downward vortex in the cavity, the bottom circumference of the conical settling chamber is uniformly provided with a plurality of compressed air spray holes, the air injected by the plurality of compressed air spray holes rotates to form an ascending air flow and forms a collision angle of 50-55 degrees with the liquid vortex, the bottom end of the conical settling chamber is provided with a large particle collecting port used for collecting large particle impurities in the liquid body, the upper cone is provided with a transition port, the transition port is communicated with a suspension inlet of the pulse membrane component, and the transition port is above the compressed air spray hole is used for enabling the suspension containing medium particles and small particles to flow to the pulse membrane component through the transition port; The pulse backflushing membrane component is provided with a suspension inlet, a first enriched liquid outlet and a solution permeation liquid outlet, the modularized membrane package is provided with a solution inlet, a second enriched liquid outlet and a high-concentration solvent outlet, the suspension inlet is communicated with the transition port, the first enriched liquid outlet is communicated with the enriched liquid inlet of the mixing tank, the solution permeation liquid outlet of the pulse backflushing membrane component is communicated with the solution inlet of the modularized membrane package, the second enriched liquid outlet is communicated with the enriched liquid inlet of the mixing tank, and the high-concentration solvent outlet is communicated with the inlet of the solvent recovery tank; The outlet of the miniature vacuum pump is communicated with the inlet of the vacuum buffer tank, and the outlet of the vacuum buffer tank is communicated with the mixing tank and the pulse recoil membrane assembly; The slurry outlet of the mixing tank is communicated with the inlet of the finished product tank and the feed inlet of the conical settling chamber through a liquid discharge pipe, a concentration detector is arranged on the liquid discharge pipe and used for detecting the concentration of medium and small particulate matters in the slurry, the control unit controls the valve opening at the inlet of the finished product tank, the valve opening at the feed inlet of the conical settling chamber and the negative pressure of the pulse backflushing membrane component according to the detection result of the concentration detector, a concentration threshold value is arranged in the control unit, the control unit compares the detection result of the concentration detector with the set concentration threshold value, if the concentration of the slurry is within the concentration threshold value range, the valve at the inlet of the finished product tank is opened, the valve at the feed inlet of the conical settling chamber is closed, the slurry meeting the requirements is discharged into the finished product tank, if the concentration of the slurry is higher than the concentration threshold value, the valve at the inlet of the finished product tank is closed, the valve at the feed inlet of the conical settling chamber is opened, the negative pressure of the pulse backflushing membrane component is reduced, and if the concentration of the slurry is lower than the concentration threshold value, the valve at the inlet of the finished product tank is closed, the valve at the feed inlet of the conical settling chamber is opened, and the negative pressure of the pulse backflushing membrane component is increased; The diameter of the feed inlet of the conical settling chamber is 15-25mm, the speed of the slurry entering the conical settling chamber is 10-12m/S, a filter screen is arranged at the feed inlet of the conical settling chamber, a booster pump is arranged at the slurry outlet of the mixing tank, the number of compressed air spray holes is 1.5-2.5mm, the compressed air spray holes are communicated with a micro air compressor, the output pressure of the micro air compressor is 0.4-0.6Mpa, the diameter of a large particle collecting port is 20-30mm, a periodically operated micro starting valve is arranged at the large particle collecting port, the periodically operated time of the micro starting valve is less than 0.5S, the distance between a transition port and the bottom end of the conical settling chamber is 150-200mm, and the diameter of the transition port is 20-30mm; The pulse recoil membrane assembly comprises a cylindrical shell, wherein 100-200 silanization modified polyamide hollow fiber membrane wires are vertically filled in the shell, a separation layer of the hollow fiber membrane wires is grafted with a C10-C12 alkyl chain, a water contact angle is 115-125 degrees, the swelling rate of common solvents for drug production is less than 2 percent, the common solvents comprise ethanol and methylene dichloride, the cylindrical shell is communicated with a micro vacuum pump, an annular micro air chamber is arranged at the top of the cylindrical shell, a plurality of air holes with downward openings are uniformly arranged on the annular micro air chamber in the circumferential direction, the annular micro air chamber is communicated with a high-pressure micro air pump, a timing electromagnetic valve is arranged between the annular micro air chamber and the high-pressure micro air pump, a suspension inlet is arranged at the bottom of the pulse recoil membrane assembly, and a first enriched liquid outlet and a solution permeation liquid outlet are both arranged at the upper part of the pulse recoil membrane assembly; The modularized membrane package comprises a rectangular shell, wherein a supporting layer, a transition layer and a separation layer are sequentially arranged in the rectangular shell from top to bottom, the supporting layer is made of terylene non-woven fabric with the diameter of 100-150 mu m, the thickness of the supporting layer is 0.2-0.3mm, the tensile strength of the supporting layer is more than 150N/cm, the transition layer is made of polyimide nanofiber membranes, the thickness of the polyimide nanofiber membranes is 50-80 mu m, the average pore diameter of the polyimide nanofiber membranes is 30-40nm, the polyimide nanofiber membranes are prepared through electrostatic spinning, the surface charge density of the polyimide nanofiber membranes is-0.8-1.0 mC/m < 2 >, the separation layer is a silanized polyamide layer, the thickness of the silanized polyamide layer is 10-15 mu m, the pore diameter of the silanized polyamide layer is 2-4nm, a C10 alkyl chain is grafted on the silanized polyamide layer, a molecular level hydrophobic barrier is formed, a solution inlet is arranged at the upper part of the rectangular shell, a high-concentration solvent outlet is arranged at the bottom of the rectangular shell, and a second enriched liquid outlet is arranged between the transition layer and the separation layer; A U-shaped siphon pipe is arranged between a first enriched liquid outlet of the pulse backflushing membrane assembly and an enriched liquid inlet of the mixing tank, the U-shaped siphon pipe is provided with a high-level port and a low-level port, the high-level port is higher than the low-level port, the first enriched liquid outlet is communicated with the high-level port of the U-shaped siphon pipe, a second enriched liquid outlet of the modularized membrane package is also communicated with the high-level port of the U-shaped siphon pipe, and the low-level port is communicated with the enriched liquid inlet of the mixing tank.
  2. 2. The separation and recovery system according to claim 1, wherein the cone angle of the lower cone in the conical settling chamber is 65 ° -75 °, the height of the conical settling chamber is 300-500mm, the maximum diameter of the conical settling chamber is 180-250mm, the conical settling chamber is made of 316L stainless steel or polytetrafluoroethylene, and a square chamber is arranged at the top point of the upper cone in the conical settling chamber.
  3. 3. The separation and recovery system according to claim 1, wherein the diameter of the cylindrical shell is 80-120mm, the height of the cylindrical shell is 200-300mm, the diameter of the silanized modified polyamide hollow fiber membrane wires is 0.6-0.8mm, the hollow pore diameter is 2-4nm, the effective filtering area is 0.8-1.5m < 2 >, the negative pressure range provided by the micro vacuum pump to the pulse back flushing membrane assembly is-0.03-0.06 Mpa, the output pressure of the high-pressure micro air pump is 0.8-1.0Mpa, the pulse frequency of the timing electromagnetic valve is 2-3Hz, the single back flushing duration is 80-120ms, and a booster pump is arranged between the solution permeation liquid outlet of the pulse back flushing membrane assembly and the solution inlet of the modularized membrane package.
  4. 4. The separation and recovery system according to claim 1, wherein a liquid discharge tank is provided between the modular membrane package and the solvent recovery tank, an inlet of the liquid discharge tank is communicated with a high concentration solvent outlet of the modular membrane package, an outlet of the liquid discharge tank is communicated with an inlet of the solvent recovery tank, a capacitance type low level gauge is provided at a lower side of the liquid discharge tank, and an ultrasonic wave high level gauge is provided at an upper side of the liquid discharge tank; the distance between the capacitance type low level meter and the lower end of the liquid draining tank is 30-50mm, the capacitance type low level meter is used for detecting the thickness of a residual liquid layer at the tank bottom of the liquid draining tank in a contact mode, so as to control residual quantity in the liquid draining tank, the distance between the ultrasonic wave high level meter and the upper end of the liquid draining tank is 50-80mm, the ultrasonic wave high level meter is used for monitoring a liquid level peak value in a non-contact mode, pollution caused by direct contact with medicine waste liquid is avoided, a large water pump and a small water pump are arranged in parallel between an outlet of the liquid draining tank and an inlet of the solvent recycling tank, the flow rate of the large water pump is larger than that of the small water pump, inlets of the large water pump and the small water pump are communicated with the outlet of the liquid draining tank, a high liquid level threshold value, a transition liquid level and a low liquid level threshold value are sequentially arranged on the liquid draining tank from top to bottom, the ultrasonic wave high level meter is triggered when the liquid level in the liquid draining tank is lower than the low liquid level threshold value, the ultrasonic wave high liquid level meter is triggered when the liquid level in the liquid draining tank is continuously triggered and the capacitance type low liquid level meter is not triggered, the liquid draining tank is judged to be in a real liquid full state, the liquid draining tank is started, the liquid draining tank is prevented from overflowing liquid level is high and the liquid level is not triggered by the liquid level meter is high liquid level meter, when the liquid level in the liquid discharge tank is positioned at a low level threshold value, an ultrasonic altimeter is not triggered, a capacitance type low level meter is triggered, the large water pump and the small water pump stop working, liquid discharge of the liquid discharge tank is closed, and the outlets of the large water pump and the small water pump are provided with one-way check valves.

Description

Medicine production waste liquid separation recovery system Technical Field The invention relates to the technical field of chemical pharmacy separation, in particular to a separation and recovery system for waste liquid in drug production. Background In the process of medicine production, waste liquid recovery is a key link for guaranteeing environment-friendly compliance and resource recycling, early medicine production depends on pressurized discharge, but air mixed in medicine liquid is easy to generate bubbles to influence product quality, and if open operation is adopted for recovery of high-toxicity solvents in chemical pharmacy, volatilization leakage is easy to cause, so that the environment and personnel safety are endangered. The miniature negative pressure separation system has become an indispensable core device in the process by virtue of the advantages of a closed low-pressure environment, compact volume and low energy consumption, and has important significance in improving the refinement level of waste liquid treatment, reducing resource waste and the like. However, the existing miniature negative pressure separation system still faces a plurality of technical bottlenecks in practical application, namely complex components of the medicine waste liquid and large viscosity fluctuation, so that the system treatment efficiency is unstable, the long-term operation reliability is insufficient, the system is limited by structural design and separation mechanisms, the stage number of the classification separation is difficult to reach three or more stages, the accurate classification recovery of multiple components in the waste liquid cannot be realized, meanwhile, the effective means for flexibly and adjustably adjusting the concentration of the discharged liquid is lacking, the differentiated requirements of different medicine production processes on the treatment of the waste liquid are difficult to adapt, and the popularization, application and the performance exertion of the system in the field of recovery of the medicine production waste liquid are severely restricted. Disclosure of Invention Aiming at the defects in the prior art, the application provides a drug production waste liquid separation and recovery system, which aims to solve the technical problems that the drug production waste liquid separation and recovery system in the prior art cannot realize accurate grading recovery of multiple components in waste liquid, the concentration of discharged liquid is difficult to adjust and the like. In order to achieve the aim of the invention, the technical scheme provided by the invention is as follows: The utility model provides a medicine production waste liquid separation recovery system, includes toper settling chamber, pulse recoil membrane module, modularization membrane package, blending tank and miniature vacuum pump, the blending tank is used for holding medicine waste liquid or enrichment liquid, and the thick liquid in the blending tank discharges to toper settling chamber, toper settling chamber is used for separating the separation thick liquid into large granule impurity and suspension, and the suspension contains medium granule and tiny particle, pulse recoil membrane module is used for separating suspension into enrichment liquid and solvent permeate, the modularization membrane package is used for separating solvent permeate into enrichment liquid and high concentration solvent, and large granule impurity indicates the material of direct >50 mu m, and medium granule is the material of diameter 5-50 mu m, and tiny particle is the material of diameter <50 mu m; The mixing tank is provided with a waste liquid inlet, an enriched liquid inlet and a slurry outlet, the waste liquid in the drug production enters the mixing tank through the waste liquid inlet, the slurry outlet is communicated with a feed inlet of the conical settling chamber, the slurry outlet is also communicated with an inlet of a finished product tank, the finished product tank is used for containing enriched liquid with the concentration reaching the standard, and a valve is arranged at the inlet of the finished product tank; The cavity of the conical settling chamber is formed by an upper cone and a lower cone, the tip end of the lower cone faces downwards, the tip end of the upper cone faces upwards, the bottom circumferences of the upper cone and the lower cone are fixedly connected, the central axes of the upper cone and the lower cone coincide, the feed inlet of the conical settling chamber is arranged on the surface of the upper cone, a valve is arranged at the feed inlet of the conical settling chamber, the feed inlet is a tangential feed inlet so that slurry is injected into the conical settling chamber along the tangential direction of the side wall of the upper cone, the slurry forms stable spiral downward vortex in the cavity, the bottom circumference of the conical settling chamber is uniformly provi