Medicine production waste liquid separation and recovery system

Abstract

The invention discloses a medicine production waste liquid separation and recovery system which comprises a conical settling chamber, a pulse back-flushing membrane assembly, a modular membrane bag, a mixing tank and a miniature vacuum pump, the mixing tank is used for containing medicine waste liquid or enriched liquid, and slurry in the mixing tank is discharged into the conical settling chamber; the conical settling chamber is used for dividing separation slurry into large-particle impurities and suspension liquid, the suspension liquid contains medium particles and small particles, the pulse back-flushing membrane assembly is used for separating the suspension liquid into enrichment liquid and solvent permeation liquid, and the modular membrane bag is used for separating the solvent permeation liquid into the enrichment liquid and a high-concentration solvent. According to the invention, the membrane pollution rate of the pulse backflushing membrane assembly is reduced, the liquid level stability and the concentration dynamic balance are realized, the solid content control precision of the enriched liquid is improved, the recovery purity of the medicine production waste liquid is improved, and the operation energy consumption of the system is reduced.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of chemical pharmaceutical separation technology, in particular to a pharmaceutical production waste liquid separation and recovery system. BACKGROUND

[0002] In the process of drug production, waste liquid recovery is a key link to ensure environmental compliance and resource recycling. Early drug production relied on pressure discharge, but the air mixed in the drug solution easily produced bubbles, affecting product quality. In the recovery of high-toxicity solvents in chemical pharmaceuticals, open operation easily causes volatile leakage, endangering the environment and personnel safety. Micro negative pressure separation system has become an indispensable core equipment in this process due to its advantages of closed low pressure environment, compact size and low energy consumption, and has important significance in improving the fine level of waste liquid treatment and reducing resource waste. However, the existing micro negative pressure separation system still faces many technical bottlenecks in actual application: the complex composition and large viscosity fluctuation of drug waste liquid lead to unstable system processing efficiency and insufficient long-term operation reliability; limited by structure design and separation mechanism, the number of stages of its fractional separation is difficult to reach three or more, which cannot realize the accurate fractional recovery of multiple components in waste liquid; at the same time, the discharge concentration lacks flexible and effective means to adapt to the differentiated requirements of different drug production processes for waste liquid treatment, which seriously restricts its popularization and application in the field of drug production waste liquid recovery and the exertion of its efficiency. SUMMARY

[0003] In view of the defects in the prior art, the present application provides a pharmaceutical production waste liquid separation and recovery system to solve the technical problems in the prior art that the waste liquid separation and recovery system cannot realize accurate fractional recovery of multiple components in waste liquid and the discharge concentration is difficult to adjust.

[0004] In order to achieve the above-mentioned purpose, the technical scheme provided by the present application is as follows: A pharmaceutical production waste liquid separation and recovery system, comprising a conical settling chamber, a pulse backflush membrane assembly, a modular membrane package, a mixing tank and a micro vacuum pump, the mixing tank is used to contain drug waste liquid or enriched liquid, the slurry in the mixing tank is discharged to the conical settling chamber, the conical settling chamber is used to separate the slurry into large particle impurities and suspended liquid, the suspended liquid contains medium particles and small particles, the pulse backflush membrane assembly is used to separate the suspended liquid into enriched liquid and solvent permeate, the modular membrane package is used to separate the solvent permeate into enriched liquid and high concentration solvent, the large particle impurities refer to substances with a diameter of > 50 pm, the medium particles are substances with a diameter of 5-50 pm, and the small particles are substances with a diameter of < 50 pm. The mixing tank is provided with a waste liquid inlet, an enriched liquid inlet and a slurry outlet. The pharmaceutical production waste liquid enters the mixing tank through the waste liquid inlet. The slurry outlet is communicated with the feed inlet of the conical sedimentation chamber and the inlet of the product tank. The product tank is used to contain the enriched liquid with a standard concentration. A valve is arranged at the inlet of the product tank. The chamber of the conical sedimentation chamber is formed by an upper cone and a lower cone. The tip of the lower cone faces downward, and the tip of the upper cone faces upward. The bottom surfaces of the upper and lower cones are fixedly connected in a circumferential manner. The central axes of the upper and lower cones coincide. The feed inlet of the conical sedimentation chamber is arranged on the surface of the upper cone. A valve is arranged at the feed inlet. The feed inlet is a tangential feed inlet, so that the slurry is injected into the conical sedimentation chamber along a direction tangent to the side wall of the upper cone. The slurry forms a stable spiral downward vortex in the chamber. A plurality of compressed air injection holes are uniformly arranged at the bottom of the conical sedimentation chamber in a circumferential manner. The air injected by the plurality of compressed air injection holes forms a rotating upward airflow, which forms a 50°-55° collision angle with the liquid vortex. A large particle collection port is arranged at the bottom end of the conical sedimentation chamber to collect large particle impurities in the liquid. A transition port is arranged on the upper cone and is communicated with the suspension inlet of the pulse backflush membrane assembly. The transition port is above the compressed air injection holes. The suspension containing medium and small particles flows to the pulse backflush membrane assembly through the transition port. The pulse backflush membrane assembly is provided with a suspension inlet, a first enriched liquid outlet and a solution permeate outlet. The modular 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 permeate outlet of the pulse backflush membrane assembly is communicated with the solution inlet of the modular membrane package. The second enriched liquid outlet is communicated with the enriched liquid inlet of the mixing tank. The high-concentration solvent outlet is communicated with the inlet of the solvent recovery tank. The outlet of the micro vacuum pump is communicated with the mixing tank and the pulse backflush membrane assembly.

[0005] In an embodiment, the outlet of the micro vacuum pump is communicated with the inlet of the vacuum buffer tank. The outlet of the vacuum buffer tank is communicated with the mixing tank and the pulse backflush membrane assembly.

[0006] In an embodiment, the slurry outlet of the mixing tank is communicated with the inlet of the product tank and the feed inlet of the conical settling chamber through a discharge pipe, a concentration detector is arranged on the discharge pipe, the concentration detector is used to detect the concentration of the small and medium-sized particulate matters in the slurry, the control unit controls the opening degree of the valve at the inlet of the product tank, the opening degree of the valve at the feed inlet of the conical settling chamber and the negative pressure of the pulse backflushing membrane assembly 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, the valve at the inlet of the product tank is opened and the valve at the feed inlet of the conical settling chamber is closed, and the slurry meeting the requirements is discharged into the product tank, if the concentration of the slurry is higher than the concentration threshold value, the valve at the inlet of the product tank is closed and the valve at the feed inlet of the conical settling chamber is opened, and the negative pressure of the pulse backflushing membrane assembly is reduced, if the concentration of the slurry is lower than the concentration threshold value, the valve at the inlet of the product tank is closed and the valve at the feed inlet of the conical settling chamber is opened, and the negative pressure of the pulse backflushing membrane assembly is increased.

[0007] In an embodiment, the diameter of the feed inlet of the conical settling chamber is 15-25 mm, the speed of the slurry entering the conical settling chamber is 10-12 m / s, a filter screen is arranged at the feed inlet of the conical settling chamber, and a booster pump is arranged at the slurry outlet of the mixing tank; the number of the compressed air injection holes is 1, the diameter of the compressed air injection hole is 1.5-2.5 mm, the compressed air injection hole is communicated with the micro air compressor, the output pressure of the micro air compressor is 0.4-0.6 Mpa; the diameter of the large particle collection port is 20-30 mm, a periodically operated micro starting valve is arranged at the large particle collection port, the periodically operated time of the micro starting valve is less than 0.5 s, the distance between the transition port and the bottom end of the conical settling chamber is 150-200 mm, and the diameter of the transition port is 20-30 mm.

[0008] In an embodiment, the cone angle of the lower conical body in the conical settling chamber is 65°-75°, the height of the conical settling chamber is 300-500 mm, the maximum diameter of the conical settling chamber is 180-250 mm, the material of the conical settling chamber is 316L stainless steel or polytetrafluoroethylene, and a square body cavity is arranged at the vertex of the upper conical body in the conical settling chamber.

[0009] In an embodiment, the pulse backflush membrane assembly comprises a cylindrical shell, 100-200 silanized modified polyamide hollow fiber membrane filaments are vertically packed inside the shell, the separation layer of the hollow fiber membrane filaments is grafted with C10-C12 alkyl chains, the water contact angle is 115°-125°, and the swelling rate against commonly used solvents for drug production is <2%, the commonly used solvents including ethanol and dichloromethane; 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 opening downward 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 backflush membrane assembly, and a first enriched liquid outlet and a solution permeate outlet are both arranged at the upper part of the pulse backflush membrane assembly.

[0010] In an embodiment, the diameter of the cylindrical shell is 80-120 mm, the height of the cylindrical shell is 200-300 mm, the diameter of the silanized modified polyamide hollow fiber membrane filament is 0.6-0.8 mm, the hollow pore size is 2-4 nm, and the effective filtration area is 0.8-1.5 m²; the micro vacuum pump provides a negative pressure range of -0.03 to -0.06 Mpa to the pulse backflush membrane assembly, the high-pressure micro air pump outputs a pressure of 0.8-1.0 Mpa, the pulse frequency of the timing electromagnetic valve is 2-3 Hz, and the single backflush duration is 80-120 ms; a booster pump is arranged between the solution permeate outlet of the pulse backflush membrane assembly and the solution inlet of the modular membrane package.

[0011] In an embodiment, the modular membrane package comprises a rectangular shell, and a support layer, a transition layer and a separation layer are sequentially arranged in the rectangular shell from top to bottom; the support layer is made of dacron non-woven fabric with a diameter of 100-150 μm, the thickness of the support layer is 0.2-0.3 mm, and the tensile strength of the support layer is >150 N / cm; the transition layer is made of polyimide nanofiber membrane, the thickness of the polyimide nanofiber membrane is 50-80 μm, the average pore size is 30-40 nm, the polyimide nanofiber membrane is prepared by electrospinning, and the surface charge density of the polyimide nanofiber membrane is -0.8 to -1.0 mC / m²; the separation layer is a silanized polyamide layer, the thickness of the silanized polyamide layer is 10-15 μm, the pore size is 2-4 nm, the silanized polyamide layer is grafted with C10 alkyl chains to form a molecular level hydrophobic barrier; the solution inlet is arranged at the upper part of the rectangular shell, the high-concentration solvent outlet is arranged at the bottom of the rectangular shell, and the second enriched liquid outlet is arranged between the transition layer and the separation layer.

[0012] In an embodiment, a drain tank is arranged between the modular membrane package and the solvent recovery tank, the inlet of the drain tank is communicated with the high-concentration solvent outlet of the modular membrane package, the outlet of the drain tank is communicated with the inlet of the solvent recovery tank, the lower side of the drain tank is provided with a capacitive low-level meter, and the upper side of the drain tank is provided with an ultrasonic high-level meter; the distance between the capacitive low-level meter and the lower end of the drain tank is 30-50 mm, which is used to contactively detect the residual liquid layer thickness at the bottom of the drain tank, so as to control the residual amount in the drain tank; the distance between the ultrasonic high-level meter and the upper end of the drain tank is 50-80 mm, which is used to non-contactively monitor the peak value of the liquid level, so as to avoid pollution caused by direct contact with the drug waste liquid; the outlet of the drain tank and the inlet of the solvent recovery tank are connected in parallel with a large water pump and a small water pump, the flow rate of the large water pump is greater than that of the small water pump, the inlets of the large water pump and the small water pump are communicated with the outlet of the drain tank, the outlets of the large water pump and the small water pump are communicated with the inlet of the solvent recovery tank, and the drain tank is sequentially provided with a high-level threshold, a transition liquid level and a low-level threshold from top to bottom; the ultrasonic high-level meter is triggered when the liquid level in the drain tank is between the high-level threshold and the transition liquid level, and the capacitive low-level meter is triggered when the liquid level in the drain tank is lower than the low-level threshold; when the ultrasonic high-level meter is continuously triggered and the capacitive low-level meter is not triggered, it is determined that the drain tank is in a true full-liquid state, the large water pump is started to work, and the liquid in the drain tank is quickly discharged, so as to avoid overflow of the drain tank; when the liquid level in the drain tank is lower than the transition liquid level and higher than the low-level threshold, neither the ultrasonic high-level meter nor the capacitive low-level meter is triggered, the large water pump stops working, and the small water pump works, so as to slowly discharge the liquid in the drain tank; when the liquid level in the drain tank is at the low-level threshold, the ultrasonic high-level meter is not triggered and the capacitive low-level meter is triggered, the large water pump and the small water pump both stop working, and the liquid discharge of the drain tank is closed, and a one-way check valve is arranged at the outlet of the large water pump and the small water pump.

[0013] In an embodiment, a U-shaped siphon is arranged between the first enriched liquid outlet of the pulse backflushing membrane assembly and the enriched liquid inlet of the mixing tank, the U-shaped siphon 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, and the second enriched liquid outlet of the modular membrane package is also communicated with the high-level port of the U-shaped siphon, and the low-level port is communicated with the enriched liquid inlet of the mixing tank.

[0014] Compared with the prior art, the present application has at least the following beneficial effects: The application forms stable spiral vortex at 10-12 m / s tangential inlet velocity by the conical angle structure and the aerodynamic vortex strengthening design of the circular flow settling chamber, realizes high-efficiency three-stage separation of >50 mu m, 5-50 mu m and <5 mu m particles in the drug production waste liquid, and completes accurate interception and non-shear return of small particles under the drive of-0.03~-0.06 MPa negative pressure by combining the pulse backflush membrane assembly and the U-shaped siphon self-return channel, so that the membrane pollution rate of the pulse backflush membrane assembly is reduced by 80%; the control unit realizes stable liquid level of the discharge tank and dynamic balance of the concentration in the discharge process by the capacitor-ultrasonic wave double liquid level sensing interlocking and the large and small pump linkage, and cooperates with the concentration detector, so that the solid content control precision of the enriched liquid reaches ±1%; the modular membrane package relies on the polyester-polyimide-silanized polyamide three-layer composite structure, maintains the swelling rate <2% in the strong solvent environment, and finally achieves the comprehensive technical effects that the drug waste liquid recovery purity is >99.5%, the energy consumption is reduced by 40%, and the modular membrane package is suitable for various drug solvent systems. BRIEF DESCRIPTION OF DRAWINGS

[0015] Figure 1 It is a structural schematic diagram of a drug production waste liquid separation and recovery system in the embodiment of the application; Figure 2 It is a structural schematic diagram of a conical settling chamber in the embodiment of the application; Figure 3 It is a structural schematic diagram of a pulse backflush membrane assembly in the embodiment of the application; Figure 4 It is a structural schematic diagram of a modular membrane package in the embodiment of the application; Figure 5 It is a structural schematic diagram of a U-shaped siphon in the embodiment of the application.

[0016] The reference signs: 1, conical settling chamber; 2, pulse backflush membrane assembly; 201, cylindrical shell; 202, hollow fiber membrane wire; 203, annular micro air chamber; 3, modular membrane package; 301, rectangular shell; 302, support layer; 303, transition layer; 304, separation layer; 4, mixing tank; 5, U-shaped siphon; 6, concentration detector; 7, control unit; 8, finished product tank; 9, solvent recovery tank; 10, discharge tank; 1001, large water pump; 1002, small water pump; 1003, ultrasonic level gauge; 1004, capacitive level gauge; 11, micro vacuum pump; 1101, vacuum buffer tank; 12, booster pump. DETAILED DESCRIPTION

[0017] In order to make the purpose, technical scheme and advantages of the application more clear and obvious, the application will be described below through specific embodiments shown in the drawings. However, it should be understood that these descriptions are only exemplary and are not intended to limit the scope of the application. In addition, in the following description, the description of the known structures and technologies is omitted to avoid unnecessary confusion of the concept of the application.

[0018] The terminology used in the disclosure is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure. As used in this disclosure and the appended claims, the singular forms "a," "an" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will also be understood that the term "and / or" as used herein refers to and encompasses any and all possible combinations of one or more of the associated listed items.

[0019] It is to be understood that the terms first, second, third, etc. can be employed merely for distinguishing between information objects that are discussed in the context of the present disclosure and are not necessarily intended to delineate between those information objects that have a relatively higher or lower importance level, unless otherwise indicated or implied by the context. Such terms are used only to distinguish between information objects of the same type. For example, a first information object can also be referred to as a second information object, and similarly, a second information object can also be referred to as a first information object, without departing from the scope of the present disclosure. Depending on the context, the word "if' as used herein can be interpreted to mean "when" or "upon the occurrence of" or "in response to the determination of" as the case can be.

[0020] In the description of the present application, unless otherwise specified and limited, it is necessary to explain that the terms "mounting", "connection", "connection" should be understood in a broad sense, for example, it can be mechanical connection, or the communication between the two elements, or direct connection, or indirect connection through intermediate media, and the specific meaning of the above terms can be understood by those skilled in the art according to the specific circumstances.

[0021] In order to better understand the technical scheme of the present application, the present application will be described in detail below in conjunction with the embodiments and the drawings.

[0022] The present embodiment provides a pharmaceutical production waste liquid separation and recovery system, as shown in the drawing, comprising a conical settling chamber 1, a pulse backflush membrane assembly 2, a modular membrane package 3, a mixing tank 4, a miniature vacuum pump 11 and a control unit 7, the mixing tank 4 is used to contain pharmaceutical waste liquid or enriched liquid, the slurry in the mixing tank 4 is discharged to the conical settling chamber 1, the conical settling chamber 1 is used to separate the slurry into large particle impurities and suspension, the suspension contains medium particles and small particles, the pulse backflush membrane assembly 2 is used to separate the suspension into enriched liquid and solvent permeate, the modular membrane package 3 is used to separate the solvent permeate into enriched liquid and high concentration solvent, the large particle impurities refer to substances with a diameter > 50 μm, the medium particles refer to substances with a diameter of 5-50 μm, and the small particles refer to substances with a diameter < 50 μm; The mixing tank 4 is provided with a waste liquid inlet, an enriched liquid inlet and a slurry outlet, the pharmaceutical production waste liquid enters the mixing tank 4 through the waste liquid inlet, the slurry outlet is communicated with the feed inlet of the conical settling chamber 1, and the slurry outlet is also communicated with the inlet of the finished product tank 8, the finished product tank 8 is used to contain enriched liquid with a concentration up to standard, and a valve is arranged at the inlet of the finished product tank 8; As shown in the accompanying drawings Figure 2 The chamber of the conical settling chamber 1 is formed by two conical bodies, the lower conical body has a downward pointed end, the upper conical body has an upward pointed end, the bottom circumferences of the two conical bodies are fixedly connected, the central axes of the two conical bodies coincide, the feed inlet of the conical settling chamber 1 is arranged on the surface of the upper conical body, a valve is arranged at the feed inlet of the conical settling chamber 1, the feed inlet is a tangential feed inlet so that the slurry is injected into the conical settling chamber 1 along a direction tangent to the side wall of the upper conical body, the slurry forms a stable downward spiral vortex in the chamber, a plurality of compressed air injection holes are uniformly arranged at the bottom of the conical settling chamber 1, the air injected by the plurality of compressed air injection holes forms a rotating upward airflow, which forms a 50°-55° collision angle with the liquid vortex to enhance the collision and agglomeration of particles (such as drug microcrystals and excipient particles) in the drug waste liquid and accelerate the sedimentation of large particles, a large particle collection port for collecting large particle impurities in the liquid is arranged at the bottom end of the conical settling chamber 1, a transition port is arranged on the upper conical body, the transition port communicates with the suspension inlet of the pulse backflush membrane module 2, the transition port is above the compressed air injection holes, and the suspension containing medium and small particles flows to the pulse backflush membrane module 2 through the transition port.

[0023] The pulse backflush membrane module 2 is provided with a suspension inlet, a first enriched liquid outlet and a solution permeate outlet, the modular membrane package 3 is provided with a solution inlet, a second enriched liquid outlet and a high-concentration solvent outlet, the suspension inlet communicates with the transition port, the first enriched liquid outlet communicates with the enriched liquid inlet of the mixing tank 4, the solution permeate outlet of the pulse backflush membrane module 2 communicates with the solution inlet of the modular membrane package 3, the second enriched liquid outlet communicates with the enriched liquid inlet of the mixing tank 4, and the high-concentration solvent outlet communicates with the inlet of the solvent recovery tank 9.

[0024] The outlet of the micro vacuum pump 11 communicates with the mixing tank 4 and the pulse backflush membrane module 2 to maintain a negative pressure working environment of the system, in order to stabilize the system operating pressure and protect the micro vacuum pump 11, in the embodiment, the outlet of the micro vacuum pump 11 communicates with the inlet of the vacuum buffer tank 1101, and the outlet of the vacuum buffer tank 1101 communicates with the mixing tank 4 and the pulse backflush membrane module 2.

[0025] The slurry outlet of the mixing tank 4 is communicated with the inlet of the product tank 8 and the feed inlet of the conical sedimentation chamber 1 through a discharge pipe, and a concentration detector 6 is arranged on the discharge pipe. The concentration detector 6 is used to detect the concentration of the small and medium-sized particulate matters in the slurry. A control unit 7 controls the opening degree of the valve at the inlet of the product tank 8, the opening degree of the valve at the feed inlet of the conical sedimentation chamber 1 and the negative pressure of the pulse backflush membrane assembly 2 according to the detection result of the concentration detector 6. The concentration threshold value is set in the control unit 7, which is determined according to the drug recovery requirements. In this embodiment, the concentration threshold value of the small and medium-sized particulate matters in the slurry is 5%-15% of the solid content. The control unit 7 compares the detection result of the concentration detector 6 with the set concentration threshold value. If the concentration of the slurry is within the concentration threshold value, the valve at the inlet of the product tank 8 is opened, the valve at the feed inlet of the conical sedimentation chamber 1 is closed, and the slurry meeting the requirements is discharged into the product tank 8. If the concentration of the slurry is higher than the concentration threshold value, the valve at the inlet of the product tank 8 is closed, the valve at the feed inlet of the conical sedimentation chamber 1 is opened, and the negative pressure of the pulse backflush membrane assembly 2 is reduced to-0.03--0.04MPa to slow down the filtration speed and dilute the slurry. If the concentration of the slurry is lower than the concentration threshold value, the valve at the inlet of the product tank 8 is closed, the valve at the feed inlet of the conical sedimentation chamber 1 is opened, and the negative pressure of the pulse backflush membrane assembly 2 is increased to-0.05--0.06MPa to accelerate the liquid to pass through the membrane and concentrate the slurry. The regulation time of the control unit 7 is less than 5S.

[0026] In this embodiment, the concentration detector 6 is a micro online refractometer. The micro online refractometer detects the refractive index of the drug waste liquid in real time, and converts the concentration through a pre-set calibration curve (obtained based on the correlation experiment between the target solute concentration in the slurry and the refractive index). The measurement range of the micro online refractometer is 0-30% Brix, the accuracy is ±0.05% Brix, and the material is 316L stainless steel.

[0027] The diameter of the feed inlet of the conical sedimentation chamber 1 is 15-25mm, and the speed of the slurry entering the conical sedimentation chamber 1 is 10-12m / s. A 100-mesh filter screen is arranged at the feed inlet of the conical sedimentation chamber 1 to preliminarily intercept the possible large impurities (such as drug residue clumps) in the drug waste liquid. In order to ensure the speed of the slurry entering the conical sedimentation chamber 1, a booster pump 12 is arranged at the slurry outlet of the mixing tank 4.

[0028] The number of compressed air injection holes is 6-8, and the diameter of the compressed air injection hole is 1.5-2.5mm. The compressed air injection hole is communicated with a micro air compressor, and the output pressure of the micro air compressor is 0.4-0.6Mpa.

[0029] The diameter of the large particle collection port is 20-30mm. A periodically operating miniature start valve is installed at the large particle collection port to periodically discharge settled large particle impurities. The periodic operation time of the miniature start valve is less than 0.5 seconds. The distance between the transition port and the bottom of the conical settling chamber 1 is 150-200mm, and the diameter of the transition port is 20-30mm.

[0030] The cone angle of the lower cone in the conical settling chamber 1 is 65°-75°, the height of the conical settling chamber 1 is 300-500mm, and the maximum diameter of the conical settling chamber 1 is 180-250mm. The material of the conical settling chamber 1 is 316L stainless steel, which is resistant to corrosion by pharmaceutical waste liquid, or polytetrafluoroethylene, which is suitable for strong solvent pharmaceutical waste liquid. A square cavity is set at the apex of the upper cone in the conical settling chamber 1 to enhance the vortex collision within the conical settling chamber 1.

[0031] As attached Figure 3 As shown, the pulse backflush membrane assembly 2 includes a cylindrical shell 201, inside which 100-200 silanized modified polyamide hollow fiber membrane filaments 202 are vertically packed. The separation layer of the hollow fiber membrane filaments is grafted with C10-C12 alkyl chains. The water contact angle is 115°-125°, and the swelling rate is <2% for commonly used solvents in drug production, including ethanol and dichloromethane. The cylindrical shell is connected to a micro vacuum pump 11. An annular micro gas chamber 203 is located at the top of the cylindrical shell. The annular micro gas chamber 203 has multiple downward-opening pores evenly distributed circumferentially. The annular micro gas chamber 203 is connected to a high-pressure micro gas pump. A timed solenoid valve is installed between the annular micro gas chamber 203 and the high-pressure micro gas pump. The suspension inlet is located at the bottom of the pulse backflush membrane assembly 2, and the first enriched liquid outlet and the solution permeate outlet are both located at the top of the pulse backflush membrane assembly 2. When the pulse backflush membrane module 2 is working, the negative pressure drives the suspension through the membrane layer, and small particles (such as drug small molecule impurities and colloidal particles) are trapped on the membrane surface to form a filter cake layer to complete the forward filtration. The annular micro gas chamber 203 is periodically introduced with high-pressure gas to reverse the pressure difference, efficiently peel off the filter cake layer, avoid the decrease in drug retention efficiency caused by membrane pore blockage, and the peeled filter cake dissolves into the suspension.

[0032] The cylindrical shell 201 has a diameter of 80-120 mm and a height of 200-300 mm. The diameter of the silanized modified polyamide hollow fiber membrane filaments is 0.6-0.8 mm, the pore size is 2-4 nm, and the effective filtration area is 0.8-1.5 m². The micro vacuum pump 11 provides a negative pressure range of -0.03 to 0.06 MPa to the pulse backflush membrane module 2, the pressure output by the high-pressure micro air pump is 0.8-1.0 MPa, the pulse frequency of the timing solenoid valve is 2-3 Hz, and the duration of a single backflush is 80-120 ms. To increase the speed at which the solvent permeate enters the modular membrane package 3, a booster pump 12 is installed between the solution permeate outlet of the pulse backflush membrane module 2 and the solution inlet of the modular membrane package 3.

[0033] As attached Figure 4 As shown, the modular membrane package 3 includes a rectangular shell 301 with dimensions of 150×80×50mm. Inside the rectangular shell 301, from top to bottom, are a support layer 302, a transition layer 303, and a separation layer 304. The support layer 302 is made of polyester nonwoven fabric with a diameter of 100-150μm and a thickness of 0.2-0.3mm. The tensile strength of the support layer 302 is >150N / cm. The support layer 302 is used to intercept impurities >100μm (such as drug residue and large-particle excipients) in drug waste. The transition layer 303 is made of polyimide nanofiber membrane with a thickness of 50-80μm and an average pore size of 30-40nm. The polyimide nanofiber membrane is prepared by electrospinning, and its surface charge density is - The transition layer 303, with a concentration of 0.8–1.0 mC / m², is used to adsorb colloidal particles (such as proteins and polymer impurities) in the pharmaceutical waste liquid. The separation layer 304 is a silanized polyamide layer with a thickness of 10–15 μm and a pore size of 2–4 nm. The silanized polyamide layer is grafted with C10 alkyl chains to form a molecular-level hydrophobic barrier, which blocks the interaction between commonly used solvents in pharmaceutical production (such as methanol and ethyl acetate) and the membrane substrate, while retaining small molecule impurities (<5 μm) to ensure that the purity of the recovered solvent is > 99.5%. The solution inlet is located at the top of the rectangular shell 301, the high-concentration solvent outlet is located at the bottom of the rectangular shell 301, and the second enrichment liquid outlet is located between the transition layer 303 and the separation layer 304.

[0034] In order to temporarily store the obtained high-concentration solvent and balance the flow fluctuation of the high-concentration solvent, a drain tank 10 is arranged between the modular membrane package 3 and the solvent recovery tank 9, the inlet of the drain tank 10 communicates with the high-concentration solvent outlet of the modular membrane package 3, the outlet of the drain tank 10 communicates with the inlet of the solvent recovery tank 9, the volume of the drain tank 10 is 5-10 L, a capacitive low-level meter 1004 is arranged at the lower side of the drain tank 10, and an ultrasonic high-level meter 1003 is arranged at the upper side of the drain tank 10; the distance between the capacitive low-level meter 1004 and the lower end of the drain tank 10 is 30-50 mm, which is used to contact type detection of the residual liquid layer thickness at the bottom of the drain tank 10, so as to control the residual amount in the drain tank 10 to be not less than 50 mL; the distance between the ultrasonic high-level meter 1003 and the upper end of the drain tank 10 is 50-80 mm, and the ultrasonic high-level meter 1003 is used to non-contact monitoring of the liquid surface peak value, so as to avoid direct contact with the drug waste liquid to cause pollution. A large water pump 1001 and a small water pump 1002 are arranged in parallel between the outlet of the drain tank 10 and the inlet of the solvent recovery tank 9, the flow of the large water pump 1001 is greater than that of the small water pump 1002, the inlets of the large water pump 1001 and the small water pump 1002 communicate with the outlet of the drain tank 10, and the outlets of the large water pump 1001 and the small water pump 1002 communicate with the inlet of the solvent recovery tank 9; from top to bottom, the drain tank 10 is sequentially provided with a high-level liquid level threshold, a transition liquid level and a low-level liquid level threshold, in the embodiment, the volume below the high-level liquid level threshold accounts for 80% of the tank volume of the drain tank 10, the volume below the transition liquid level accounts for 30% of the tank volume of the drain tank 10, and the volume below the low-level liquid level threshold accounts for 20% of the tank volume of the drain tank 10; when the liquid level in the drain tank 10 is between the high-level liquid level threshold and the transition liquid level, the ultrasonic high-level meter 1003 is triggered, and when the liquid level in the drain tank 10 is lower than the low-level liquid level threshold, the capacitive low-level meter 1004 is triggered; when the ultrasonic high-level meter 1003 is continuously triggered and the capacitive low-level meter 1004 is not triggered, it is determined that the drain tank 10 is in a true full-liquid state, the large water pump 1001 is started to work, and the liquid in the drain tank 10 is quickly discharged, so as to avoid overflow of the drain tank 10; when the liquid level in the drain tank 10 is lower than the transition liquid level and higher than the low-level liquid level threshold, neither the ultrasonic high-level meter 1003 nor the capacitive low-level meter 1004 is triggered, the large water pump 1001 stops working, and the small water pump 1002 works, so as to slowly discharge the liquid in the drain tank 10; when the liquid level in the drain tank 10 is at the low-level liquid level threshold, the ultrasonic high-level meter 1003 is not triggered and the capacitive low-level meter 1004 is triggered, then the large water pump 1001 and the small water pump 1002 both stop working, and the drain of the drain tank 10 is closed, so as to retain the liquid seal at the bottom of the tank to maintain the negative pressure (-0.03--0.05 MPa) of the drain tank 10. A one-way check valve is arranged at the outlet of the large water pump 1001 and the small water pump 1002, so as to avoid liquid backflow in the negative pressure environment and cross contamination.

[0035] In this embodiment, the measurement accuracy of the capacitive low-level meter is ±0.5 mm, and the material is PTFE. The measurement accuracy of the ultrasonic high-level meter is ±1 mm, and the range is 0-500 mm. The large water pump 1001 is a micro pneumatic diaphragm pump. The flow rate of the large water pump 1001 is 50-100 L / h, and the lift is 5-8 m. The small water pump 1002 is a micro gear pump. The flow rate of the small water pump 1002 is 10-20 L / h, and the lift is 3-5 m. The materials of the large water pump 1001 and the small water pump 1002 are both 316L stainless steel to prevent corrosion by the drug waste liquid.

[0036] A U-shaped siphon 5 is provided between the first concentrate outlet of the pulse backflush membrane assembly 2 and the concentrate inlet of the mixing tank 4. The U-shaped siphon 5 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 concentrate outlet communicates with the high-level port of the U-shaped siphon 5. The second concentrate outlet of the modular membrane package 3 also communicates with the high-level port of the U-shaped siphon. The low-level port communicates with the concentrate inlet of the mixing tank 4. By providing the U-shaped siphon, the concentrate automatically flows back to the mixing tank 4 under the action of system negative pressure (-0.02--0.04 MPa). The present particulate concentrate is transported without mechanical impeller shearing.

[0037] A vacuum break valve with an opening pressure of -0.01 MPa is provided at the top of the U-shaped siphon 5 to prevent liquid backflow when the system negative pressure is abnormal. A one-way valve is provided at the low-level port to prevent the liquid in the mixing tank 4 from flowing back to the U-shaped siphon. The diameter of the U-shaped siphon is 10-15 mm, and the material is PTFE.

[0038] In this embodiment, the working principle of the drug production waste liquid separation and recovery system is as follows: A portion of the drug production waste liquid enters the mixing tank 4 and then enters the conical sedimentation chamber 1 through the booster pump 12. The waste liquid is separated into large particulate impurities and a suspension containing small and medium-sized particles in the conical sedimentation chamber 1. The suspension enters the pulse backflush membrane assembly 2 and is separated into a concentrate containing small and medium-sized particles and a solvent permeate. The solvent permeate enters the modular membrane package 3 and is separated into a concentrate and a high-concentration solvent with a concentration of up to 99.5%. The high-concentration solvent enters the solvent recovery tank 9 through the drain tank 10. The high-concentration solvent in the solvent recovery tank 9 is used for solvent recovery. The concentrate separated by the pulse backflush membrane assembly 2 and the concentrate separated by the modular membrane package 3 re-enter the mixing tank 4. The concentration detector detects the concentrate discharged from the mixing tank 4. If the concentrate concentration meets the standard, it enters the finished product tank 8. The concentrate in the finished product tank 8 is used to recover antibiotics, etc. If the concentrate concentration does not meet the standard, it re-enters the conical sedimentation chamber 1 to start a new round of separation and filtration until the concentrate concentration meets the standard and enters the finished product tank 8. New drug production waste liquid re-enters the mixing tank 4 to start separation and recovery. The concentrate in the finished product tank 8 can be used to extract antibiotics, and the high-concentration solvent in the solvent recovery tank 9 can be used to extract IPA (isopropyl alcohol).

[0039] It should be noted that the above examples are only used to illustrate the technical solutions of the present application but not to limit the present application; although the present application has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the specific implementation of the present application can be modified or some technical features can be replaced by equivalent; without departing from the spirit of the technical solutions of the present application, they should be covered in the technical solution range of the present application claimed.

Claims

1. A pharmaceutical production waste liquid separation and recovery system, characterized in that, The system includes a conical settling chamber, a pulse backflush membrane assembly, a modular membrane pack, a mixing tank, and a micro vacuum pump. The mixing tank is used to contain drug waste liquid or enrichment liquid. The slurry in the mixing tank is discharged into the conical settling chamber, which is used to separate the slurry into large particulate impurities and a suspension. The suspension contains medium and small particles. The pulse backflush membrane assembly is used to separate the suspension into an enrichment liquid and a solvent permeate. The modular membrane pack is used to separate the solvent permeate into an enrichment liquid and a high-concentration solvent. Large particulate impurities refer to substances with a diameter >50μm, medium particles are substances with a diameter of 5-50μm, and small particles are substances with a diameter <50μm. The mixing tank is equipped with a waste liquid inlet, an enrichment liquid inlet, and a slurry outlet. The pharmaceutical production waste liquid enters the mixing tank through the waste liquid inlet. The slurry outlet is connected to the feed inlet of the conical settling chamber. The slurry outlet is also connected to the inlet of the finished product tank. The finished product tank is used to contain the enrichment liquid with the required concentration. A valve is installed at the inlet of the finished product tank. The conical settling chamber is formed by two cones, an upper cone and an lower cone. The pointed end of the lower cone faces downwards, and the pointed end of the upper cone faces upwards. The bottom surfaces of the two cones are circumferentially connected, and their central axes coincide. The inlet of the conical settling chamber is located on the surface of the upper cone. A valve is installed at the inlet, which is tangential, allowing the slurry to be sprayed into the conical settling chamber tangentially to the side wall of the upper cone. The slurry forms a stable downward spiral vortex within the chamber. The bottom of the conical settling chamber is uniformly provided with multiple compressed air nozzles. The air jets from the multiple compressed air nozzles rotate and rise, forming a collision angle of 50°-55° with the liquid vortex. The bottom of the conical settling chamber is provided with a large particle collection port for collecting large particulate impurities in the liquid. The upper cone is provided with a transition port, which is connected to the suspension inlet of the pulse backflush membrane module. The transition port is above the compressed air nozzles. The suspension containing medium and small particles flows to the pulse backflush membrane module through the transition port. The pulse backflush membrane assembly is provided with a suspension inlet, a first enriched liquid outlet, and a solution permeate outlet. The modular membrane package is provided with a solution inlet, a second enriched liquid outlet, and a high-concentration solvent outlet. The suspension inlet is connected to the transition port, the first enriched liquid outlet is connected to the enriched liquid inlet of the mixing tank, the solution permeate outlet of the pulse backflush membrane assembly is connected to the solution inlet of the modular membrane package, the second enriched liquid outlet is connected to the enriched liquid inlet of the mixing tank, and the high-concentration solvent outlet is connected to the inlet of the solvent recovery tank. The outlet of the micro vacuum pump is connected to the mixing tank and the pulse backflush membrane assembly.

2. The separation and recovery system according to claim 1, characterized in that, The outlet of the micro vacuum pump is connected to the inlet of the vacuum buffer tank, and the outlet of the vacuum buffer tank is connected to the mixing tank and the pulse backflush membrane assembly.

3. The separation and recovery system according to claim 1, characterized in that, It also includes a control unit. The slurry outlet of the mixing tank is connected to the inlet of the finished product tank and the feed inlet of the conical settling chamber through a drain pipe. A concentration detector is installed on the drain pipe to detect the concentration of small and medium-sized particles in the slurry. The control unit controls the opening of the valve at the inlet of the finished product tank, the opening of the valve at the feed inlet of the conical settling chamber, and the negative pressure of the pulse backflushing membrane assembly based on the detection results of the concentration detector. The control unit is set with a concentration threshold. The control unit compares the detection results of the concentration detector with the set concentration threshold. If the slurry concentration is within the concentration threshold range, the valve at the inlet of the finished product tank is opened and the valve at the feed inlet of the conical settling chamber is closed, and the slurry that meets the requirements is discharged into the finished product tank. If the slurry concentration is higher than the concentration threshold, the valve at the inlet of the finished product tank is closed and the valve at the feed inlet of the conical settling chamber is opened, and the negative pressure of the pulse backflushing membrane assembly is reduced. If the slurry concentration is lower than the concentration threshold, the valve at the inlet of the finished product tank is closed and the valve at the feed inlet of the conical settling chamber is opened, and the negative pressure of the pulse backflushing membrane assembly is increased.

4. The separation and recovery system according to claim 3, characterized in that, The diameter of the feed inlet of the conical settling chamber is 15-25mm, and the velocity of the slurry entering the conical settling chamber is 10-12m / s. A filter screen is installed at the feed inlet of the conical settling chamber, and a booster pump is installed at the slurry outlet of the mixing tank. The number of compressed air nozzles is [number missing], and the diameter of the compressed air nozzles is 1.5-2.5mm. The compressed air nozzles are connected to a micro air compressor, and the output pressure of the micro air compressor is 0.4-0.6Mpa. The diameter of the large particle collection port is 20-30mm, and a periodically operating micro start valve is installed at the large particle collection port. The periodic operation time of the micro start valve is less than 0.5S. The distance between the transition port and the bottom of the conical settling chamber is 150-200mm, and the diameter of the transition port is 20-30mm.

5. The separation and recovery system according to claim 4, characterized in that, 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 material of the conical settling chamber is 316L stainless steel or polytetrafluoroethylene, and a square cavity is provided at the apex of the upper cone in the conical settling chamber.

6. The separation and recovery system according to claim 4, characterized in that, The pulse backflush membrane assembly includes a cylindrical shell, inside which 100-200 silanized modified polyamide hollow fiber membrane filaments are vertically packed. The separation layer of the hollow fiber membrane filaments is grafted with C10-C12 alkyl chains. The water contact angle is 115°-125°, and the swelling rate is <2% for commonly used solvents in drug production, including ethanol and dichloromethane. The cylindrical shell is connected to a micro vacuum pump. An annular micro gas chamber is provided at the top of the cylindrical shell. The annular micro gas chamber has multiple downward-opening pores evenly arranged circumferentially. The annular micro gas chamber is connected to a high-pressure micro gas pump. A timed solenoid valve is provided between the annular micro gas chamber and the high-pressure micro gas pump. The suspension inlet is located at the bottom of the pulse backflush membrane assembly, and the first enriched liquid outlet and the solution permeate outlet are both located at the top of the pulse backflush membrane assembly.

7. The separation and recovery system according to claim 6, characterized in that, The cylindrical shell has a diameter of 80-120mm and a height of 200-300mm. The silanized modified polyamide hollow fiber membrane filaments have a diameter of 0.6-0.8mm and a hollow pore size of 2-4nm, with an effective filtration area of ​​0.8-1.5m². The micro vacuum pump provides a negative pressure range of -0.03 to 0.06MPa to the pulse backflush membrane module, the high-pressure micro air pump outputs a pressure of 0.8-1.0MPa, the pulse frequency of the timer solenoid valve is 2-3Hz, and the duration of a single backflush is 80-120ms. A booster pump is installed between the solution permeate outlet of the pulse backflush membrane module and the solution inlet of the modular membrane package.

8. The separation and recovery system according to claim 6, characterized in that, The modular membrane package includes a rectangular shell, within which a support layer, a transition layer, and a separation layer are sequentially arranged from top to bottom. The support layer is made of polyester nonwoven fabric with a diameter of 100-150 μm and a thickness of 0.2-0.3 mm, with a tensile strength > 150 N / cm. The transition layer is made of polyimide nanofiber membrane with a thickness of 50-80 μm, an average pore size of 30-40 nm, and is prepared by electrospinning. The surface charge density of the polyimide nanofiber membrane is -0.8 to -1.0 mC / m². The separation layer is a silanized polyamide layer with a thickness of 10-15 μm and a pore size of 2-4 nm. The silanized polyamide layer is grafted with C10 alkyl chains to form a molecular-level hydrophobic barrier. The solution inlet is located at the top of the rectangular shell, the high-concentration solvent outlet is located at the bottom of the rectangular shell, and the second enrichment liquid outlet is located between the transition layer and the separation layer.

9. The separation and recovery system according to claim 6, characterized in that, A drain tank is installed between the modular membrane pack and the solvent recovery tank. The inlet of the drain tank is connected to the high-concentration solvent outlet of the modular membrane pack, and the outlet of the drain tank is connected to the inlet of the solvent recovery tank. A capacitive low-level gauge is installed on the lower side of the drain tank, and an ultrasonic high-level gauge is installed on the upper side. The distance between the capacitive low-level gauge and the lower end of the drain tank is 30-50mm, which is used to detect the thickness of the residual liquid layer at the bottom of the drain tank in a contact manner, thereby controlling the residual amount in the drain tank. The distance between the ultrasonic high-level gauge and the upper end of the drain tank is 50-80mm. The ultrasonic high-level gauge is used to monitor the peak liquid level non-contactly, avoiding direct contact with the drug waste liquid and causing contamination. A large water pump and a small water pump are connected in parallel between the outlet of the drain tank and the inlet of the solvent recovery tank. The flow rate of the large water pump is greater than that of the small water pump. The inlets of both the large and small water pumps are connected to the outlet of the drain tank, and the outlets of both the large and small water pumps are connected to the inlet of the solvent recovery tank. The drain tank is arranged from top to bottom. The system is equipped with high-level, transitional, and low-level liquid thresholds. When the liquid level in the drain tank is between the high-level and transitional thresholds, an ultrasonic high-level gauge is triggered. When the liquid level is below the low-level threshold, a capacitive low-level gauge is triggered. When the ultrasonic high-level gauge is continuously triggered and the capacitive low-level gauge is not triggered, the drain tank is determined to be truly full, and the large water pump is activated to quickly drain the liquid from the drain tank to prevent overflow. When the liquid level in the drain tank is below the transitional level but above the low-level threshold, neither the ultrasonic high-level nor the capacitive low-level gauge is triggered, the large water pump stops working, and the small water pump operates to slowly drain the liquid from the drain tank. When the liquid level in the drain tank is at the low-level threshold, the ultrasonic high-level gauge is not triggered, but the capacitive low-level gauge is triggered, both the large and small water pumps stop working, and the drain tank's drainage is shut off. One-way check valves are installed at the outlets of both the large and small water pumps.

10. The separation and recovery system according to claim 6, characterized in that, A U-shaped siphon is provided between the first enrichment outlet of the pulse backflushing membrane assembly and the enrichment inlet of the mixing tank. The U-shaped siphon has a high-level port and a low-level port, with the high-level port being higher than the low-level port. The first enrichment outlet is connected to the high-level port of the U-shaped siphon, and the second enrichment outlet of the modular membrane package is also connected to the high-level port of the U-shaped siphon. The low-level port is connected to the enrichment inlet of the mixing tank.

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