CN113797583A - Extraction pilot test method based on bulk drug centrifugal solvent extraction system - Google Patents
Extraction pilot test method based on bulk drug centrifugal solvent extraction system Download PDFInfo
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0207—Control systems
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0215—Solid material in other stationary receptacles
- B01D11/0223—Moving bed of solid material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
- B01D11/0284—Multistage extraction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0292—Treatment of the solvent
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Automation & Control Theory (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention belongs to the technical field of solvent extraction, and particularly relates to an extraction pilot test method based on a bulk drug centrifugal solvent extraction system. The extraction pilot test method comprises an extraction system, wherein a light phase inlet of a centrifugal extractor of the extraction system is communicated to an outlet end of a solvent storage tank through a solvent feeding pump, and a heavy phase inlet of the centrifugal extractor is communicated to an outlet end of a material blending tank through a material feeding pump; the light phase outlet of the centrifugal extractor is communicated with the inlet end of the loaded organic phase storage tank, the heavy phase outlet of the centrifugal extractor is communicated with the inlet end of the raffinate storage tank, the outlet end of the raffinate storage tank is communicated with the pumping end of the material feeding pump, and the extraction system further comprises an intermediate storage tank; the extraction pilot-plant process can be carried out based on the extraction system. The invention takes the centrifugal extractor with pilot scale throughput model as the core of the system, can reliably and rapidly complete the extraction pilot process and obtain the optimal value of the extraction stage number.
Description
Technical Field
The invention belongs to the technical field of solvent extraction, and particularly relates to an extraction pilot test method based on a bulk drug centrifugal solvent extraction system.
Background
A drug substance, api (active Pharmaceutical ingredient), refers to any substance or mixture of substances used in the manufacture of drugs, and when used in the preparation of drugs, it becomes an active ingredient of the drugs. The raw material medicaments are mainly used as raw materials of various patent medicaments or preparations, are basic components of the patent medicaments or the preparations, but cannot be directly taken by patients, and are mostly powder, crystals, extractum and the like prepared by chemical synthesis, plant extraction or biotechnology.
The chemical synthesis of raw material medicine generally consists of production processes of multistep chemical reaction, physical treatment of some materials and the like, and production operation units are relatively complex and relate to reaction, extraction, decoloration, filtration, crystallization, centrifugation, drying and the like. The centrifugal solvent extraction integrates two operation units of mixing mass transfer and centrifugal separation, can replace the traditional stirring tank, reaction kettle, mixing tank and settling tank, realizes closed, continuous and quick operation, has the advantages of high extraction efficiency, high phase equilibrium speed, low solvent consumption and the like, and becomes a new trend of technical development. Before a centrifugal solvent extraction process is applied to replace the traditional gravity settling process (equipment mainly comprises a stirring tank, a reaction kettle, a mixing tank, a settling tank and the like), most of raw material medicine enterprises need small and medium tests. The bench test is generally carried out in a laboratory, and the materials are either actual materials in production or materials obtained by mixing and simulating reagents in proportion, namely alternative test materials, and the aim is to explore reaction mechanisms, process flows, process parameters, process characteristics and the like. The pilot plant test is mostly carried out in a workshop, and directly enters a production link, and an upstream working section and a downstream working section are linked by using actual materials and production parameters, so that the production process, the operation parameters, the actual effect and the like are searched. In production, because of various raw material medicines, complicated production links, scattered workshop sections, high integration level required for a centering and testing device, convenient and quick access or detachment of the production workshop sections, rich test units, small occupied space and the like. Meanwhile, most of the main chemical raw materials for synthesizing the bulk drugs are listed in a list of dangerous chemicals which are monitored in an important way, such as inorganic compounds like sodium hydroxide, sulfuric acid, aluminum trichloride, ammonia and the like, and organic compounds like formic acid, diethyl ester, phenol, acetaldehyde, nitrobenzene and the like; moreover, the extractant used as the reactant carrier, such as toluene, ether, acetone, ethanol, chloroform, ethyl acetate, etc., is also mostly flammable and explosive, corrosive, toxic, etc., so that the factory area of the bulk drug factory is mostly flammable and explosive class A factory buildings and warehouses, and the safety risk is extremely high. According to relevant specifications, raw material medicine production equipment needs to meet the requirement of full process automation; therefore, the centrifugal extraction pilot plant also needs to realize full process automation from the aspect of intrinsic safety, and comprehensive consideration is given to the aspects of automatic control, process monitoring, data monitoring, safety interlocking, emergency refuge and unloading and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an extraction pilot test method based on a bulk drug centrifugal solvent extraction system, which takes a pilot test scale throughput type centrifugal extractor as a system core and can reliably and quickly complete an extraction pilot test flow and obtain an optimal value of extraction stages.
In order to achieve the purpose, the invention adopts the following technical scheme:
an extraction pilot test method based on a bulk drug centrifugal solvent extraction system is characterized by comprising an extraction system, wherein the extraction system comprises a centrifugal extractor, a light phase inlet of the centrifugal extractor is communicated to an outlet end of a solvent storage tank through a solvent feed pump, and a heavy phase inlet of the centrifugal extractor is communicated to an outlet end of a material blending tank through a material feed pump; a light phase outlet of the centrifugal extractor is communicated with an inlet end of the loaded organic phase storage tank, a heavy phase outlet of the centrifugal extractor is communicated with an inlet end of the raffinate storage tank, and an outlet end of the raffinate storage tank is communicated with a pumping end of the material feeding pump; the extraction system also comprises an intermediate storage tank, wherein the intermediate storage tank and the loaded organic phase storage tank form a parallel pipeline so as to be communicated with a light phase outlet of the centrifugal extractor through a branch switch valve; the extraction system also comprises a liquid level meter and a thermometer T which are used for correspondingly monitoring the current states of the solvent storage tank, the material blending tank, the loaded organic phase storage tank, the raffinate storage tank and the intermediate storage tank, wherein flow meters F are arranged on sections of pipelines at the pump-out ends of the material feeding pump and the solvent feeding pump; a pH meter for monitoring the current pH value of the internal liquid is also arranged at the material blending tank; each pipeline is provided with a pipeline switch valve for opening and closing the corresponding pipeline;
the operation flow of the extraction pilot test method is as follows:
1) the extractant enters a solvent storage tank, is displayed in real time through a liquid level meter arranged on a tank body of the solvent storage tank, and stops feeding and controls the temperature when the volume of the extractant in the tank body reaches a specified liquid level;
2) the materials enter a material preparation tank, and feeding is stopped when the volume of preorder reaction liquid in the tank body reaches a specified liquid level through a liquid level meter arranged on the tank body of the material preparation tank; then, adding acid or alkali to adjust the pH value of the material;
3) pumping the prepared material in the step 2) into a centrifugal extractor by a material feeding pump, preliminarily setting the material feeding amount according to the machine type of the used centrifugal extractor, controlling the flow by a flowmeter, pumping an extracting agent into the centrifugal extractor by a solvent feeding pump when liquid flows out from a heavy phase outlet of the centrifugal extractor, controlling the phase comparison of two phases, extracting and separating the two phases, and sampling and analyzing after the two phases are stable;
4) repeating the step 3), keeping the material feeding amount unchanged, changing the feeding amount of the extracting agent to change the phase ratio of the two phases, sampling and analyzing, and comparing to determine the optimal phase ratio of the two phases;
5) under the condition that the material process condition and the two-phase ratio are determined, carrying out primary extraction according to the extraction operation, enabling the loaded organic phase subjected to primary extraction to enter a loaded organic phase storage tank, and carrying out sampling analysis on raffinate in the raffinate storage tank to finish primary extraction operation; through pipeline switching, pumping the primary raffinate from a raffinate storage tank into a centrifugal extractor through a material feeding pump for secondary extraction, and allowing the loaded organic phase after the secondary extraction to enter an intermediate storage tank; repeating the steps, and comparing the impurity content analysis results of the raffinate all times after repeating the specified times, thereby obtaining the optimal value of the extraction stages.
Preferably, the heights of the inlet ends of the loaded organic phase storage tank, the raffinate storage tank and the intermediate storage tank are lower than the heights of the corresponding heavy phase outlet and the light phase outlet which are communicated with the loaded organic phase storage tank, the raffinate storage tank and the intermediate storage tank, so that the light phase effluent and the heavy phase effluent enter the corresponding tanks in a self-flowing mode.
Preferably, the loaded organic phase storage tank, the raffinate storage tank and the intermediate storage tank are all horizontal tank bodies.
Preferably, a solvent storage tank, a material blending tank, a loaded organic phase storage tank, a raffinate storage tank and an intermediate storage tank are all provided with washing liquid inlets, and the solvent storage tank is also provided with an organic solvent inlet; the material preparation tank is also provided with a material inlet and a hydrochloric acid inlet, and the hydrochloric acid inlet is communicated with an outlet of an acid-base metering tank for adding and metering hydrochloric acid; the stirring assembly used for playing an internal stirring function is arranged in the material blending tank, and comprises a stirring paddle and a power source for driving the stirring paddle to generate a stirring action.
Preferably, the tank bodies of the solvent storage tank, the material blending tank, the loaded organic phase storage tank, the raffinate storage tank and the intermediate storage tank are designed in a hollow sandwich mode, and hollow jackets of the tank bodies are communicated with external medium equipment through a heat medium inlet and outlet pipe and/or a refrigerant inlet and outlet pipe.
Preferably, a pipeline filter is further arranged on a section of pipeline at the pump-out end of the material feeding pump and the solvent feeding pump; pipeline sight glass and sampling ports are respectively arranged at the heavy phase outlet and the light phase outlet; the solvent storage tank, the material blending tank, the loaded organic phase storage tank, the raffinate storage tank and the intermediate storage tank are respectively provided with a sanitary breather valve inside the communicating tank, and each tank body is respectively provided with a rotary cleaning nozzle used for cleaning the environment inside the tank.
Preferably, the solvent storage tank, the material blending tank, the loaded organic phase storage tank, the raffinate storage tank, the intermediate storage tank, the corresponding pump, the switch valve and the central control assembly are all arranged on the prying frame.
Preferably, the skid-mounted frame is provided with a leaked liquid collecting tank which is in the shape of an annular groove and is used for collecting leaked liquid falling onto the panel of the skid-mounted frame; and a leakage liquid emptying valve communicated with the leakage liquid collecting tank is also arranged on the prying frame.
Preferably, the centrifugal extractor comprises a rotor assembly module for generating a centrifugal force field and realizing a mixing and separating function and a rack shell module for realizing material storage, collection, guidance and separation of each phase, and the two groups of modules are connected with each other through quick-opening bolts.
Preferably, the rack housing module is provided with a guide pin which facilitates the rotor assembly module to be inserted and pulled in a centering manner along the vertical direction.
Preferably, the solvent reservoir temperature is maintained at 26 ℃.
The invention has the beneficial effects that:
1) by adopting the scheme, the centrifugal solvent extraction purpose is realized by taking a pilot scale throughput type centrifugal extractor as a system core; of course, during actual operation, test units such as back extraction, washing, saponification and the like can be naturally formed, so that the aim of one-machine multi-purpose operation of integration and modularization is fulfilled. In actual operation, a material blending tank is arranged at the feed end of the preorder reaction liquid, and the pH value of the material can be blended. The material blending tank pumps the blended preorder reaction liquid into the centrifugal extractor through a material output pump. The solvent feed end is provided with a solvent storage tank for storing a certain amount of organic solvent; the solvent storage tank pumps the solvent into the centrifugal extractor through the solvent output pump. After centrifugal extraction operation, the raffinate flowing out of the heavy phase outlet automatically flows into a raffinate storage tank through gravity; the loaded organic phase flowing out from the light phase outlet also automatically flows into the loaded organic phase storage tank through gravity, and the primary extraction effect is realized. By arranging the intermediate storage tank, the invention not only can flexibly realize the purpose of multiple times of extraction, but also can realize the separate storage of each batch of liquid so as to achieve the maximization of functions.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention;
FIG. 2 is a front view of one embodiment of the present invention;
FIG. 3 is a top view of one embodiment of the present invention;
fig. 4 is a view showing a state of modular assembly of the centrifugal extractor.
The actual correspondence between each label and the part name of the invention is as follows:
10-centrifugal extractor
11-rotor assembly module 12-rack housing module 13-quick-opening bolt 14-guide pin
20-solvent feed pump 30-Material feed pump
40-solvent storage tank 50-material blending tank 51-acid-base metering tank 52-stirring assembly
60-loaded organic phase storage tank 70-raffinate storage tank 80-intermediate storage tank
91-branch switch valve 92-heating medium inlet and outlet pipe 93-pipeline filter
94-pipeline sight glass 95-sampling port 96-sanitary breather valve 97-rotary cleaning spray head
98-prizing frame 98 a-leakage collecting tank 98 b-leakage emptying valve
Detailed Description
For ease of understanding, the specific structure and operation of the present invention is further described herein with reference to FIGS. 1-4:
the specific structure of the invention is shown in fig. 1-4, which takes a pilot-scale centrifugal extractor 10 as a core, and is a processing unit of a centrifugal solvent extraction process, materials and an extracting agent are mixed and transferred in the centrifugal extractor 10, and finally separation is realized, and the whole structure forms an extraction unit. Correspondingly, according to the difference of the operation flows, the same set of the invention can also be used as a back extraction unit, namely: the loaded organic phase and the stripping agent enter the centrifugal extractor 10. When the present invention is used as a washing unit, it is the material and detergent that enter the centrifugal extractor 10. When the present invention is used as a saponification unit, the material and saponifier are fed into the centrifugal extractor 10. That is, the centrifugal extractor 10 of the present invention can perform tests of various chemical engineering units according to the purpose of work.
In actual pilot plant test, the general treatment capacity is less than or equal to 1-3 m3Therefore, the centrifugal extractor 10 of the present invention can be selected to have the CTX150 and CTX250 specifications. Because most of the tested materials are corrosive, in order to ensure that the test adaptability of the invention is larger, the material of the contact part of the centrifugal extractor 10 and the materials is preferably steel-based sprayed with polytetrafluoroethylene, the sealing material is polytetrafluoroethylene, and the electrical appliance has the explosion-proof property; under the conditions, the centrifugal extractor 10 can have higher rotating speed, larger separation factor and wider test adjusting range. The centrifugal extractor 10 is arranged on the platform, and the height of the heavy phase outlet of the centrifugal extractor 10 is higher than that of the light phase outlet; during assembly, due to the design of the platform, the heights of the heavy phase outlet and the light phase outlet of the centrifugal extractor 10 are raised, and light and heavy phase outlet liquid can automatically flow into a corresponding storage tank, so that the conveying of a pump is avoided, and the whole system is compact. The heavy phase outlet and the light phase outlet are both provided with sampling ports 95, and the effluent can be sampled and analyzed in time in the test process; the heavy phase outlet and the light phase outlet are also provided with pipeline sight glasses 94, so that the liquid outlet condition can be checked in time in the test process, and the phase splitting effect can be known; the light phase inlet, the heavy phase outlet and the light phase outlet are all connected with the outside through hoses: firstly, avoid the vibration of centrifugal extraction machine 10 during operation to cause the influence to the pipeline, secondly make things convenient for the change, the connection of pipeline.
In order to further adapt to the characteristics of various raw material medicines, easy generation of intermediate phase in the extraction process and frequent internal cleaning, the centrifugal extractor 10 is designed in a modularized way, and as shown in fig. 4, the whole machine is divided into two parts, namely a rotor assembly module 11 and a frame shell module 12. The rotor assembly module 11 is a core assembly of the centrifugal extractor 10 and is used for generating a centrifugal force field and realizing mixing and separation; the rack housing module 12 is used for collecting and guiding each phase after material storage and separation and providing support for the whole machine. The rotor assembly module 11 and the rack housing module 12 are quickly connected by quick-opening bolts 13. To achieve rotor centering, guide pins 14 are also provided on the housing shell module 12. When the material variety is changed or a third phase appears in the interior of the centrifugal extractor in the test, and the centrifugal extractor needs to be thoroughly cleaned, the whole centrifugal extractor can be quickly opened, and the rotor assembly module 11 is lifted out of the rack shell module 12, so that the aim of quickly cleaning the interior of the centrifugal extractor 10 is fulfilled.
The solvent reservoir 40 may be vertical or horizontal for solvent monitoring. A thermometer is arranged at the tank body of the solvent storage tank 40, so that the temperature of the solvent in the tank can be monitored in real time; a liquid level meter is also arranged to monitor the liquid level of the solvent in the tank in real time; the tank top is provided with a sanitary breather valve 96, and the pressure in the tank can be kept balanced when the liquid level in the tank changes; the tank top is also provided with a rotary cleaning spray head 97 which can carry out omnibearing cleaning on the tank; the outer part of the tank body is provided with a jacket, and heat medium or refrigerant can be introduced through a heat medium inlet and outlet pipe 92 or a refrigerant inlet and outlet pipe, so that the materials in the tank body can be heated or cooled according to the process requirements.
In the extraction process, most materials need to be subjected to pH value adjustment; by adding a certain amount of acid or alkali and then stirring and mixing, the material blending tank 50 can achieve the purpose of adjusting the pH value. The material blending tank 50 is provided with a stirring component 52, and the stirring component 52 is explosion-proof, variable-frequency and adjustable in rotating speed and can be properly adjusted according to the process requirement; the tank body is provided with a thermometer T, so that the temperature of materials in the tank is monitored in real time; a liquid level meter is arranged to monitor the liquid level of the materials in the tank in real time; a pH meter is arranged to monitor the pH value in the tank in real time; the tank top is provided with a sanitary breather valve 96, and the pressure in the tank can be kept balanced when the liquid level in the tank changes; the tank top is also provided with a rotary cleaning spray head 97 which can carry out omnibearing cleaning on the tank; in order to add acid and alkali conveniently, the top of the tank is also provided with an acid and alkali metering tank 51, and the proper amount of acid and alkali can be quantitatively added into the tank by controlling the valve. In order to check the blending condition in the tank, the tank top is provided with a viewing mirror viewing port.
The inlet of the material feeding pump 30 is connected with the outlet of the material blending tank 50 through a pipeline, and the material blended in the material blending tank 50 is pumped to the heavy phase inlet of the centrifugal extractor 10 and enters the centrifugal extractor 10. A pipeline filter 93 and a flow meter F are sequentially arranged at a proper position of a pipeline between the outlet of the material feeding pump 30 and the heavy phase inlet. The pipeline filter filters and intercepts solid-phase substances possibly contained in the material, avoids damaging the flowmeter F, and also avoids entering the centrifugal extractor 10 to cause blockage of an internal flow passage and unclear phase splitting and equipment vibration. The type, medium material and filtering precision of the pipeline filter can be selected according to the specific material condition; the flowmeter F can be selected from a liquid turbine flowmeter, a vortex shedding flowmeter or an electromagnetic flowmeter and the like according to a specific flow range and material characteristics. In order to ensure the integral compactness of the system, the pipeline filter and the flowmeter are vertically arranged as much as possible.
The inlet of the solvent feed pump 20 is connected with the outlet of the solvent storage tank 40 through a pipeline, and the organic solvent in the solvent storage tank 40 is pumped to the light phase inlet of the centrifugal extractor 10 and enters the centrifugal extractor 10. As most organic solvents are flammable and explosive, the solvent feeding pump 20 can be a magnetic pump, a diaphragm pump and the like, so that the safety is ensured. A line filter and a flow meter are also provided in sequence in the line between the outlet of the solvent feed pump 20 and the inlet of the light phase. The pipeline filter filters and intercepts solid-phase substances possibly contained in the organic solvent, so that the flowmeter is prevented from being damaged, and the phenomenon that an internal flow passage is blocked to cause unclear phase splitting and equipment vibration when the solid-phase substances enter the centrifugal extractor 10 is also avoided. The type, medium material and filtering precision of the pipeline filter can be selected according to the specific material condition; the flowmeter can be selected from a liquid turbine flowmeter, a vortex shedding flowmeter and the like according to a specific flow range and material characteristics. Most organic solvents do not have conductivity or have extremely low conductivity, so an electromagnetic flowmeter is generally not selected for the flowmeter. In order to ensure the integral compactness of the system, the pipeline filter and the flowmeter are vertically arranged as much as possible.
The raffinate storage tank 70 is connected to the heavy phase outlet of the centrifugal extractor 10 through a pipeline, and after centrifugal separation, the raffinate enters the raffinate storage tank 70. The raffinate storage tank 70 can be vertical or horizontal, and in order to monitor the raffinate condition, a thermometer is arranged on the body of the raffinate storage tank 70 to monitor the temperature of the raffinate in the tank in real time; a liquid level meter is also arranged to monitor the liquid level of raffinate in the tank in real time; the tank top is provided with a sanitary breather valve 96, and the pressure in the tank can be kept balanced when the liquid level in the tank changes; the tank top is also provided with a rotary cleaning spray head 97 which can clean the tank in all directions. The centrifugal extractor 10 is lifted by the platform, which is necessary to ensure that the raffinate can automatically flow into the raffinate storage tank 70, and the connecting pipeline is smooth, so that back pressure phenomena such as sharp bend, diameter change, climbing and the like can not occur.
The loaded organic phase storage tank 60 is connected with the light phase outlet of the centrifugal extractor 10 through a pipeline. The organic solvent picks up solute from the material to form a loaded organic phase, which enters the loaded organic phase storage tank 60 after centrifugal separation. The loaded organic phase storage tank 60 can be vertical or horizontal, and in order to monitor the condition of the loaded organic phase, a thermometer is arranged on the tank body of the loaded organic phase storage tank 60 to monitor the temperature of the loaded organic phase in the tank in real time; a liquid level meter is also arranged to monitor the liquid level of the loaded organic phase in the tank in real time; the tank top is provided with a sanitary breather valve 96, and the pressure in the tank can be kept balanced when the liquid level in the tank changes; the tank top is also provided with a rotary cleaning spray head 97 which can clean the tank in all directions. The loaded organic phase storage tank 60 is also provided with a jacket for temperature regulation of the loaded organic phase. The centrifugal extractor 10 is lifted up by the platform, which ensures that the loaded organic phase can automatically flow into the loaded organic phase storage tank 60, and the connecting pipeline is smooth, and has no back pressure phenomena such as sharp bend, diameter change, climbing and the like.
When the centrifugal extractor 10 needs to implement a washing process, the solvent storage tank 40 contains a detergent, and the detergent washes the material to remove salts, impurities or other components from the material. The washing liquid enters the loaded organic phase storage tank 60 from the light phase outlet of the centrifugal extractor 10, and a washing process is completed. But when the washing is needed for a plurality of times, the washing liquid needs to be separately collected; other operational flows are similar, and therefore an intermediate storage tank 80 is added to make up the last part of the modularity of the present invention.
The intermediate storage tank 80 is also connected to the light phase outlet of the centrifugal extractor 10 by a line. The intermediate storage tank 80 can be vertical or horizontal, and for the condition of liquid phase in the tank, a thermometer is arranged on the tank body of the intermediate storage tank 80 to monitor the temperature of negative liquid phase in the tank in real time; a liquid level meter and the like are also arranged to monitor the liquid level of the liquid phase in the tank in real time; the tank top is provided with a sanitary breather valve 96, and the pressure in the tank can be kept balanced when the liquid level in the tank changes; the tank top is also provided with a rotary cleaning spray head 97 which can clean the tank in all directions. The intermediate tank 80 is also provided with a jacket for temperature regulation of the liquid phase in the tank. The centrifugal extractor 10 is lifted up by the platform, which is necessary to ensure that the liquid phase can automatically flow into the intermediate storage tank 80, and the connecting pipeline is smooth, and has no back pressure phenomena such as sharp bend, diameter change, climbing and the like. The light phase effluent enters the loaded organic phase storage tank 60 or the intermediate storage tank 80 and can be controlled by a pipeline switching valve.
The main devices of the solvent storage tank 40, the material blending tank 50, the material feeding pump 30, the solvent feeding pump 20, the raffinate storage tank 70, the centrifugal extractor 10, the intermediate storage tank 80, the loaded organic phase storage tank 60 and the like are organically connected together through pumps, pipelines, hoses, flow meters, pipe fittings, switch valves and the like to form the extraction system of the invention. For experimental convenience, whole extraction system installs on sled dress frame 98, and sled dress frame 98 possesses enough intensity and rigidity, convenient hoist and mount and transport. The control unit of the present invention is also mounted on the prying frame 98 to facilitate field operation. In the test process, materials are inevitably leaked, emitted and leaked; in order to prevent the leakage from polluting the environment, leakage collecting grooves 98a are formed around the skid-mounted frame 98. The leaked liquid collecting tank 98a is in the shape of an annular groove, and can collect leaked liquid falling onto the panel of the prying frame 98, and finally the leaked liquid emptying valve 98b can be opened to discharge the leaked liquid, which is specifically shown in fig. 2.
In actual work, the invention can realize various chemical unit operations through pipeline adjustment:
the material blending tank 50 can be used for blending materials with acid and base, and can also be used for blending organic solvents, such as diluting and blending organic solvents and sulfonated kerosene, and pumping the organic solvents into the solvent storage tank 40 through the solvent feeding pump 20 by virtue of pipelines for later use; the use of solvent feed pump 20 and even material feed pump 30 can be accomplished with line adjustments.
And (3) extraction operation: the material enters a material preparation tank 50 for standby, the extractant enters a solvent storage tank 40 for standby, the material is pumped to a heavy phase inlet of the centrifugal extractor 10 by a material feeding pump 30 according to a certain flow rate, and the extractant is pumped to a light phase inlet of the centrifugal extractor 10 by a solvent feeding pump 20 according to a certain flow rate. Mixing the material and the extractant in the centrifugal extractor 10 for mass transfer, allowing solute in the material to enter the extractant to form a loaded organic phase, and allowing the loaded organic phase to enter a loaded organic phase storage tank 60 after centrifugal separation; the solute-removed material forms raffinate, which is centrifugally separated and then enters a raffinate storage tank 70 to complete the first-stage extraction operation.
The density of the materials is higher than that of the organic solvent by default in the extraction operation, when the organic solvent is chloroform and other organic phases with higher density, a pipeline can be unchanged, only the heavy phase outlet of the centrifugal extractor 10 flows out to be loaded with the organic phase, and the light phase outlet flows out to be raffinate.
The following description is given for a specific example in conjunction with the above extraction system:
prostaglandin is a kind of unsaturated fatty acid with physiological activity, is an active ingredient for preparing patent drugs, and belongs to the category of raw material drugs. In the production of prostaglandin, the material is subjected to multi-step chemical reaction to obtain preorder reaction liquid containing prostaglandin, and then extraction operation is carried out to obtain purified prostaglandin. The extraction unit on the existing prostaglandin production line of a certain medicine enterprise is a traditional gravity settling process, and extraction pilot test is carried out in a production workshop for exploring a centrifugal solvent extraction production process, operation parameters, actual effects and the like, as follows:
1) taking the preorder reaction liquid as a material, taking ethyl acetate as an extracting agent, and adding 31 wt% hydrochloric acid to adjust the pH value of the preorder reaction liquid. And (3) allowing the ethyl acetate to enter a solvent storage tank 40, and displaying in real time through a liquid level meter arranged on the tank body, wherein when the volume of the ethyl acetate in the tank reaches 700L, a feeding valve is closed, and feeding is stopped. The preorder reaction liquid enters a material preparation tank 50, when the volume of the preorder reaction liquid in the tank reaches 270L through a liquid level meter arranged on the tank body, a feeding valve is closed, feeding is stopped, a stirring component is started at the same time, and stirring is carried out at a rated rotating speed of 70r/min, so that the preorder reaction liquid is uniform in component.
According to laboratory parameters, when the pH value of the preoperative reaction liquid is 4 and the temperature of ethyl acetate is 26 ℃, the extraction efficiency is optimal. Therefore, when the step 1) is carried out, it is necessary to pay attention to the pH adjustment and ethyl acetate temperature adjustment of the reaction solution in the previous step, that is:
and (3) blending the pH value of the material: controlling the adding speed and flow of the hydrochloric acid, operating according to the real-time display value of the pH meter, stopping adding the hydrochloric acid when the pH value reaches 4, and continuously stirring for 20min by the stirring assembly.
Ethyl acetate temperature adjustment: the embodiment is carried out in summer, the room temperature is higher than 26 ℃, the refrigerant is introduced into the jacket at the position 40 of the solvent storage tank, the temperature in the tank is adjusted according to real-time display of a thermometer, and the temperature in the tank is guaranteed to be maintained at 26 ℃.
2) Determination of the two-phase ratio: in this example, the centrifugal extractor 10 is of the CTX150 type, and the material feed pump 30 and the solvent feed pump 20 are both metering pumps, and the flow meters are both turbine flow meters. The pre-mixed reaction liquid is pumped into the centrifugal extractor 10 by a material feeding pump 30, the feeding amount of the pre-mixed reaction liquid is preliminarily set according to the model of the centrifugal extractor 10, and the flow meter displays 200L/h at the moment. When liquid flows out from the heavy phase outlet of the centrifugal extractor 10, ethyl acetate is pumped into the centrifugal extractor 10 by the solvent feed pump 20, the phase ratio of the two phases is controlled to be 1:0.8, and the flow meter displays 160L/h. And (4) extracting and separating the two phases, and sampling and analyzing after the two phases are stable. Then, the feeding amount of the reaction solution was kept constant, and the extraction was performed by changing the feeding amount of ethyl acetate so that the two phase ratio was 1:1 and 1:1.2, respectively, and sampling was performed for analysis. And (4) comprehensively considering factors such as analysis results, extraction efficiency and the like, and determining that the phase ratio of the two phases is 1:1 to be optimal.
3) And determining the extraction stage number: under the condition that the material process condition is determined by comparing the two phases, the extraction is carried out for the first time according to the extraction operation, the loaded organic phase after the extraction for the first time enters a loaded organic phase storage tank 60, and the raffinate is sampled and analyzed to complete the extraction operation for the first time. Through pipeline switching, the primary raffinate is pumped into the centrifugal extractor 10 from the raffinate storage tank 70 through the material feed pump 30 to perform secondary extraction according to the extraction operation, and the loaded organic phase after the secondary extraction enters the intermediate storage tank 80. The method is the same as the above, and three extraction operations and four extraction operations are carried out. And obtaining the optimum extraction stage number of three according to the analysis result of the solute content of the raffinate.
It will, of course, be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, but rather includes the same or similar structures that may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
The techniques, shapes, and configurations not described in detail in the present invention are all known techniques.
Claims (10)
1. An extraction pilot test method based on a bulk drug centrifugal solvent extraction system is characterized by comprising an extraction system, wherein the extraction system comprises a centrifugal extractor (10), a light phase inlet of the centrifugal extractor (10) is communicated to an outlet end of a solvent storage tank (40) through a solvent feed pump (20), and a heavy phase inlet of the centrifugal extractor (10) is communicated to an outlet end of a material blending tank (50) through a material feed pump (30); a light phase outlet of the centrifugal extractor (10) is communicated to an inlet end of the loaded organic phase storage tank (60), a heavy phase outlet of the centrifugal extractor (10) is communicated to an inlet end of the raffinate storage tank (70), and an outlet end of the raffinate storage tank (70) is communicated to a pumping end of the material feeding pump (30); the extraction system also comprises an intermediate storage tank (80), wherein the intermediate storage tank (80) and the loaded organic phase storage tank (60) form a parallel pipeline so as to be communicated with a light phase outlet of the centrifugal extractor (10) through a branch switch valve (91); the extraction system also comprises a thermometer T and a liquid level meter which are used for correspondingly monitoring the current states of the solvent storage tank (40), the material blending tank (50), the loaded organic phase storage tank (60), the raffinate storage tank (70) and the intermediate storage tank (80), wherein flow meters F are arranged on a section of pipeline at the pump-out ends of the material feeding pump (30) and the solvent feeding pump (20); a pH meter for monitoring the current pH value of the internal liquid is also arranged at the material blending tank (50); each pipeline is provided with a pipeline switch valve for opening and closing the corresponding pipeline;
the operation flow of the extraction pilot test method is as follows:
1) the extractant enters a solvent storage tank (40), real-time display is carried out through a liquid level meter arranged on a tank body of the solvent storage tank (40), and when the volume of the extractant in the tank body reaches a specified liquid level, feeding is stopped, and the temperature is controlled;
2) the material enters a material blending tank (50), and feeding is stopped when the volume of the preorder reaction liquid in the tank body is monitored to reach a specified liquid level by a liquid level meter arranged on the tank body of the material blending tank (50); then, adding acid or alkali to adjust the pH value of the material;
3) pumping the prepared material in the step 2) into a centrifugal extractor (10) by a material feeding pump (30), preliminarily setting the material feeding amount according to the machine type of the centrifugal extractor (10), and controlling the flow rate by a flowmeter; when liquid flows out from a heavy phase outlet of the centrifugal extractor (10), an extracting agent is pumped into the centrifugal extractor (10) by a solvent feed pump (40), a two-phase ratio is controlled, extraction and separation are carried out on the two phases, and sampling analysis is carried out after the two phases are stable;
4) repeating the step 3), keeping the material feeding amount unchanged, changing the feeding amount of the extracting agent to change the phase ratio of the two phases, sampling and analyzing, and comparing to determine the optimal phase ratio of the two phases;
5) under the condition that the material process condition and the two-phase ratio are determined, primary extraction is carried out according to the extraction operation, the loaded organic phase after the primary extraction enters a loaded organic phase storage tank (60), and the raffinate is sampled and analyzed to complete the primary extraction operation; through pipeline switching, the primary raffinate is pumped into a centrifugal extractor (10) from a raffinate storage tank (70) through a material feeding pump (30) to carry out secondary extraction according to the extraction operation, and a loaded organic phase after the secondary extraction enters an intermediate storage tank (80); and repeating the steps for specified times, comparing the analysis results of the impurity solute content of the raffinate for all times, and comprehensively considering factors such as cost and the like to obtain the optimal value of the extraction stage.
2. The extraction pilot test method based on the bulk drug centrifugal solvent extraction system according to claim 1, characterized in that: the heights of the inlet ends of the loaded organic phase storage tank (60), the raffinate storage tank (70) and the intermediate storage tank (80) are all lower than the heights of the corresponding heavy phase outlet and light phase outlet which are communicated with the loaded organic phase storage tank, so that the light phase effluent and the heavy phase effluent enter the corresponding tanks in a self-flowing mode.
3. The extraction pilot test method based on the bulk drug centrifugal solvent extraction system according to claim 1, characterized in that: the loaded organic phase storage tank (60), the raffinate storage tank (70) and the intermediate storage tank (80) are all horizontal tank bodies.
4. An extraction pilot plant method based on a bulk drug centrifugal solvent extraction system according to claim 1, 2 or 3, characterized in that: washing liquid inlets are respectively arranged on the solvent storage tank (40), the material blending tank (50), the loaded organic phase storage tank (60), the raffinate storage tank (70) and the intermediate storage tank (80), and an organic solvent inlet is also arranged on the solvent storage tank (40); a material inlet and a hydrochloric acid inlet are also arranged at the material preparation tank (50), and the hydrochloric acid inlet is communicated with an outlet of a hydrochloric acid-base metering tank (51) for adding and metering hydrochloric acid; the stirring assembly (52) used for playing an internal stirring function is arranged in the material blending tank (50), and the stirring assembly (52) comprises a stirring paddle and a power source for driving the stirring paddle to generate a stirring action.
5. An extraction pilot plant method based on a bulk drug centrifugal solvent extraction system according to claim 1, 2 or 3, characterized in that: the tank bodies of the solvent storage tank (40), the material blending tank (50), the loaded organic phase storage tank (60), the raffinate storage tank (70) and the intermediate storage tank (80) are all designed in a hollow sandwich mode, and hollow jackets of the tank bodies are communicated with external medium equipment through a heat medium inlet and outlet pipe (92) and/or a cold medium inlet and outlet pipe.
6. An extraction pilot plant method based on a bulk drug centrifugal solvent extraction system according to claim 1, 2 or 3, characterized in that: a pipeline filter (93) is arranged on a section of pipeline at the outlet end of the material feeding pump (30) and the solvent feeding pump (20); pipeline sight glass (94) and sampling port (95) are arranged at the heavy phase outlet and the light phase outlet; sanitary breather valves (96) in the communicating tank are respectively arranged at the solvent storage tank (40), the material blending tank (50), the loaded organic phase storage tank (60), the raffinate storage tank (70) and the intermediate storage tank (80), and rotary cleaning nozzles (97) used for cleaning the environment in the tank are respectively arranged at the tank bodies.
7. An extraction pilot plant method based on a bulk drug centrifugal solvent extraction system according to claim 1, 2 or 3, characterized in that: the solvent storage tank (40), the material blending tank (50), the loaded organic phase storage tank (60), the raffinate storage tank (70), the intermediate storage tank (80) and corresponding pumps, switch valves and central control assemblies are all arranged on the prying frame (98).
8. The pilot scale skid-mounted system based on bulk drug centrifugal solvent extraction process of claim 7, wherein: a leaked liquid collecting tank (98a) is arranged on the prying frame (98), and the leaked liquid collecting tank (98a) is in the shape of an annular groove and is used for collecting leaked liquid falling onto a panel of the prying frame (98); and a leakage liquid emptying valve (98b) communicated with the leakage liquid collecting tank (98a) is also arranged on the prying frame (98).
9. A pilot scale skid based on a bulk drug centrifugal solvent extraction process as claimed in claim 1 or 2 or 3 wherein: the centrifugal extractor (10) comprises a rotor assembly module (11) for generating a centrifugal force field and realizing a mixing and separating function and a rack shell module (12) for realizing storage, collection, guide and separation of materials and each phase, wherein the two groups of modules are connected with each other through a quick-opening bolt (13); and a guide pin (14) which is convenient for the rotor assembly module (11) to be inserted and pulled in a centering way along the vertical direction is arranged on the frame shell module (12).
10. An extraction pilot plant method based on a bulk drug centrifugal solvent extraction system according to claim 1, 2 or 3, characterized in that: the solvent reservoir (40) temperature was maintained at 26 ℃.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102616955A (en) * | 2012-03-21 | 2012-08-01 | 武汉巍川环保科技有限责任公司 | Process and device for treating and recycling chromium-containing waste liquor |
| CN108004420A (en) * | 2017-12-08 | 2018-05-08 | 中国科学院青海盐湖研究所 | The technique that lithium is extracted from the bittern of alkalescence containing lithium based on centrifugal extractor |
| CN108101843A (en) * | 2018-02-01 | 2018-06-01 | 湖南正清制药集团股份有限公司 | A kind of Sinomenine and its circular centrifugal preparation method |
| CN213446234U (en) * | 2020-10-16 | 2021-06-15 | 瀚蓝工业服务(嘉兴)有限公司 | Waste phosphoric acid extraction phosphoric acid treatment system |
-
2021
- 2021-08-25 CN CN202110981483.8A patent/CN113797583A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102616955A (en) * | 2012-03-21 | 2012-08-01 | 武汉巍川环保科技有限责任公司 | Process and device for treating and recycling chromium-containing waste liquor |
| CN108004420A (en) * | 2017-12-08 | 2018-05-08 | 中国科学院青海盐湖研究所 | The technique that lithium is extracted from the bittern of alkalescence containing lithium based on centrifugal extractor |
| CN108101843A (en) * | 2018-02-01 | 2018-06-01 | 湖南正清制药集团股份有限公司 | A kind of Sinomenine and its circular centrifugal preparation method |
| CN213446234U (en) * | 2020-10-16 | 2021-06-15 | 瀚蓝工业服务(嘉兴)有限公司 | Waste phosphoric acid extraction phosphoric acid treatment system |
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Application publication date: 20211217 |