CN109350993B - Automatic extraction method of noble and fine traditional Chinese medicines - Google Patents
Automatic extraction method of noble and fine traditional Chinese medicines Download PDFInfo
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- CN109350993B CN109350993B CN201811300711.5A CN201811300711A CN109350993B CN 109350993 B CN109350993 B CN 109350993B CN 201811300711 A CN201811300711 A CN 201811300711A CN 109350993 B CN109350993 B CN 109350993B
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Abstract
The invention relates to an automatic extraction method of noble and fine traditional Chinese medicines, which can improve the extraction efficiency and the transfer rate of effective components, and also adopts three-stage solid-liquid separation equipment, can carry out continuous operation, does not generate filtration bottleneck and blockage, can realize continuous production, and has high production efficiency, low cost, good dissolubility of the separated product, high clarity and less precipitation.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine production, in particular to an automatic extraction process technology of traditional Chinese medicines.
Background
The extraction is the primary link and important operation unit of traditional Chinese medicine production, and the quality of the process directly influences the quality of the product. The traditional Chinese medicine extraction method comprises a decoction method, an immersion method, a reflux method, a percolation method, an improved gelatin method and the like, but the traditional method has more defects: 1) the loss of effective components, especially water-insoluble components, is high in the decocting method; 2) the organic solvent may react with the effective components during the extraction process, so that the original effect of the organic solvent is lost; 3) the extraction yield is low, the extraction time is long, and the process is complicated; 4) traditional Chinese medicine production enterprises commonly use a multifunctional extraction tank to directly feed and extract materials at present, and because a conventional multifunctional tank cannot enable a solvent around the materials to always keep a certain concentration difference in the extraction process, the extraction efficiency is low, 1-2 times of liquid medicine is generally remained in discharged dregs of a decoction, and certain waste is easily caused.
With the development of science and technology, the application of ultrasonic waves, microwaves and supercritical CO is gradually promoted in recent years2The extraction method is used for extraction, and the ultrasonic and microwave extraction methods can obviously shorten the extraction time and reduce the energy consumption, but are not easy to realize industrial scale and influence the health of people; the microwave has a heat effect, and simultaneously, the microwave can influence the composition and the property of the material, thereby influencing the quality of the product, and the use of the microwave is also limited; supercritical CO2Is suitable for extracting fat-soluble substances, has rigorous extraction conditions, is not beneficial to industrial production, and has narrow application range.
Patent CN101912460B discloses a preparation method for improving the quality of ginsenoside-containing traditional Chinese medicine extract. The method comprises the steps of taking ginseng, red ginseng, American ginseng or pseudo-ginseng and leech, schisandra chinensis, hawthorn or dogwood acid medicinal materials as raw materials, heating and refluxing the raw materials by ethanol or water, combining extracting solutions, concentrating, adjusting the pH value of the concentrated solution by using a sodium hydroxide solution or an ammonia test solution, drying the concentrated solution, and preparing dry paste powder. However, the method only adopts ethanol or water for heating reflux extraction, and can not always keep a certain concentration difference of the solvent around the material, so the extraction efficiency is low, and 1 to 2 times of liquid medicine is generally remained in the discharged dregs of a decoction, which is easy to cause certain waste.
CN106727018A discloses a method for extracting ginseng extract, which comprises the steps of carrying out low-temperature thermal transformation on ginseng crude extract after water extraction and alcohol precipitation, and separating the ginseng crude extract by D101 or AB8 type macroporous resin after redissolution to obtain the ginseng extract. However, this method is not only complicated in the extraction process of ginseng extract, but also low in extraction efficiency and extraction yield, and the residue of liquid medicine in the residue is serious.
CN105663195A discloses a ginsenoside rich in ginsenoside Rg3 and an extraction method thereof. The extraction method comprises the following steps: extracting Ginseng radix with ethanol as extraction solvent by microwave extraction method, adding certain amount of vitamin C into the extraction solution, and extracting under microwave heating for a certain time to obtain crude extractive solution of total saponins of Ginseng radix; the crude extract of the total ginsenoside is further enriched and purified by adopting a macroporous resin adsorption method to obtain the total ginsenoside extract. However, the extraction method not only needs to adopt ethanol solvent for extraction, but also needs to adopt microwave heating, the obtained crude extraction liquid also needs to use macroporous resin for further extraction, the extraction process is complex, the conditions are harsh, the cost is high, and the extraction rate and the paste yield are not high.
CN102258883A discloses a dynamic circulation extraction method of plant extract, wherein the plant material is extracted by extraction solvent for multiple times of dynamic circulation in the extraction process, and forced solvent circulation is adopted. The extraction solvent used each time is 1.5-3 times of the raw material by mass, and the solvent circulation times are 2-5 times; the total extraction times are 2-5 times. Compared with the conventional dynamic countercurrent extraction process, the method has the advantages of high utilization rate of unit extraction equipment, wide equipment adaptability, simple and easy process and the like, can be applied to the production of plant extracts, and is particularly suitable for extracting plant effective components with heat sensitivity, easy deterioration and the like. However, the document does not specifically show the extraction examples and extraction effects of precious and fine Chinese herbs such as ginseng, red ginseng, etc.
The process after the traditional Chinese medicine is extracted is solid-liquid separation, the physical characteristics of the medicine residues generated by different extraction processes, such as viscosity, water content, solid granularity and the like, are different, the forms of the medicine residues after the different traditional Chinese medicines are extracted are also different, and the medicine residues have light floaters, suspended matters and precipitates.
Patent CN107913543A discloses a quick solid-liquid separation device for traditional Chinese medicines, which comprises a box body, wherein parts such as a transverse partition plate, a material pipe, a gear, a booster pump stirring rod, a heating rod and the like are arranged in the box body.
Patents CN205659433U and CN204951634U both disclose a solid-liquid separation device for Chinese medicine extract, which respectively adopts a single centrifugal separation mode and a filter screen for solid-liquid separation.
Patent CN206492274U discloses a traditional chinese medicine solid-liquid separation equipment to specifically disclose this separator include by high to low two filters that connect gradually: the filter I and the filter II are detachably connected. The filter is to include a filter screen, the filter is two-position to filter the jar, and this solid-liquid separation equipment only separates through the filtration mode, and separation efficiency is lower, and the separation effect is relatively poor, can not be applicable to the separation of different types of traditional chinese medicine.
In addition, in the prior art, ceramic membrane is adopted for solid-liquid separation, which is mainly applied to Chinese medicine injections and other preparations with extremely high requirements on clarity or purity of active ingredients, but the problems of large interception loss of active ingredients, incomplete membrane pollution prevention and treatment, low production efficiency and the like can occur when ceramic membrane separation is adopted for Chinese medicine formula granules or common Chinese medicine solid oral preparations.
However, the above solid-liquid separation devices all adopt a simple solid-liquid separation mode, the separation efficiency is low, the separation effect is poor, and the separation device has clear requirements on the types and properties of the Chinese traditional medicine to be separated.
Therefore, how to improve the extraction efficiency of the noble and fine Chinese medicines, improve the cream yield and the index component transfer rate of the product, and effectively and efficiently separate the extracting solution is the core problem of improving the quality and the economic benefit of the noble and fine Chinese medicines.
Disclosure of Invention
Problems to be solved by the invention
In order to solve the technical problems in the prior art, the invention aims to design an automatic extraction and separation method of noble and fine traditional Chinese medicines so as to improve the extraction efficiency and separation efficiency of noble and fine traditional Chinese medicines, and improve the cream yield, index component transfer rate and clarity of finished products; meanwhile, the separation efficiency is improved, the separation effect is improved, and the production cost and the energy consumption are reduced.
Means for solving the problems
The invention provides an automatic extraction method of noble and fine traditional Chinese medicines, which comprises the following steps,
(1) feeding:
adding solvent and noble fine raw materials to be extracted into the dynamic extraction tank body according to the measurement;
(2) dynamic extraction:
after feeding is finished, heating precious and fine raw materials to be extracted and a solvent in a tank, and automatically controlling the process to set a temperature value, wherein the set temperature is 85-100 ℃;
and starting forced circulation of the dynamic extraction tank and stirring in the dynamic extraction tank, automatically recording the set time of extraction and decoction by a program while heating the dynamic extraction tank, setting the decoction time to be 0.5-4 h, preferably setting the decoction time to be 1-3 h, and obtaining an extracting solution after the set time of extraction and decoction is reached.
Preferably, the method further comprises (3) a solid-liquid separation step of the extracted liquid, wherein the separation step sequentially utilizes a primary centrifuge or a slag remover, a filtering solid-liquid separator and a secondary centrifuge to carry out combined solid-liquid separation on the extracted liquid and the dregs flowing out of the dynamic extraction tank.
Preferably, the primary centrifuge or the slag remover is a decanter centrifuge or a slag remover, and preferably a horizontal screw type slag remover; the filtering type solid-liquid separator is a wet oscillating screen; the secondary centrifuge is a decanter centrifuge, preferably a disk separator.
Preferably, the liquid inlet amount of the primary centrifugal machine or the slag remover is set to be 4-6T/h, the rotating speed of a main motor of the primary centrifugal machine or the slag remover is 2300-2450 rpm, and the rotating speed of an auxiliary motor is 1500-1700 rpm.
Preferably, the number of the vibrating meshes of the wet oscillating screen is 100-250 meshes.
Preferably, the liquid inlet amount of the secondary centrifuge is set to be 3-4T/h, and the slag discharge period is as follows: 150-300 seconds, and the slag discharge time is 0.1-0.5 seconds.
Preferably, the raw materials to be extracted from the noble and fine class are selected from one or more of centipede, scorpion, dragon's blood, scalded leech, rhizoma paridis, aspongopus, zaocys dhumnade, edible tulip, tianlong dragon, gecko, American ginseng, red ginseng, dendrobe, cistanche, musk, antelope horn and cordyceps sinensis.
Preferably, the solvent is water, and the volume mass ratio of the addition amount of the solvent to the noble fine raw materials to be extracted is 8-20.
Preferably, the forced circulation in the step (2) has 8-15 times of circulation per hour.
ADVANTAGEOUS EFFECTS OF INVENTION
Compared with the prior art, the invention has the advantages that:
1) the method adopts a specific dynamic extraction tank, utilizes the high-frequency control of a stirring motor T-M1 of the dynamic extraction tank and a circulating pump T-M2 of the dynamic extraction tank to achieve the forced circulation times of the process requirements, makes full use of the diffusion principle to quickly dissolve the active ingredients of the medicinal materials in the solvent, improves the extraction production efficiency, and forces the active ingredients on the surface of the medicinal materials to reach a certain concentration difference, thereby improving the extraction efficiency and the index ingredient transfer rate.
2) The invention adopts three-stage solid-liquid separation equipment, can carry out continuous operation, does not generate filtration bottleneck and blockage, can realize continuous production, and has high production efficiency, low cost, good dissolubility of the separated product, high clarity, high transmittance and less precipitation; the decocted extract is filtered at high temperature in the whole process, the health is safe, the automatic residue discharge can be realized, the automatic control can be adopted, the labor cost is saved, and the labor intensity is reduced.
3) The original process for extracting the noble and fine traditional Chinese medicines adopts a 3T multifunctional tank with the feeding amount of 100-250 kg, the total addition amount of a solvent is 14-24 times of the feeding amount, and the extraction is carried out for 1-2 times, wherein each time lasts for 0.5-2 hours. The invention adopts dynamic extraction and three-stage separation to extract and separate precious traditional Chinese medicines, and optionally regulates and controls the process parameters such as extraction time, extraction temperature, cycle times and the like, so that the transfer rate of the effective components of the product is obviously improved, the transmittance of the finished product is improved by 2.18 times compared with the prior art, and the daily yield is also improved by more than 15 percent compared with the prior art. Compared with the method which only adopts two-stage solid-liquid separation, the invention can realize continuous production by combining three solid-liquid separation devices, not only the transfer rate of the effective components is improved to a certain extent, but also the extract has high light transmittance and better dissolubility after being dissolved.
Drawings
FIG. 1 is a schematic structural diagram of an automated extraction and separation apparatus for Chinese herbs used in the automated extraction method of the present invention.
FIG. 2 is a schematic view of a horizontal screw centrifuge used in the present invention.
Description of the reference numerals
T-1-dynamic extraction tank
T-2-horizontal screw type slag remover
T-3-wet type oscillating screen
T-4-intermediate tank 1
T-5-intermediate storage tank 2
T-6-disc type separator
T-7-extracting solution storage tank
T-M1-dynamic extraction tank stirring motor
T-M2-circulating pump of dynamic extraction tank
T-N1-dynamic extraction tank stirring paddle
T-N2-circulating pipeline of dynamic extraction tank
T-N3-extraction tank heating jacket
T-N4-extract liquid outlet control valve
TQRV-1-extraction tank jacket steam regulating valve
TQPT-1-extraction tank jacket steam pressure gauge
TQPT-2-extract jar interior steam manometer
TQTT-1-extracting pot internal thermometer
TQPV-1-extraction tank feed liquid control valve
TQLS-1-dynamic extraction tank liquid level switch
1-auxiliary motor
2-main motor
3-differential mechanism
4-rotating drum
5-spiral discharger
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
The invention provides an automatic extraction method of noble and fine traditional Chinese medicines, which adopts a specific automatic traditional Chinese medicine extraction and separation device.
< automatic extraction and separation apparatus for Chinese herbs >
As shown in figure 1, the automatic traditional Chinese medicine extracting and separating device comprises a dynamic extracting tank T-1 and a combined solid-liquid separating component.
The dynamic extraction tank T-1 is characterized in that a tank body of the dynamic extraction tank T-1 is provided with a circulating pipeline T-N2 which leads circulating materials out and into the tank body in a circulating manner in the extraction process, the circulating materials comprise solvent and extract, namely noble and fine traditional Chinese medicines, the circulating pipeline is provided with a circulating pump T-M2, the circulating pipeline and the circulating pump are designed to meet the requirement that the solvent and the extract circulate together, the properties of the materials are not damaged in the circulating process, the materials in the whole tank can be quickly and uniformly mixed, an extraction tank material liquid control valve TQPV-1 and a dynamic extraction tank liquid level switch TQLS-1 can be arranged on the circulating pipeline T-N2, and a sewage branch pipe for discharging residue liquid can also be arranged on the circulating pipeline. The inner chamber of the dynamic extraction tank is provided with a plurality of layers of stirring paddles T-N1, the stirring paddles are driven by a dynamic extraction tank stirring motor T-M1, the stirring paddles are preferably arranged at positions not on the central axis of the tank body, the stirring paddles are preferably three-layer stirring paddles, the uppermost layer is a downward pressing type, some floating materials can be sunk through stirring, the middle layer is a horizontal type, the materials can be horizontally and outwards pushed to be diffused, dynamic exchange of the materials is promoted, the lowermost layer is an upward turning type, the materials are upwards rolled through pushing, and material deposition is avoided at the bottom of the tank. The design of the stirring paddle can enable the tank to achieve better stirring effect. The invention utilizes the high-frequency control of a stirring motor T-M1 of the dynamic extraction tank and a circulating pump T-M2 of the dynamic extraction tank to achieve the forced circulation times of the process requirements, fully utilizes the diffusion principle to quickly dissolve the active ingredients (such as saponins, flavonoids, alkaloids and the like) of precious traditional Chinese medicines in the solvent, and forcibly makes the active ingredients on the surface of the medicines reach a certain concentration difference.
The dynamic extraction tank is also provided with a feeding unit and a heating unit. The feeding unit finishes the feeding of the solvent and the raw materials to be extracted, controls the feeding time and the feeding amount, and starts circulation and stirring at the feeding end point. The heating unit heats the extraction system to enable the temperature in the extraction tank to reach the temperature set by the process and keep at the temperature set by the process, and the extraction time at the temperature set by the process is recorded. The heating unit comprises a extracting tank heating jacket T-N3, a temperature gauge TQTT-1 in the extracting tank for detecting the temperature in the extracting tank, a steam pipe communicated with the extracting tank heating jacket, an extracting tank jacket steam regulating valve TQRV-1 arranged on a steam pipe, an extracting tank inner steam pressure gauge TQPT-2 for detecting the steam pressure in the extracting tank, and an extracting tank jacket steam pressure gauge TQPT-1 for detecting the steam pressure in the extracting tank. According to the invention, the opening of the steam regulating valve TQRV-1 of the jacket of the extraction tank is regulated by PID, the decocting temperature is stably reached, and the phenomena of too fast temperature rise and material leakage during decoction of medicinal materials after manual regulation of a manual steam valve are effectively solved. Preferably, each valve of the dynamic extraction tank is controlled by a PLC controller. After extraction is finished, the extracting solution and the dregs in the dynamic extraction tank are led into a combined solid-liquid separation component together under the control of an extracting solution outlet control valve T-N4 for solid-liquid separation. The liquid outlet unit of the dynamic extraction tank comprises a liquid outlet pipeline with an extracting liquid outlet control valve T-N4, one end of the liquid outlet pipeline is connected to the circulating pipeline in a branch mode, and the other end of the liquid outlet pipeline is connected with the combined solid-liquid separation assembly. In a possible embodiment of the invention, the bottom cover of the dynamic extraction tank is not provided with a filtering device.
The combined solid-liquid separation component comprises three solid-liquid separation devices, and is sequentially provided with a primary centrifuge or a slag remover, a filtering solid-liquid separator and a secondary centrifuge, wherein the primary centrifuge or the slag remover, the filtering solid-liquid separator and the secondary centrifuge are sequentially communicated through a feeding pipeline.
Further, the primary centrifuge or the slag remover is a decanter centrifuge or a slag remover and is used for primarily separating slag liquid and most of solid slag by specific gravity difference, and the primary centrifuge or the slag remover is preferably a horizontal screw type slag remover T-2 in a specific embodiment of the invention. The horizontal screw type slag remover is generally used in the fields of water treatment and the like, the horizontal screw type slag remover with larger treatment capacity is creatively used in the traditional Chinese medicine extraction and separation process, and compared with a three-foot centrifuge or a flat plate centrifuge with larger treatment capacity conventionally used in traditional Chinese medicine extraction and separation, the horizontal screw type slag remover can realize continuous production and is provided with a spiral mechanical structure inside to facilitate the cleaning of medicine dregs. In one embodiment of the invention, as shown in fig. 2, the horizontal screw centrifuge comprises a rotary drum (4), a screw discharger (5), a motor and a differential (3), wherein the screw discharger (5) is arranged in the rotary drum (4), a material feeding pipe is inserted into the screw discharger (5), one end of the material feeding pipe is a feeding hole, the other end of the material feeding pipe is a discharging hole, one end of the rotary drum (4) close to the feeding hole is used as a clear liquid outlet, and one end close to the discharging hole is used as a sediment outlet, and the motor comprises a main motor (2) for controlling feeding and an auxiliary motor (1) for controlling the differential (3).
The effluent enters a filtering type solid-liquid separator through a horizontal screw type slag remover, and the filtering type solid-liquid separator has the function of separating and filtering a small amount of impurities through particle size difference so that the filtrate can meet the requirement of liquid inlet of a disc type separator. In one embodiment of the invention, the filtering type solid-liquid separator is a wet oscillating screen T-3, compared with the conventional filtering equipment, the wet oscillating screen adopts dynamic filtering, so that the problem that a large amount of fine powder blocks the filter screen holes is avoided, the treatment capacity is high, and continuous production can be realized.
The secondary centrifuge according to the invention, which serves to remove pulp and impurities and the majority of the impurities accumulated in the sediment zone, mainly has the effect of fine filtration, is preferably a decanter centrifuge, in one embodiment of the invention a disk separator T-6. Compared with the tubular centrifuges of the same type, the disc type separator has higher capacity and can realize continuous production. In consideration of the difference of the processing capacity between the disc-type separator and the solid-liquid separation equipment of the previous two stages, an intermediate storage tank 1T-4 and a high-level intermediate storage tank 2T-5 are preferably arranged between the filtering solid-liquid separator and the two-stage separator, so that the working mode of the top liquid inlet of the disc-type separator is adapted.
The secondary centrifugal machine can achieve a separation result with high efficiency and good separation effect only by being sequentially combined with the primary centrifugal machine and the filtering type solid-liquid separation machine. If the horizontal screw type slag remover is used independently, the separation effect is poor, the turbidity of the extracting solution is high, if the wet oscillating screen is used independently, large solid particles easily block the screen holes, and if the disc type separator is used independently, the liquid slag cannot be removed in time due to large particle size and large impurity amount, so that the blockage is easy to occur. If only a horizontal screw type slag remover and a wet oscillating screen are combined, the clarity and the dissolubility of the product are greatly influenced without a fine filtering step. In addition, the three solid-liquid separation devices are specific in sequence due to the action, the solid-liquid separation principle and the difference of productivity, the good separation effect of the invention can be realized only by sequentially passing through the three solid-liquid separation devices, if the three solid-liquid separation devices are connected in different sequences, the treatment capacity and the separation efficiency are influenced, and meanwhile, the device is easy to block.
< automated extraction and separation method of precious and fine Chinese herbs >
Based on the automatic extraction and separation device for traditional Chinese medicines, the automatic extraction and separation method for precious and fine traditional Chinese medicines comprises dynamic extraction and optional solid-liquid separation after the dynamic extraction.
The invention relates to an automatic extraction and separation method of noble and fine traditional Chinese medicines, which mainly comprises the following steps:
(1) feeding:
moving the noble and fine raw materials to be extracted to a feeding port, firstly opening a solvent adding control valve, beginning to measure the solvent added into an extraction tank body by using an electromagnetic flow meter, wherein the volume-mass ratio of the adding amount of the solvent to the raw materials to be extracted is 8-20, and when the amount of the solvent reaches a preset process set value, the medicinal materials are fed into the extraction tank T-1 from the feeding port. If the addition amount of the solvent is too high, the circulation load of the system is increased, the production cost is increased, and if the addition amount of the solvent is too low, the effective components cannot be sufficiently extracted, so that the cream yield and the index component transfer rate of the product are influenced. The solvent is one or more of water and alcohol solvents, halogenated hydrocarbons, and the like, such as methanol, ethanol, n-propanol, isopropanol, dichloromethane, dichloroethane, and the like, and can be selected according to the solubility of the medicinal materials.
(2) Dynamic extraction:
after the material feeding is finished, automatically opening a steam regulating valve to start introducing steam into a heating jacket of the extraction tank, and heating the raw materials and the solvent in the tank; while the extraction tank heating jacket T-N3 is heated, the temperature of the extracting solution is detected on line in real time by the temperature gauge in the extraction tank arranged at the bottom of the side of the tank body, the PLC program controls the opening of the steam regulating valve TQRV-1 of the extraction tank jacket in a PID regulating mode according to the steam pressure and the target value of the temperature in the extraction tank, so that the temperature of the extracting solution rises stably, and when the temperature gauge in the extraction tank reaches the temperature set by the process, the temperature is kept at the temperature set by the process, and the set temperature is 85-100 ℃.
Starting a circulating pump T-M2 in an extracting solution circulating system while heating, forcibly circulating the extracting solution, continuously pumping the liquid in the extracting tank from the bottom of the extracting tank, pumping the liquid back to the extracting tank from the upper part of the extracting tank by a pump through a pipeline, enhancing the contact between a solid phase and a liquid phase through the circulating flow of the liquid, and enhancing the dissolution of active ingredients from the inside of the medicinal material. The circulating pump T-M2 controls the flow of the circulating liquid through the frequency conversion of the frequency converter to achieve corresponding circulating times, wherein the circulating times per hour are 8-15; and simultaneously, a stirring motor T-M1 of the dynamic extraction tank is started by frequency conversion to stir the solvent so as to achieve the concentration difference of the effective components on the surface of the medicinal material decoction pieces. Regarding the number of cycles per hour, if the number of cycles per hour is small, it is not favorable for maintaining a certain concentration difference around the medicinal material and for dissolving out the effective components, but if the number of cycles is too large, the medicinal material is repeatedly collided and squeezed by a pump, and pressure is easily brought to the solid-liquid separation process after the medicinal material tissue is boiled.
In addition, the PLC program can automatically record the set time of extraction decoction, generally speaking, the decoction time is 0.5-4 h, and the preferred decoction time range is 1-3 h. When the set time of extraction and decoction is reached, the steam regulating valve of the jacket of the extraction tank is closed, the extraction is finished and liquid discharge is started. The problems of too short manual decoction time, low medicinal material yield, long decoction time and low efficiency can be effectively solved by automatically and accurately recording the decoction time.
In the process of taking and discharging liquid, firstly, an extracting liquid discharging control valve T-N4 is opened, solid-liquid separation is carried out through an extracting liquid circulating pump T-M2, after the liquid level detection switch of the dynamic extraction tank is detected to judge that the liquid is emptied, the extracting tank circulating pump T-M2 and the extracting tank stirring motor T-M1 are stopped, and the corresponding control valve is closed. In the process of extracting the liquid from the extracting solution, the extraction yield of the batch of materials can be deduced by using a formula in the program and compared with the past set empirical value, and the parameters of the batch amount, the water adding amount, the temperature and the time for dynamically extracting the next batch of materials are automatically and finely adjusted in the program.
(3) And (3) combined solid-liquid separation:
the extract and the dregs obtained by dynamic extraction can be separated by a conventional solid-liquid separation device, and preferably combined solid-liquid separation is carried out on the extract and the dregs by a primary centrifuge or a slag remover, preferably a horizontal screw type slag remover T-2, a filtering type solid-liquid separator, preferably a wet oscillating screen T-3, and a secondary centrifuge, preferably a disc type separator T-6 in sequence.
In order to better separate the precious and fine traditional Chinese medicine extracting solution from the decoction dregs, the liquid inlet speed and the screw rotating speed of the primary centrifuge or the residue remover, the vibrating screen mesh number of the wet vibrating screen, the rotating speed of the secondary centrifuge, the residue discharge gap and other process parameters need to be controlled. The inventors found that the separation effect was excellent when the following parameters were used:
the liquid inlet amount of the primary centrifuge or the slag remover is set to be 4-6T/h, the rotating speed of a main motor of the primary centrifuge or the slag remover is 2300-2450 rpm, and the rotating speed of an auxiliary motor is 1500-1700 rpm
The liquid outlet with less residue and dry residue can be realized; when the number of the vibrating screen meshes of the wet vibrating screen is 100-250 meshes, the treatment capacity can be ensured, and the medicine dregs with larger grain diameter can be removed; the liquid inlet amount of the secondary centrifuge is set to be 3-4T/h, and the slag discharge period is as follows: 150-300 seconds and 0.1-0.5 second for slag discharge, which is beneficial to obtaining clear filtrate.
In a preferred embodiment of the present invention, after the dynamic extraction step is completed, the software automatically determines whether the automatic clearing program needs to be executed according to the issued order sheet: the method comprises hot water cleaning and alkali cleaning after whether batch and variety need to be replaced or not; after entering the automatic cleaning program, the verified control parameters are set in the CIP online cleaning program to complete the automatic cleaning of the equipment and the pipeline.
The control parameters comprise flushing time, cleaning liquid inlet time, cleaning cycle time and cleaning discharge completion delay time of the dynamic extraction tank; the liquid inlet time for cleaning the pipeline and the delay time for finishing the cleaning and discharging of the pipeline are prolonged; the flushing time and the liquid inlet time of the primary centrifugal machine or the slag remover, the filtering solid-liquid separator and the sedimentation type centrifugal machine are respectively the cleaning time of the pipeline; flushing time of an extracting solution storage tank, cleaning liquid inlet time and cleaning discharge completion delay time.
Generally, the extraction and separation device of traditional Chinese medicines in the prior art has no CIP online cleaning process program for independent alkali cleaning and heating water, and the cleaning process of the extraction and separation device is also according to the original extraction and separation process flow program, and no corresponding cleaning record can be inquired in a production server system. The invention creatively introduces a CIP online cleaning process program, can independently select equipment and pipeline alkaline cleaning or hot water cleaning, and can independently set cleaning and discharging time and the like.
According to the verified site cleaning time, the invention utilizes an automatic control program to complete the site cleaning purposes of all equipment (a dynamic extraction tank, a horizontal screw centrifuge, a wet-type vibrating screen, a disc centrifuge and the like) and all process pipelines, automatically completes the site cleaning requirements of closed equipment and pipelines without dead angles, manual intervention and timing and quantitative online site cleaning, and ensures that all process equipment and pipelines meet the GMP online site requirements.
Examples
The technical solution of the present invention will be further described with reference to specific examples. It should be understood that the following examples are only for illustrating and explaining the present invention and are not intended to limit the scope of the present invention.
Example 1
The present embodiment relates to a method for extracting and separating ginseng. It adopts the automatic extraction and separation device for traditional Chinese medicine shown in figure 1 to carry out automatic extraction and separation.
(1) Feeding:
preprocessing ginseng slices, cutting or crushing the ginseng slices to obtain particles with the particle size less than 1 cm;
moving the ginseng slice 160KG with particle size less than 1cm to the feeding port, opening the solvent (water) adding control valve, and starting to measure to 3M by using an electromagnetic flowmeter3The dynamic extraction tank body is added with 2400L of solvent, and after the amount of the solvent reaches a preset process set value, ginseng slices are put into the extraction tank T-1 from a feeding port.
(2) Dynamic extraction:
after the material feeding is clicked, automatically opening a steam regulating valve to enable steam to be introduced into a heating jacket of the extraction tank, and heating the ginseng slices and water in the tank; while the extracting tank heating jacket T-N3 is heating, the temperature of the extracting solution is detected on line in real time by the extracting tank inner thermometer arranged at the bottom of the tank side, and the PLC program controls the opening of the extracting tank jacket steam adjusting valve TYRV-1 in a PID adjusting mode according to the steam pressure and the target value of the extracting tank inner temperature, so that the temperature of the extracting solution rises stably, and when the extracting tank inner thermometer reaches the process set temperature, the temperature is kept at the process set temperature value, and the set temperature is 98 ℃.
Heating and starting circulation pump T-M2 in the extractive solution circulation system to forcibly circulate extractive solution. The circulating pump T-M2 controls the flow of the circulating liquid through the frequency conversion of the frequency converter so as to achieve 12 times of circulation per hour; and simultaneously, a stirring motor T-M1 of the dynamic extraction tank is started by frequency conversion to stir the solvent so as to achieve the concentration difference of the effective components on the surface of the medicinal material decoction pieces.
The PLC program automatically records the set time of extraction and decoction, and the decoction time is 2 h. When the set time of extraction and decoction is reached, the steam regulating valve of the jacket of the extraction tank is closed, the extraction is finished and liquid discharge is started.
In the process of extracting the liquid from the extracting solution, firstly, an extracting solution outlet control valve T-N4 is opened, solid-liquid separation is carried out through an extracting solution circulating pump T-M2, after the liquid level detection switch of the dynamic extraction tank is detected to judge that the liquid is emptied, the extracting tank circulating pump T-M2 and an extracting tank stirring motor T-M1 are stopped, and the corresponding control valve is closed.
(3) And (3) combined solid-liquid separation:
and (3) introducing the extracting solution in the extracting tank into a combined solid-liquid separation component for solid-liquid separation, and sequentially passing through a horizontal screw type slag remover T-2, a wet type oscillating screen T-3 and a disc type separator T-6.
Extracting solution in the extraction tank is pumped into a horizontal screw type slag remover, the liquid inlet amount is set to be about 4T/h, the rotating speed of a main motor is set to be 2500 revolutions per minute, the rotating speed of an auxiliary motor is set to be 1800 revolutions per minute, the extracting solution after slag removal passes through a wet type oscillating screen, the mesh number of the oscillating screen is 200 meshes, the extracting solution is pumped into an intermediate storage tank, the extracting solution flows into a disc type separator, the liquid inlet amount is set to be about 2.5T/h, and the slag removal period is as follows: 300 seconds and 0.3 second of slag discharge time. The extract after passing through the disc type separator can enter the next working procedure.
Example 2
The present embodiment relates to a method for extracting and isolating red ginseng. It also adopts the automatic extraction and separation device for traditional Chinese medicine shown in figure 1.
(1) Feeding:
pretreating Ginseng radix Rubri, cutting or pulverizing Ginseng radix Rubri to particle size less than 1 cm;
moving Ginseng radix Rubri 160KG with particle diameter less than 1cm to the feeding port, opening the solvent (water) addition control valve, and starting to measure to 3M by electromagnetic flowmeter32400L of solvent is added into the dynamic extraction tank, and when the amount of the solvent reaches a preset process set value, the red ginseng is put into the extraction tank T-1 from a feeding port.
(2) Dynamic extraction:
after clicking the feeding is finished, automatically opening a steam regulating valve to enable steam to be introduced into a heating jacket of the extraction tank, and heating the red ginseng and the water in the tank; while the extracting tank heating jacket T-N3 is heating, the temperature of the extracting solution is detected on line in real time by the extracting tank inner thermometer arranged at the bottom of the tank side, and the PLC program controls the opening of the extracting tank jacket steam adjusting valve TYRV-1 in a PID adjusting mode according to the steam pressure and the target value of the extracting tank inner temperature, so that the temperature of the extracting solution rises stably, and when the extracting tank inner thermometer reaches the process set temperature, the temperature is kept at the process set temperature value, and the set temperature is 98 ℃.
Heating and starting circulation pump T-M2 in the extractive solution circulation system to forcibly circulate extractive solution. The circulating pump T-M2 controls the flow of the circulating liquid through the frequency conversion of the frequency converter so as to achieve 12 times of circulation per hour; and simultaneously, a stirring motor T-M1 of the dynamic extraction tank is started by frequency conversion to stir the solvent so as to achieve the concentration difference of the effective components on the surface of the medicinal material decoction pieces.
The PLC program automatically records the set time of extraction and decoction, and the decoction time is 2 h. When the set time of extraction and decoction is reached, the steam regulating valve of the jacket of the extraction tank is closed, the extraction is finished and liquid discharge is started.
In the process of extracting the liquid from the extracting solution, firstly, an extracting solution outlet control valve T-N4 is opened, solid-liquid separation is carried out through an extracting solution circulating pump T-M2, after the liquid level detection switch of the dynamic extraction tank is detected to judge that the liquid is emptied, the extracting tank circulating pump T-M2 and an extracting tank stirring motor T-M1 are stopped, and the corresponding control valve is closed.
(3) And (3) combined solid-liquid separation:
and (3) introducing the extracting solution in the extracting tank into a combined solid-liquid separation component for solid-liquid separation, and sequentially passing through a horizontal screw type slag remover T-2, a wet type oscillating screen T-3 and a disc type separator T-6.
Extracting solution in the extraction tank is pumped into a horizontal screw type slag remover, the liquid inlet amount is set to be about 4T/h, the rotating speed of a main motor is set to be 2500 revolutions per minute, the rotating speed of an auxiliary motor is set to be 1800 revolutions per minute, the extracting solution after slag removal passes through a wet type oscillating screen, the mesh number of the oscillating screen is 200 meshes, the extracting solution is pumped into an intermediate storage tank, the extracting solution flows into a disc type separator, the liquid inlet amount is set to be about 2.5T/h, and the slag removal period is as follows: 300 seconds and 0.3 second of slag discharge time. The extract after passing through the disc type separator can enter the next working procedure.
Comparative example 1
The present comparative example relates to the same method for extraction and separation of ginseng as in example 1. With the difference that conventional 3M is used3A multifunctional extraction tank and a PD1250 punching bag discharge centrifuge of a conventional solid-liquid separation device. Specifically, ginseng slices are put into a multifunctional extraction tank, water is added for extraction twice, water with the amount 10 times that of decoction pieces is added for the first time, and boiling extraction is carried out for 2 hours; adding water 8 times the amount of the decoction pieces for the second time, boiling and extracting for 1 hr, and centrifuging with PD1250 punching bag discharge centrifuge.
Comparative example 2
The present comparative example relates to the same method for extraction and separation of ginseng as in example 1. With the difference that conventional 3M is used3The multifunctional extraction tank and the 200-mesh bag filter are used for extraction and separation. Specifically, ginseng slices are put into a multifunctional extraction tank, water is added for extraction twice, water with the amount 10 times that of decoction pieces is added for the first time, and boiling extraction is carried out for 2 hours; adding water 8 times of the decoction pieces for the second time, boiling and extractingFor 1 hour, the extract was passed through a 200 mesh bag filter.
Comparative example 3
The comparative example relates to the same extraction and separation method of ginseng as in example 1, with the same raw material charge and water as the solvent. Except that the extraction temperature in step (2) was 70 ℃.
Comparative example 4
The comparative example relates to the same extraction and separation method of ginseng as in example 1, with the same raw material charge and water as the solvent. Except that the extraction temperature in step (2) was 110 ℃.
Comparative examples 5 to 6
Comparative example 5
The comparative example relates to the same extraction and separation method of ginseng as in example 1, with the same raw material charge and water as the solvent. Except that the number of hourly cycles of step (2) was 7/hr.
Comparative example 6
The comparative example relates to the same extraction and separation method of ginseng as in example 1, with the same raw material charge and water as the solvent. Except that the number of cycles per hour of step (2) was 16 cycles/hour.
Comparative example 7
The comparative example relates to the same extraction and separation method of ginseng as in example 1, with the same raw material charge and water as the solvent. The dynamic extraction equipment and process and the subsequent concentration, drying and granulation processes are the same as those in example 1, except that only two-stage solid-liquid separation equipment (horizontal screw type slag remover + disc centrifuge) is adopted in step (3). The operating parameters of the horizontal screw type slag remover and the disc centrifuge are consistent with those of the embodiment 1.
Comparative example 8
The comparative example relates to the same extraction and separation method of ginseng as in example 1, with the same raw material charge and water as the solvent. The dynamic extraction equipment and process and the subsequent concentration, drying and granulation processes are the same as those in example 1, except that only two-stage solid-liquid separation equipment (horizontal screw type slag remover + wet type oscillating screen) is adopted in step (3). The operating parameters of the horizontal screw type slag remover and the wet type oscillating screen are consistent with those of the embodiment 1.
Comparative example 9
The comparative example relates to the same extraction and separation method of ginseng as in example 1, with the same raw material charge and water as the solvent. The dynamic extraction equipment and process and the subsequent concentration, drying and granulation process are the same as those in example 1, except that the horizontal screw type slag remover in step (3) is changed into a three-foot type lower slag discharge centrifugal filter, the disc type centrifuge is changed into a tubular clarification type ultracentrifuge, and the equipment parameters of the three-foot type lower slag discharge centrifugal filter and the tubular clarification type ultracentrifuge are adjusted according to the actual conditions. The operating parameters of the wet shaker were in accordance with example 1.
The production efficiency and energy consumption of the processes of examples 1 and 2 and comparative examples 1 to 9 of the present invention, and the solubility, clarity, effective component transfer rate of the product were comprehensively analyzed, and the specific results are shown in table 1.
The total content of the ginsenoside Rg1 and the ginsenoside Re in the ginseng extracts prepared in the embodiment 1, the embodiment 2 and the comparative examples 1 to 9 related by the invention is determined by adopting a high performance liquid chromatography, and the specific method comprises the following steps: octadecylsilane chemically bonded silica is used as a filling agent; acetonitrile-water is used as a mobile phase; the detection wavelength was 203 nm. The flow rate is 1.0ml/min, the sample volume of the sample is 10 μ l, and the sample volume of the ginsenoside Rg1 and the ginsenoside Re reference sample is 10 μ l with the concentration of 0.2 mg/ml.
The total transfer rate (%) of ginsenoside Rg1 and ginsenoside Re in the extract is multiplied by the total content (%) of ginsenoside Rg1 and ginsenoside Re in the extract/the total content (%) of ginsenoside Rg1 and ginsenoside Re in decoction pieces
TABLE 1 comparison of the production Process and product quality for different groups
As can be seen from the comparison in Table 1, compared with the conventional multi-functional extraction tank for multiple times of decoction, the invention adopts dynamic extraction and three-stage solid-liquid separation processes for production, so that the transfer rate of the effective components of the product is obviously improved, the transmittance of the finished product is improved by 2.18 times compared with the prior art, and the daily yield is also improved by more than 15% compared with the prior art. Compared with the method which only adopts two-stage solid-liquid separation, the invention can realize continuous production by combining three solid-liquid separation devices, not only the transfer rate of the effective components is improved to a certain extent, but also the extract has high light transmittance and better dissolubility after being dissolved.
In addition to the above embodiments, the present invention also includes other embodiments, and any technical solutions formed by equivalent transformation or equivalent replacement should fall within the scope of the claims of the present invention.
Claims (5)
1. An automatic extraction method of noble and fine traditional Chinese medicines is characterized by comprising the following steps: the method comprises the following steps of,
(1) feeding:
adding solvent and noble fine raw materials to be extracted into the dynamic extraction tank body according to the measurement; the extract is prepared from one or more of Scolopendra, Scorpio, sanguis Draxonis, Hirudo, rhizoma paridis, Aspongopus, Zaocys, Pseudobulbus Cremastrae seu pleiones, Gekko Swinhonis, radix Panacis Quinquefolii, Ginseng radix Rubri, herba Dendrobii, Cistanchis herba, Moschus, cornu Saigae Tataricae and Cordyceps,
(2) dynamic extraction:
after feeding is finished, heating precious and fine raw materials to be extracted and a solvent in a tank, and automatically controlling the process to set a temperature value, wherein the set temperature is 85-100 ℃;
starting forced circulation of the dynamic extraction tank and stirring in the dynamic extraction tank, automatically recording the set time of extraction and decoction by a program while heating the dynamic extraction tank, setting the decoction time to be 0.5-4 h, and obtaining an extracting solution after liquid outlet when the set time of extraction and decoction is reached;
(3) a solid-liquid separation step of the extract obtained by liquid discharge, wherein the separation step sequentially utilizes a first-stage slag remover, a filtering solid-liquid separator and a second-stage centrifuge to carry out combined solid-liquid separation on the extract and the dregs flowing out of the dynamic extraction tank, an intermediate storage tank 1 and a high-level intermediate storage tank 2 are arranged between the filtering solid-liquid separator and the second-stage centrifuge,
the first-stage slag remover is a horizontal screw type slag remover, the filtering type solid-liquid separator is a wet oscillating screen, the second-stage centrifuge is a disc type separator,
the liquid inlet amount of the primary slag remover is set to be 4-6T/h, the rotating speed of a main motor of the primary slag remover is 2300-,
the number of the vibrating screen meshes of the wet oscillating screen is 100-250 meshes.
2. The automatic extraction method of precious traditional Chinese medicine according to claim 1, characterized in that: the decocting time range is 1-3 h.
3. The automatic extraction method of precious traditional Chinese medicine according to claim 1 or 2, characterized in that: the liquid inlet amount of the secondary centrifuge is set to be 3-4T/h, and the slag discharge period is as follows: 150-300 seconds, and the slag discharge time is 0.1-0.5 seconds.
4. The automatic extraction method of precious traditional Chinese medicine according to claim 1 or 2, characterized in that: the solvent is water, and the volume-mass ratio of the addition amount of the solvent to the noble fine raw materials to be extracted is 8-20.
5. The automatic extraction method of precious traditional Chinese medicine according to claim 1 or 2, characterized in that: the circulation times per hour of the forced circulation in the step (2) are 8-15.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202860175U (en) * | 2012-04-09 | 2013-04-10 | 王新 | Complete device capable of continuously producing and dynamically extracting traditional Chinese medicines |
| CN204671929U (en) * | 2015-04-02 | 2015-09-30 | 广州市络捷生物科技有限公司 | A kind of integrated continuous microjet low temperature extracts and clarification production system |
| CN205659433U (en) * | 2016-05-17 | 2016-10-26 | 北京和利康源医疗科技有限公司 | Traditional chinese medicine draws and separation solid -liquid apparatus |
| CN206950707U (en) * | 2017-06-19 | 2018-02-02 | 武汉爱民制药股份有限公司 | A kind of Chinese medicine extracts energy-efficient integrated complexes |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202860175U (en) * | 2012-04-09 | 2013-04-10 | 王新 | Complete device capable of continuously producing and dynamically extracting traditional Chinese medicines |
| CN204671929U (en) * | 2015-04-02 | 2015-09-30 | 广州市络捷生物科技有限公司 | A kind of integrated continuous microjet low temperature extracts and clarification production system |
| CN205659433U (en) * | 2016-05-17 | 2016-10-26 | 北京和利康源医疗科技有限公司 | Traditional chinese medicine draws and separation solid -liquid apparatus |
| CN206950707U (en) * | 2017-06-19 | 2018-02-02 | 武汉爱民制药股份有限公司 | A kind of Chinese medicine extracts energy-efficient integrated complexes |
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