CN111569523A - Automatic control device for separation of traditional Chinese medicine alcohol precipitation liquid medicine - Google Patents
Automatic control device for separation of traditional Chinese medicine alcohol precipitation liquid medicine Download PDFInfo
- Publication number
- CN111569523A CN111569523A CN201910116976.8A CN201910116976A CN111569523A CN 111569523 A CN111569523 A CN 111569523A CN 201910116976 A CN201910116976 A CN 201910116976A CN 111569523 A CN111569523 A CN 111569523A
- Authority
- CN
- China
- Prior art keywords
- alcohol precipitation
- pipette
- liquid
- traditional chinese
- chinese medicine
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000007788 liquid Substances 0.000 title claims abstract description 146
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 238000001556 precipitation Methods 0.000 title claims abstract description 77
- 239000003814 drug Substances 0.000 title claims abstract description 58
- 238000000926 separation method Methods 0.000 title abstract description 10
- 239000006228 supernatant Substances 0.000 claims abstract description 52
- 238000007667 floating Methods 0.000 claims description 15
- 238000003860 storage Methods 0.000 claims description 15
- 238000010521 absorption reaction Methods 0.000 claims description 10
- 238000005213 imbibition Methods 0.000 claims description 9
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 5
- 230000037452 priming Effects 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 239000000428 dust Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 25
- 238000010586 diagram Methods 0.000 description 15
- 238000000605 extraction Methods 0.000 description 14
- 230000035772 mutation Effects 0.000 description 13
- 239000000284 extract Substances 0.000 description 12
- 239000000047 product Substances 0.000 description 11
- 238000002474 experimental method Methods 0.000 description 10
- 230000001376 precipitating effect Effects 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000004364 calculation method Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000013049 sediment Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 241000304195 Salvia miltiorrhiza Species 0.000 description 4
- 235000011135 Salvia miltiorrhiza Nutrition 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000012869 ethanol precipitation Methods 0.000 description 4
- 239000010231 banlangen Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000006187 pill Substances 0.000 description 3
- 239000009636 Huang Qi Substances 0.000 description 2
- 235000003143 Panax notoginseng Nutrition 0.000 description 2
- 241000180649 Panax notoginseng Species 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000009277 Panax notoginseng extract Substances 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 235000019206 astragalus extract Nutrition 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 230000007012 clinical effect Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000007721 medicinal effect Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- -1 organic acid salt Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000008247 solid mixture Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 238000010977 unit operation Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/04—Combinations of filters with settling tanks
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses an automatic control device for separating traditional Chinese medicine alcohol precipitation liquid medicine, belongs to the field of pharmaceutical devices, and aims to solve the problem of effective separation of supernatant of a dust removal tank.
Description
Technical Field
The invention relates to the field of pharmacy, in particular to an automatic control device for separating traditional Chinese medicine alcohol precipitation liquid medicine.
Background
The chemical components contained in the traditional Chinese medicinal materials are very complex, and not only contain various effective components, but also have ineffective components and also contain toxic components. Extracting the effective components of the effective monomers, and further separating and purifying the effective components to obtain the effective monomers is an important content in the research field of traditional Chinese medicines. The extraction of the traditional Chinese medicine is to extract the effective components in the traditional Chinese medicine to the maximum extent by utilizing some extraction technologies, so that the internal quality and the clinical treatment effect of the traditional Chinese medicine preparation are improved, and the effect of the traditional Chinese medicine is exerted to the maximum extent.
The extraction of Chinese medicine is an important unit operation in the production process of Chinese medicine, and the selection of the technological process and the equipment configuration of the method are directly related to the quality and the clinical effect of the Chinese medicine. The extract of traditional Chinese medicine materials obtained by decocting, soaking, alcohol extraction and other methods is a liquid-solid mixture, generally contains a lot of mud sand, dregs of a decoction pieces and particles, and impurities such as macromolecular colloids without medicinal effects, which are usually main factors influencing the volume, clarity, taste and the like of a medicinal preparation, so that the liquid medicine needs to be separated from the dregs of a decoction.
The ethanol precipitation method is a commonly used method for purifying and refining the traditional Chinese medicine water extract. The principle of the method is as follows: the medicinal materials are decocted with water for extraction, wherein the effective components of the water solution of alkaloid, organic acid salt, amino acid and the like are extracted, and a plurality of water-soluble impurities are extracted. The alcohol precipitation method is to dissolve the effective components in ethanol and precipitate the impurities after adding ethanol by utilizing the characteristic that the effective components can be dissolved in ethanol and the impurities are not dissolved in ethanol. The aim of alcohol precipitation is to remove impurities and retain effective components of the medicine, so the operation process of the alcohol precipitation unit and the applicability of the equipment thereof are closely related to the safety, stability and effectiveness of the traditional Chinese medicine product and are inseparable organic whole with the dosage form and quality of the product.
During the extraction process of the traditional Chinese medicine, after the ethanol precipitation and standing, the liquid medicine is layered, the upper layer is clear liquid, and the lower layer is sediment. The traditional operation method is that supernatant is manually sucked into a storage tank, and the operation is finished after the supernatant reaches the layered liquid level by visual observation. The traditional solid-liquid separation end point judgment method comprises the following steps: the visual clarification has strong subjectivity, incomplete or excessive suction, waste of supernatant or the phenomenon that a suction pipe enters a medicine residue area to cause sediment to be mixed into a product, and the quality stability of the product is influenced; the separation end point is judged manually, and digital and automatic control is difficult to realize. The quantification of the method for judging the solid-liquid separation endpoint of traditional Chinese medicine extraction and alcohol precipitation is one of the technical control problems in the traditional Chinese medicine industry.
Disclosure of Invention
In order to solve the technical problem, the application provides a traditional chinese medicine alcohol precipitation liquid medicine separation automatic control device, and this device can realize the effective separation of supernatant and sediment dregs of a decoction in the alcohol precipitation jar automatically.
In order to achieve the purpose, the invention adopts the following technical scheme:
an automatic control device for separating Chinese medicinal alcohol precipitation medicinal liquid comprises alcohol precipitation tank, pipette, limiting device, PLC (programmable logic controller), filter, supernatant storage tank, liquid absorption power source, turbidity meter and/or pressure sensor; the inlet end of the pipette extends into the supernatant layer in the alcohol precipitation tank, and the outlet end of the pipette is positioned outside the alcohol precipitation tank and is movably connected to the alcohol precipitation tank through a limiting device so that the inlet end of the pipette moves at different heights; one end of the filter is connected with the outlet end of the pipette, and the other end of the filter is connected with the supernatant storage tank; the turbidity meter is connected to the liquid outlet pipe between the filter and the supernatant storage tank; the two pressure sensors are respectively arranged at the front and the rear parts of the filter; PLC is through collecting pressure sensor and turbidity appearance feedback's pressure differential and turbidity information to the start-stop of control pipette imbibition.
Further, the pipette is sealed and movably connected to the side wall or the upper end enclosure of the alcohol precipitation tank.
Further, when the pipette is movably connected to the side wall of the alcohol precipitation tank, the pipette is a hard bent pipe consisting of an outlet end of the vertical pipe wall and an inlet end which is not in contact with the pipe wall and forms an angle of 0-90 degrees; the limiting device is a rotary liquid discharging device connected to the outlet end of the pipette, the rotary liquid discharging device comprises a fixed part and a rotatable rotating part nested in the fixed part, the fixed part is used for connecting the pipette to the side wall of the alcohol precipitation tank in a sealing manner, and the rotating part is fixedly connected with the pipette and is rotatably connected with a motor; the rotation speed, the steering and the starting and stopping of the motor are regulated and controlled by the PLC according to the feedback pressure difference and turbidity information.
Furthermore, a gear is sleeved on the rotating part of the rotary liquid outlet device and is in meshed connection with a shaft rod; the shaft is connected directly or through a three-way connector to the motor, which transfers the rotation of the motor to the gear through which the rotating part and the pipette are driven to rotate.
Further, when the axostylus axostyle passes through three way connection ware to be connected in the motor, be equipped with a hand wheel on the axostylus axostyle, rotate with the drive axostylus axostyle through rotatory this hand wheel.
Further, when the pipette is movably connected to the upper end enclosure of the alcohol precipitation tank, the pipette is a vertically arranged hard hollow screw rod with threads on the outer wall; the limiting device comprises a screw rod nut in threaded fit with the liquid suction pipe, the screw rod nut is sleeved on the liquid suction pipe and is connected to a motor in a rotating mode, and the motor drives the screw rod nut to rotate so as to enable the liquid suction pipe to move in the vertical direction; the rotation speed, the steering and the starting and stopping of the motor are regulated and controlled by the PLC according to the feedback pressure difference and turbidity information.
Further, the motor is a servo motor or a stepping motor.
Further, when the pipette is movably connected to the upper end enclosure of the alcohol precipitation tank, the pipette is a hose which is vertically arranged; the limiting device comprises a floating ball and a guide rail, the guide rail is fixed on the side wall of the alcohol precipitation tank in parallel, and the floating ball is fixedly connected to the inlet end of the liquid suction pipe and is connected with the guide rail in a sliding mode.
Further, the imbibition power source is a vacuum system, negative pressure is formed through the vacuum system, and supernatant in the alcohol precipitation tank is imbibed from the imbibition pipe, and the vacuum system comprises a vacuum display instrument and a vacuum proportion adjusting valve.
Further, the imbibition power supply is a delivery pump by PLC control, inhales the supernatant in the alcohol precipitation jar from the pipette through this delivery pump, and this delivery pump includes self priming pump, centrifugal pump, measuring pump.
Furthermore, valves are arranged on the liquid suction pipe and the liquid outlet pipe, and the opening and the closing of the valves are controlled by the PLC.
The liquid suction pipe of the device sucks the supernatant in the alcohol precipitation tank, along with the sucking of the supernatant, the pressure difference between two ends of the filter changes when the liquid level exceeds the position of the liquid suction pipe, and simultaneously signals are input to the PLC; when the floating ball is adopted to control the position of the liquid washing pipe, the floating ball can drive the liquid suction pipe to descend along with the descending of the liquid level, suspended matters are gradually increased along with the descending of the liquid level, the pressure difference of the filter is increased, the turbidity is gradually increased, and the descending speed is checked according to the liquid outlet flow rate. After the pipette was close the layering liquid level, the liquid turbidity of output increased, and the dregs of a decoction also can be more and more simultaneously, and the numerical value change of turbidity appearance can feed back to PLC this moment, and after turbidity was greater than product technological requirement, PLC will control the pipette and stop, and control liquid pipeline valve closed simultaneously. In the same way, the pressure difference between the two ends of the filter is increased along with the increase of the medicine residues, the pressure difference value is returned to the PLC, and if the pressure difference value exceeds the process set value, the PLC controls the liquid suction pipe and the liquid outlet pipe valve to stop and close. When any signal of the two feedback signals exceeds a set value, the liquid discharge is judged to be finished, and the pipette returns to the initial position.
The flow rate of supernatant in the tank body is kept stable in the output process, the inlet end of a supernatant liquid suction pipe is required to descend along with the descending of the liquid level, the inlet end of the liquid suction pipe is always covered by the liquid level so as to keep the supernatant liquid in a stable state when passing through a turbidity meter, and the detected data is stable and accurate. When the value detected by the turbidity meter is increased and reaches the liquid suction end point standard value range, the PLC controls the driving motor to stop and the liquid suction pipe is stopped, and liquid discharge is finished. The pressure difference between the two ends of the filter can also reach the standard range value before reaching the end point, the value can be used as an auxiliary index for judging the end point, and meanwhile, the filter can prevent medicine dregs from entering a product when liquid outlet is abnormal.
The method has the advantages that the liquid absorption end point can be quickly judged by online detection of the alcohol precipitation liquid through the turbidity meter, and the phenomenon that the liquid absorption end point is incompletely or excessively absorbed due to subjectivity of manual judgment to cause supernatant waste or the phenomenon that the liquid absorption tube enters a medicine residue area to cause sediment to be mixed into a product to influence the quality stability of the product is avoided. The device solves the problem that the separation end point is judged manually and the digital and automatic control is difficult to realize. Turbidity appearance mainly carries out the turbidity detection of quality of water in fields such as municipal water supply, drinking water treatment plant, sewage treatment plant, chemical industry, does not have the application yet in traditional chinese medicine extraction field, and traditional chinese medicine alcohol precipitation liquid medicine is the ethanol solution, and this device uses turbidity appearance to detect the ethanol solution turbidity, is the first application in traditional chinese medicine extraction field.
Drawings
Fig. 1 is a structural diagram of an automatic control device for separating a traditional Chinese medicine alcohol precipitation liquid medicine in embodiment 1.
In the figure: 101-alcohol precipitation tank, 102-pipette, 103-filter, 104-pressure sensor, 105-turbidimeter, 106-supernatant storage tank, 107-rotary liquid outlet device, 108-servo motor, 109-three-way connector and 110-hand wheel.
Fig. 2 is a structural diagram of a liquid suction device in the alcohol precipitation tank in example 1.
In the figure: 201-an alcohol precipitation tank, 202-a pipette, 203-a filter, 204-a pressure sensor, 205-a turbidimeter, 206-a supernatant storage tank, 207-a screw rod and 208-a stepping motor.
Fig. 3 is a structural diagram of an automatic control device for separating a traditional Chinese medicine alcohol precipitation solution in embodiment 2.
In the figure: 301-alcohol precipitation tank, 302-pipette, 303-filter, 304-pressure sensor, 305-turbidimeter, 306-supernatant storage tank, 307-floating ball and 308-guide rail.
Fig. 4 is a structural diagram of a liquid suction device in an alcohol precipitation tank in example 2.
Fig. 5 is a structural diagram of an automatic control device for separating a traditional Chinese medicine alcohol precipitation solution in embodiment 3.
Fig. 6 is a structural diagram of a liquid suction device in an alcohol precipitation tank in example 3.
Fig. 7 is a diagram of the pipette inlet end position in example 1.
Fig. 8 is a schematic view of a pipette rotating shaft in example 1.
FIG. 9 is a turbidity curve diagram of the process of extracting, alcohol precipitating and sucking clear liquid from compound Saviae Miltiorrhizae radix dripping pill.
FIG. 10 is a partially enlarged view of turbidity curve of compound Saviae Miltiorrhizae radix dripping pill during extraction, alcohol precipitation and clear liquid suction.
FIG. 11 is a turbidity curve diagram of the process of extracting, alcohol precipitating and sucking clear liquid from the water extract of nourishing blood and refreshing brain.
FIG. 12 is a partial enlarged view of turbidity curve of blood-nourishing and brain-refreshing water extract during extraction, alcohol precipitation and clear liquid suction.
FIG. 13 is a turbidity curve diagram of the process of extracting, alcohol precipitating and sucking clear liquid from the extract of Salvia miltiorrhiza Bunge and Panax notoginseng.
FIG. 14 is a partial enlarged view of turbidity curve during the process of extracting, alcohol precipitating and sucking clear liquid from Salvia miltiorrhiza Bunge and Panax notoginseng Burk extract.
FIG. 15 is a turbidity curve diagram of the process of extracting, alcohol precipitating and sucking clear liquid from radix astragali extract.
FIG. 16 is a partial enlarged view of turbidity curve of the process of extracting, alcohol precipitating and sucking clear liquid from radix astragali extract.
FIG. 17 is a turbidity curve diagram of the process of extracting radix Isatidis extract, precipitating with ethanol, and sucking clear liquid.
FIG. 18 is a partially enlarged view of turbidity curve of the process of extracting radix Isatidis extract, precipitating with ethanol, and sucking clear liquid.
Detailed Description
In order to make the aforementioned and other features and advantages of the invention more comprehensible, embodiments accompanied with figures are described in detail below.
Fig. 1 is a structural diagram of an automatic control device for separating a traditional Chinese medicine alcohol precipitation liquid medicine disclosed in this embodiment 1, wherein a pipette 102 is fixed on a side wall of an alcohol precipitation tank 101, a limiting device is a rotary liquid discharge device 107, and as shown in fig. 2, a motor is connected above the rotary liquid discharge device 107, the motor is a servo motor or a stepping motor, and the servo motor 108 is selected in this embodiment. The pipette 102 is a hard bent pipe with a corner, the outlet end of the pipette 102 is hermetically fixed on the side wall of the alcohol precipitation tank 101 through a rotary liquid discharging device 107, the inlet end entering the tank body and the tank wall form 0-90 degrees, the pipette 102 can rotate 360 degrees by taking the outlet end as an axis, the inlet end is optimally close to the vertical position, but the inner wall and the stirring paddle cannot be touched. The rotary liquid outlet device 107 comprises a fixed part and a rotating part, the rotating part is connected with a gear, and the gear is rotationally connected with a servo motor 108 through a shaft rod and a three-way connector 109. The servo motor 108 controls the intake end of the pipette 102 to rotate at a technically set angular velocity with high precision, thereby decreasing the arc-shaped velocity of the pipette 102.
The upper end of the shaft of the rotary tapping device 107 is provided with a hand wheel 110 for manual rotation to change the height of the inlet end of the pipette 102. The outlet end of the pipette 102 is connected to a filter 103, and the filter 103 is connected to a supernatant reservoir 106. A turbidity meter 105 for detecting the turbidity of the liquid is arranged on the liquid outlet pipe between the filter 103 and the supernatant storage tank 106. Pressure sensors 104 are provided before and after the filter 103 to detect a liquid pressure difference before and after the filter 103. The PLC (not shown) collects the liquid pressure difference and turbidity information fed back from the pressure sensor 104 and the turbidity meter 105, and performs PID control on the servo motor 108 to control the height of the inlet end of the pipette 102.
Fig. 3 is a structural diagram of an automatic control device for separating a traditional Chinese medicine alcohol precipitation liquid disclosed in this embodiment 2, wherein a pipette 202 is fixed to an upper head of an alcohol precipitation tank 201, and a limiting device is a lead screw nut 207, as shown in fig. 4. The sealed rotation of pipette 202 is connected at alcohol precipitation jar 201 upper cover, and the outer wall of pipette 202 contains the screw thread, is stereoplasm spiral lead screw structure. The pipette 207 can be linearly moved at a uniform speed in the direction perpendicular to the liquid level by the rotation of the feed screw nut 207. The device for driving the feed screw nut 207 can be a high-precision controllable device such as a servo motor or a stepping motor, and the stepping motor 208 is selected in the embodiment. The stepper motor 208 controls the pipette 202 outlet end to rotate in the vertical direction at a process-set angular velocity with high precision, thereby causing the pipette 202 to descend linearly. The structure of other parts of the automatic control device for separating the traditional Chinese medicine alcohol precipitation liquid medicine is the same as that of the previous embodiment, and the details are not repeated herein.
Fig. 5 is a structural diagram of an automatic control device for separating a traditional Chinese medicine alcohol precipitation liquid disclosed in this embodiment 3, wherein a pipette 302 is fixed to an upper head of an alcohol precipitation tank 301, and a limiting device is a floating ball 307 and a guide rail 308, as shown in fig. 6. The pipette 302 enters the tank body from the upper end socket of the alcohol precipitation tank 301 and is a hose, the floating ball 307 is positioned at the lower end of the pipette 302, the inlet end of the pipette 302 is connected with the floating ball 307, the guide rail 308 is installed on the side wall of the alcohol precipitation tank 301 and is parallel to the side wall of the alcohol precipitation tank 301, and one end of the floating ball 307 is connected with the guide rail 308. The float 307 moves with the liquid level by buoyancy and the constraint of the guide rail 308. The device does not need to be provided with a motor, so that the PLC only needs to control the valves on the liquid suction pipe and the liquid outlet pipe to be opened and closed. The structure of other parts of the automatic control device for separating the traditional Chinese medicine alcohol precipitation liquid medicine is the same as that of the previous embodiment, and the details are not repeated herein.
After the alcohol precipitation liquid level in the alcohol precipitation tank is layered, the initial position of the pipette is at the supernatant position, the pipette generates vacuum under the power of the liquid absorption power source, and liquid discharge is started. As in one embodiment, the suction power source employs vacuum delivery: a supernatant storage tank connected with the supernatant conveying pipeline is vacuumized, and the supernatant is sucked into the storage tank under the condition of negative pressure of the pipeline; the vacuum power can be a public vacuum system of a workshop, and can also be independently connected with a vacuum pump for use, and the vacuum can be more stable by installing a vacuum display instrument in the system and installing a proportion regulating valve on a vacuum pipeline, so that the aim of stabilizing the flow rate of the conveyed liquid is fulfilled. In another embodiment, the suction power source is delivered using a self-priming pump: and connecting a supernatant liquid outlet pipeline to an inlet of a self-sucking pump, and conveying the material to a storage tank through an outlet of the self-sucking pump. In another embodiment, the liquid suction power source is delivered by pumps such as a centrifugal pump and a metering pump: the precondition for the use of such a pump is that the reservoir and the pump can be filled with material in a communicating state before starting.
Device regulation principle of example 1
In the initial position, the pipette is in horizontal position, the supernatant is higher than the pipe orifice, and the residue is lower than the pipe orifice. After the supernatant liquid begins to flow out, the liquid level is reduced, and after the liquid level is reduced to a specified distance above the pipe orifice (distance standards can be established according to the allowable loss of products and the precision of the device), the liquid outlet is driven by a motor to be reduced at a constant speed. According to the effluent flow rate Q (m)3H) and the sectional area M (M) of the cylindrical tank body2) The velocity V (m/h) at which the pipette entry end needs to descend along the liquid surface can be calculated. After the calculation result of the descending speed of the inlet end, the rotating speed N (r/min) of the pipette can be calculated according to the size of the pipette, and the rotating speed ratio coefficient K of the motor and the rotating speed of the pipette can be used for calculating the rotating speed of the pipetteSo as to calculate the rotating speed of the transmission motor and control the rotation speed through a PLC. And stopping the vehicle after the turbidity meter detects that the vehicle meets the parking standard.
The calculation process is specifically described as follows (as shown in fig. 8):
the known conditions are: h (m) is the initial liquid level of the supernatant (detected value of the liquid level sensor), R (m) is the contribution length of the pipette on the vertical surface, L (m) is the vertical distance from the initial position of the inlet end to the rotating shaft of the pipette, theta (DEG) is the initial position angle of the pipette, and Q (m)3And/h) is the effluent flow rate of the supernatant (detected value of the flow rate sensor).
The control requirements are as follows: the intake end of the pipette descends at a constant speed in the vertical direction and, at the ith position, descends by L relative to the initial positioniAt the i +1 th position, L is decreasedi+1Requires Li+1＝Li；
Calculating the requirement: the rotation angle change at the i-th and i + 1-th positions is θi+1；
The control calculation formula is as follows:
after the program sets the liquid level to reach the distance h above the initial position of the intake end of the pipette, the pipette begins to descend, namely the pipette begins to run after the time T after the liquid discharge begins.
T ═ H)/[ Q/cylinder can cross-sectional area]＝(H-h)/Q*πr2(r is the radius of the can body);
operation equation L of liquid outlet pipei＝Li+1Q/cylinder can body section area Q/pi r2；
According to the triangular relationship:
θn＝90-θ-θi-θi+1；
L+Li+Li+1＝Rcosθn＝Rcos(90-θ-θi-θi+1)；
deducing:
Li+L＝Rcos(90-θ-θi-θi+1)-Li+1；
in the same way, the method for preparing the composite material,
L＝Rcos(90-θ)；
Li+L＝Rcos(90-θ-θi)；
therefore, the temperature of the molten metal is controlled,
Rcos(90-θ-θi-θi+1)-Li+1＝Rcos(90-θ-θi)。
multiplying the transmission coefficient K by the formula angle change relationship, and converting the result into a PLC program to drive the motor.
Device regulation principle of example 2
And (3) setting the initial position, wherein the pipe orifice of the liquid absorption pipeline in the tank is positioned below the liquid level of the supernatant for a specified distance (a distance standard can be set according to the allowable loss of the product and the precision of the device). The liquid level of the supernatant liquid drops after the supernatant liquid begins to flow out, and the liquid outlet pipe is driven by the motor to drop at the same speed as the liquid level. According to the effluent flow rate Q (m)3H) and the sectional area M (M) of the cylindrical tank body2) The velocity V (m/h) at which the pipette tip needs to descend along the liquid level can be calculated. After the calculation result of the descending speed of the liquid outlet is obtained, the rotating speed of the transmission motor can be calculated through the speed ratio coefficient K of the motor and the screw nut, and the rotating speed is controlled through the PLC. And stopping the vehicle after the turbidity meter detects that the vehicle meets the parking standard.
And (3) calculating:
the control calculation formula is as follows:
Before imbibition, according to the liquid level position H and the initial position H of imbibition inlet end1And the liquid absorption requires the depth h of the inlet end entering the liquid level, calculates the distance S required to be lowered at the inlet end, and controls the inlet end to be lowered to a specified position through a PLC.
S＝H1-H+h；
After the liquid absorption is started, the vertical descending speed of the device is equal to the liquid level descending speed;
V＝Q/πr2；
calculating the rotation speed of the motor according to the transmission coefficient K;
V1＝KV；
and converting the formula into a PLC program for control.
Device regulation principle of example 3
At the initial position, the floating ball floats on the liquid level of the supernatant, and the pipe orifice of the liquid outlet pipe below the floating ball is arranged below the liquid level. The liquid level of the supernatant liquid drops after the supernatant liquid begins to go out, the floating ball synchronously drops along with the liquid level under the action of buoyancy, and the turbidity meter stops after detecting that the turbidity meter meets the parking standard.
And (3) calculating:
according to the buoyancy and the gravity action of the floating ball, the inlet end of the liquid suction port can be kept below the liquid level, so that a motor for controlling the operation of the liquid suction inlet end does not need to be added.
The device provided by the invention can realize the solid-liquid separation effect, automatically and intelligently operate, and improve the automatic control level of the traditional Chinese medicine industry; the second-time end point judgment is scientific, stable and improves the product quality.
To prove the advantages of the device provided by the invention, five groups of detection experiments are used for explaining, the turbidity of the liquid entering the supernatant liquid storage tank is detected by a turbidity meter, and if the turbidity of the liquid is always within an allowable range in the whole allowable process of the device, the device provided by the invention is proved to be capable of automatically separating the supernatant liquid and the sediment dregs.
TABLE 1
| Time of day | Turbidity Range NTU | Mean value NTU | Less than or equal to 55NTU percent of pass |
| 5min later until the mutation point | 9.3-40.6 | 24.2 | 100％ |
TABLE 2
| Time of day | Turbidity Range NTU | Mean value NTU | Less than or equal to 55NTU percent of pass |
| 5min later until the mutation point | 17.5-31.5 | 25.0 | 100％ |
TABLE 3
| Time of day | Turbidity Range NTU | Mean value NTU | Less than or equal to 55NTU percent of pass |
| 5min later until the mutation point | 6.2-44.4 | 23.4 | 100％ |
TABLE 4
| Time of day | Turbidity Range NTU | Mean value NTU | Less than or equal to 55NTU percent of pass |
| 5min later until the mutation point | 9.7-47.8 | 19.7 | 100％ |
TABLE 5
| Time of day | Turbidity Range NTU | Mean value NTU | Less than or equal to 55NTU percent of pass |
| 5min later until the mutation point | 14.4-47.0 | 24.1 | 100％ |
From the five experiments, it can be known that the device provided in the embodiment stops liquid suction when the turbidity reaches the mutation point, so that the turbidity of the sucked supernatant is in the allowable range, and the turbidity qualification rate of the collected supernatant is 100 percent, so that the device can effectively and automatically separate the supernatant from the precipitated dregs.
As for the judgment of mutation point, the above experiment was conducted by judging the mutation point by a nephelometer alone. The mutation point can also be judged by two pressure sensors positioned in front of and behind the filter independently, namely after the supernatant is absorbed, the sediment dregs below are blocked at the filter after being absorbed, the pressure difference between the front of and behind the filter can be caused to generate mutation, and the mutation point is judged. Therefore, the device to be protected in the invention can adopt a turbidity meter independently, can also adopt a pressure sensor independently, and can also adopt the turbidity meter and the pressure sensor to judge the mutation point simultaneously.
The above embodiments are only intended to illustrate the technical solution of the present invention and not to limit the same, and a person skilled in the art can modify the technical solution of the present invention or substitute the same without departing from the spirit and scope of the present invention, and the scope of the present invention should be determined by the claims.
Claims (10)
1. An automatic control device for separating traditional Chinese medicine alcohol precipitation liquid medicine is characterized by comprising an alcohol precipitation tank, a pipette, a limiting device, a PLC (programmable logic controller), a filter, a supernatant storage tank, a liquid absorption power source, a turbidity meter and/or a pressure sensor; the inlet end of the pipette extends into the supernatant layer in the alcohol precipitation tank, and the outlet end of the pipette is positioned outside the alcohol precipitation tank and is movably connected to the alcohol precipitation tank through a limiting device so that the inlet end of the pipette moves at different heights; one end of the filter is connected with the outlet end of the pipette, and the other end of the filter is connected with the supernatant storage tank; the turbidity meter is connected to the liquid outlet pipe between the filter and the supernatant storage tank; the two pressure sensors are respectively arranged at the front and the rear parts of the filter; PLC is through collecting pressure sensor and turbidity appearance feedback's pressure differential and turbidity information to the start-stop of control pipette imbibition.
2. The automatic control device for separating traditional Chinese medicine alcohol precipitation liquor as claimed in claim 1, wherein the pipette is hermetically and movably connected to the side wall or the upper end enclosure of the alcohol precipitation tank.
3. The automatic control device for separating traditional Chinese medicine alcohol precipitation liquor according to claim 2, wherein the pipette is a hard bent tube composed of an outlet end of a vertical tube wall and an inlet end which is not in contact with the tube wall and forms an angle of 0-90 degrees when being movably connected to the side wall of the alcohol precipitation tank; the limiting device is a rotary liquid discharging device connected to the outlet end of the pipette, the rotary liquid discharging device comprises a fixed part and a rotatable rotating part nested in the fixed part, the fixed part is used for connecting the pipette to the side wall of the alcohol precipitation tank in a sealing manner, and the rotating part is fixedly connected with the pipette and is rotatably connected with a motor; the rotation speed, the steering and the starting and stopping of the motor are regulated and controlled by the PLC according to the feedback pressure difference and turbidity information.
4. The automatic control device for separating Chinese medicinal alcohol precipitation liquor according to claim 3, wherein a gear is sleeved on the rotating part of the rotary liquor discharge device, and the gear is engaged with a shaft rod; the shaft is connected directly or through a three-way connector to the motor, which transfers the rotation of the motor to the gear through which the rotating part and the pipette are driven to rotate.
5. The automatic control device for separating the liquid medicine after traditional Chinese medicine alcohol precipitation according to claim 4, wherein when the shaft lever is connected to the motor through the three-way connector, a hand wheel is provided on the shaft lever, and the hand wheel is rotated to drive the shaft lever to rotate.
6. The automatic control device for separating the traditional Chinese medicine alcohol precipitation liquor as claimed in claim 2, wherein the pipette is a vertically arranged hard hollow screw rod with threads on the outer wall when movably connected to the upper end enclosure of the alcohol precipitation tank; the limiting device comprises a screw rod nut in threaded fit with the liquid suction pipe, the screw rod nut is sleeved on the liquid suction pipe and is connected to a motor in a rotating mode, and the motor drives the screw rod nut to rotate so as to enable the liquid suction pipe to move in the vertical direction; the rotation speed, the steering and the starting and stopping of the motor are regulated and controlled by the PLC according to the feedback pressure difference and turbidity information.
7. The automatic control device for separating traditional Chinese medicine alcohol precipitation liquor as claimed in claim 2 or 6, wherein the motor is a servo motor or a stepping motor.
8. The automatic control device for separating traditional Chinese medicine alcohol precipitation liquor as claimed in claim 1, wherein the pipette is a vertically arranged hose when movably connected to the upper end enclosure of the alcohol precipitation tank; the limiting device comprises a floating ball and a guide rail, the guide rail is fixed on the side wall of the alcohol precipitation tank in parallel, and the floating ball is fixedly connected to the inlet end of the liquid suction pipe and is connected with the guide rail in a sliding mode.
9. The automatic control device for separating traditional Chinese medicine alcohol precipitation liquor as claimed in claim 1, wherein the liquid suction power source is a vacuum system, negative pressure is formed through the vacuum system, and supernatant in the alcohol precipitation tank is sucked from the liquid suction pipe, and the vacuum system comprises a vacuum display instrument and a vacuum proportion regulating valve; the imbibition power supply can also be by a transfer pump of PLC control, inhales the supernatant in the alcohol precipitation jar from the pipette through this transfer pump, and this transfer pump includes self priming pump, centrifugal pump, measuring pump.
10. The automatic control device for separating traditional Chinese medicine alcohol precipitation liquor as claimed in claim 1, wherein valves are arranged on the liquid suction pipe and the liquid outlet pipe, and the valves are controlled to be opened and closed by PLC.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910116976.8A CN111569523A (en) | 2019-02-15 | 2019-02-15 | Automatic control device for separation of traditional Chinese medicine alcohol precipitation liquid medicine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910116976.8A CN111569523A (en) | 2019-02-15 | 2019-02-15 | Automatic control device for separation of traditional Chinese medicine alcohol precipitation liquid medicine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111569523A true CN111569523A (en) | 2020-08-25 |
Family
ID=72114800
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910116976.8A Pending CN111569523A (en) | 2019-02-15 | 2019-02-15 | Automatic control device for separation of traditional Chinese medicine alcohol precipitation liquid medicine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111569523A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114100208A (en) * | 2022-01-24 | 2022-03-01 | 江苏中有信科技有限公司 | Alcohol precipitation solvent flow rate step control method, alcohol precipitation tank and artificial intelligence alcohol precipitation system |
Citations (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10230108A (en) * | 1997-02-20 | 1998-09-02 | Kurita Water Ind Ltd | Method and device for filtration |
| CN2298052Y (en) * | 1997-01-16 | 1998-11-25 | 黄永德 | Internal flow filter |
| JPH11128158A (en) * | 1997-10-27 | 1999-05-18 | Olympus Optical Co Ltd | Endoscope washing/sterilizing device |
| JP2001112863A (en) * | 1999-10-15 | 2001-04-24 | Kita Kyushu Biophysics Kenkyusho:Kk | On-line blood-dialyzing-filtering device, and blood- dialyzing-filtering process using the device |
| US20020099174A1 (en) * | 1996-03-08 | 2002-07-25 | Anna Johnston | Filtration of plasma mixtures using cellulose-based filter aids |
| CN102698484A (en) * | 2012-05-24 | 2012-10-03 | 靖江康爱特环境工程有限公司 | Full-automatic filter cake layer filter and filtering method thereof |
| CN203108280U (en) * | 2013-01-15 | 2013-08-07 | 武汉纽威制药机械有限公司 | Alcohol precipitation tank |
| CN103520949A (en) * | 2013-10-15 | 2014-01-22 | 四川省砚山中药饮片有限公司 | Complete equipment for continuous counter-current ultrasonic extraction |
| CN203598588U (en) * | 2013-09-02 | 2014-05-21 | 嵩县开拓者钼业有限公司 | Filtering system for collecting solid mineral grains from dilute phase superfine mineral suspension |
| CN103908798A (en) * | 2013-01-05 | 2014-07-09 | 天津天士力现代中药资源有限公司 | Method for extracting medicinal material by using turbidity detection |
| CN104014157A (en) * | 2013-03-01 | 2014-09-03 | 中石化上海工程有限公司 | Method for separating traditional Chinese medicine alcohol precipitation stewing liquid |
| CN105477901A (en) * | 2015-12-11 | 2016-04-13 | 苏州泽达兴邦医药科技有限公司 | Blockage judging and preventing device for liquid outlet in traditional Chinese medicine extraction process and control method |
| CN205340241U (en) * | 2016-01-18 | 2016-06-29 | 温州市洪都轻工机械有限公司 | Alcohol precipitation tank |
| CN106237706A (en) * | 2016-08-31 | 2016-12-21 | 广州市海同机电设备有限公司 | High-efficient automatic purifying plant |
| CN107088316A (en) * | 2017-07-06 | 2017-08-25 | 江苏北松健康产业有限公司 | Alcohol precipitation concentration systems and alcohol sinking system |
| CN206613349U (en) * | 2017-04-13 | 2017-11-07 | 合肥茂腾环保科技有限公司 | It is a kind of to handle the device that stripper reclaims the on-condensible gas produced |
| CN107335277A (en) * | 2017-06-22 | 2017-11-10 | 杭州利群环保纸业有限公司 | A kind of tobacco extract membrane separation device and control method |
| CN206965191U (en) * | 2017-07-06 | 2018-02-06 | 江苏北松健康产业有限公司 | Alcohol precipitation concentration systems and alcohol sinking system |
| CN108392896A (en) * | 2018-05-07 | 2018-08-14 | 山东胜星化工有限公司 | A kind of amine liquid removes the control system of coke powder purifier |
| CN207838379U (en) * | 2017-12-12 | 2018-09-11 | 江西和明制药有限公司 | A kind of efficiently automatic Alcohol-settling tank |
| CN108911276A (en) * | 2018-09-07 | 2018-11-30 | 刘寅平 | A kind of coal mine ceramic water film purifying device and its filtering and backwash method |
| CN109011734A (en) * | 2018-08-20 | 2018-12-18 | 中石化上海工程有限公司 | A kind of device and method of traditional Chinese medicine extraction alcohol precipitation automatic feed/discharge |
| CN209646030U (en) * | 2019-02-15 | 2019-11-19 | 天津天士力现代中药资源有限公司 | A kind of Chinese medicine alcohol precipitation separating liquid medicine automatic control device |
-
2019
- 2019-02-15 CN CN201910116976.8A patent/CN111569523A/en active Pending
Patent Citations (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020099174A1 (en) * | 1996-03-08 | 2002-07-25 | Anna Johnston | Filtration of plasma mixtures using cellulose-based filter aids |
| CN2298052Y (en) * | 1997-01-16 | 1998-11-25 | 黄永德 | Internal flow filter |
| JPH10230108A (en) * | 1997-02-20 | 1998-09-02 | Kurita Water Ind Ltd | Method and device for filtration |
| JPH11128158A (en) * | 1997-10-27 | 1999-05-18 | Olympus Optical Co Ltd | Endoscope washing/sterilizing device |
| JP2001112863A (en) * | 1999-10-15 | 2001-04-24 | Kita Kyushu Biophysics Kenkyusho:Kk | On-line blood-dialyzing-filtering device, and blood- dialyzing-filtering process using the device |
| CN102698484A (en) * | 2012-05-24 | 2012-10-03 | 靖江康爱特环境工程有限公司 | Full-automatic filter cake layer filter and filtering method thereof |
| CN103908798A (en) * | 2013-01-05 | 2014-07-09 | 天津天士力现代中药资源有限公司 | Method for extracting medicinal material by using turbidity detection |
| CN203108280U (en) * | 2013-01-15 | 2013-08-07 | 武汉纽威制药机械有限公司 | Alcohol precipitation tank |
| CN104014157A (en) * | 2013-03-01 | 2014-09-03 | 中石化上海工程有限公司 | Method for separating traditional Chinese medicine alcohol precipitation stewing liquid |
| CN203598588U (en) * | 2013-09-02 | 2014-05-21 | 嵩县开拓者钼业有限公司 | Filtering system for collecting solid mineral grains from dilute phase superfine mineral suspension |
| CN103520949A (en) * | 2013-10-15 | 2014-01-22 | 四川省砚山中药饮片有限公司 | Complete equipment for continuous counter-current ultrasonic extraction |
| CN105477901A (en) * | 2015-12-11 | 2016-04-13 | 苏州泽达兴邦医药科技有限公司 | Blockage judging and preventing device for liquid outlet in traditional Chinese medicine extraction process and control method |
| CN205340241U (en) * | 2016-01-18 | 2016-06-29 | 温州市洪都轻工机械有限公司 | Alcohol precipitation tank |
| CN106237706A (en) * | 2016-08-31 | 2016-12-21 | 广州市海同机电设备有限公司 | High-efficient automatic purifying plant |
| CN206613349U (en) * | 2017-04-13 | 2017-11-07 | 合肥茂腾环保科技有限公司 | It is a kind of to handle the device that stripper reclaims the on-condensible gas produced |
| CN107335277A (en) * | 2017-06-22 | 2017-11-10 | 杭州利群环保纸业有限公司 | A kind of tobacco extract membrane separation device and control method |
| CN107088316A (en) * | 2017-07-06 | 2017-08-25 | 江苏北松健康产业有限公司 | Alcohol precipitation concentration systems and alcohol sinking system |
| CN206965191U (en) * | 2017-07-06 | 2018-02-06 | 江苏北松健康产业有限公司 | Alcohol precipitation concentration systems and alcohol sinking system |
| CN207838379U (en) * | 2017-12-12 | 2018-09-11 | 江西和明制药有限公司 | A kind of efficiently automatic Alcohol-settling tank |
| CN108392896A (en) * | 2018-05-07 | 2018-08-14 | 山东胜星化工有限公司 | A kind of amine liquid removes the control system of coke powder purifier |
| CN109011734A (en) * | 2018-08-20 | 2018-12-18 | 中石化上海工程有限公司 | A kind of device and method of traditional Chinese medicine extraction alcohol precipitation automatic feed/discharge |
| CN108911276A (en) * | 2018-09-07 | 2018-11-30 | 刘寅平 | A kind of coal mine ceramic water film purifying device and its filtering and backwash method |
| CN209646030U (en) * | 2019-02-15 | 2019-11-19 | 天津天士力现代中药资源有限公司 | A kind of Chinese medicine alcohol precipitation separating liquid medicine automatic control device |
Non-Patent Citations (1)
| Title |
|---|
| 陈勇;李页瑞;金胤池;蔡圣;程翼宇;瞿海斌;: "中药醇沉工艺及装备研究进展与思考", 世界科学技术-中医药现代化, no. 05, 15 October 2007 (2007-10-15) * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114100208A (en) * | 2022-01-24 | 2022-03-01 | 江苏中有信科技有限公司 | Alcohol precipitation solvent flow rate step control method, alcohol precipitation tank and artificial intelligence alcohol precipitation system |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101032447A (en) | Alcohol precipitating method and device based on the principle of hydraulic cyclone | |
| CN207237390U (en) | A kind of inclined-tube sedimentation tank for being provided with automatic mud removing system | |
| CN111569523A (en) | Automatic control device for separation of traditional Chinese medicine alcohol precipitation liquid medicine | |
| CN203971473U (en) | Alcohol-settling tank | |
| CN209646030U (en) | A kind of Chinese medicine alcohol precipitation separating liquid medicine automatic control device | |
| CN203803394U (en) | Automatic medicine dissolving device | |
| CN207699386U (en) | A kind of wastewater treatment equipment for breathing out fragrant slot workshop | |
| CN206886776U (en) | A kind of efficient dephosphorization fast reaction settler | |
| CN206334389U (en) | Astragalus polyose multistage continuous extracting device | |
| CN208711613U (en) | A kind of accurate dispensation apparatus | |
| CN206886925U (en) | A kind of heparin sodium wastewater processing unit | |
| CN107551956A (en) | Chemicals dosing plant | |
| CN215516780U (en) | Precipitation device for wastewater treatment | |
| CN205933460U (en) | Integration sewage treatment sedimentation tank | |
| CN2650844Y (en) | Automatic acid supplier of ceramic filter | |
| CN105664556B (en) | A kind of helixseal continuous pulp discharge filter for supercritical water treatment technique | |
| CN107050921A (en) | A kind of traditional Chinese medicine extraction acid adjustment device and traditional Chinese medicine extraction system | |
| CN110812884B (en) | Traditional Chinese medicine alcohol precipitation tank and alcohol precipitation method | |
| CN204588781U (en) | A kind of automatic drug feeding machine | |
| CN219429734U (en) | Accurate dosing device of sewage treatment | |
| CN208200564U (en) | A kind of sewage disposal system based on flocculation | |
| CN206965183U (en) | A kind of traditional Chinese medicine extraction acid adjustment device and traditional Chinese medicine extraction system | |
| CN220845706U (en) | Acidizing flow-back fluid treatment device | |
| CN207072835U (en) | The complete Airfloat filtering pond device of integration | |
| CN106237706A (en) | High-efficient automatic purifying plant |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |