CN109499094A - A kind of automation extraction separation method of powder decoction pieces Chinese medicine - Google Patents
A kind of automation extraction separation method of powder decoction pieces Chinese medicine Download PDFInfo
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- CN109499094A CN109499094A CN201811475864.3A CN201811475864A CN109499094A CN 109499094 A CN109499094 A CN 109499094A CN 201811475864 A CN201811475864 A CN 201811475864A CN 109499094 A CN109499094 A CN 109499094A
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0207—Control systems
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0215—Solid material in other stationary receptacles
- B01D11/0253—Fluidised bed of solid materials
- B01D11/0257—Fluidised bed of solid materials using mixing mechanisms, e.g. stirrers, jets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
- B01D11/0284—Multistage extraction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0292—Treatment of the solvent
-
- 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
- B01D36/045—Combination of filters with centrifugal separation devices
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Automation & Control Theory (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The present invention relates to a kind of automation extraction separation methods of powder decoction pieces Chinese medicine, this method includes that solid-liquid separation step is carried out to the extracting solution obtained by Dynamic Extraction, and the separating step is successively combined formula to the extracting solution and the dregs of a decoction that flow out out of dynamic extraction pot using first-stage centrifugal machine or slag remover, filtering type solid-liquid separating machine and two-stage centrifugal machine and is separated by solid-liquid separation.The present invention uses three-level solid-liquid separating equipment, can work continuously, will not generate filtering bottleneck, will not generate blocking, it can be achieved that continuous production, high production efficiency is at low cost, and the product light transmittance after separation is high, precipitating is few.
Description
Technical field
The present invention relates to Chinese medicine production technical field more particularly to a kind of automation extraction process technologies of Chinese medicine.
Background technique
Extraction is the primary link and important operation unit of Chinese medicine production, and the superiority and inferiority of technique directly influences the matter of product
Amount.Traditional Chinese medicine extracting method includes decocting method, infusion process, circumfluence method, percolation, Gelatin improving method etc., but conventional method is deposited
In more disadvantage: 1) decocting method loss of effective components is more, especially water insoluble active ingredient；2) organic solvent in extraction process
It is possible that acting on effective component, it is made to lose original effectiveness；3) extract yield is low, extraction time is long, technique is cumbersome；4) Chinese medicine
Manufacturing enterprise is often used multi-function extractor at present and directly feeds intake extraction, since conventional Multifunction tank during the extraction process cannot
The solvent around material is set to remain certain concentration difference, therefore extraction efficiency is lower, and the dregs of a decoction discharged can generally remain 1-2
Medical fluid again, easily causes certain waste.
Ultrasonic wave, microwave, supercritical CO are applied with the development of science and technology, gradually rising in recent years2The method of extraction carries out
It extracts, ultrasonic wave, multistage microwave amplifier can be obviously shortened extraction time, reduce energy consumption, but be not easy to realize commercial scale, and influence people
Health；Microwave has a fuel factor, at the same microwave may composition to material and property have an impact, and then influence product
Quality, microwave use be also restricted；Supercritical CO2Suitable for extracting liposoluble substance, and extraction conditions are harsh, are unfavorable for
Industrialized production, application range are relatively narrow.
CN102258883A discloses the dynamic circulation extracting method of a Plant Extracts, and plant material is in extraction process
It is middle that multiple dynamic circulation extraction is carried out using Extraction solvent, and use and force solvent circulation.Extraction solvent used is every time
1.5-3 times of material quality, solvent cycle-index are 2-5 times；Extracting total degree is 2-5 times.Work is extracted with conventional dynamic countercurrent
Skill is compared, and is had many advantages, such as that the raising of unit extract equipment utilization rate, apparatus adaptability are wide, simple for process, be can be applied to plant
The production of object extract is particularly suitable for the extraction of the plants active princlple such as thermal sensitivity, perishable.But the document is not specific
Provide such as cattail pollen, the extraction example of Liu Yi San powder decoction pieces Chinese medicine and extraction effect.
Traditional Chinese medicine extraction subsequent process is to be separated by solid-liquid separation, and dregs of a decoction physical features caused by different extraction processes are such as
The equal different froms such as viscosity, water content, solid granularity, and the form of the different Chinese medicine dregs of a decoction after extraction is also different, there is matter
Light floating material, also has sediment at suspended matter, for powder decoction pieces Chinese medicine, since powder decoction pieces have viscosity, are not readily separated,
Even the simple separation of solid and liquid of tradition, which configures advanced solid-liquid separating equipment, which to be also difficult to realize, both can guarantee filter efficiency and had divided
From effect, ensure that product quality indicator and economic indicator.
Patent CN107913543A discloses a kind of quick equipment for separating liquid from solid of Chinese medicine, including cabinet, the inside of cabinet are set
There are the components such as diaphragm plate, expects pipe, gear, booster pump stirring rod and heating pole, the device of the invention structure novel divides Chinese medicine
Good from effect, speed is fast, and the dregs of a decoction are removed conveniently, is conducive to promote.
Patent CN205659433U and CN204951634U disclose a kind of equipment for separating liquid from solid of Chinese medicine extract, on
Equipment for separating liquid from solid is stated single centrifuge separation mode is respectively adopted and is separated by solid-liquid separation with strainer.
Patent CN206492274U discloses a kind of Chinese medicine equipment for separating liquid from solid, and specifically discloses the separator and include
Filter there are two being sequentially connected from high to low: filter one and filter two, the filter and two detachable connections.It crosses
Filter is to include a filter screen, two filtering tanks of filter, which only passes through filter type and separated, point
Lower from efficiency, separating effect is poor, is not applied for the separation of different types of Chinese medicine.
Be separated by solid-liquid separation in addition, the prior art also has using ceramic membrane, which are mainly applied to clarity or effectively at
In the preparations such as the traditional Chinese medicine for dividing purity requirement high, but for Chinese medicinal granule or general Chinese medicine solid orally ingestible
Such as effective component will appear using ceramic membrane separation instead and shut off and is lost that big, membrane fouling control, which is not thorough, production efficiency is low asks
Topic.
However, above-mentioned equipment for separating liquid from solid is all made of simple solid-liquid separation method, separative efficiency is lower, separating effect compared with
Difference, and the type and property of Chinese medicine to be separated are clearly required, the separation for powder decoction pieces Chinese medical extract, by
It is easily adhered to filter cloth surface after powder veriety is decocted a drug wrapped, so that filter cloth mesh is become smaller and causes that extraction efficiency is low and drawing liquid difficulty etc.
Factor, it is difficult to use above-mentioned general solid-liquid separating equipment.
In addition, patent CN108125990A and CN102068464A disclose the extracting method of Medicated Leaven, but not
It is open to be extracted using dynamic extraction pot, it is also not publicly separated, is extracted and isolated effect using three-level separator
It is relatively low with efficiency.
Therefore, the extraction efficiency for how improving powder decoction pieces Chinese medicine improves paste-forming rate, the index components rate of transform of product,
And the key problem that separation is promotion powder decoction pieces traditional Chinese medicine quality and economic benefit effectively and efficiently is carried out to extracting solution.
Summary of the invention
Problems to be solved by the invention
In order to solve the above-mentioned technical problem of the prior art, it is an object of the invention to design a kind of powder decoction pieces Chinese medicine
Automation extraction separation method to improve the extraction efficiency and separative efficiency of powder decoction pieces Chinese medicine, improve product paste-forming rate,
The light transmittance of the index components rate of transform and finished product；Meanwhile separative efficiency is improved, improve separating effect, reduces production cost and energy
Consumption.
The solution to the problem
Technical solution provided by the present invention is a kind of automation extraction separation method of powder decoction pieces Chinese medicine, this method packet
Include following steps,
(1) it feeds intake:
Metered solvent and raw material to be extracted are pressed into dynamic extraction pot body；
(2) Dynamic Extraction:
After the completion of feeding intake, opens and the raw material and solvent to be extracted in tank are heated, automation control technique initialization temperature value；
The stirring in dynamic extraction pot is opened, while dynamic extraction pot heating, program automatically begins to record and extracts the setting decocted
Time, after extraction, which decocts setting time, to be reached, liquid obtains extracting solution out；
(3) solid-liquid separation step for the extracting solution that liquid out is obtained, the separating step successively utilize first-stage centrifugal machine or
Slag remover, filtering type solid-liquid separating machine and two-stage centrifugal machine are combined the extracting solution and the dregs of a decoction that flow out out of dynamic extraction pot
Formula is separated by solid-liquid separation.
Preferably, the first-stage centrifugal machine or slag remover are sedimentation-type centrifuge or slag remover, and preferably horizontal helical type removes the gred
Machine, the first-stage centrifugal machine or 2300-2600 revs/min of revolving speed of slag remover main motor, auxiliary-motor revolving speed be 1500-1900 turn/
Minute.
Preferably, the first-stage centrifugal machine or slag remover liquid inlet volume are set as 4~6T/ hours.
Preferably, the filtering type solid-liquid separating machine is wet type shaking screen, and the vibration grit number of the wet type shaking screen is
100~300, preferably 250 mesh.
Preferably, the two-stage centrifugal machine is sedimentation-type centrifuge, preferably disc separator, the two-stage centrifugal machine
Liquid inlet volume be set as 2~4T/ hours, the deslagging period: 150-350 seconds, the deslagging time be 0.1~0.5 second.
Preferably, the liquid inlet volume of the two-stage centrifugal machine is set as 3~4T/ hours, the deslagging period: 150-350 seconds, deslagging
Time is 0.1~0.5 second.
Preferably, the raw material to be extracted be selected from burnt Medicated Leaven, Liu Yi San, cattail pollen, charred POLLEN TYPHAE, excrementum pteropi, stir-baked FAECES TROGOPTERORI with vinegar,
Medicated Leaven one of builds bent and arisaema cum bile or a variety of.
Preferably, the solvent is water, the volume mass ratio of the additive amount of the solvent and raw material to be extracted is 8~
18:1.
Preferably, the temperature that step (2) Dynamic Extraction is set is 60~100 DEG C.
Preferably, step (2) decocts the time set as 30~180min.
The effect of invention
Compared with the prior art, the advantages of the present invention are as follows:
1) specific dynamic extraction pot is used, the circulating pump of dynamic extraction pot stirring motor T-M1 and dynamic extraction pot are utilized
The control of T-M2 high frequency reaches technique and requires forced circulation number, makes full use of diffusion principle, be quickly dissolved in medicinal material effective component
It in solvent, improves and extracts production efficiency, pressure makes the effective component on medicinal material surface reach certain concentration difference, and then improves and extract
Efficiency, the clarity of the index components rate of transform and product.
2) existing technique of decocting a drug wrapped is added water to cook after a certain amount of material to be packed into the small filter cloth bag of mesh, due to powder
Veriety is easily adhered to filter cloth surface after decocting a drug wrapped, and so that filter cloth mesh is become smaller and causes extraction efficiency low and drawing liquid difficulty, the present invention
It using three-level solid-liquid separating equipment, can work continuously, filtering bottleneck will not be generated, blocking will not be generated, it can be achieved that even
Continuous production, high production efficiency is at low cost, and the product melting after separation is good, and clarity is high, and light transmittance is high, and precipitating is few；It decocts
Automation control can be used, it can be achieved that automatic discharge in extracting solution whole process high temperature filtration afterwards, hygiene safety, save manpower at
This, reduces labor intensity.
3) present invention extracts separation to powder decoction pieces Chinese medicine by using Dynamic Extraction and three-level separation, and optionally right
The technological parameters such as master/motor speed of horizontal helical type slag remover, vibration grit number regulate and control, and the effective component rate of transform of product mentions
High 70% or more, finished product light transmittance improves 40% or more compared with original process, and the daily output also improves 32% or more compared with original process.
It compares and is separated by solid-liquid separation only with second level, the solid-liquid separating equipment that the present invention is applied in combination three kinds allows continuous production, no
Only the effective component rate of transform improves, at the same extract rush it is molten after light transmittance is high, melting is more preferable.
Detailed description of the invention
Fig. 1 is the structural schematic diagram that separator is extracted in Chinese medicine automation used in present invention automation extracting method.
Fig. 2 is the structural schematic diagram of Horizontal helical type centrifuge used in the present invention.
Description of symbols
T-1-dynamic extraction pot
T-2-horizontal helical type slag remover
T-3-wet type shaking screen
T-4-intermediate storage tank 1
T-5-intermediate storage tank 2
T-6-disc separator
T-7-extraction liquid storage tank
T-M1-dynamic extraction pot stirring motor
T-M2-dynamic extraction pot circulating pump
T-N1-dynamic extraction pot agitating paddle
T-N2-dynamic extraction pot circulation line
T-N3-extractor heating jacket
T-N4-extracting solution liquid control valve
TQRV-1-extractor jacket steam regulating valve
TQPT-1-extractor jacket steam pressure gauge
Steam pressure gauge in TQPT-2-extractor tank
Thermometer in TQTT-1-extractor tank
TQPV-1-extractor feed liquid control valve
TQLS-1-dynamic extraction pot liquid-level switch
1-auxiliary motor
2-main motors
3-differential mechanisms
4-rotary drums
5-discharge with endless screw devices
Specific embodiment
The present invention will be described in further detail below with reference to the embodiments of the drawings.
The present invention provides a kind of automation extraction separation method of powder decoction pieces Chinese medicine, which employs specific Chinese medicines certainly
Dynamicization extracts separator.
<separator is extracted in Chinese medicine automation>
As shown in Figure 1, separator is extracted in the automation of Chinese medicine used in the present invention comprising dynamic extraction pot T-1, combination
Formula is separated by solid-liquid separation component.
The tank body of the dynamic extraction pot T-1 is equipped with during the extraction process that recycle stock circulation extraction introducing tank is intracorporal
Circulation line T-N2, recycle stock include solvent and object to be extracted, and circulation line is equipped with circulating pump T-M2, circulation line and are followed
The design of ring pump to meet solvent and extract recycles together, and does not destroy the character of material in cyclic process, can make whole tank
Material can be quickly uniformly mixed, and extractor feed liquid control valve TQPV-1, dynamic extraction pot can be equipped on circulation line T-N2
Liquid-level switch TQLS-1 is also provided with the blow down branch for slag liquid discharge on circulation line.In the dynamic extraction pot
Chamber is equipped with multiple impellers T-N1, and agitating paddle is driven by dynamic extraction pot stirring motor T-M1, and agitating paddle is preferably provided with not in tank
Body axial centerline, agitating paddle are preferably three layers of agitating paddle, and top layer is press-down type, and the material of some floatings can be made to pass through
Stirring is sunk, and middle layer is horizontal, can promote diffusion horizontally outward, promotes material dynamic exchange, and lowest level is upper-turn-type,
By promoting rolling material upwards, material is avoided to be deposited on tank bottom.The design of the above agitating paddle, which can make to reach in tank, preferably to be stirred
Mix effect.The present invention is controlled using the circulating pump T-M2 high frequency of dynamic extraction pot stirring motor T-M1 and dynamic extraction pot, is reached
Technique requires forced circulation number, makes full use of diffusion principle, makes the effective elements of the medicine in powder decoction pieces (such as saponins, Huang
Ketone, alkaloids etc.) it is quickly dissolved in solvent, pressure makes the effective component on medicinal material surface reach certain concentration difference.
Dynamic extraction pot is additionally provided with feed intake unit and heating unit.The throwing of the unit that feeds intake completion solvent and raw material to be extracted
It puts, and delivering opportunity, injected volume is carried out and controlled, and open circulation and stirring launching terminal.Heating unit is to extraction body
System's heating makes temperature in extractor tank reach the temperature of technique initialization and be maintained at the temperature value of the technique initialization, is recorded in the work
Extraction time under the temperature value of skill setting.Heating unit includes extractor heating jacket T-N3, temperature in Detection and Extraction tank tank
Extractor tank in thermometer TQTT-1, be connected to extractor heating jacket steam pipe, the extraction on steam pipe pipeline is set
Tank jacket steam regulating valve TQRV-1, steam pressure gauge TQPT-2 in the extractor tank of steam pressure, inspection in Detection and Extraction tank tank
Survey the extractor jacket steam pressure gauge TQPT-1 of extractor jacket steam pressure.The present invention adjusts extractor collet by PID
Steam control valve TQRV-1 opening size, steadily reaches decoction temperature, effectively solves medicinal material after manual adjustment manual steam valve
The too fast, material that heats up when decoction runs material phenomenon.Preferably, each valve of dynamic extraction pot is controlled by PLC controller.Extraction terminates
Afterwards, by dynamic extraction pot extracting solution and the dregs of a decoction import combined type gas-liquid-solid together under the control of extracting solution liquid control valve T-N4
Liquid separation assembly is separated by solid-liquid separation.The dispensing unit of dynamic extraction pot includes the outlet tube with extracting solution liquid control valve T-N4
One end branch on road, the outlet tube road connects on circulation line, and the other end connects combined solid-liquid separation assembly.Of the invention one
In a possible embodiment, the bottom cover of dynamic extraction pot is not provided with filter plant.
Combined solid-liquid separation assembly of the present invention includes three solid-liquid separating equipments, is disposed with first-stage centrifugal machine
Or slag remover, filtering type solid-liquid separating machine and two-stage centrifugal machine, the first-stage centrifugal machine or slag remover, filtering type solid-liquid separating machine
Feed lines connection is passed sequentially through between two-stage centrifugal machine three.
Further, the first-stage centrifugal machine or slag remover are sedimentation-type centrifuge or slag remover, and effect is to by slag liquid
Carry out initial gross separation, with the difference of specific gravity separating most solid dregs of a decoction, in the specific embodiment of the present invention level-one from
Scheming or slag remover are preferably horizontal helical type slag remover T-2.Horizontal helical type slag remover is generally used for the fields such as water process, the invention
Property the biggish horizontal helical type slag remover for the treatment of capacity is used for traditional Chinese medicine extraction separation process, the traditional Chinese medicine extraction that compares separation is conventional to be used
The biggish link-suspended basket centrifuge for the treatment of capacity or flat centrifuge, horizontal helical type slag remover allow continuous production and inside it
Be conducive to the cleaning of the dregs of a decoction with screw machine structure.In the specific embodiment of the present invention, as shown in Fig. 2, sleeping spiral shell
Formula centrifuge includes rotary drum (4), discharge with endless screw device (5), motor, differential mechanism (3), and the discharge with endless screw device (5) is arranged in rotary drum
(4) in, walking feeding tube is inserted in discharge with endless screw device (5), one end of walking feeding tube is feed inlet, and the other end is as discharge port, rotary drum
(4) it close to one end of feed inlet as purified liquor outlet, is exported close to one end of discharge port as sediment, the motor includes being used for
Control the main motor (2) of charging and the auxiliary motor (1) for controlling differential mechanism (3).
By horizontal helical type slag remover, liquid enters filtering type solid-liquid separating machine out, and the effect of filtering type solid-liquid separating machine is logical
Partial size difference is crossed to separate, filter a small amount of impurity so that filtrate can satisfy the requirement of disc separator feed liquor.In this hair
Filtering type solid-liquid separating machine is wet type shaking screen T-3 in a bright specific embodiment, and wet type shaking screen is relative to routine
Filter plant, what is taken due to wet type shaking screen is dynamic filtration, avoids a large amount of fine powders blocking opening of sieves, and treating capacity
Greatly, it can be achieved that continuous production.
The effect of two-stage centrifugal machine of the invention is to remove pulp and impurity and most of impurity for being gathered in sediment area,
The main effect for playing refined filtration, preferably sedimentation-type centrifuge, separate in the specific embodiment of the present invention for disc-type
Machine T-6.For disc separator for the tube centrifuge of same type, production capacity is bigger and is able to achieve continuous production.Consider
It is variant to the processing capacity between disc separator and the solid-liquid separating equipment of preceding second level, preferably it is separated by solid-liquid separation in filtering type
Intermediate storage tank 1T-4 and high-order intermediate storage tank 2T-5 are set between machine and two-stage centrifugal machine, to adapt to disc centrifuge top
The operating mode of portion's feed liquor.
The two-stage centrifugal machine needs successively to be used in combination and could reach with above-mentioned first-stage centrifugal machine and filtering type solid-liquid separating machine
To high efficiency and the separating resulting of good separating effect.If horizontal helical type slag remover is used alone, separating effect is bad, extracting solution
Turbidity is high, if wet type shaking screen is used alone, solid bulky grain is easy blocking sieve screen apertures, if disc separator is used alone,
Also due to melt cinder partial size is big, impurity level is big, cannot exclude in time, is easy to happen blocking.If only combination horizontal helical type slag remover and
Wet type shaking screen, no refined filtration step can clarity to product and melting have large effect.In addition, three separation of solid and liquid
Equipment is because of its effect and is separated by solid-liquid separation principle and production capacity difference, and the sequence of three is specific in the present invention, only successively
It is just able to achieve good separating effect of the present invention by three solid-liquid separating equipments, if connected using different order
It will affect its treating capacity and separative efficiency, while being also easy to that equipment is caused to block.
<powder decoction pieces Chinese medicine automates extraction separation method>
Separator is extracted based on above-mentioned Chinese medicine automation, separation side is extracted in powder decoction pieces Chinese medicine automation of the invention
Method includes Dynamic Extraction and the separation of solid and liquid that is arranged in after Dynamic Extraction.
The present invention relates to powder decoction pieces Chinese medicine automation extraction separation method key step is as follows:
(1) it feeds intake:
Raw material to be extracted is moved at feeding port, solvent addition control valve is first turned on, is started using electromagnetic flowmeter
Measuring the solvent being added into extractor body, the volume mass ratio (L/Kg) of the additive amount of solvent and raw material to be extracted is 6~20,
Preferably 8-18.The raw material to be extracted can selected from burnt Medicated Leaven, Liu Yi San, cattail pollen, charred POLLEN TYPHAE, excrementum pteropi, stir-baked FAECES TROGOPTERORI with vinegar,
Medicated Leaven one of builds bent and arisaema cum bile or a variety of.After solvent amount reaches predetermined process setting value, medicinal material is thrown from feeding port
Enter in extractor T-1.Solvent adding too much then increases system circulating load, increases production cost, and solvent additive amount is too low then
Meeting extracts effective component with being unable to fully, influence the paste-forming rate and the index components rate of transform of product.Solvent is this
Common solvent water and alcohols solvent of the field for extraction, one of halogenated hydrocarbons etc. or a variety of, such as methanol, ethyl alcohol, positive third
Alcohol, isopropanol, methylene chloride, dichloroethanes etc., preferably water can be selected according to the dissolubility of medicinal material.
(2) Dynamic Extraction:
After the completion of click feeds intake, automatically turning on steam control valve makes to start to be passed through steam in extractor heating jacket, to tank
Interior raw material and solvent is heated；While extractor heating jacket T-N3 heating, by being mounted on mentioning for tank body side bottom
The temperature of thermometer real-time online Detection and Extraction liquid in tank tank is taken, and PLC program is according to the mesh of temperature in steam pressure, extractor
Scale value is controlled the aperture of extractor jacket steam regulating valve TQRV-1 by PID regulative mode, made on the temperature plateau of extracting solution
It rises, when thermometer reaches the temperature of technique initialization in extractor tank and is maintained at technique initialization temperature value, set temperature 60
~100 DEG C.
The circulating pump T-M2 in fluid circulation is extracted in starting while heating, to extracting solution forced circulation, constantly
The liquid in extractor from pot bottom is extracted, extractor is returned from the top of extractor from newly by pipeline with pump, passes through liquid
Body circulates, and enhances the contact between solid-liquid two-phase, and enhancing effective component dissolves out inside medicinal material.Circulating pump T-M2 is logical
The flow of frequency converter frequency control circulation fluid is crossed to reach corresponding cycle-index, cycle-index is 8~15 times per hour；Simultaneously
Dynamic extraction pot stirring motor T-M1 variable frequency starting is stirred solvent to reach the concentration of pharmaceutical decocting piece surface effective component
Difference.About cycle-index per hour, if cycle-index is few per hour, it is unfavorable for keeping certain concentration difference around medicinal material, no
Conducive to the dissolution of effective component, if but cycle-index it is excessive, medicinal material impact several times and by pump squeeze, easily cause medicinal material tissue
Pressure is brought to solid-liquid separation process after well-done.
In addition, PLC program can automatically record the setting time extracted and decocted, it is however generally that decocting time is 0.5~4h, excellent
Select 1~3h of decocting time range.After extraction, which decocts setting time, to be reached, extractor jacket steam regulating valve is closed, extracts knot
Beam simultaneously starts liquid out.The too short medicinal material yield of artificial decocting time can be effectively solved by automatically accurate recording decocting time
It is low, the problem of decocting time is long, low efficiency.
During taking liquid to go out liquid, be first turned on extracting solution liquid control valve T-N4, by extracting solution circulating pump T-M2 into
Enter to be separated by solid-liquid separation, after determining feed liquid emptying by detection dynamic extraction pot liquid level detecting switch, extractor circulating pump T-M2, extract
Tank stirring motor T-M1 is shut down, and closes corresponding control valve.Extracting solution can also be derived during going out liquid using program inner equation
The extraction yield of this batch materials and compared with setting empirical value in the past, inside program under automatic fine tuning batch materials Dynamic Extraction throwing
Doses, amount of water, temperature, time parameter.
(3) combined solid-liquid separates:
The resulting extracting solution of Dynamic Extraction and the dregs of a decoction can be separated using conventional equipment for separating liquid from solid, preferably according to
It is secondary to utilize first-stage centrifugal machine or the preferred horizontal helical type slag remover T-2 of slag remover, the preferred wet type shaking screen T-3 of filtering type solid-liquid separating machine
Formula is combined to extracting solution and the dregs of a decoction with the preferred disc separator T-6 of two-stage centrifugal machine to be separated by solid-liquid separation.
In order to preferably carry out the separation of powder decoction pieces Chinese medicine extract and the dregs of a decoction, need to control first-stage centrifugal machine or slagging-off
The vibration grit number and revolving speed, the deslagging gap of two-stage centrifugal machine etc. of the feed speed and screw speed of machine, wet type shaking screen
Technological parameter.The inventors discovered that separating excellent effect when using following parameter:
First-stage centrifugal machine or slag remover liquid inlet volume are set as 4~6T/ hours, first-stage centrifugal machine or slag remover main motor revolving speed
It is 2300-2600 revs/min, preferably 2400-2550 revs/min, auxiliary-motor revolving speed is 1500-1900 revs/min, preferably
1700-1850 revs/min, it may be implemented out that liquid slag inclusion is few, the dregs of a decoction are dry, the clarity of product is high, while can reduce energy consumption, prolongs
Long service life of equipment；The vibration grit number of wet type shaking screen can not only guarantee treating capacity but also can remove when being 100~300 mesh
The dregs of a decoction of greater particle size；The liquid inlet volume of the two-stage centrifugal machine is set as 2~4T/ hours, the deslagging period: 150~350 seconds, row
The slag time 0.1~0.5 second, it help to obtain clear filtrate.
In a preferred embodiment of the present invention, after the completion of Dynamic Extraction step, software is automatically according to assigning
Instruction sheet judges whether to need to be implemented program of clearing out a gathering place automatically: the alkali after cleaning and whether needing replacing batch, kind including hot water
Cleaning heating water cleaning；After program is cleared out a gathering place in entrance automatically, setting has been subjected to the control ginseng of verifying in CIP on-line cleaning program
Count up to the automatic cleaning of pairs of equipment, pipeline.
The control parameter includes the washing time of dynamic extraction pot, cleaning feed liquor time, clean cycle time, cleaning row
Discharge into delay time；Delay time is completed in pipeline-cleaning feed liquor time, pipeline-cleaning discharge；First-stage centrifugal machine or slag remover,
The washing time of filtering type solid-liquid separating machine and sedimentation-type centrifuge, pipeline-cleaning feed liquor time；When extracting the flushing of liquid storage tank
Between, cleaning the feed liquor time, cleaning discharge complete delay time.
In general the extraction separator of prior art Chinese medicine has no the CIP on-line cleaning stream of independent alkali cleaning heating water
Cheng Chengxu, the general separator that extracts clear out a gathering place program also according to former extraction and separation process process program, in production server system
It can be inquired in system without corresponding cleaning record.The invention introduces CIP on-line cleaning process program, can be individually right
Equipment, pipeline alkali cleaning or hot water wash are selected, and cleaning and drain time etc. can be separately provided.
Respectively cleared out a gathering place the time according to what is had verified that, the present invention using automation control program complete each equipment (dynamic extraction pot,
Horizontal helical type centrifuge, wet type shaking screen, disc centrifuge etc.), the purpose of clearing out a gathering place of each process pipeline, automatically complete to closing
Formula equipment and pipeline ensure that each process equipment meets with pipeline without dead angle, no manual intervention, requirement of clearing out a gathering place online at regular time and quantity
The online site requirement of GMP.
Embodiment
Carry out the technical solution during the present invention is further explained below with reference to specific embodiment.Under it should be understood that
Column embodiment is only used for the explanation and illustration present invention, and the protection scope being not intended to restrict the invention.
Embodiment 1
The present embodiment is related to extracting cattail pollen and isolated method.It uses Chinese medicine automation shown in FIG. 1 to extract
Separator carries out automation and extracts separation.
(1) it feeds intake:
Cattail pollen is pre-processed, removal of impurities is picked；
Cattail pollen 150KG is moved at feeding port, solvent (water) addition control valve is first turned on, is opened using electromagnetic flowmeter
Begin to measure to 3M3Dynamic extraction pot body in solvent 1950L is added, after solvent amount reaches predetermined process setting value, from feeding intake
Mouth puts into cattail pollen in extractor T-1.
(2) Dynamic Extraction:
After the completion of click feeds intake, automatically turning on steam control valve makes to start to be passed through steam in extractor heating jacket, to tank
Interior cattail pollen and water is heated；While extractor heating jacket T-N3 heating, by the extraction for being mounted on tank body side bottom
The temperature of thermometer real-time online Detection and Extraction liquid in tank tank, and PLC program is according to the target of temperature in steam pressure, extractor
Value is controlled the aperture of extractor jacket steam regulating valve TQRV-1 by PID regulative mode, made on the temperature plateau of extracting solution
It rises, when thermometer reaches the temperature of technique initialization in extractor tank and is maintained at technique initialization temperature value, set temperature 98
℃。
The circulating pump T-M2 in fluid circulation is extracted in starting while heating, to extracting solution forced circulation.Circulating pump
T-M2 is reached by the flow of frequency converter frequency control circulation fluid to be recycled 12 times per hour；Dynamic extraction pot stirring motor simultaneously
T-M1 variable frequency starting is stirred solvent to reach the concentration difference of pharmaceutical decocting piece surface effective component.
PLC program automatically records the setting time extracted and decocted, decocting time 2h.Reach when extracting decoction setting time
Afterwards, extractor jacket steam regulating valve is closed, extracting terminates and start liquid out.
During extracting solution goes out liquid, it is first turned on extracting solution liquid control valve T-N4, passes through extracting solution circulating pump T-M2
It extractor circulating pump T-M2, is mentioned after determining feed liquid emptying by detection dynamic extraction pot liquid level detecting switch into separation of solid and liquid
It takes tank stirring motor T-M1 to shut down, closes corresponding control valve.
(3) combined solid-liquid separates:
Extracting solution in extractor is imported combined solid-liquid separation assembly to be separated by solid-liquid separation, is successively removed by horizontal helical type
Slag machine T-2, wet type shaking screen T-3, disc separator T-6.
Extracting solution in extractor is pumped into horizontal helical type slag remover, and liquid inlet volume is set as about 4T/ hours, and main motor revolving speed is set
2500 revs/min fixed, auxiliary-motor revolving speed sets 1800 revs/min, and the extracting solution after slagging-off passes through wet type shaking screen, vibrates sieve mesh
Number is 250 mesh, then is pumped into relay reservoir, flows into disc separator afterwards, liquid inlet volume is set as about 2.5T/ hours, the deslagging period:
300 seconds, the deslagging time 0.3 second.Extracting solution after disc separator can enter next procedure.
Embodiment 2
The present embodiment is related to extracting Liu Yi San and isolated method.It is also automated using Chinese medicine shown in FIG. 1
Extract separator.
(1) it feeds intake:
Liu Yi San powder 170KG is moved at feeding port, solvent (water) addition control valve is first turned on, utilizes electromagnetic current
Meter starts metering to 3M3Dynamic extraction pot body in be added solvent 2040L, after solvent amount reaches predetermined process setting value,
It is put into extractor T-1 from feeding port by Liu Yi San.
(2) Dynamic Extraction:
After the completion of click feeds intake, automatically turning on steam control valve makes to start to be passed through steam in extractor heating jacket, to tank
Interior Liu Yi San and water is heated；While extractor heating jacket T-N3 heating, by being mounted on mentioning for tank body side bottom
The temperature of thermometer real-time online Detection and Extraction liquid in tank tank is taken, and PLC program is according to the mesh of temperature in steam pressure, extractor
Scale value is controlled the aperture of extractor jacket steam regulating valve TQRV-1 by PID regulative mode, made on the temperature plateau of extracting solution
It rises, when thermometer reaches the temperature of technique initialization in extractor tank and is maintained at technique initialization temperature value, set temperature 98
℃。
The circulating pump T-M2 in fluid circulation is extracted in starting while heating, to extracting solution forced circulation.Circulating pump
T-M2 is reached by the flow of frequency converter frequency control circulation fluid to be recycled 12 times per hour；Dynamic extraction pot stirring motor simultaneously
T-M1 variable frequency starting is stirred solvent to reach the concentration difference of pharmaceutical decocting piece surface effective component.
PLC program automatically records the setting time extracted and decocted, decocting time 1h.Reach when extracting decoction setting time
Afterwards, extractor jacket steam regulating valve is closed, extracting terminates and start liquid out.
During extracting solution goes out liquid, it is first turned on extracting solution liquid control valve T-N4, passes through extracting solution circulating pump T-M2
It extractor circulating pump T-M2, is mentioned after determining feed liquid emptying by detection dynamic extraction pot liquid level detecting switch into separation of solid and liquid
It takes tank stirring motor T-M1 to shut down, closes corresponding control valve.
(3) combined solid-liquid separates:
Extracting solution in extractor is imported combined solid-liquid separation assembly to be separated by solid-liquid separation, is successively removed by horizontal helical type
Slag machine T-2, wet type shaking screen T-3, disc separator T-6.
Extracting solution in extractor is pumped into horizontal helical type slag remover, and liquid inlet volume is set as about 4T/ hours, and main motor revolving speed is set
2500 revs/min fixed, auxiliary-motor revolving speed sets 1800 revs/min, and the extracting solution after slagging-off passes through wet type shaking screen, vibrates sieve mesh
Number is 250 mesh, then is pumped into relay reservoir, flows into disc separator afterwards, liquid inlet volume is set as about 2.5T/ hours, the deslagging period:
250 seconds, the deslagging time 0.3 second.Extracting solution after disc separator can enter next procedure.
Comparative example 1
This comparative example is using conventional 3M3Multi-function extractor and conventional solid-liquid separating equipment PD1250 hanging bag discharging from
The cattail pollen that scheming is related to embodiment 1 extracts.Specifically, cattail pollen 170kg is put into multi-function extractor, using decocting a drug wrapped
5~6kg cattail pollen is first fitted into the filter cloth bag of 50*50cm (250 mesh) by technique, and extracting in water is secondary, adds cattail pollen 12 for the first time
Water again boils extraction 1 hour；Second plus 10 times of cattail pollen of water, is boiled extraction 1 hour, is carried out using link-suspended basket centrifuge
Centrifugal filtration.
Comparative example 2
This comparative example is related to the method substantially the same manner as Example 1 for extracting separation to cattail pollen.Difference is step
(3) main motor revolving speed sets 2300 revs/min, and auxiliary-motor revolving speed sets 1600 revs/min.
Comparative example 3
This comparative example is related to the method substantially the same manner as Example 1 for extracting separation to cattail pollen.Main motor revolving speed is set
2600 revs/min fixed, auxiliary-motor revolving speed sets 1900 revs/min.
Comparative example 4
This comparative example is related to the method substantially the same manner as Example 1 for extracting separation to cattail pollen.Difference is step
(3) vibration grit number is 150 mesh.
Comparative example 5
This comparative example is related to the method substantially the same manner as Example 1 for extracting separation to cattail pollen.Difference is step
(3) vibration grit number is 300 mesh.
Comparative example 6
This comparative example is related to the method substantially the same manner as Example 1 for extracting separation to cattail pollen.Difference is to walk
Suddenly (3) are only with second level solid-liquid separating equipment (horizontal helical type slag remover+disc centrifuge).Horizontal helical type slag remover and disc-type from
The job parameter and embodiment 1 of scheming are consistent.
Comparative example 7
This comparative example is related to the method substantially the same manner as Example 1 for extracting separation to cattail pollen.Difference is to walk
Suddenly (3) are only with second level solid-liquid separating equipment (horizontal helical type slag remover+wet type shaking screen).Horizontal helical type slag remover and wet type shaking screen
Job parameter and embodiment 1 it is consistent.
Comparative example 8
This comparative example is related to the method substantially the same manner as Example 1 for extracting separation to cattail pollen.Difference is to walk
Suddenly the horizontal helical type slag remover of (3) is changed to slag dumping filter centrifugal under 3-foot, and disc centrifuge is changed to tubular type clarification type and is surpassed
Fast centrifuge, according to the practical device parameter for adjusting slag dumping filter centrifugal and tubular type clarification type ultracentrifuge under 3-foot.
The job parameter and embodiment 1 of wet type shaking screen are consistent.
To the embodiment of the present invention 1, embodiment 2, the production efficiency of the technique of comparative example 1 to comparative example 8 and at yield and
The light transmittance of product, effective component rate of transform etc. carry out comprehensive analysis, and concrete outcome is shown in Table 1.
Isorhamnetin -3-O- in prepared Pollen Tyjphae extract in embodiment 1 according to the present invention and comparative example 1~8
Neohesperidin content uses high effective liquid chromatography for measuring, method particularly includes: using octadecylsilane chemically bonded silica as filler；
Using -0.05% phosphoric acid solution of acetonitrile as mobile phase；Detection wavelength is 254nm.Flow velocity is 1.0ml/min, and test sample sample volume is
10 μ l, concentration are that 50 μ g/ml Isorhamnetin-3-O-neohespeidoside reference substance sample volumes are 10 μ l.
Glycyrrhizic acid content uses high-efficient liquid phase color in prepared Liu Yi San extract in embodiment 2 according to the present invention
Spectrometry measurement, method particularly includes: using octadecylsilane chemically bonded silica as filler；It is stream with methanol-ammonium dihydrogen phosphate
Dynamic phase；Detection wavelength is 250nm.Flow velocity is 1.0ml/min, and test sample sample volume is 10 μ l, and concentration is 0.2mg/ml glycyrrhizic acid
Ammonium reference substance sample volume is 10 μ l.
Index components content (%)/drink in the total rate of transform of index components (%)=paste-forming rate (%) × extract in extract
Index components content (%) in piece
The other production technology of the different groups of table 1 and product quality compare
By the comparison of table 1 it is found that the technique that the multi-function extractor conventional compared to use is repeatedly decocted, this hair
It is bright to be produced by using Dynamic Extraction and three-level solid-liquid separation process, the effective component rate of transform of product improves 70% or more,
Finished product light transmittance improves 40% or more compared with original process, and the daily output also improves 32% or more compared with original process.Compare only with
Second level is separated by solid-liquid separation, and the solid-liquid separating equipment that the present invention is applied in combination three kinds allows continuous production, and not only effective component turns
Shifting rate improves, while extract rushes molten rear light transmittance height.
In addition to the implementation, all to use equivalent transformation or equivalent replacement the invention also includes there is an other embodiments
The technical solution that mode is formed should all be fallen within the scope of the hereto appended claims.
Claims (10)
1. a kind of automation extraction separation method of powder decoction pieces Chinese medicine, it is characterised in that: this method comprises the following steps,
(1) it feeds intake:
Metered solvent and raw material to be extracted are pressed into dynamic extraction pot body；
(2) Dynamic Extraction:
After the completion of feeding intake, opens and the raw material and solvent to be extracted in tank are heated, automation control technique initialization temperature value；It opens
Stirring in dynamic extraction pot, while dynamic extraction pot heating, program automatically begins to record and extracts the setting time decocted,
After extraction, which decocts setting time, to be reached, liquid obtains extracting solution out；
(3) solid-liquid separation step of the extracting solution obtained to liquid out, the separating step successively utilize first-stage centrifugal machine or slagging-off
It is solid that machine, filtering type solid-liquid separating machine and two-stage centrifugal machine are combined formula to the extracting solution and the dregs of a decoction that flow out out of dynamic extraction pot
Liquid separation.
2. a kind of automation extraction separation method of powder decoction pieces Chinese medicine according to claim 1, it is characterised in that: described
First-stage centrifugal machine or slag remover are sedimentation-type centrifuge or slag remover, preferably horizontal helical type slag remover, the first-stage centrifugal machine or
2300-2600 revs/min of revolving speed of slag remover main motor, auxiliary-motor revolving speed is 1500-1900 revs/min.
3. a kind of automation extraction separation method of powder decoction pieces Chinese medicine according to claim 1, it is characterised in that: described
First-stage centrifugal machine or slag remover liquid inlet volume are set as 4~6T/ hours.
4. a kind of automation extraction separation method of powder decoction pieces Chinese medicine according to claim 1, it is characterised in that: described
Filtering type solid-liquid separating machine is wet type shaking screen, and the vibration grit number of the wet type shaking screen is 100~300, preferably 250
Mesh.
5. a kind of automation extraction separation method of powder decoction pieces Chinese medicine according to claim 1, it is characterised in that: described
Two-stage centrifugal machine is sedimentation-type centrifuge, preferably disc separator, the liquid inlet volume of the two-stage centrifugal machine is set as 2~
4T/ hours, the deslagging period: 150-350 seconds, the deslagging time was 0.1~0.5 second.
6. a kind of automation extraction separation method of powder decoction pieces Chinese medicine according to claim 5, it is characterised in that: described
The liquid inlet volume of two-stage centrifugal machine is set as 3~4T/ hours, the deslagging period: 150-350 seconds, the deslagging time was 0.1~0.5 second.
7. a kind of automation extraction separation method of powder decoction pieces Chinese medicine according to claim 1 or 2, it is characterised in that:
The raw material to be extracted is selected from burnt Medicated Leaven, Liu Yi San, cattail pollen, charred POLLEN TYPHAE, excrementum pteropi, stir-baked FAECES TROGOPTERORI with vinegar, Medicated Leaven, builds bent and gallbladder
One of Southern Star is a variety of.
8. a kind of automation extraction separation method of powder decoction pieces Chinese medicine according to claim 1 or 2, it is characterised in that:
The solvent is water, and the volume mass ratio of the additive amount of the solvent and raw material to be extracted is 8~18:1.
9. a kind of automation extraction separation method of powder decoction pieces Chinese medicine according to claim 1 or 2, it is characterised in that:
The temperature that step (2) Dynamic Extraction is set is 60~100 DEG C.
10. a kind of automation extraction separation method of powder decoction pieces Chinese medicine according to claim 1, it is characterised in that: step
Suddenly (2) decoct the time set as 60~180min.
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| CN201811475864.3A Pending CN109499094A (en) | 2018-12-04 | 2018-12-04 | A kind of automation extraction separation method of powder decoction pieces Chinese medicine |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109126191A (en) * | 2018-09-10 | 2019-01-04 | 江阴天江药业有限公司 | Separator and extraction separation method and its application are extracted in a kind of automation of Chinese medicine |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109126191A (en) * | 2018-09-10 | 2019-01-04 | 江阴天江药业有限公司 | Separator and extraction separation method and its application are extracted in a kind of automation of Chinese medicine |
Non-Patent Citations (1)
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| 张锲: "《中国改革经纬录-科技文论卷》", 31 October 1996, 北京：经济日报出版社 * |
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