CN109432146A - The automation extraction separation method and its granule preparation method of the sterculia seed - Google Patents
The automation extraction separation method and its granule preparation method of the sterculia seed Download PDFInfo
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
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- A61K36/185—Magnoliopsida (dicotyledons)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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Abstract
The present invention relates to the automation extraction separation method of the sterculia seed and its granule preparation methods.The three-level separation of solid and liquid for automating extraction separation method and including Dynamic Extraction and being arranged in after Dynamic Extraction.The present invention can effectively solve the problems, such as that production efficiency is low in sterculia seed extraction process, energy consumption is serious, it is halfway to be separated by solid-liquid separation, and the clarity of obtained finished product, melting are greatly improved.
Description
Technical field
The present invention relates to the automations of Chinese medicine production technical field more particularly to the sterculia seed to extract separation and granule system
Standby technique.
Background technique
The sterculia seed is the dry mature seed of Sterculiaceae sterculia nobilis platymiscium, is the medicinal and edible Chinese medicine of traditional throat-clearing throat-moistening
Material.Sterculia seed kind skin contains galactolipin, pentose, and there are also the microelements such as active constituent sterculin (duckweed mother-in-law element) and calcium, magnesium, embryos
Cream is containing the viscous element of tragacanth, the fatty substance of kernel.Modern research shows that the polysaccharide in the sterculia seed is its main function
Ingredient has certain anti-inflammatory activity, can be with clearing heat and moistening lung, relieving sore-throat disinfection, relax bowel and defecation.
Extraction for the sterculia seed, generallys use water boiling method and ultrasonic method.But when using water boiling method, sterculia seed category
In the very big herbal species of water absorption rate, required Extraction solvent is excessive, and the isolated process energy consumption of whole extraction is excessive, and high temperature
Prolonged hot water extracts the partial hydrolysis that will cause sterculia seed polysaccharide branch, if i.e. will be a certain amount of to be extracted using decocting a drug wrapped
Solubilization matchmaker decocts after raw material is packed into the small filter cloth bag of mesh, since the sterculia seed is easy expansion, generates many lymphatic temperaments, causes
Filtration difficulty, paste-forming rate is too low, and is easy to paste extractor bed coke.In addition, being often used multi-function extractor at present carries out water
It decocts, conventional Multifunction tank cannot make the solvent around material remain certain concentration difference during the extraction process, therefore mention
Take efficiency lower.Ultrasonic wave extraction is then that energy is generated and transmitted by ultrasonic activation, cause medium point with big speed into
Enter vibrational state, is that medium structure changes, effective component is promoted to enter in solvent, but due to sterculia seed nonsoluble mucous matter
Content is high, and the ultrasonic treatment of pure short time is difficult to for effective component being fully dissolved out, and at high-power or the long period ultrasound
Comprehend cause solution temperature rise it is too fast, should not control, influence branched structure and energy consumption be very big.
In order to obtain the sterculia seed polysaccharide compared with high yield pulp1 and purity, CN101372514A disclose a kind of sterculia seed polysaccharide and
Sterculia seed raw material is added water first through ultrasonication, to be again heated to 55~65 DEG C and extract, so by preparation method and application
Afterwards routinely by extracting solution concentration, alcohol precipitation and purifying.The invention extracts to obtain by the water-bath of ultrasonication and lower temperature
Sterculia seed water-soluble polysaccharide yield with higher and purity.But this application, which refers to that water added at the extraction is at least, to pass through
70~80 times of weight of pretreated sterculia seed raw material, and need to extract 2~3 times, each extraction time is 1~2 hour, by
This visible this application equally exists energy consumption and consumes excessive problem, and in addition the process route is complicated, the production cycle is long.
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 does not refer to
The technique is suitble to water absorption rate big and is also easy to produce mucilagenous medicinal material.
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, how preferably to improve the rate of transform of the index components of drug quality and can reduce
Production cost needs to study solid-liquid separation process according to specific dregs of a decoction property to be separated.CN102552400A is disclosed
It is filtered for Chinese medicine extract using plate and frame filter press, the second-order separation of disk plate centrifuge is then carried out, later using sub-prime
Concentration, it is effective to retain thermal sensitivity, oxidisability, volatile ingredient in Chinese medical extract；The advantage being concentrated using film, by target
Ingredient is retained, and be will transmit through liquid and is concentrated, and by the integrated of membrane technology and concentration technique, can both solve thermal sensitivity, oxidation
Property, the rate of transform problem of volatility pharmacodynamics index ingredient.But this method is at high cost, for Chinese medicinal granule or general Chinese medicine
Solid orally ingestible such as uses film concentration to will appear effective component instead and shut off and is lost that big, membrane fouling control is not thorough, production is imitated
The problems such as rate is low.For the separation of solid and liquid of the sterculia seed, because of the high-hydroscopicity of the sterculia seed, how utmostly to retain effective component,
It ensures that product quality indicator and economic indicator is also the problem to merit attention.CN101372514A discloses each extraction
After using the nylon cloth of 200 mesh or so carry out filter remove sediment, but use method residual moisture can relatively it is more.
Chinese medicinal granule is made of the extracted concentration of single medicinal material medicine materical crude slice, for the particle of tcm clinical practice formula.
It is used under instruction of Chinese Medicine theory based on the clinical use of traditional Chinese herbal decoction, but compared with traditional traditional Chinese herbal decoction, it
Has the characteristics that convenient to take, easy storage, Portable belt, quality controllable.At present not for the preparation method of sterculia seed granule
Seeing has detailed research, and with the development of granule industry, need the preparation method of sterculia seed granule to optimize
And improvement, extraction efficiency and quality are further increased, separating effect is improved, reduces production energy consumption, improves granule product matter
Amount.
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 the automatic of the sterculia seed
Change extraction separation method and its granule preparation method utmostly to retain effective component, production cost and energy can be reduced again
Consumption improves extraction efficiency, improves separating effect.
The solution to the problem
The present invention provides the automation extraction separation methods of the sterculia seed, and this method comprises the following steps,
(1) it feeds intake:
Solvent and sterculia seed powder to be extracted, the sterculia seed powder to be extracted are sequentially added into dynamic extraction pot body
The size controlling at end is in≤0.5cm；The volume mass ratio (L/Kg) of the solvent and the sterculia seed powder to be extracted is 30-
60:1；
(2) Dynamic Extraction:
After the completion of feeding intake, open in tank raw material and solvent heat, open in the forced circulation and tank of dynamic extraction pot
Stirring, automation control makes the temperature of extracting solution rise the Extracting temperature for reaching technique initialization and keeps the temperature, while program
It automatically begins to record and extracts the setting time decocted, after extraction, which decocts setting time, to be reached, close extractor heating, extract and tie
Beam and out liquid；
(3) combined solid-liquid separates:
Successively using first-stage centrifugal machine or slag remover, filtering type solid-liquid separating machine and the second-order separation machine to from dynamic extraction pot
The extracting solution and the dregs of a decoction of interior outflow are combined formula separation of solid and liquid；Wherein the first-stage centrifugal machine or slag remover liquid inlet volume are set as
3-6T/ hours, first-stage centrifugal machine or slag remover main motor revolving speed were 2400-2500 revs/min, and auxiliary-motor revolving speed is 1500-
1700 revs/min.
Further, Extracting temperature is set as 60~95 DEG C, further preferably 60~90 DEG C, is still more preferably extracted
Temperature is 70 DEG C.
Further, decocting time is set as 20~45 minutes, further preferred 30 minutes.
Further, the first-stage centrifugal machine or slag remover are sedimentation-type centrifuge or slag remover, and preferably horizontal helical type removes
Slag machine；The second-order separation machine is sedimentation-type centrifuge, preferably disc separator.
Further, the solvent is water, C1-6Alcohols solvent, one of halogenated hydrocarbons or a variety of, it is preferably described
Solvent is water.
The present invention also provides a kind of sterculia seed granule preparation method, this method includes the present invention sterculia seed above-mentioned
Automation extraction separation method and concentration, drying and granulation step.
Further, the concentration is concentrated using vacuum and low temperature, and the vacuum pressure of concentration is -0.070~-0.099MPa,
Thickening temperature is 45~70 DEG C.
Further, described dry using spray drying, dry inlet air temperature control is at 165~195 DEG C, leaving air temp control
System is at 80~105 DEG C.
The effect of invention
Compared with the prior art, the advantages of the present invention are as follows:
1) water absorption rate for efficiently solving the sterculia seed using dynamic extraction process and combined solid-liquid separate mode is big, energy consumption
Serious problem.Using specific dynamic extraction pot, pass through the circulation of dynamic extraction pot stirring motor T-M1 and dynamic extraction pot
The control of T-M2 high frequency is pumped, reaches technique and requires forced circulation number, make full use of diffusion principle, make sterculia seed medicinal material effective component
It is quickly dissolved in solvent, improves and extract production efficiency, pressure makes the effective component on medicinal material surface reach certain concentration difference, in turn
The usage amount of solvent can be effectively reduced while improving extraction efficiency, in addition during the extraction process control Extracting temperature and
Extraction time to prevent medical fluid system from becoming cloudy as far as possible, guarantees the melting and clarity of product.The present invention uses combined type gas-liquid-solid
Liquid separate mode, wherein use Horizontal helical type centrifuge as first-stage centrifugal machine or slag remover, by regulation to technological parameter and
The mode of extruding can make the sterculia seed dregs of a decoction remove a large amount of water rapidly, using extraction separation method of the invention, can make
30% or more Power dissipation reductions make production efficiency improve 20% or more.
2) present invention mainly using decanter type and filtering type combined type gas-liquid-solid liquid separating method (first through Horizontal helical type centrifuge, then
Through Wet oscillating screen and butterfly centrifugal machine) medical filtration difficult problem is effectively solved, and can work continuously, it will not produce
Raw filtering bottleneck, high production efficiency is at low cost, and the product melting after separation is good, and clarity is high, and precipitating is few.
3) present invention is optimized and improves to the preparation method of sterculia seed one-component formulation particle, using vacuum and low temperature
Concentration and spray dried form can obtain the granule that aridity is high and melting, clarity are good.
Detailed description of the invention
Fig. 1 is the structural representation that separator is extracted in Chinese medicine automation used in present invention automation extraction separation method
Figure.
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 the automation extraction separation methods of the sterculia seed, extract and divide which employs the automation of specific Chinese medicine
From device.
<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 sterculia seed powder to be extracted, and circulation line is equipped with circulating pump T-M2, follows
The design on endless tube road and circulating pump to meet solvent and sterculia seed powder to be extracted recycles together, and does not break in cyclic process
The character of bad material can enable whole tank material quickly be uniformly mixed, and the control of extractor feed liquid can be equipped on circulation line T-N2
Valve TQPV-1 processed, dynamic extraction pot liquid-level switch TQLS-1 are also provided with the blowdown for slag liquid discharge on circulation line
Branch pipe.The dynamic extraction pot inner cavity is equipped with multiple impellers T-N1, and agitating paddle is driven by dynamic extraction pot stirring motor T-M1,
Agitating paddle is preferably provided with not in tank body axial centerline, and agitating paddle is preferably three layers of agitating paddle, and top layer is press-down type, can be with
Sink the material of some floatings by stirring, middle layer is horizontal, can promote diffusion horizontally outward, promotes material dynamic
Exchange, 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
It can make to reach better mixing effect in tank.The present invention utilizes the circulation of dynamic extraction pot stirring motor T-M1 and dynamic extraction pot
The control of T-M2 high frequency is pumped, reaches technique and requires forced circulation number, make full use of diffusion principle, keep the effective component of the sterculia seed fast
It is instantly 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 the second-order separation machine, the first-stage centrifugal machine or slag remover, filtering type solid-liquid separating machine
Feed lines connection is passed sequentially through between the second-order separation 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, the sterculia seed dregs of a decoction residual moisture being in addition discharged after horizontal helical type slag remover
Can control within 80%, greatly reduce this kind as water absorption rate is high and caused by produce loss.Of the invention one
In a specific embodiment, as shown in Fig. 2, Horizontal helical type centrifuge includes rotary drum (4), discharge with endless screw device (5), motor, differential mechanism
(3), discharge with endless screw device (5) setting is inserted with walking feeding tube, one end of walking feeding tube in discharge with endless screw device (5) in rotary drum (4)
For feed inlet, the other end is as discharge port, and one end of the close feed inlet of rotary drum (4) is as purified liquor outlet, close to the one of discharge port
End is exported as sediment, and the motor includes the main motor (2) for controlling charging and the auxiliary electricity for controlling differential mechanism (3)
Motivation (1).
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 the second-order separation 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 the second-order separation machine, to adapt to disc centrifuge top
The operating mode of portion's feed liquor.
The second-order separation 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, and filter efficiency is low, and the sterculia seed dregs of a decoction
Containing large quantity of moisture, the waste of material is easily caused, if disc separator is used alone, also due to melt cinder partial size is big, impurity level
Greatly, it cannot exclude in time, be easy to happen blocking.If horizontal helical type slag remover and wet type shaking screen are only combined, without refined filtration step meeting
There is large effect to the clarity and melting of product.In addition, three solid-liquid separating equipments are because of its effect and are separated by solid-liquid separation former
Reason and production capacity difference, the sequence of three is specific in the present invention, only successively by three solid-liquid separating equipments
It is able to achieve good separating effect of the present invention, if will affect its treating capacity and separation effect using different order connection
Rate, while being also easy to that equipment is caused to block.
<the automation extraction separation method of the sterculia seed>
Separator, the automation extraction separation method packet of the sterculia seed of the invention are extracted based on above-mentioned Chinese medicine automation
Include feed intake, Dynamic Extraction and the combined solid-liquid separation being arranged in after Dynamic Extraction.
The present invention relates to the automation extraction separation method key step of the sterculia seed is as follows:
(1) it feeds intake:
The sterculia seed needs pulverization process, and size controlling is in 0.5cm or less.
By sterculia seed powder moving to be extracted at feeding port, it is first turned on solvent addition control valve, utilizes electromagnetic current
Meter starts to measure the solvent being added into extractor body, and the additive amount of solvent is generally 30-60 times of the sterculia seed to be extracted
The inventory of powder, after solvent amount reaches predetermined process setting value, sterculia seed powder to be extracted puts into from feeding port and extracts
In tank T-1.Solvent adding too much will increase system circulating load, and yield does not change much but energy consumption can improve, and increase life
Produce cost, solvent additive amount is too low, extracts to sterculia seed effective component with being unable to fully, influence the paste-forming rate of product with
And the index components rate of transform.The common solvent of the present invention be one of water, the alcohols solvent of C1-6, halogenated hydrocarbons or a variety of, it is excellent
Select water or ethyl alcohol, more preferable water.
(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 is general
It is 60~95 DEG C, further preferred 60~90 DEG C, still more preferably Extracting temperature is 70 DEG C, and Extracting temperature should not boil, temperature
It spends the high easily well-done separation of solid and liquid to rear process and brings difficulty.
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 10~15 times per hour；Together
When dynamic extraction pot stirring motor T-M1 variable frequency starting solvent is stirred to reach the concentration difference of medicinal material surface effective component.
The pressure inside the tank of dynamic extraction pot is normal pressure.About cycle-index per hour, if cycle-index is few per hour, it is unfavorable for medicinal material
Around keep certain concentration difference, be unfavorable for the dissolution of effective component, if but cycle-index it is excessive, medicinal material impact several times and warp
It crosses pump to squeeze, easily leads to the well-done a large amount of stickums of generation of the sterculia seed to solid-liquid separation process and bring pressure.
In addition, PLC program can automatically record the setting time extracted and decocted, it is however generally that decocting time (decocts heat preservation
Time) it is 20~45 minutes, further preferred 30 minutes.After extraction, which decocts setting time, to be reached, closes extractor collet and steam
Steam control valve, extracting terminates and starts liquid out.It can effectively solve manually to decoct by automatically accurate recording decocting time
The problem of time, too short medicinal material yield was low, decocting time long low efficiency.The present invention is by using relatively low Extracting temperature and phase
To short decocting time to prevent medical fluid system from becoming cloudy as far as possible, guarantee the melting and clarity of product.
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:
It is successively preferably wet using first-stage centrifugal machine or the preferred horizontal helical type slag remover T-2 of slag remover, filtering type solid-liquid separating machine
The formula shaking screen T-3 and preferred disc separator T-6 of the second-order separation machine is combined formula to extracting solution and the dregs of a decoction and is separated by solid-liquid separation.
In order to preferably carry out the sterculia seed Chinese medicine extract and the dregs of a decoction separation, preferably to first-stage centrifugal machine or slag remover
Operating parameter carry out priority control to exclude the moisture in the dregs of a decoction mostly to the greatest extent.In a specific embodiment of the invention, level-one
Centrifuge or slag remover liquid inlet volume are set as 3~6T/ hours, and 2400~2500 revs/min of main motor revolving speed, auxiliary-motor revolving speed
1500~1700 revs/min, it may be implemented out that liquid slag inclusion is few, the dregs of a decoction are dry.If liquid inlet volume is excessive, solid-liquid separation effect is influenced；
If liquid inlet volume is too small, production efficiency will affect；If major-minor machine revolving speed is too low, it may appear that separation of solid and liquid is not thorough, part medicine
Slag enters rear process, brings pressure to the separation of solid and liquid of rear process；If major-minor motor speed is excessive, easily cause material unrestrained
Take, influences the yield of finished product.
In the specific embodiment of the present invention, the vibration grit number of wet type shaking screen is 100~250 mesh Shi Jike
It can remove the dregs of a decoction of greater particle size to guarantee treating capacity again, the liquid inlet volume of the second-order separation machine is set as 2-4T/ hours, row
The slag period: 150-300 seconds, the deslagging time 0.1-1 seconds, 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.
<sterculia seed granule preparation method>
The present invention also provides a kind of sterculia seed granule preparation method, this method includes present invention automation above-mentioned
Extraction separation method and concentration, drying and granulation step.This method is especially suitable for sterculia seed one-component formulation particle manufacture.
The clear filtrate pump of gained will be separated by solid-liquid separation to be used as medicine liquid storage tank, then drawing liquid is to concentration tank, in order to farthest mention
The aridity of high final sterculia seed granule, the present invention is concentrated using cryogenic vacuum, in order to reduce to polysaccharide material
Destroy, the vacuum pressure of concentration is -0.070~-0.099MPa, and thickening temperature is 45~70 DEG C, be concentrated into specific gravity be 1.01~
1.05 (60 DEG C), gained concentrate is spray-dried, and clear cream will be obtained by vacuum concentration, and drawing liquid is dry to spray drying tower again
When 165~195 DEG C of inlet air temperature and 80~105 DEG C of leaving air temp, material residence time 15~60 seconds in the high temperature environment；It is dry
Material later is crushed, and xeraphium directly pelletizes or is added necessary auxiliary material in spray dried powder；It pelletizes
One-component formulation particle.Auxiliary material can be carbohydrate auxiliary material, such as starch, soluble starch, dextrin, sucrose or mannitol.These are auxiliary
Material can be used alone, and several can also be used in mixed way, to improve the mouthfeel of particle.Method of granulating of the present invention includes dry-pressing
Method granulation and fluidized bed granulation.
Using this method simple production process, the sterculia seed formula that aridity is high and melting, clarity are good can be obtained
Particle.
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 sterculia seed one-component formulation preparation method of granules.It uses Chinese medicine automation shown in FIG. 1 to mention
It takes separator to carry out automation and extracts separation.
(1) it feeds intake:
The sterculia seed needs pulverization process, and size controlling is in 0.5cm or less；
Sterculia seed powder 40Kg to be extracted is moved at feeding port, solvent (water) addition control valve, benefit are first turned on
Start metering to 3M with electromagnetic flowmeter3Dynamic extraction pot body in be added solvent 2000L, set when solvent amount reaches predetermined process
It, will be in sterculia seed powder investment extractor T-1 to be extracted from feeding port after definite value.
(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 sterculia seed powder and water to be extracted is heated；While extractor heating jacket T-N3 heating, by being mounted on tank
The temperature of thermometer real-time online Detection and Extraction liquid in the extractor tank of side bottom, and PLC program is according to steam pressure, extraction
The target value of temperature in tank is controlled the aperture of extractor jacket steam regulating valve TQRV-1 by PID regulative mode, makes extracting solution
Temperature plateau rise, when thermometer reaches the temperature of technique initialization in extractor tank and be maintained at technique initialization temperature value,
Set temperature is 70 DEG C.
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 medicinal material surface effective component.
PLC program automatically records the setting time extracted and decocted, decocting time 0.5h.It is reached when extracting decoction setting time
After arriving, 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 4T/ hours, the setting of main motor revolving speed
2500 revs/min, auxiliary-motor revolving speed sets 1700 revs/min, and the extracting solution after slagging-off passes through wet type shaking screen, vibrates grit number
For 150 mesh, then it is pumped into relay reservoir, flows into disc separator afterwards, liquid inlet volume is set as 2.5T/ hours, the deslagging period: 250
Second, the deslagging time: 0.3 second.Extracting solution after disc separator can enter next procedure.
(4) it is concentrated, dry and granulation
The clear filtrate pump of gained after disc separator is used as medicine liquid storage tank, then drawing liquid is to concentration tank, using true
Empty low-temperature concentration equipment, the vacuum pressure of concentration are -0.08~-0.095MPa, and concentration time is 1.5~2.5h, thickening temperature
It is 55~70 DEG C, is concentrated in vacuo to the clear cream that specific gravity is 1.01~1.03, then drawing liquid to spray drying tower, spray drying air inlet is warm
Degree 175 DEG C and 90~95 DEG C of leaving air temp, material residence time 15~60 seconds in the high temperature environment, it is dry after material by its
Crushed, add the auxiliary materials such as maltodextrin carry out granulation can obtain sterculia seed one-component formulation particle.
Embodiment 2
The present embodiment is related to sterculia seed one-component formulation preparation method of granules substantially the same manner as Example 1.Difference is
Solvent amount is 2400L.
Comparative example 1
This comparative example is using conventional 3M3Multi-function extractor, the sterculia seed that embodiment 1 is related to using water boiling method into
Row extracts.
Specifically, 40Kg sterculia seed powder investment multi-function extractor extracts, using processing of decocting a drug wrapped, respectively by 5
~6kg sterculia seed is fitted into the filter cloth bag of 50*50cm (150 mesh), and extracting in water is secondary, the water that 50 times of the first time sterculia seed,
Boil extraction 0.5 hour；Second plus 20 times of the sterculia seed of water, boils extraction 0.5 hour, and bag type filtering is utilized after having extracted
Device filters (200 mesh).
Concentration, drying and the granulation as described in 1 step of embodiment (4) are carried out later, obtain sterculia seed one-component formulation
Grain.
Comparative example 2
This comparative example is related to sterculia seed one-component formulation preparation method of granules substantially the same manner as Example 1.Difference is
Solvent additional amount is 2480L.
Comparative example 3
This comparative example is related to sterculia seed one-component formulation preparation method of granules substantially the same manner as Example 1.Difference is
Solvent additional amount is 1120L.
Comparative example 4
This comparative example is related to sterculia seed one-component formulation preparation method of granules substantially the same manner as Example 1.Difference is
Extracting temperature is 98 DEG C.
Comparative example 5
This comparative example is related to sterculia seed one-component formulation preparation method of granules substantially the same manner as Example 1.Difference is
The main motor revolving speed of horizontal helical type slag remover is 2600.
Comparative example 6
This comparative example is related to sterculia seed one-component formulation preparation method of granules substantially the same manner as Example 1.Difference is
The main motor revolving speed of horizontal helical type slag remover is 2300.
Comparative example 7
This comparative example is related to sterculia seed one-component formulation preparation method of granules substantially the same manner as Example 1.Difference is
By step (3) 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 vibration
Job parameter and the embodiment 1 for swinging sieve are consistent.
Comparative example 8
This comparative example is related to sterculia seed one-component formulation preparation method of granules same as Example 1.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.
Production efficiency and energy consumption and extract to the technique of 1-3 of the embodiment of the present invention, comparative example 1 to comparative example 8
Clarity, melting of dry extract etc. carry out comprehensive analysis, and concrete outcome is shown in Table 1.
Clarity result indicates:
◎ is clear and bright；Zero is slightly clear and bright；△ is slightly muddy.
Melting result indicates:
◎, which is stirred 30 seconds, to be dissolved；Zero stirring 60 seconds is dissolved.
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
Bright to produce by using Dynamic Extraction and three-level solid-liquid separation process, the paste-forming rate of product, which has, to be obviously improved, and energy consumption has bright
Aobvious reduction；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 may be implemented to connect
Continuous production, while extract rushes molten rear clarity and melting is more preferable.In addition, the present invention uses the extracting mode of relative low temperature,
It can effectively guarantee the clarity and melting of product.
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 (8)
1. the automation extraction separation method of the sterculia seed, it is characterised in that: this method comprises the following steps,
(1) it feeds intake:
Solvent and sterculia seed powder to be extracted are sequentially added into dynamic extraction pot body, the sterculia seed powder to be extracted
Size controlling is in≤0.5cm；The volume mass ratio of the solvent and the sterculia seed powder to be extracted is 30-60:1；
(2) Dynamic Extraction:
After the completion of feeding intake, open in tank raw material and solvent heat, open dynamic extraction pot forced circulation and tank in stirring,
Automation control makes the temperature of extracting solution rise the Extracting temperature for reaching technique initialization and keeps the temperature, while program is opened automatically
The setting time that record extraction decocts that begins is closed extractor and is heated after extraction, which decocts setting time, to be reached, and extracts end and simultaneously goes out
Liquid；
(3) combined solid-liquid separates:
Successively flowed using first-stage centrifugal machine or slag remover, filtering type solid-liquid separating machine and the second-order separation machine to out of dynamic extraction pot
Extracting solution and the dregs of a decoction out is combined formula separation of solid and liquid；Wherein the first-stage centrifugal machine or slag remover liquid inlet volume are set as 3-
6T/ hours, first-stage centrifugal machine or slag remover main motor revolving speed were 2400-2500 revs/min, and auxiliary-motor revolving speed is 1500-1700
Rev/min.
2. the automation extraction separation method of the sterculia seed according to claim 1, it is characterised in that:
Extracting temperature is set as 60~95 DEG C, preferably Extracting temperature is 70 DEG C.
3. the automation extraction separation method of the sterculia seed according to claim 1 or 2, it is characterised in that:
Decocting time is set as 20~45 minutes, further preferred 30 minutes.
4. the automation extraction separation method of the sterculia seed according to claim 1-3, it is characterised in that:
The first-stage centrifugal machine or slag remover are sedimentation-type centrifuge or slag remover, preferably horizontal helical type slag remover；The second level
Seperator is sedimentation-type centrifuge, preferably disc separator.
5. the automation extraction separation method of the sterculia seed according to claim 1-4, it is characterised in that:
The solvent is water, C1-6Alcohols solvent, one of halogenated hydrocarbons or a variety of, the preferably solvent is water.
6. a kind of sterculia seed granule preparation method, it is characterised in that: this method includes as described in claim any one of 1-5
The sterculia seed automation extraction separation method and concentration, drying and granulation step.
7. sterculia seed granule preparation method according to claim 6, it is characterised in that: the concentration is low using vacuum
Temperature concentration, the vacuum pressure of concentration are -0.070~-0.099MPa, and thickening temperature is 45~70 DEG C.
8. sterculia seed granule preparation method according to claim 6 or 7, it is characterised in that:
Described dry using spray drying, at 165~195 DEG C, leaving air temp is controlled 80~105 for dry inlet air temperature control
℃。
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