CN100342839C - Chinese medicine preparation and set of apparatuses thereof - Google Patents
Chinese medicine preparation and set of apparatuses thereof Download PDFInfo
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- CN100342839C CN100342839C CNB2005100106257A CN200510010625A CN100342839C CN 100342839 C CN100342839 C CN 100342839C CN B2005100106257 A CNB2005100106257 A CN B2005100106257A CN 200510010625 A CN200510010625 A CN 200510010625A CN 100342839 C CN100342839 C CN 100342839C
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 230
- 238000000605 extraction Methods 0.000 claims abstract description 108
- 238000010438 heat treatment Methods 0.000 claims abstract description 78
- 238000000034 method Methods 0.000 claims abstract description 40
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- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 239000004480 active ingredient Substances 0.000 claims abstract description 3
- 238000001694 spray drying Methods 0.000 claims description 49
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 230000008020 evaporation Effects 0.000 claims description 23
- 238000005516 engineering process Methods 0.000 claims description 20
- 238000007670 refining Methods 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000284 extract Substances 0.000 claims description 12
- 239000010692 aromatic oil Substances 0.000 claims description 8
- 239000008187 granular material Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 239000012141 concentrate Substances 0.000 claims description 4
- 239000010419 fine particle Substances 0.000 claims description 3
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- A—HUMAN NECESSITIES
- 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
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/81—Solanaceae (Potato family), e.g. tobacco, nightshade, tomato, belladonna, capsicum or jimsonweed
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/10—Vacuum distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/38—Steam distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
- B01D5/006—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes with evaporation or distillation
-
- 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
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- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The present invention relates to a traditional Chinese medicine preparation process and a complete set of equipment thereof. The preparation process has the steps of extraction (I) solid-liquid separation (II) heating sterilization (III) and vacuum concentration (IV) which are orderly carried out. The complete set of equipment comprises extraction equipment (A), solid-liquid separation equipment (B), sterilization equipment (C) and vacuum condensation equipment (D) which are orderly connected through liquid feed pipelines. The processes of extracting active ingredients in traditional Chinese medicine raw materials, separating impurities in physic liquor, sterilizing the physic liquor and concentrating the physic liquor can be continuously accomplished in one time, dried powder or thick paste can be respectively produced and obtained according to requirements, and the present invention has the advantages of high equipment automation degree, high production efficiency, low energy consumption, convenient cleaning, low bacterium content (of products obtained in the production) and stable quality of the products.
Description
Technical field
The invention belongs to the continuous production processes technical field that raw material of Chinese medicine is prepared as thick paste shape product or dry powder finished product, the invention still further relates to the complete set of equipments technical field of structures that is used for this technology.
Background technology
Existing Chinese drug preparation technique normally with the extraction of Chinese medicine, concentrate and finish in different workshop sections respectively with dried, can not directly be produced the finished product material continuously.Even divide workshop section to handle, also being manually or needing the equipment of the artificial auxiliary semiautomatic control of finishing of employing.What for example extraction process adopted is legacy equipments such as water liquid decoction pot or rustless steel extraction pot, or employing percolation extracting technology etc., these extraction equipment and technology are keeping the characteristics of traditional decoction technology substantially, have a series of problems such as leaching the fluid coefficient is big, impurity content is high, energy consumption is big, yield is low, lixiviate is thorough inadequately, cleaning inconvenience, supernatant separation difficulty.And reinforced, the discharging of equipment and the control of whole leaching process is still to be operating as the master manually, and it is bigger that quality of liquid medicine is influenced by anthropic factor, is difficult to guarantee the quality of tcm product.Concentrator mainly contains tilting-type reaction pot, vacuum concentration reaction pot, thin film concentration evaporation equipment, economic benefits and social benefits and triple effect outer circulation concentration and evaporation equipment etc. at present.Tilting-type reaction pot evaporating temperature height, the material heated time is long, the easy coking of thermal sensitivity composition, a large amount of steam that evaporate easily make plant and equipment grow mycete, have a strong impact on the health of pharmaceutical production environment; The vacuum concentration reaction pot can not accurately be controlled the every technological parameter in the concentration process, and concentrated effect is relatively poor; The thin film concentration evaporation equipment is higher because of evaporating temperature, and evaporating temperature and inlet amount can't control automatically, and coking phenomenon is often arranged; Each density of imitating of economic benefits and social benefits and triple effect outer circulation concentration and evaporation equipment can't detect automatically, and input and output material all needs manually-operated, no temperature, pressure and vacuum automatic control system, and vacuum and condenser system energy consumption are big.And in the drying means of concentrated medicament commonly used, the drying effect of vacuum drying, lyophilization and heated-air circulation oven is all undesirable, not only uneven drying even, easily caking, efficient is low and drying time is long, and input and output material all needs manually-operated, vulnerable to pollution, severe operational environment; Boiling-bed drying easily makes dry thing caking and noise big.Freeze-drying and boulton process need large-scale equipment, but also are difficult to adopt successive production stage, production method trouble effort; Simultaneously, after lyophilization or the vacuum lyophilization, necessary additional step such as grind and homogenize and make production process become more loaded down with trivial details again; The existing spray drying process that has some producers to use, but its technology and low, the poor product quality of equipment control level also are difficult to handle the bigger extractum of viscosity, and its dry tenacity is low, returning charge is bigger.Existing Chinese medicinal preparation method, its medicinal residues are not thorough with separating of medicinal liquid, it is more that the medicinal liquid that enters vacuum concentration contains impurity, not only wearing and tearing, the occluding device pipeline, also reduce the quality of finished product material greatly, add that sterilization is insufficient, it is too high to cause the finished product material that finally obtains to contain equal bacterium amount, is difficult to reach the bacteria containing amount requirement of GMP to medicine.And existing concentration generally just carries out just entering the subsequent drying processing after the once concentration; directly produce dry traditional Chinese medicine granule or powder; and the medicinal liquid after the once concentration is because enrichment factor is low; be difficult to be directly used in production extractum series products; cause the finished product material kind that makes single, be difficult to satisfy the requirement of product diversity.In addition,, clean also inconvenience because the automatic control level of existing equipment is low, the feasible unstable product quality of producing, production efficiency is low.
Summary of the invention
Purpose of the present invention provides separate impurities, the sterilization of medicinal liquid and the concentration process of medicinal liquid in a kind of extraction that can disposablely finish the raw material of Chinese medicine effective ingredient continuously, the medicinal liquid just in order to solve above-mentioned the deficiencies in the prior art, and produce respectively as required and obtain dry powder or thick paste, the automaticity height, the production efficiency height, energy consumption is low, it is convenient to clean, the product bacteria containing amount that production obtains is low, stay-in-grade Chinese medicine preparation technology, the present invention also is provided for the complete set of equipments of this technology.
The objective of the invention is to be achieved through the following technical solutions.
A kind of Chinese medicine preparation technology, comprise the extraction, solid-liquid separation, pasteurization and the vacuum concentration that carry out successively, 1., extract concrete technology is:, be on extraction pot, to connect condenser and oil water separator and form a closed circuit, and on extraction pot, form another closed circuit by pipeline connection circulating pump by pipeline; Raw material of Chinese medicine is contained in the basket in crack with holes, basket is packed in the extraction pot, again liquid solvent is added extraction pot, carry out heat temperature raising with the Steam Heating extraction pot, raw material of Chinese medicine is soaked into into rare medicinal liquid, rare medicinal liquid is squeezed in the extraction pot by closed circuit once more by circulating pump, carries out dynamic circulation and extracts; Simultaneously, aromatic oil in the raw material of Chinese medicine is evaporated, the vapours that is mixed with aromatic oil enters oil water separator after by condenser separates, and the solvent after the separation flows back in the extraction pot from the extraction pot top through closed circuit as novel solvent and thermal source, carries out the next round circulation again; Said process carries out synchronously, and circulation repeatedly finishes until the extracts active ingredients of raw material of Chinese medicine; 2., solid-liquid separation, be that the extracting solution that extraction process is obtained carries out isolated by filtration through equipment for separating liquid from solid, separate medicinal residues and medicinal liquid, obtain the little medicinal liquid of dregginess; 3., pasteurization, be the medicinal liquid that solid-liquid separation obtains to be flowed through be arranged on pasteurization device on the transfer pipeline, medicinal liquid is heated to 110～130 ℃ of sterilizations 10～30 seconds; 4., vacuum concentration, be traditional Chinese medicine liquid to be joined internal medium be in the closed circuit that connects to form up and down by evaporator and heating tank of vacuum state and use the Steam Heating evaporation and concentration, technical process is: with vacuum extractor to whole concentrator system evacuation, after absolute pressure reaches 9500～20000Pa to the evaporator, in evaporator, infeed medicinal liquid, after setting liquid level, adjust the feed flow flow, stable with control jar inner liquid medicine liquid level, add steam to heating tank then, to flow to the medicinal liquid heating of heating tank from evaporator, when the medicinal liquid liquid level reaches the requirement height, medicinal liquid is in sharply boiling of 45～60 ℃ of beginnings, and circulation and evaporation between heating tank and evaporator, until being concentrated to desired concentration; Simultaneously, the boil-off gas in the evaporator is drawn carry out gas-liquid separation.
Technology of the present invention through behind the pasteurization, to medicinal liquid is carried out refinement treatment before concentrating at medicinal liquid, being about to medicinal liquid sends in the centrifugal separating device, remaining fine particle in the medicinal liquid is separated, made medicinal liquid purer, the content of solid matter approaches zero in the medicinal liquid; Through after the concentration, again medicinal liquid is carried out secondary concentration at medicinal liquid, further improve the medicinal liquid viscosity; Described secondary concentration is to handle carrying out vacuum concentration once more through the traditional Chinese medicine liquid of preliminary concentration in the feed tank, technical process is: start vacuum extractor, be in vacuum state to whole concentrator system, infeed medicinal liquid by feed tank to heater then, and adjust the feed flow flow, feeding the Steam Heating medicinal liquid to heater again vaporizes medicinal liquid, medicinal liquid after the vaporization falls into vacuum evaporator, condense into thick paste shape finished product after the cooling gradually in the process that in vaporizer, descends, simultaneously, solvent enters vapour liquid separator and carries out vapor-liquid separation.Also can be at medicinal liquid through after the concentration, concentrated medicament is carried out spray drying treatment, technical process is: need add feed tank internal heating, stirring by exsiccant concentrated medicament, and in the closed circuit of forming by feed tank, solution feed pump and connecting pipe, circulate, limit heating, the circulation of stirring limit, carrying out the pretreatment that homogenizes of medicinal liquid, and the follow-up flow that enters spray drying tower of stable solution feed pump; Send into simultaneously in the spray drying tower with pretreated concentrated medicament and through the hot-air after filtration, the heat treated then, concentrated medicament, fully contact with high-temperature hot air, and rapid draing is become granule by the high speed rotating atomisation by aerosol apparatus; At last, dried granule is entered separation and the collection that cyclone separator carries out final products by air conveying.At medicinal liquid through after the concentration, carry out spray drying before, also can be to the concentrated medicament sterilization processing of heating once more, the sterilization temperature of heating is 80～95 ℃; The present invention is in extraction process, and the solvent of employing is water or ethanol; When solvent was water, adding the raw material of Chinese medicine of extraction pot and the mass ratio of water was 1: 8～10, and extracting temperature is 90～99 ℃, and the extracting solution cycle-index is per hour 8～10 times; When solvent was ethanol, adding the raw material of Chinese medicine of extraction pot and the mass ratio of ethanol was 1: 4～8, and extracting temperature is 70～85 ℃, and the extracting solution cycle-index is per hour 8～10 times; In vacuum Concentrating Process, the absolute pressure in the evaporator remains on 9500～20000Pa, and temperature remains on 45～60 ℃, and steam pressure remains on 0.1～0.3M Pa in the heating tank; In secondary concentration technology, medicinal liquid preheats earlier before entering heater, and from the medicinal liquid that feed tank comes out, the temperature before preheating is 40～60 ℃, and the temperature after preheating is 80～90 ℃; The heater via heated temperatures is 110～120 ℃; In the secondary concentration processing procedure, the absolute pressure in the vacuum evaporator remains on 8000Pa～12000Pa, and temperature remains on 60～80 ℃, and steam pressure remains on 0.1～0.3MPa in the heater; Temperature in spray-drying process in the feed tank is 60～90 ℃, and the hot air temperature that enters spray drying tower is 150～160 ℃, and the temperature in the cyclone separator is 80～100 ℃; Concentrated medicament is 50～100 μ m by the drop size after spraying during spray drying.
Complete set of equipments of the present invention includes extraction equipment, equipment for separating liquid from solid, sterilizing unit and the vacuum concentration equipment that is linked in sequence by feed liquid pipeline.
Between sterilizing unit and vacuum concentration equipment, be provided with refining plant; Be connected with secondary concentration equipment in the vacuum concentration equipment back; Be connected with spray drying device in the vacuum concentration equipment back; Described extraction equipment comprises the extraction pot of band heating jacket and discharging opening, the steam pipework and the steam supply that are connected with the extraction pot heating jacket, by pipeline and the tank connected solvent supply of extraction, connect the extracting solution closed circuit of forming by extraction pot and circulating pump by pipeline, connect the closed circuit of forming by extraction pot, condenser and oil water separator by pipeline, in extraction pot, be provided with the Chinese medicine basket in crack with holes, be provided with the top cover that to open entirely at the extraction pot top; Described pasteurization device includes heater, insulating tube and the cooler that is linked in sequence along the medicinal liquid transfer pipeline; Described vacuum concentration equipment includes the feed tank by pipeline connection, communicate up and down and form the evaporator and the heating tank of closed circuit, vapour liquid separator and condensing unit, last connection tube and the evaporator of connecting heating tank and evaporator are tangent, the internal diameter of last connection tube is less than the internal diameter of heating tank upper cavity, be connected with vacuum extractor in the condensing unit back by pipeline, evaporator is provided with vacuum-breaking valve, the liquid-transport pipe-line that connects feed tank and evaporator is higher than connection tube from evaporator top position enters and also extends to the tank body bottom in the tank body always, liquid-transport pipe-line is provided with electrically-controlled valve, evaporator is provided with upper liquidometer and the next liquidometer, and two liquidometers all link to each other with control system with electrically-controlled valve; Heating and evaporating unit, vapour liquid separator, condenser and vacuum extractor that described secondary concentration equipment includes the feed tank that connects by pipeline, connected to form by heater and vacuum evaporator, connecting pipe between feed tank and the heating and evaporating unit is provided with solution feed pump, the vaporizer lower end is provided with medicine liquid outlet, and the outlet of condenser is connected with vacuum extractor; Described spray drying device includes heater in addition, in establish the feed tank of agitating device, have a spray drying tower that aerosol apparatus and attachment are swept dropping control device by pipeline and feed flow are tank connected, feed the hot-blast pipe line of spray drying tower, and the cyclone separator that is connected the spray drying tower back, before spray drying tower, be provided with heating apparatus medicinal liquid is carried out sterilization processing, the connecting line of feed tank and spray drying tower is provided with solution feed pump, and behind solution feed pump, be connected with the pipeline of single-revolution to feed tank, between feed tank and solution feed pump, form a closed circuit, on hot-blast pipe line, be disposed with thick effect air filter, air heater and accurate air filter, cyclone separator adopts secondary cyclone, and second level cyclone separator adopts bispin wind knockout tower structure, described bispin wind knockout tower structure is an air intake vent, inside is divided into two cyclone separating tower that the wind-force rotation direction is opposite, to two products of separated outlets should be arranged; Described air heater is the two-stage air heater, and its first order is steam-heated air heater, and the second level is electrically heated air heater; Described refining plant mainly comprises a centrifugal separating device; On extraction equipment, equipment for separating liquid from solid, sterilizing unit, vacuum concentration equipment, refining plant, secondary concentration equipment and spray drying device, be provided with automatic control system and rinser.
Technology of the present invention has realized Chinese medicine extraction, has removed impurity, sterilization, once concentration, secondary concentration or dryly finish continuously on a streamline.Medicinal liquid repeatedly circulates and enters extraction pot during extraction, begins once more and the medical material contact lysis from tank deck, realizes that dynamic circulation extracts, to the extraction ratio height of Chinese medicine effective ingredient; In addition, the condensing solvent of extraction pot top after oil water separator separates got back in the extraction pot from the extraction pot overhead stream as novel solvent and thermal source, carries out the next round circulation again, forms while extracting separating process, and solvent is fully utilized; Aromatic oil in the medical material rises with steam and enters reflux condenser, carries out the extraction and the separation of aromatic oil then by oil water separator.Chinese crude drug is to put in the powder charge basket in crack with holes in extraction pot, as long as porosity determines suitably both can to guarantee the contact lysis that solvent and medical material are even, smooth, can guarantee that again useless medicinal residues can not sneak in the medicinal liquid, extracting solution is even, makes slagging-off simultaneously and clean tank body very convenient.The medicinal residues that equipment for separating liquid from solid will be mixed in the extracting solution further sieve, and have thoroughly solved the problem of medicinal residues obstruction and wearing and tearing drawing liquid pump.Set sterilizing unit can kill the most of thermoduric bacteria in the medicinal liquid, and the finished product material bacteria containing amount of not only guaranteeing follow-uply to concentrate, obtaining after the dried is low, can also effectively keep the effective ingredient in the medicinal liquid, reduces the drug effect loss.Medicinal liquid is carried out refinement treatment, the remaining fine particle in the medicinal liquid can be separated, make medicinal liquid purer.Vacuum concentration process of the present invention can reduce medicinal liquid greatly and become the heat that gaseous state absorbs from liquid state, and the temperature in the heating tank can be controlled at lower temperature, can effectively keep the effective ingredient of some thermal sensitivity medicines and biologics; The used evaporator of its concentrated medicament both linked to each other for independent tank body and by pipeline with heating tank, formed a closed circuit, can make medicinal liquid carry out dynamic circulation and concentrate, and improved thickening efficiency; Last connection tube between heating tank and the evaporator is set to the structure tangent with evaporator, the internal diameter of last connection tube is less than the internal diameter of heating tank upper cavity, and the liquid-transport pipe-line that connects feed tank and evaporator enters from evaporator top and also extends to the tank body bottom in the tank body always, can make medicinal liquid enter evaporator and in evaporator, form eddy current along inner tank wall from the heating tank high velocity jet, form the medicinal liquid thin film in inner tank wall, increase the medicinal liquid evaporation surface, with the rapid evaporation and concentration of medicinal liquid, and medicinal liquid does not foam when being heated circulation and flow in the jar, guarantee a jar intravital vacuum, the recovery of avoiding causing the drug effect loss and influencing solvent.Secondary concentration technology can be highly concentrated to the medicinal liquid after the once concentration is carried out once more, directly obtains the extractum series products, and whole concentration process medicine is difficult for coking, and the drug effect loss is little, thickening efficiency height, the extractum concentration height of making.In the spray drying, the closed circuit that is provided with is to desiring to carry out the processing that homogenizes in advance of spray-dired medicinal liquid, make that to enter spray-dired medicinal liquid viscosity, composition, temperature even, and can stablize medicinal liquid flow, be convenient to stablize follow-up atomizing effect to guarantee the dried finished products quality; Set air filtration and heating process make the dry air cleaning enters spray drying tower and keep sufficiently high temperature, with raising be dried finished product cleanliness factor and improve drying efficiency; Set two stage cyclone segregation apparatus and bispin wind knockout tower structure can improve the finished product recovery rate effectively; The filtration drying device that is provided with on compressed air line can filter and drying in advance to the compressed air that the feeding attachment is swept in the dropping control device, in order to avoid bring clean and the higher air of moisture into spray drying tower; Heating apparatus is set to the medicinal liquid sterilization of heating before spray drying, can effectively kill the antibacterial in the medicinal liquid, make medicinal liquid reach the hygienic requirements of pharmaceutical production, the finished product that dried obtains does not lump, be small graininess, be convenient to follow-up Cyclonic separating apparatus rewinding and recovery rate height, simultaneously short grained dry thing in follow-up processes such as compression forming because the pressure that puts on the granule is very little, be difficult for producing electrostatic interaction, be convenient to make tablet.
Technology of the present invention is provided with rationally, and compact equipment can all realize automatic control, high efficiency.Complete equipment is the working environment of a sealing, and energy consumption is low, and environmental pollution is little, and cleans conveniently.The finished product material steady quality that production makes, bacteria containing amount is low, can satisfy the code requirement of GMP to pharmaceutical production fully.
Further set forth content of the present invention below in conjunction with Figure of description and embodiment.
Description of drawings
Fig. 1 is a process schematic representation of the present invention;
Fig. 2 finally carries out the equipment sketch map that spray drying treatment obtains dry finished product material for the present invention;
Fig. 3 handles the equipment sketch map that obtains thick paste finished product material for the present invention finally carries out secondary concentration.
The specific embodiment
As shown in Figure 1, technology of the present invention comprises extraction I, solid-liquid separation II, pasteurization III, refining V and the vacuum concentration IV that carries out successively, just after handling, the medicinal liquid vacuum concentration carries out secondary concentration VI again if produce thick paste shape finished product material, if produce dry finished product material, just after handling, the medicinal liquid vacuum concentration carries out spray drying VI.
As shown in Figure 2, the present invention's equipment of preparing thick paste finished product material comprises extraction device A, equipment for separating liquid from solid B, sterilizing unit C, refining plant E, vacuum concentration equipment D and the secondary concentration equipment that is linked in sequence by feed liquid pipeline.As shown in Figure 3, the equipment for preparing dry finished product material comprises extraction device A, equipment for separating liquid from solid B, sterilizing unit C, refining plant E, vacuum concentration equipment D and the spray drying device G that is linked in sequence by feed liquid pipeline.
Extract the extraction pot a1 that device A comprises band heating jacket a6 and discharging opening, the steam pipework a7 and the steam supply a8 that are connected with extraction pot heating jacket a6, by pipeline and the tank connected solvent supply a9 of extraction, connect the extracting solution closed circuit of forming by extraction pot a1 and circulating pump a4 by pipeline, connect the closed circuit of forming by extraction pot a1, condenser a2 and oil water separator a3 by pipeline, in extraction pot a1, be provided with the Chinese medicine basket a5 in crack with holes, be provided with the top cover a10 that can open entirely at the extraction pot top.Pasteurization device C includes heater c1, insulating tube c2 and the cooler c3 that is linked in sequence along the medicinal liquid transfer pipeline.Vacuum concentration equipment D comprises feed tank d3 by pipeline connection, communicates and form evaporation d1 and heating tank d2, vapour liquid separator d4 and the condensing unit d5 of closed circuit up and down, last connection tube d6 and the evaporator of connecting heating tank d2 and evaporator d1 are tangent, and the internal diameter of last connection tube d6 is less than the internal diameter of heating tank d1 upper cavity; Be connected with vacuum extractor d7 in condensing unit d5 back by pipeline, evaporator d1 is provided with vacuum-breaking valve d8; The liquid-transport pipe-line d9 that connects feed tank d3 and evaporator d1 is higher than connection tube d6 from evaporator top position enters and also extends to the tank body bottom in the tank body always; Liquid-transport pipe-line d9 is provided with electrically-controlled valve d10, and evaporator d1 is provided with upper liquidometer d11 and the next liquidometer d12, and two liquidometers all link to each other with control system with electrically-controlled valve d10.Heating and evaporating unit, vapour liquid separator f4, condenser f5 and vacuum extractor f6 that secondary concentration equipment F includes the feed tank f1 that connects by pipeline, connected to form by heater f2 and vacuum evaporator f3; Be provided with agitating device f11 in feed tank f1, the connecting pipe between feed tank f1 and the heating and evaporating unit is provided with solution feed pump f7, and vaporizer f3 lower end is provided with medicine liquid outlet f10, and the outlet of condenser f5 is connected with vacuum extractor f6.Spray drying device G include heater in addition, in establish the feed tank g1 of agitating device g6, have a spray drying tower g3 that aerosol apparatus g4 and attachment are swept dropping control device g7 by what pipeline was connected with feed tank g1, feed the hot-blast pipe line g8 of spray drying tower g3, and the cyclone separator g5 that is connected spray drying tower g3 back; Before spray drying tower g3, be provided with heating apparatus g9 medicinal liquid is carried out sterilization processing; The connecting line of feed tank g1 and spray drying tower g3 is provided with solution feed pump g2, and is connected with the pipeline of single-revolution to feed tank g1 behind solution feed pump g2, forms a closed circuit g10 between feed tank g1 and solution feed pump g2; On hot-blast pipe line f8, be disposed with thick effect air filter g11, air heater and accurate air filter g14, air heater is the two-stage air heater, its first order is steam-heated air heater g12, and the second level is electrically heated air heater g13; Cyclone separator adopts secondary cyclone g5 and g18, and second level cyclone separator g18 adopts bispin wind knockout tower structure, described bispin wind knockout tower structure is an air intake vent, and inside is divided into two cyclone separating tower that the wind-force rotation direction is opposite, to two products of separated outlets should be arranged.Refining plant E mainly comprises a centrifugal separating device e1.On extraction device A, equipment for separating liquid from solid B, sterilizing unit C, vacuum concentration equipment D, refining plant E, secondary concentration equipment F and spray drying device G, be provided with control device and automatic control system, being as indication in the dashed rectangle among Fig. 1 needs the parameter controlled in technology, corresponding i.e. equipment is provided with control instrument.Rinser all is set to be used for cleaning equipment on this external extraction device A, equipment for separating liquid from solid B, sterilizing unit C, vacuum concentration equipment D, refining plant E, secondary concentration equipment F and the spray drying device G.Rinser can be to be directly installed in each tank body or the high-pressure cleaning device of pipeline, also can be to insert by ready-packaged joint.
Work process is as follows:
At first, set to extract the operating condition of device A, as set the solvent addition, extract temperature, running time started, extraction time, medicinal liquid is at tank body internal recycle number of times etc.Solvent can adopt Purified Water or the ethanol through heating, and described Purified Water is purified processing, removed the water behind antibacterial, the impurity, the also available pure water of selling on the market.When solvent was Purified Water, the raw material of Chinese medicine of adding extraction pot was 1: 8～10 with the ratio of solvent, and extracting temperature is 90～99 ℃, and the extracting solution cycle-index is per hour 8～10 times; When solvent was ethanol, extracting temperature was 75～80 ℃, and the extracting solution cycle-index is per hour 8～10 times.Present embodiment selective finishing water is as solvent.Then, open top cover a10, the basket a5 that is loaded with raw material of Chinese medicine is hung in the extraction pot a1, close top cover a10, and locking top cover and tank body.Subsequently, for Purified Water, the Purified Water that comes out from solvent supply a9 enters heat exchanger a13 heating to extraction pot a1.After the Purified Water addition arrives setting value, electromagnetic valve a12 closes, thermoindicating controller a11 starts working, open electromagnetic valve a14 to extraction pot chuck a6 supply steam, the heating steam of coming out from steam supply a8 enters extraction pot chuck a6 from steam pipework a7 through electromagnetic valve a14, heating extraction jar, heating-up temperature are about 95 ℃, and the condensed water of heating steam is discharged from the outlet that is located at extraction pot heating jacket bottom; All link to each other with electromagnetic valve a14 on the steam pipework a7 at the temperature sensor a15 that is provided with on the extraction pot, thermoindicating controller a11 with control system, can control the temperature of extracting solution automatically, when the extracting solution temperature is crossed when low, electromagnetic valve a14 connects, feed steam, heating extraction liquid to the extraction pot heating jacket; When the extracting solution temperature reached setting value, electromagnetic valve a14 disconnected, and stops to feed steam.Can insert steam on the extracting solution closed circuit, directly to feed Steam Heating in tank body, increase a jar intravital temperature and pressure, carry out pressurised extraction, when the pressure in the jar reached setting value, the beginning dynamic circulation was extracted.Pressure transducer a16 that is provided with on extraction pot and set electromagnetic valve a17 all are connected with control system, can control the pressure in the extraction pot automatically, when the beginning pressurised extraction, electromagnetic valve a17 connects, and feeds steam in extraction pot, heating extraction liquid, improve a jar intravital pressure, when the jar internal pressure reached setting value, electromagnetic valve a17 disconnected, and stops to feed steam.The first medicinal liquid that extracts enters extracting solution circulating pump a4 through circulation line, and extracting solution circulating pump a4 starts working; Just carry medicinal liquid and squeeze into extraction pot a1 by circulating pump a4 after medicinal liquid flow meter a18 metering, carry out dynamic circulation and extract, the medicinal material extract in extraction pot finishes.General cycle-index is per hour 8～10 times.The operating parameters of flow-control circulating pump a4 that can be by effusion meter a18 is regulated the flow of circulation medicinal liquid, thereby is regulated the cycle-index in the unit interval, and each leaching process is finished approximately and needed 1～3 hour.Because the extraction pot inner liquid medicine repeatedly circulates when extracting and enters extraction pot, add the structural design of basket a5, medicinal liquid is begun once more and the medical material contact lysis from tank deck, in the decline process, form reverse exchange with medical material, reach dynamic hot reflux effect, keep a jar interior spice gradient simultaneously, realize the dynamic circulation extraction.When reclaiming the operation of aromatic oil, at first open extraction pot upper pipeline valve, make the interior aromatic oil of extraction pot along with steam rises, after reflux condenser a2 cooling, it is separated to enter oil water separator a3, and condensed fluid is in reflux pipe flow back into extraction pot a1, and this condensed liquid is got back in the tank body from the extraction pot top as novel solvent and thermal source, carry out the next round circulation again, form while extracting separating process.After extraction finishes, take out powder charge basket a5, take out medicinal residues and focus on.
Then, the medicinal liquid that extracts enters solid-liquid separating equipment B by pipeline.Through equipment for separating liquid from solid b1 the residual medicinal residues in the extracting solution are separated, separated to store among the fluid reservoir b2 that the medicinal liquid that obtains is drawn into the back and prepare to enter sterilization process.
Subsequently, liquid-feeding pump is sent medicinal liquid into sterilizing unit C, medicinal liquid is pumped among the heater c1, in heater c1, feed steam, fluid temperature is risen to about 120 ℃ instantaneous, medicinal liquid flows through thermophore c2 insulation 10～30 seconds after heater comes out, flow to cooler c3 again, fluid temperature from 120 ℃ of instantaneous reducing to about 60 ℃, is finished sterilization process.Medicinal liquid after sterilization flows into follow-up storage tank c4.
In order to make medicinal liquid purer,, improve end product quality to reduce the impurity content of final products as far as possible, can again medicinal liquid be imported refining plant E medicinal liquid is carried out refinement treatment, be about to medicinal liquid and pump among the centrifugal separating device e1, further the impurity in the medicinal liquid is separated, obtain the medicinal liquid of high cleanliness.
Afterwards, the medicinal liquid after the refinement treatment is sent into vacuum concentration equipment D and carried out the vacuum concentration processing.In evaporator d1 tank body, feed steam and carry out disinfection, finish sterilization after, confirm that fluid temperature in the feed tank d3 and amount of liquid medicine start working after up to specification.Open device d5 with fixed attention, start vacuum extractor d7 and begin evacuation, the absolute pressure that is evacuated in the evaporator d1 also keeps about 10600Pa.By liquid-transport pipe-line d9 feed flow in evaporator d1, pipeline d9 extends to the evaporator bottom always in evaporator d1 then, makes medicinal liquid flow directly into evaporator d1 bottom, avoids destroying the evaporating surface of medicinal liquid taper eddy current.Medicinal liquid again through evaporator d1 outlet at bottom by and heating tank d2 between connection tube d14 flow in the heating tank d2.In heating tank d2, be blown into Steam Heating, feed flow reach a certain amount of after, medicinal liquid is evaporated and circulates between evaporator d1 and heating tank d2, upper and lower liquidometer d11, d12 that evaporator d1 go up to be provided with are connected with control system with electrically-controlled valve d10, can Comprehensive Control evaporator d1 interior amount of liquid medicine and the liquid supply rate of feed tank d3.Medicinal liquid tangentially flows back to evaporator d1 from heating tank d2 at a high speed by last connection tube d6, and forms the eddy current of taper in the evaporation tank body, can enlarge disengagement area, improves evaporation efficiency, eliminates foamed phenomenon.Medicinal liquid carries out dynamic circulating and evaporating in the thin film evaporation mode always in the tubulation of heating cylinder and in the evaporator, gradually medicinal liquid is concentrated.The gas that comes out in the evaporator d1 enters gas-liquid separator d4 and carries out gas-liquid separation, the steam suction condensing unit d5 of vacuum evaporation cools off, enter at last and reclaim liquid storage tank d13, carry out separating of gas and liquid once more, wherein gas is discharged by the pipeline that links to each other with vacuum extractor d7, and remaining condensed fluid is then sent in the retracting device.Reach when setting value when medicinal liquid is concentrated into proportion, get final product discharging.In whole vacuum concentration process flow process, the absolute pressure in the evaporator remains on 9500～20000Pa, and temperature remains on 45～60 ℃, and steam pressure remains on 0.1～0.3MPa in the heating tank.After concentration process is finished, open vacuum-breaking valve d8, eliminate vacuum.
At last, according to demand, send into concentrated medicament among the secondary concentration equipment F or spray among the thing drying equipment G and do respective handling the final finished material.
After entering secondary concentration equipment F, heating feed tank f1 starts agitating device f11 concentrated medicament is stirred to add the concentrated medicament of thermmal storage; Open condenser f5, start vacuum extractor f6 and begin evacuation, the absolute pressure that is evacuated in the vacuum evaporation cylinder f3 also keeps at 10600Pa.With solution feed pump f7 concentrated medicament is delivered into pre-heater f8, the while infeeds steam to vacuum evaporator f3's with pre-heater f8, and steam is along medicinal liquid mobile reverse feeding in pre-heater f8 and heater f2.Medicinal liquid falls into vacuum evaporator f3 after being vaporized in heater f2, cooling and condense into the thick paste shape in the process that the medicinal liquid of vaporization descends in vaporizer f3.The residue vapor of separating in the vacuum evaporator f3 enters carries out vapor-liquid separation in the vapour liquid separator f4, steam reclaims after stram condenser f5 condensation.In concentration process, to be controlled at about 60 ℃ by the fluid temperature that feed tank comes out to enter before the pre-heater f8, fluid temperature after the pre-heater heating is controlled at about 85 ℃, the fluid temperature of heater via f2 heating back vaporization is controlled at about 115 ℃, absolute pressure in the control vacuum evaporator f3 is at 10600Pa, temperature is about 70 ℃, and steam pressure is 0.25MPa.Thick paste shape finished product material after concentrating imports receiving vessel from outlet f10.Open vacuum-breaking valve f9, eliminate vacuum.
After entering spray drying device G, feed tank g1 is to add thermmal storage concentrated medicament wherein in heating, starts the agitating device g6 in the feed tank simultaneously, and running quantitative liquid feeding pump g2 makes concentrated medicament at closed circuit g10 internal recycle, to the concentrated medicament processing that homogenizes.Confirm steam and compressed-air actuated pressure, open the chiller of aerosol apparatus g4 and adjust the rotating speed of centrifugal atomizer g4, adjust the liquid supply rate of quantitative liquid feeding pump g2, below cyclone separator g5, g18, place dry finished product material receptor, set the control temperature of each workshop section, the general temperature of setting in the feed tank g1 is 60～90 ℃, and the hot air temperature that enters spray drying tower g3 is 150～160 ℃, and the temperature in the first order cyclone separator g5 is 80～100 ℃.The attachment that starts in centrifugal atomizer g4, the spray drying tower g3 is swept dropping control device g7, compressed air is fed attachment sweep winding-up pipe on the dropping control device g7, running air draft blower fan g15 and breeze fan g16, air filters through just imitating air filter g11, enter steam-heated air heater g12, after passing through electrically heated air heater g13 again, after filtering, accurate air filter g14 enters centrifugal atomizer g4 by hot-blast pipe line g8.When the concentrated medicament among the feed tank g1 homogenize handle reach requirement after, when the temperature in the first order cyclone separator g5 reaches setting value, opens solenoid valve g17, the liquor charging of quantitative liquid feeding pump g2 changes, medicinal liquid is carried by quantitative liquid feeding pump g2 and enter centrifugal atomizer g4 behind heating apparatus g9, the atomizer of high speed rotating becomes medical liquid atomizing the fine droplet of 50～100 μ m, this moment, droplet fully mixed in the spray dryer tower body with the hot-air of coming from accurate air filter g14, because droplet generally all is controlled between 50～100 μ m, so the surface area that the drop of per unit weight contacts with dry-heat air is very big, and the efficient of dry run is very high.A small amount of dried particles attached to spray drying tower g3 inwall is arranged, sweep dropping control device g7 by attachment and sweep.Dried solid product is transported to primary cyclone g5 with wind-force, fall in the finished product material receiving vessel by the product after the cyclone separator separation, receive 92%～95% finished product approximately, the wind that other is mixed with a small amount of dry products enters separation once more in the secondary cyclone g18 again, product after the separation falls in the finished product receiving vessel, can receive 92%～95% in the surplus products approximately.Last gas is drained by discharge duct.When the production of last batch of concentrated medicament is finished, stop agitating device g6, when liquid level drops to pot liquid and almost do not have, add low amounts of water as the washings in the pipe arrangement.
After whole Chinese medicine preparation process is finished, start rinser, the pipeline that each tank body and medicinal liquid are flowed through cleans.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101897649A (en) * | 2009-06-01 | 2010-12-01 | 王学永 | Microcomputer Chinese medicine tonic paste machine |
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