A kind of Chinese medicine material extraction process and equipment
Technical field
The present invention relates to a kind of technology of extracting the contained active ingredient of Chinese medicine raw material, and the equipment that is used for this explained hereafter herb liquid.
Background technology
At present, the water liquid decoction pot that domestic most of pharmaceutical factories of traditional Chinese medicine have also continued to use nearly one thousand years in use just adds chuck in the decoction pot bottom as the Chinese medicine extraction equipment, adopts the coil pipe in chuck to feed Steam Heating.Also have part producer to adopt the multi-function extractor of stainless steel manufacturing Chinese medicine to be carried out water is carried or alcohol extracting, be aided with and install stirring system additional at the extractor top cover and carry out Dynamic Extraction, strengthen the mass transfer of leaching process and increase heat-exchanger circuit, the lixiviate that refluxes operation.These extraction equipment 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.Because reinforced, the discharging of this kind equipment and the control of whole leaching process are so far still to be operating as the master manually, it is bigger that quality of liquid medicine is influenced by human factor, is difficult to guarantee the quality of tcm product.In addition, also have some producers to adopt the diacolation extracting technology, this technological operation cycle is long, the solvent consumption is big, production cost is high, and still has the essence weakness of traditional extracting technology.Now, most pharmaceutical factories of traditional Chinese medicine are the many variety production of small lot, adopt the andnon-continuous operation manner lixiviate, and production equipment frequently has enough to meet the need, and cleaning equipment is simple and crude, and cleaning performance lacks necessary examination criteria, and the possibility of soup cross pollution is very big.
Summary of the invention
Purpose of the present invention provides a kind of both energy savings to make just and extracts concentrated difference maintenance high gradient in order to overcome above-mentioned the deficiencies in the prior art, can quicken the leaching of medicinal material active ingredient, simultaneously can solve of the setting of different extracts to customized parameters such as solvent ratio, temperature, time, pressure, cycle-indexes, help the raising of stable, the efficient of quality, and it is more even to extract liquor strength, and the dynamic circulation that can control automatically of not having precipitation, slag tap and cleaning very convenient and production safety is extracted the technology and the equipment of Chinese medicine material.
The objective of the invention is to be achieved through the following technical solutions.
A kind of Chinese medicine material extraction process, its technical process is: connect condenser and oil water separator and form a closed circuit by pipeline on extractor, and form another closed circuit by pipeline connection circulating pump on extractor; Chinese medicine material is contained in the basket in crack with holes, basket is packed in the extractor, again liquid solvent is added extractor and carry out heat temperature raising with the Steam Heating extractor, Chinese medicine material is soaked into into rare soup, rare soup is squeezed in the extractor by closed circuit once more by circulating pump, carries out dynamic circulation and extracts; Simultaneously, aromatic oil in the Chinese medicine material is evaporated the vapours that is mixed with aromatic oil and enters oil water separator after by condenser and separate, solvent after the separation flows back in the extractor from the extractor 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 Chinese medicine material.
In technology of the present invention, described solvent can be water or alcohol, and when solvent was water, adding the Chinese medicine material of extractor and the mass ratio of solvent was 1: 8~10, and extracting temperature is 90~99 ℃, and the extract cycle-index is per hour 8~10 times; When solvent was alcohol, the mass ratio of raw material and solvent was 1: 4~8, and extracting temperature is 70~85 ℃, and the extract cycle-index is per hour 8~10 times.In leaching process, in extractor, feed steam, carry out pressurised extraction, pressure ranges up to 2.0Mpa.
For realizing extraction process of the present invention, the traditional Chinese medicine extraction equipment that is adopted is the Chinese medicine basket that is provided with crack with holes in extractor, is provided with the top cover that can open entirely at the extractor top.
For ease of extracting and improving extraction efficiency, be arranged at Chinese medicine basket in the extractor and be set at least 2 and stack for ease of uncapping, on the top cover of extractor, be connected with hood-opening device, hood-opening device can adopt oil pressure hood-opening device or air pressure hood-opening device; Described oil pressure hood-opening device comprises oil pressure pumping plant, driving oil cylinder and the connecting rod that is linked in sequence, and the middle part of connecting rod is hinged on the pedestal, and the other end and the top cover of connecting rod are hinged; Circulating line on the extract closed circuit tangentially enters tank body from extractor top along tank body; This equipment extractor is provided with the steam inlet, and this steam inlet can be set directly on the tank body, or inserts on the extract closed circuit by connector; For realizing automatic control, the connecting pipe between extractor and the solvent supply is provided with flowmeter, magnetic valve and heat exchanger, and heat exchanger is connected with steam supply; Connecting pipe between extractor heating jacket and the steam supply is provided with magnetic valve, and extractor is provided with temperature sensor and thermoindicating controller, and temperature sensor, thermoindicating controller and magnetic valve all link to each other with control system; Between extractor and circulating pump, be provided with the medicinal liquid flow meter; Connecting pipe between extractor and the steam supply is provided with magnetic valve, and extractor is provided with pressure sensor, and pressure sensor all is connected with control system with magnetic valve; For ease of cleaning, on the pipeline of extractor and soup process, be provided with the interface that is connected with cleaning device.
Extractor inner liquid medicine of the present invention repeatedly circulates when extracting and enters extractor, begin once more and the medicinal material contact lysis from tank deck, the soup of decline becomes reverse exchange with medicinal material, reach dynamic hot reflux effect, keep a jar interior spice gradient simultaneously, realize the dynamic circulation extraction.In addition, the condensing solvent of extractor top after oil water separator separates got back in the extractor from the extractor 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.Adopt different solvent and process conditions, can satisfy extraction requirement the different qualities medicinal material.Aromatic oil in the medicinal material is mingled in the steam, and rising with steam enters reflux condenser, then by oil water separator, utilizes water different with the proportion of oil, can carry out the extraction and the separation of aromatic oil easily.Chinese medicine is to put in the powder charge basket in crack with holes in extractor, as long as porosity is determined suitably, both can guarantee the contact lysis that solvent and medicinal material are even, smooth, and can guarantee that again the useless dregs of a decoction can not sneak in the soup, make slagging-off simultaneously and cleaned tank body very convenient.Basket in the tank body takes the multilayer basket to stack, and can reduce the volume and weight of single basket on the one hand, is convenient to put into and take out tank body, on the other hand, it is blocked up effectively to avoid medicinal material to pile up in basket, and solvent is fully contacted with medicinal material, with the active ingredient in the abundant extraction medicinal material.Top at extractor is provided with the hood-opening device that can open entirely, is convenient to the turnover of basket.Set hood-opening device can be realized automatic lid closing/opening easily.Circulating line on the extract closed circuit tangentially enters tank body from extractor top along tank body, extract is tangentially passed back in the extractor, forms eddy flow in jar, can quicken circulating of extract, increases the soup mass transfer and improves extraction efficiency.All link to each other with control system with magnetic valve on the steam pipework at the temperature sensor that is provided with on the extractor, can control the temperature of extract automatically, cross when low when the extract temperature, magnetic valve is connected, and feeds steam to the extractor heating jacket, the heating extract; And when the extract temperature was too high, magnetic valve disconnected, and stopped to feed steam.The steam inlet is set on extractor, can in tank body, feed Steam Heating, increase the pressure in the tank body, carry out pressurised extraction, the magnetic valve that steam pipework is provided with all links to each other with control system with pressure sensor on the tank body, the pressure in the control tank body, pressurised extraction has impelled solvent to circulate between medicinal material, dynamically hot reflux makes a jar interior spice remain on certain gradient, and has increased friction wash-out dynamics, has accelerated the dissolving of centering pharmaceutically active ingredient and has leached.By-pass valve control that is provided with on each pipeline that communicates with extractor and instrument can realize that the automatic control of whole extraction process and operating personnel observe the extraction working condition at any time, in time adjust duty.All be provided with cleaning device on the pipeline of extractor and soup process, make extractor and soup transfer pipeline obtain cleaning comparatively easily, guarantee to meet the hygienic requirements of GMP standard.As long as the present invention controls extraction conditions well, the operation that the entire equipment system can be automatic, stable.By the accurate control of set control components and parts, make traditional Chinese medicine extraction process quantification, standardization, scientific more simultaneously, reduced the interference of human factor.Technology of the present invention and equipment have to Chinese medicine effective ingredient recovery rate height, extract evenly (do not have precipitation), extraction time is short, power consumption is low, take up an area of advantages such as few, realized the operation of soup closed circulation simultaneously, Automatic Control has satisfied the requirement of GMP to pharmaceutical production.Multiple extracting modes such as this equipment is applicable to that water is carried, alcohol extracting and high pressure extraction.
Further set forth content of the present invention below in conjunction with Figure of description.
Description of drawings
Fig. 1 is a Processes and apparatus connection diagram of the present invention;
Fig. 2 is the structural representation of extractor part in the present device;
Fig. 3 is the left view of Fig. 2;
Fig. 4 circulates the mode schematic diagram for soup of the present invention in extractor.
The specific embodiment
As Fig. 1, Fig. 2 and shown in Figure 3, at first according to producing the selected extractor 14 of running automatically of needs, three powder charge baskets 17 that stack are set in extractor, at the extractor outer bottom heating jacket 8 is set, the top is provided with the top cover 31 that can open entirely by hood-opening device 32, and present embodiment adopts the oil pressure hood-opening device, is linked in sequence by oil pressure pumping plant 13, driving oil cylinder 34 and connecting rod 35 and forms, the middle part of connecting rod 35 is hinged on the pedestal, and the other end of connecting rod and top cover 31 are hinged; On extractor 14, connect reflux condenser 11, oil water separator 13, circulating pump 7, solvent supply 4 and steam supply 12 respectively with pipeline; Wherein, extractor 14 and reflux condenser 11, oil water separator 13 are connected to form closed circuit by pipeline; Extractor 14 and circulating pump 7 are also connected to form closed circuit by circulating line 36, and circulating line 36 tangentially feeds extractor 14; Extractor heating jacket 8 is connected with steam supply 12 with steam pipework 21, and extractor 14 is connected with steam supply 12 with steam pipework 15; Bottom at extractor 14 is provided with discharging opening, at external ready-packaged joint 30 of discharging opening and flexible pipe.Flowmeter 6, magnetic valve 5 and heat exchanger 2 are set on the connecting pipe between extractor 14 and the solvent supply 4, again heat exchanger are connected with steam supply 12, a magnetic valve 16 is set on the connecting pipe between heat exchanger 2 and the extractor 14 again; Be provided with magnetic valve 1 leading on the jet chimney of heat exchanger 2 into, the solvent pipeline is provided with thermoindicating controller 3; On the connecting pipe between extractor heating jacket 8 and the steam supply 12, magnetic valve 20 is set, temperature sensor 27 and thermoindicating controller 22 are set on extractor, temperature sensor 27, thermoindicating controller 22 and magnetic valve 20 all link to each other with control system, and the temperature sensor of each tank body all links to each other with moisture recorder 26; Between extractor 14 and circulating pump 7, medicinal liquid flow meter 19 is set; On the connecting pipe 15 between extractor 14 and the steam supply 12 magnetic valve 9 is set, pressure sensor 10 is set on extractor, pressure sensor 10 all is connected with control system with magnetic valve 9.On the pipeline of extractor 14 and soup process cleaning device is set all, according to demand, cleaning device can be selected high-pressure cleaning device or connect cleaning device with pipe interface.
Technical process is as follows: at first, the set device operating condition is set flowmeter 6 flows and is determined to add the solvent amount, the temperature of design temperature indicating controller 22 determines to extract temperature, set timer and determine the running time started, set extraction time, soup circulates in tank body.Solvent can adopt Purified Water or the alcohol through heating, and described Purified Water is purified processing, removed the water behind bacterium, the impurity, the also available pure water of selling on the market.When solvent was Purified Water, the Chinese medicine material of adding extractor was 1: 8~10 with the ratio of solvent, and extracting temperature is 90~99 ℃, and the extract cycle-index is per hour 8~10 times; When solvent was alcohol, extracting temperature was 75~80 ℃, and the extract cycle-index is per hour 8~10 times.Present embodiment selective finishing water is as solvent.Then, 33 pressurizations of oil pressure pumping plant drive oil cylinder 34 by petroleum pipeline, open top cover 31 by connecting rod 35, three baskets 17 that are loaded with Chinese medicine material are hung in after stack places in the extractor 14 successively 33 pressure releases of oil pressure pumping plant, close top cover 31, and lock top cover and tank body with bolt.Subsequently, open moisture recorder 26, open magnetic valve 16, supply Purified Water to extractor 14, start Purified Water flowmeter 6 simultaneously, open magnetic valve 5, the Purified Water in the solvent supply 4 enters heat exchanger 2 heating by flowmeter 6, and the Purified Water heating is decided by the magnetic valve 1 of thermoindicating controller 3 by control steam supply.When the Purified Water addition after flowmeter 6 is confirmed to arrive setting value, magnetic valve 5 cuts out, thermoindicating controller 22 is started working, open magnetic valve 20 to extractor chuck 8 supply steam, heating steam enters extractor chuck 8 from jet chimney 21 through magnetic valve 20, heating extractor, heating-up temperature are about 95 ℃, and the condensed water of heating steam is discharged from the outlet 28 that is located at extractor heating jacket 8 bottoms; The temperature sensor 27 that is provided with on the extractor, thermoindicating controller 22 with steam pipework 21 on magnetic valve 20 all link to each other with control system, can control the temperature of extract automatically, when the extract temperature is crossed when low, magnetic valve 20 is connected, feed steam to extractor heating jacket 8, the heating extract; And when the extract temperature was too high, magnetic valve 20 disconnected, and stopped to feed steam and can pass through moisture recorder 26, the temperature in track record and the observation extractor.Insert steam by connector 29 on the extract closed circuit, can directly feed Steam Heating in tank body, increase the temperature and pressure in the tank body, carry out pressurised extraction, when the pressure in the jar reached setting value, the beginning dynamic circulation was extracted.Pressure sensor 10 that is provided with on extractor and set magnetic valve 9 all are connected with control system, the temperature that can control extract is automatically crossed when low when the extract temperature, magnetic valve 9 is connected, feed steam to extractor heating jacket 8, the heating extract, and when the extract temperature was too high, magnetic valve 9 disconnected, and stopped to feed steam.When needs carry out pressurised extraction to Chinese medicine material, directly feed in the tank body the soup pressurization of heating with steam, the valve closing before the condenser prevents that pressure scatters and disappears.The first soup that extracts enters extract circulating pump 7 through circulation line, carry soup at the beginning of extract circulating pump 7 is started working and after 19 meterings of medicinal liquid flow meter, squeeze into extractor 14 by circulating line 36 by circulating pump 7, carry out dynamic circulation and extract, the medicinal material extract in extractor finishes.General cycle-index is per hour 8~10 times.The operating parameters of flow-control circulating pump 7 that can be by flowmeter 19 is regulated the flow of circulation soup, thereby is regulated the cycle-index in the unit interval, and each leaching process is finished approximately and needed 2~3 hours.Because repeatedly circulating and tangentially enter extractor along tank body, the extractor inner liquid medicine forms eddy flow when extracting, add the structural design of basket, make soup begin once more quick and medicinal material contact lysis from tank deck, in the decline process, form reverse exchange with medicinal material, reach dynamic hot reflux effect, as shown in Figure 4, keep a jar interior spice gradient simultaneously, realize the dynamic circulation extraction.When reclaiming the operation of aromatic oil, at first open extractor upper pipeline valve, make the interior aromatic oil of extractor along with steam rises, after reflux condenser 11 coolings, enter oil water separator 13, utilize profit proportion difference, the aromatic oil of light specific gravity reclaims from recovery fragrance oil pipe 18 outflows of a high position, condensate liquid is in return line flow back into extractor 14, this condensed liquid is got back in the tank body from the extractor top as novel solvent and thermal source, carry out the next round circulation again, form while extracting separating process.Reflux condenser 11 adopts multi tube heat exchanger.If extract in fixing time and finish, just close magnetic valve 20 this moment to pipe box supply steam, stop heating; Close extract circulating pump 7, soup is carried out subsequent treatment from drawing after ready-packaged joint 30 connects flexible pipe.Take out powder charge basket 17, take out the dregs of a decoction and focus on.Cooling water inlet 25 and coolant outlet 24 are set on extractor chuck 8, can feed cooling water the extractor chuck is cooled off; After the extractor inner liquid medicine is drawn, the pipeline that cleaning fluid inserts extractor and soup process is cleaned, guarantee to meet the hygienic requirements of GMP standard with set cleaning device.
Extraction equipment of the present invention can also install the vacuum switching device shifter additional, makes the extractor internal environment be in vacuum state, carries out the dynamic alcohol extraction process of Chinese medicine, to satisfy the specific (special) requirements of some medicinal materials.