CN1579592A - New-type technological equipment and method for plant extraction - Google Patents

New-type technological equipment and method for plant extraction Download PDF

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CN1579592A
CN1579592A CN 03132385 CN03132385A CN1579592A CN 1579592 A CN1579592 A CN 1579592A CN 03132385 CN03132385 CN 03132385 CN 03132385 A CN03132385 A CN 03132385A CN 1579592 A CN1579592 A CN 1579592A
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extract
plant
microwave
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王锡康
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Abstract

The invention relates to a new multifunctional assorted equipment of plant extraction and its technics. Extraction rate of the equipment is high; time is short; energy consumption is low; impregnant is little; control is easy; operation is flexible and applied range is wide. Five extraction units is made through improving current homogenate, braking wall, ultrasonic, microwave and conventional extraction equipment. In term of design idea of predominance complementation and overall consideration, the five units are organically combined as uniquely functional equipment and create fine grinding, intermittence countercurrent and extraction of fresh matters without water. Merits of the invention are that extraction time can be shorted one second to two thirds; impregnant dosage is reduced 50-70 percent and energy consumption is reduced 40-60 percent. Quantity of pesticide, fertilizer and heavy metal remnants is lower than current standard. Plants of the invention include Chinese herbal medicine, wilding and agricultural and sideline products. Impregnants include organic solvent, inorganic solvent and water.

Description

A kind of new process equipment and process that is used for plant extract
Technical field the invention relates to a kind of new process equipment and process that plant (comprising Chinese herbal medicine, wild plant, agricultural byproducts, down together) is extracted that be used for.
The background technology plant is the extremely abundant renewable resource of occurring in nature, and the Chinese herbal medicine in the plant, wild plant, agricultural byproducts then are medicine, food, cosmetics and other industrial important source material.The most frequently used processing method is exactly by extracting, with solvent desirable ingredients is therefrom extracted, with methods such as film separate solvent being separated by concentrated, absorption, precipitation, crystallization with solute again, for further processing.The extraction of plant functional component claims leaching, lixiviate or extraction again, and the many examples that are extracted as with Chinese medicine of this specification except that specific term, are referred to as extraction by the custom of Chinese medicinal material industry with extraction, leaching and lixiviate.
Traditional extracting method mainly contains infusion process, percolation, decocting method, reflux extraction and continuous backflow extraction method etc.
(1) the infusion process infusion process is with in the powder of extract or the fragment dress people proper container, adds The suitable solvent with the stripping method of composition wherein.This law is relatively simple, but leaching rate is relatively poor, is solvent as water, and its extract is easy to moldy metamorphism.
(2) the percolation percolation is that powder with extract is contained in the percolator, constantly adds novel solvent, makes it penetrate extract, flows out a kind of extracting method of leachate from top to bottom from the percolator bottom.When solvent infilters that Chinese herbal medicine stripping composition proportion strengthens and when moving down, its position is just replaced in the solution on upper strata or rare immersion liquid, causes good concentration difference, and diffusion energy is carried out preferably, so extraction effect is better than infusion process.
(3) the decocting method decocting method is the extracting method that China uses the earliest, adopts big reaction pot, big copper pot, barrel more, or feeds Steam Heating in the pond of cement block, also several can be decocted device and be connected to each other by pipeline, fries in shallow oil continuously and soaks.
(4) reflux extraction is used organic solvent heating extraction, needs to adopt the backflow heater, in order to avoid the solvent evaporates loss.Solvent soaked the about 1~2cm in Chinese herbal medicine surface.Add hot reflux in water-bath, keep putting cold filtration behind the boiling number hour, solubilizer in Chinese herbal medicine is done second and third time and is added hot reflux again, till carrying most functional component substantially.
(5) continuous extraction is used the functional component that volatile organic solvent extracts plant, and what suitability for industrialized production was the most frequently used at present is exactly continuous extraction.Compare with other conventional method, continuous extraction need be less with quantity of solvent, and it is also more complete to extract composition.But continuous extraction generally needs a few hours could extract fully, and it is longer to extract the composition heated time, and the labile composition of case of thermal instability should not adopt this method.
There are three intrinsic weakness in the tradition extraction method: the one, and solvent load is big, and loss is big, and extraction time is long, and yield is low, purity difference, energy consumption height.The 2nd, some heat-sensitive substances are often oxidized decomposition in leaching process, causes damage.The 3rd, the agricultural chemicals in the extract, chemical fertilizer and heavy-metal residual exceed standard easily.
With the Chinese medicinal material industry is example, and the Chinese herbal medicine ingredient is very complicated, and existing active ingredient has invalid components and toxic component again.In order to improve the result of treatment of Chinese herbal medicine, will use up effective component extracting to greatest extent, remove invalid components and toxic component.Therefore, Chinese herbal medicine extracts for the inherent quality and the clinical efficacy that improve Chinese medicine preparation the most important.But extracting method commonly used is removed the invalid components aspect keeping active ingredient, exists that loss of effective components is big, the cycle long, operation is many, the not high shortcoming of recovery rate.China's Chinese medicine exists production Technology to fall behind, and the through engineering approaches level is low, and process facility modernization degree is low, traditional Chinese medicine enterprise is one little, more than two, three low, Chinese medicine preparation falls behind, and each link lacks the standard criterion control of international endorsement, has problems such as constant product quality is relatively poor.Along with the quickening and the China joined WTO of economic globalization process, the negative effect of this situation will highlight more.
Over nearly 10 years, many new technologies, new method have appearred aspect plant extract, many research reports show, these new technologies, new method have advantages such as recovery rate height, loss of effective components is few, the cycle is short really, and these advantages demonstrate them and are with a wide range of applications in industrial production such as Chinese medicine preparation.
(1) supercritical liquid extraction technique supercritical fluid extraction (SC FEFE) is a kind ofly to replace conventional organic solvent that Chinese herbal medicine effective ingredients is extracted and the new technique that separates with supercritical fluid (be called for short SCF), its principle be utilize fluid (solvent) near critical point in certain zone (supercritical region) with mixture to be separated in solute have the behavior that balances each other unusually and transmit performance, and the solvability to solute changes in quite wide scope with the change of pressure and temperature, utilize this SCF to make solvent, can from multiple liquid state or solid mixt, extract component to be separated.SCF commonly used is CO 2, because CO 2Nontoxic, nonflammable explosive, inexpensive, lower critical pressure and temperature are arranged, be easy to from mixture, separate safely.Supercritical CO 2Extraction is compared with traditional extraction process, and biggest advantage is to extract separation under the condition of near ambient temperature, whole active ingredients in the retained product almost, and organic solvent-free is residual, and the product purity height is simple to operate, energy-conservation.The SCFE technology demonstrates unique advantage for the active ingredient of extracting separating volatile composition, liposoluble substance, high-thermosensitive material and valuable medicinal.But the extraction that is used for Chinese medicine, wild plant and agricultural byproducts functional component exists: 1. lack biologic artifact solubility and equilibrium under high pressure in design, in most of the cases, need measure by experiment; 2. SC-CO commonly used at present 2Be difficult to effectively extract for many strong polarity and polymer substance.Though 3. the supercritical fluid extraction process is an energy-conservation process, the economy of process depends on the ability that recovers energy or reduces the required energy of gas compression that small-sized and discontinuity production will make its superiority have a greatly reduced quality greatly; 4. the output investment ratio that comprises high-tension apparatus is expensive, and the high pressure technique of employing also embarrasses people to accept, and heavy industrialization plant extraction device does not come out so far, so this technology also is difficult to popularize at present in industrial production.
(2) basic principle of ultrasound assisted extraction technique ultrasound assisted extraction technique mainly is to utilize cavitation effect of ultrasonic waves to quicken the leaching of effective ingredients in plant, hyperacoustic in addition second order effect, as mechanical oscillation, emulsification, spread, smash, chemical effect etc. can quicken also that desire extracts that the diffusion of composition discharges and fully and solvent, be beneficial to extraction.Compare with conventional extraction method have extraction time short, productive rate is high, need not advantages such as heating.The ultrasonic technique extracting method is simple, the recovery rate height, and low-consumption high-efficiency has wide application prospect as a kind of means of extracting.Ultrasound assisted extraction technique can be avoided the destruction of HTHP to active ingredient, but it has relatively high expectations to the thickness and the container placement location of chamber wall, otherwise can influence the medicinal material leaching effect.And experimental study all is to be in very on a small scale at present, be used for large-scale production, the scale-up problem of the relevant works equipment that awaits further to solve.
(3) the microwave-assisted extraction technique microwave abstracting is the new technology that a kind of latest development of utilizing microwave energy to improve extraction yield is got up.Its principle is in microwave field, the difference that absorbs the microwave ability makes some zone of base matter or some component in the extraction system be heated by selectivity, thereby make that be extracted material separates from matrix or system, advance that the people is less to dielectric constant, in the extractant of microwave absorption capacity relative mistake; Microwave abstracting has that equipment is simple, applied widely, extraction efficiency is high, favorable reproducibility, save time, save reagent, pollute characteristics such as little.At present, except that being mainly used in the environmental sample preliminary treatment, also be used for fields such as biochemistry, food, Industrial Analysis and natural product extraction.At home, microwave-assisted extraction technique is used for Chinese herbal medicine to extract the research report of this respect also fewer.It is a kind ofly to save time conveniently that this technology is applied to that medicinal material leaches, and the Chinese medicine that is worthy to be popularized universal leaches new method.Microwave-assisted extraction technique is compared with the traditional decoction method, has overcome the easily disadvantage of the easy coking of cohesion of medicinal material fine powder, and extraction time is extremely short, and equipment is simple, invests less.But this technology is used for Chinese herbal medicine extracts genus starting still, and its extraction mechanism also needs further research.
(4) impurity of enzyme process Chinese medicine preparation mostly is starch, pectin, protein etc. greatly, can select for use suitable enzyme to be decomposed at impurity and remove.Enzyme reaction is more leniently decomposed plant tissue, can improve yield by a relatively large margin, a kind of one of method of effective component extracting in the plant to greatest extent so enzymolysis be can yet be regarded as, and this is a up-and-coming new technology.Cellulase is used for the Chinese medicine effective component extracting based on cellulose, really can improve the yield of active ingredient, but will widen its application, also need further deeply to inquire into the concentration of enzyme, the concentration of substrate, temperature, acid-base value, what influence inhibitor and activator etc. have to extract.Enzyme process is being used comparatively extensively at present aspect the animal medicinal material extraction.
(5) semi-bionic extraction semi-bionic extraction (being called for short the SBE method) is that whole medicine organon is combined with the molecular medicine organon, from biopharmaceutical angle, simulation oral administration and medicine be through the principle of intestines and stomach transhipment, is a kind of new extraction process through the Chinese medicine preparation design of alimentary canal administration.Be about to spice and extract with the sour water of certain pH earlier, continue with the buck extraction of certain pH, extract filters, concentrates, makes preparation respectively.It unites analytic thinking and system's thinking, forms the new approaches of observation problem, has promptly adhered to " the composition opinion is arranged, and the theory of the unique importance of class origin not focuses on the pharmacodynamics reaction of body " in traditional Chinese medicine extraction.More active ingredient can be extracted and keep to this new extraction method, can shorten the production cycle, reduce cost, and the research prompting of multiple compound preparation, " SBE method " might substitute " WE method " (being water extraction method).And this extracting method also has wide application prospect in the granular research of the prepared slices of Chinese crude drugs." semi-bionic extraction " can embody the comprehensive function characteristics of tcm clinical practice medication, meets the principle that oral administration absorbs through the intestines and stomach transhipment.But this method still follows the high temperature decocting method at present, and long-time high temperature decocts can influence many effective active compositions, reduces drug effect.
(6) homogenate extraction method is compared with above several extracting methods, homogenate extract be a kind of application early but the extraction method that superiority is not fully realized by people.The homogenate extraction method is simple except equipment, the processing ease, outstanding advantage is to extract at normal temperatures, can keep little element, amino acid, trace element and heat-sensitive substance of giving birth in the extract preferably, be particularly useful for being rich in the extraction of the both for medicine and food Chinese medicine of starch.But the yield of extract is lower than other method, and existing extraction equipment is open basically, and solution usage is big, loses also big.
(7) this method of broken wall extraction method is by to vegetable material fully broken purpose that reaches extraction in appropriate solvent.Extractor mainly is made up of high-speed electric expreess locomotive, crushing cutter, container, base, principal post and speed-regulating switch etc.Motor speed divides fast, slow two grades, the broken extraction only needs 1-2min 1 time, extracts the back medicinal material and is fractured into pulpous state.By selecting the medicinal material of various character for use, carry out cold soaking extraction method, diacolation extraction method, reflux extraction and extract obtained recovery rate of broken wall extraction method and thin-layer chromatography contrast test respectively.The result shows that it is quick, complete that the broken wall extraction method is extracted, and need not heat, thereby can save a large amount of time, solvent and the energy.Though the broken wall extraction method is simple to operate, the yield of extract is not the highest, and is confined to experimental study yet, be applied to big production, also needs further research.
Comparing with the optimization of operating condition, extract the improvement of equipment and do still quite fewly, also only have a few devices that mechanical agitation and pneumatic agitating device are arranged at present, is an aspect being badly in need of reinforcement.Work on hand mainly is the simple modifications to special process, and significant limitation is arranged, and lacks theoretical direction.
Generally speaking, at present domestic above-mentioned The application of new technique research is lagged behind theoretical research, equipment research lags behind technical research.Except that the existing pilot-plant of supercritical fluid extraction, other Industrial Application of Technology is also under test, up to now, does not also have the single device of manufacturer production maturation, and Technology Equipment still is a blank.
Any new technology and new equipment all have advanced person and weak point, if but with they organic assembling, form technical equipment and even technical system, that will be a qualitative leap, to bring a revolution to the extraction of the high efficiency, low cost of China's Chinese medicine, wild plant and agricultural byproducts and the intensive processing of high added value, and the reinforcement technique of chemical separating and mass transfer will provide strong assurance for this reason.Still with the example that is extracted as of Chinese herbal medicine, realization traditional Chinese medicine subject intersects with Chemical Engineering, to help realizing the modernization of Chinese medicine production equipment, with the notion of Chemical Engineering, the separation process of theoretical introducing traditional Chinese medicine extraction, utilize available research achievements,, start with from the research of basic influence factor in conjunction with the concrete condition that Chinese medicine is produced, technological process, production equipment, operating condition are done modernization overlay and careful groping, provide feasible design.By applying the outfield, adopting mode such as novel extraction process to carry out leaching process strengthens, the research new technology is to the influence of different pharmaceutical and different component extraction thereof, on the basis of going deep into efficacy factor research, seek the optimum operation condition and the possible mechanism of action, and then the design of carrying out back yard industry equipment is a practical way.
Combination is not simple stack, must be to meet the very strong organic combination of the principles of science, operability.In above-mentioned 7 kinds of novel extraction technology, the supercritical fluid extraction high-tension apparatus, one-time investment is bigger, the operating cost height; Enzyme process will be set up a whole set of biochemical system, and involves great expense; Semi-bionic extraction does not have the precedent of success in the extraction of wild plant and agricultural byproducts functional component.Supercritical fluid, enzyme process and semi-bionic extraction adhere to physics, three different categories of biochemistry and medicineization separately, are difficult to integrate.By contrast, homogenate, broken wall, ultrasonic and microwave abstracting all belong to physics and extract, be extracted under the normal pressure and carry out, less demanding to equipment, safety relatively, the temperature of extraction are normal temperature normally, and maximum temperature can be above 60 ℃, biochemistry and chemical reaction generally do not take place in the leaching process, and the possibility of combination is arranged.
But at present there are many deficiencies at the homogenate of usefulness, broken wall, ultrasonic and microwave abstracting equipment, also immature on the technology, mainly be:
(1) the main equipment refiner of homogenate extraction is generally selected JMJ40-T type colloid mill for use, feed size<3mm, and discharging particle 75~100 μ m, production capacity is little, and is easy to wear, relatively poor to high fiber-like plant homogenate effect.The at present employing contacted 3~5 groups of identical colloid mill, agitator, head tanks of structure more, carries out counter-flow extraction, and except the yield of extract was not really high, solution usage was big, loses also big.
(2) stability, the continuity of the operation of the extractor of wall-breaking abstraction are relatively poor, feed size<3mm, discharging-material size 50~75 μ m.All adopting compartment to extract at present, is the solvent of 5~8 times of disposable adding materials, carries out Separation of Solid and Liquid after the extraction, and recovery rate is higher than the homogenate method and is lower than ultrasonic and microwave method, and the concentrated amount of solvent load and back operation is all bigger.To the material of some both for medicine and food, after extracting medicinal ingredient, remaining is main component when being made as food with starch and dietary fiber, coarse mouthfeel, and commodity rate is not high.
(3) Chinese patent 01223085 discloses a kind of intensified by ultrasonic wave traditional Chinese medicine extraction jar, and its formation is the extractor inwall at the carrying vapour chuck, by hanger, the fixing some board-like ultrasonic wave vibration plates towards tank body central authorities of suspension ring.The weak point of this board-like ultrasonic wave vibration plate periphery wall built-up structure, the one, the ultrasonic machinery of opposed wall built-up can all be utilized, and the interference of ripple easily takes place, and surpasses into the loss of ultrasonic mechanical energy, thereby the ultrasonic energy effective rate of utilization is low.Extraction time is still long, generally needs 20~40min.The 2nd, board-like wall built-up body structure surface abnormity, perforate of tank body perisporium or pad and suspension member are more, clean complexity, and difficulty reaches the GMP requirement.Chinese patent 02213449 discloses another kind of ultrasonic wave traditional Chinese medicine extraction jar, is several ultrasonic vibrators are sealed in the same transducing box, this transducing box is placed top in the extractor again, by setting up agitator, improves the ultrasonic effect of the herbal medicine of jar middle and lower part.This structure is the same with above-mentioned patent, still can cause the loss of ultrasonic energy, make the ultrasonic energy effective rate of utilization reduce, and the ultrasonic vibrator of this structure is changed difficulty.Above-mentioned two kinds of ultrasonic wave extractors all adopt compartment to extract, and are the solvents of 5~8 times of disposable adding materials, carry out Separation of Solid and Liquid after the extraction, and the concentrated amount of solvent load and back operation is all bigger.
(4) up to now, it is fewer both at home and abroad microwave technology to be used for the research report of plant extract this respect, does not also have the suitability for industrialized production equipment of microwave plant extract.Existing testing equipment structure is equivalent to a household microwave oven that has amplified, and extractor is placed in the microwave irradiation chamber, microwave by around to middle irradiation, the tank deck of extractor has respiratory siphon to communicate with atmosphere.Extracting method is disposable a certain amount of plant meal and the solvent of adding in extractor, soaks into about 20min earlier, extracts by the fuel factor of microwave irradiation again.There are 7 deficiencies in this extraction element and method: the thickness that has 1. surpassed microwave frequency effective irradiation 50mm because of the radius of extractor, the less effective irradiation of accepting microwave of the material of core, integral energy is irregular, reduced extraction efficiency, though bigger extractor has been installed agitating device, effect is still undesirable.2. control measures deficiency.Under the set situation of extraction equipment, extract, extractant, can only be on the technology according to the physicochemical property of extract, by extraction time, the regulation and control of extracting these 2 parameters of temperature being improved the efficient of Microwave Extraction.And it is also wayward to extract temperature, extracts usually because of overtemperature interrupts, and to carry out again after the equitemperature reduction again, and extraction time generally needs 20~40min; When 3. using low boiling point solvent to extract, can make the solvent boiling that heats up rapidly, cause the extractor internal pressure to rise sharply and cause and burn and explosion accident, can not give full play to the superiority of Microwave Extraction because of the fuel factor of microwave irradiation.4. extractor must be made of the good material of microwave penetrations such as polyene PVF or quartz glass, has increased cost and manufacture difficulty; 5. can only extract with microwave method, can not with common extracting method dual-purpose; The soup content of 6. discharging in the dregs of a decoction is higher, needs by other measure the dregs of a decoction to be squeezed, and when using solvent extraction, need join a cover desolventizing equipment in addition, has increased the operation of the work of extracting; 7. solvent load is still bigger, is generally 5~8 times of extract.
This shows, if only existing homogenate, broken wall, ultrasonic and microwave abstracting equipment are combined, still can not reach safety, efficient, low consumption, be applicable to the original intention of suitability for industrialized production.
Summary of the invention is in order to overcome the above-mentioned deficiency of existing plant extract equipment and method, the present invention is to several equipment improvement or upgrade the back organic assembling, a kind of extract yield height is provided, the time is short, energy consumption is low, solvent load is few, controllability is strong, operating flexibility is big, the Multifunction combined type plant extract technical equipment of applied range, and the supporting process that its superiority is given full play to.
The technical solution adopted for the present invention to solve the technical problems is, by to the improvement of existing homogenate, broken wall, ultrasonic wave, microwave and traditional extraction device or optional can better equipment, form 5 extraction cells, then with the design of having complementary advantages, making overall plans, its organic combination is become to have the technical equipment of original effect, and created that micro mist is broken with growing with each passing hour, three kinds of new process for extracting such as batch (-type) adverse current and the anhydrous extraction of bright product.
Concrete scheme is:
1, in the configuration of equipment, adopts the design of having complementary advantages, making overall plans.
Whole extraction element is made up of homogenate, broken wall, ultrasonic, microwave, 5 unit of extraction, center and 9 auxiliary equipment; The capital equipment of 1. homogenate extraction cells is material moistening device and refiner.The material moistening device is the cylindrical device that the anchor gate stirrer is housed, and refiner replaces the generally colloid mill of use with the online high shear homogeneous dispersion of QDL machine.Feed size<the 3mm of this homogenizer, discharging particle 50~100 μ m, operating pressure 0.5Mpa; 2. the wall-breaking abstraction unit replaces the broken extractor of being made up of high-speed electric expreess locomotive, crushing cutter etc. with a SRH type high pressure homogenizer.This high pressure homogenizer structure tube list operates steadily, and maximum working pressure reaches 70Mpa, average working pressure 56Mpa, and when feed size<100 μ m, discharging particle grain size<5 μ m, average 2~3 μ m; 3. the capital equipment of ultrasonic extraction unit is the ultrasonic extraction device, is made up of tubular type extractor and electrical control cubicles.Extractor is a upright pipeline, inwardly respectively adorns one group of bar type ultrasonic vibrator that power is powerful from the top and the bottom centre of pipeline, and structure is very simple; 4. the microwave abstracting unit essential equipment (UEE) is a microwave extracter, is made up of waveguide tubular type extractor and microwave source, fuses.Extractor adopts the design of box multimode cavity (be called for short irradiation chamber), and interior installation tubular type processor to the distributed energy regenerative of cavity, can obtain extraordinary heating uniformity with the 2450MHz magnetron of several rated power.The irradiation chamber has import and export, the thermometric port of chokes shielding and has the chamber door of good chokes, the replacing of convenient dissimilar extractors, and microwave leakage is up to state standards fully.Microwave source adopts the compound magnetic system of ancillary coil of permanent magnetism and the design of water-cooling structure, adds good safety interlocking protective device, makes this microwave source have good stability, and is easy to adjust, multiple functional, safe and reliable.5. the center extractor is the still formula equipment of jacket type, and backflow, cooling and solvent recovery unit are equipped with in top, and the outlet at bottom of extractor is a quick operating valve of being furnished with the ultra-fine filter plate of stainless steel.Large and small double-deck anchor gate stirrer is housed in the device, the paddle that the upper strata is big is close to extractor cylindrical shell and bottom bulkhead inwall, paddle that lower floor is little and outlet inwall are close to, rivet with polyene PVF engineering plastics plate and paddle the bottom of little paddle, and sheet moulds the material bottom and scrapes mutually with the filter plate flexibility of outlet.6. other auxiliary equipment: is made up of filtering type lower discharging centrifuge, water-ring vacuum pump, shell and tube water cooler, high-order slurry bucket and 5 head tanks, high-order slurry barrel and head tank are cylindrical device.7. main operating process realizes automatic control, and steam condensate (SC) and cooling water are reusable.
The technological process of this Multifunction combined type plant extract technical equipment is: will put into the material moistening jar through the plant meal after cleaning (cleaning), impurity elimination, the pulverizing, after adding the time about solvent material moistening 30min, extract in advance with homogenate earlier, then around the center extractor, by the extraction of broken wall, ultrasonic and microwave abstracting unit, carry substantially to the greatest extent for this reason until solute.Residue precipitation after the extraction is discharged, and extract then further separates processing.In case of necessity, the extract after concentrating can be carried out reextraction with microwave, so that agricultural chemicals, chemical fertilizer and heavy-metal residual are up to standard,
Below briefly introduce purpose, function and the technical characterictic of this Multifunction combined type plant extract technical equipment configuration:
(1) one of purpose that disposes like this in the homogenate extraction cells is, through after wetting, automatically sucked by the import of the mixed material of solute, solvent composition from online high shear homogeneous dispersion machine, through strong shearing, grinding, bump and cavitation, make material reach the even matter effect of dispersion, refinement.It is characterized in that making solute and solvent to obtain the mass transfer space of large surface area, improved extraction efficiency; Two of purpose is, because the output services pressure of homogeneous dispersion machine is up to 0.5Mpa, so replace screw pump commonly used to become unique conveying equipment for fluid substances of whole extraction system with it.Material carries out homogenate extraction continuous high-efficient ground by circulating between homogeneous dispersion machine and material moistening device; It is characterized in that cycling extraction between small number of devices replaces the counter-current extraction of many complete equipments, saved power, improved efficient.
(2) in one of purpose of this configuration in wall-breaking abstraction unit be, micron Chinese medicine technology of Chu Xianing and method are affirmed by Chinese medicine circle and are paid attention in recent years, micron Chinese medicine is meant that adopting modern high technology to combine with traditional processing technique and preparation technique develops, and the granularity that can keep the intrinsic pharmacodynamics material base of traditional Chinese medicine is micron-sized new medicine.Micron Chinese medicine comprises micron Chinese medicine material, Chinese medicine micron extract and micron Chinese medicine preparation.It is generally acknowledged that its particle grain size should be in 1~75 mu m range, most of micron Chinese medicine average grain diameters≤15 μ m.SRH type high pressure homogenizer discharging particle grain size<5 μ m, average 2~3 μ m are just in the scope of micron Chinese medicine.It is characterized in that this configuration provides the condition that helps the effective ingredient stripping most and do not change extract effect characteristic, thereby improved the utilization rate of plant functional component; Two of purpose is, particle diameter 2~3 μ m of high pressure homogenizer discharging average grain, and it is broken that the dietary fiber in the both for medicine and food plant has been carried out micro mist, do not have rough mouthfeel.It is characterized in that this configuration makes thinks that originally the dietary fiber of invalid components is used effectively.(the soymilk factory original production process of domestic maximum is, earlier the soybean defibrination pulverized, and carries out screenings and separates, and bean dregs are as feed.Use this high pressure homogenizer, it is connected in fiberizer after, the skin of beancurd that originally separates from bean powder, bean dregs have become the part of soymilk powder, have improved commodity rate greatly.)
(3) one of purpose that disposes like this in the ultrasonic extraction unit is, single hose ultrasonic extraction utensil has dead angle simple in structure, no, the field of force that the ultrasonic vibrator of same model and same equifrequent, power, quantity applies material is far superior to pot type ultrasonic extraction device, the thickness of chamber wall and container placement location are required not harsh yet, and cleaning equipment and change ultrasonic vibrator easily.It is characterized in that reaching the highest efficient with the most succinct equipment; Two of purpose is, different with pot type ultrasonic extraction device is, material no longer applies the extraction that the field of force adds stirring action, makes displacement-type in extractor by the ultrasonic vibrator of board-like wall built-up or overhead transducing box structure, but be power with high shear homogeneous dispersion machine, between ultrasonic wave and center extractor, circulate extraction, because of the bar type ultrasonic vibrator is exceedingly fast to the field of force frequency that material applies, even under the flow velocity of tens meters of per seconds, extraction yield is still very high, and whole being extracted in 5~10min finished.It is characterized in that replacing fixed mobile extraction by the mobile extraction of outer circulation type.
(4) in the configuration of microwave abstracting unit, will extract and the microwave irradiation device separates, the waveguide tube extractor is installed in the microwave irradiation chamber, extract and then do not serve as fully by the center extractor.The center extractor is equipped with safety valve and bursting diaphragm, and compressed air hose is equipped with on top, and vacuum-pumping tube is equipped with in the bottom, forms a microwave circulation extraction system by center extractor, microwave irradiation chamber, high shear homogeneous dispersion machine and cooler.Doing one of purpose like this is, the radius of tube extractor generally is no more than 50mm, within optimum Microwave Extraction frequency effective irradiation 50mm thickness, thereby has improved extraction efficiency.It is characterized in that being improved to tubular type by the pot type extraction extracts; Two of purpose is, in the process of extracting, extract time of staying in tube extractor of frequency that temperature can be by microwave irradiation, intensity, material, the size of chiller water amount is more directly regulated and control, and extraction is carried out continuously, each leaching process only needs 30~120s.It is characterized in that circulating extraction by leaving standstill or move to extract to be improved between several equipment in same container, controllability is stronger; Three of purpose is because whole device carries out under air-tight state, when using low boiling point solvent to extract, can extraction normally be carried out by improving the boiling point that pressure improves this solvent.Various reliable because of regulate and control method, the situation that seldom has temperature, pressure to rise sharply can not lead to a disaster even take place yet.It is characterized in that to carry out carrying out under vacuum, normal pressure and the pressurized conditions safety operation; Four of purpose is, after extraction and the microwave irradiation device separates, accept being only limited to of microwave irradiation and be installed in tube extractor in the microwave irradiation chamber, still be made into good materials of microwave penetration such as polyene PVF or quartz glass, materials only are 1/5 of original structure, miscellaneous equipment is no longer carried and is subjected to microwave irradiation, makes of stainless steel, greatly reduces the difficulty and the cost of making.
(5) the center extraction cells like this one of purpose of configuration be, the extraction of broken wall, ultrasonic and three kinds of modes of microwave all with the center extractor as buffering, heating, equilibrium and intermediate storage equipment, it is characterized in that realizing distributing rationally of resource; Two of purpose is, the center extractor both can extract with usual ways such as infiltration, decoction, backflows, also can extract with the method a kind of or that several are connected in wherein a kind of and broken wall, ultrasonic and three kinds of modes of microwave.It is characterized in that can carrying out the extraction of method more than five kinds with same extractor, applicability is wider; Three of purpose is that because the special construction of agitator makes material not have the dead angle in the extractor of center, it is very even to be heated, and has solved the easily disadvantage of the easy coking of cohesion of traditional decoction method medicinal material fine powder, has also shortened the time of refluxing extraction.It is characterized in that becoming Dynamic Extraction, improved extraction efficiency by the static state extraction.Four of purpose is, when extracting with traditional approach, extract finish after, can tackle the dregs of a decoction on the ultra-fine filter plate of outlet at bottom stainless steel of center extractor, wherein moisture is extruded (or extract organic solvent), improved yield.The special construction that it is characterized in that agitator makes soup can not stop up filter plate in the process that extrudes (or extracting out); Five of purpose is, after discharging soup, feeds steam by the chuck to extractor, makes dregs of a decoction precipitation on the spot in the extractor of center under stirring state, need not to establish in addition desolventizing equipment.It is characterized in that extracting, precipitation finishes in same container, reduced the operation of the work of extracting.
(6) be that head tank simple in structure with 5, that cost is lower replaces the extractor group, realizes counter-flow extraction by method of the present invention between center extractor and head tank in one of purpose of this configuration of auxiliary equipment.It is characterized in that having realized once more distributing rationally of resource.Two of purpose is, the rotating speed of filtering type lower discharging centrifuge is up to 6000r/min, and separation factor surpasses 2000, and particle grain size is still had preferably with the liquid separating effect at 2~3 μ m and the bigger extract of viscosity.It is characterized in that dissolving meticulous pulverizing and separated difficult contradiction; Three of purpose is to extract temperature by the size of adjusting shell and tube water cooler water consumption and how many controls easily of steam consumption of center extractor steam jacket.It is characterized in that strengthening the controllability of extracting operation.
In sum, the most original technical characterictic of Multifunction combined type plant extract technical equipment is: the one, maximize favourable factors and minimize unfavourable ones to greatest extent.Below chat, homogenate, broken wall, common advantage ultrasonic, microwave abstracting be extraction time short, energy consumption is low, can keep the functional component of extract preferably, but deficiency is arranged respectively.The deficiency of homogenate and wall-breaking abstraction is that the yield of extract is not the highest, and ultrasonic very high with yield microwave abstracting; Though the efficient of ultrasonic extraction is high, the agricultural chemicals in the extract, chemical fertilizer and heavy-metal residual still do not reach the current standard of developed country, and behind microwave abstracting, even the residues of pesticides of trace can also reduce more than 85% again.But the selectivity of microwave abstracting is very strong, is " opening different locks with different keys ", tends to heating in the process of microwave abstracting.Their organic assembling are got up, allow homogenate and wall-breaking abstraction extract earlier functional component more than 60%, ultrasonic extraction is extracted more than 30% again, and rest parts is gone to finish by microwave abstracting.This really is that each doing his best, has complementary advantages, and Zhu Lianbi closes.The 2nd, existing pot type is ultrasonic and microwave extracter has only ultrasonic or microwave frequency intensity, extractant, extraction time, 4 control devices of extraction temperature, with the homogeneous dispersion machine is that the outer circulation type extractor of power has increased extraction process state, mass flow, extracting pressure and 4 control devices of extraction environment.Like this, technological parameter that the overwhelming majority has a direct impact extraction and parameter are all in and have in one's pocket, and make extraction more safe and efficient.
2, on process, grow with each passing hour, carry out three innovations.
Along with the enhancing day by day of health of people and health care consciousness, the curative effect of Chinese medicine and the effect of health food are proposed higher requirement, the new market demand has appearred.Wherein representational is that micron Chinese medicine, dietary fiber and bright product extract.People go back idea price and do not want growth thereupon, and this just requires to fall as far as possible few solvent load technically, with treating capacity, the reduction extraction cost that reduces extract.To this, solution of the present utility model is:
(1) common element of having created broken extraction micron Chinese medicine of micro mist and dietary fiber is the fineness of extract will be reduced to below the 15 μ m.Such Chinese medicine can effectively be absorbed by human body, can not change original pharmacodynamic profiles again, and dietary fiber does not have rough mouthfeel yet.This point, traditional extracting mode is difficult to accomplish.Also the degree of grinding with Chinese medicine is an example, traditional extracting mode thinks that the degree of grinding of raw material can not be meticulous, generally is no more than 40 orders (635 μ m), and reason is: though 1. meticulous powder can improve its leaching effect when leaching, but suction-operated also increases, thereby diffusion velocity is affected; 2. if pulverize meticulously, a large amount of cell ruptures in the medicinal material tissue cause a large amount of insoluble matters in the cell and more resin, mucilaginous substance etc. to sneak into or leach, make to leach impurity and increase, and the viscosity increase, diffusion is slow, leaching liquor filtration difficulty, product muddiness; 3. meticulous powder brings difficulty to operation, and when leaching with percolation, because the space between them is too little, the solvent flow resistance increases, and causes obstruction easily, makes diacolation incomplete or lixiviate is difficult.But from materia medica, the dissolution rate of medicine amasss into positive correlation with the specific grain surface of medicine, and specific area and particle diameter are inversely proportional to.Therefore, the particle diameter of medicine is thin more, and then its specific area is big more, helps the stripping of effective ingredient more.If but the particle diameter of medicine<100 nanometers just changed original pharmacodynamic profiles, produce some known and toxic and side effects the unknown, the particle diameter of micron Chinese medicine<15 μ m and not change original pharmacodynamic profiles be exactly ultimate challenge to traditional extracting mode.
How to solve the contradiction of extraction rate and smashing fineness? the inventor thinks, traditional extracting mode to the field of force that is extracted material and applies too a little less than, extract slowly, inefficiency, separation equipment function restriction in addition has to adopt suitable degree of grinding, higher temperature, bigger concentration difference and long time, adopt methods such as hot reflux, solid-liquid counter-current, time expand, continuous replacement solvent, quicken diffusion to improve extraction rate.
The technical scheme that the present invention takes is that elder generation shears material, be milled to 2~3 μ m with homogeneous dispersion machine and high pressure homogenizer, by ultrasonic wave, microwave extract is applied the strong field of force then, reaches the purpose of the broken extraction of micro mist.Its mechanism is: the extraction of plant functional component belongs to solid---liquid extraction category.General extraction process comprises following three steps: 1. solvent soaks into and enters in the solid, the solute dissolving; 2. Rong Xie solute is diffused into the surface of solids from the solid interior fluid; 3. solute continues to arrive by the liquid film diffusion from the surface of solids main body of external solvent.Under common condition, 1., 3. two steps are not the governing factors of mass transfer, 2. the speed of extraction do not depend mainly on step, i.e. extraction is actually the mass transfer operation of diffusion inside.Therefore, the speed of extraction depends primarily on extracting process and choice of Solvent.After solvent was determined, extracting process played decisive influence.In addition, factor such as poor, extraction time of the degree of grinding of raw material, extraction temperature, solvent strength, extraction times also influences extraction rate to some extent.No matter how technology and equipment is innovated, these basic principles can not be run counter to, but design and control the above-mentioned factor that influences extraction rate accurately, go after profits and advoid disadvantages, and be possible fully.Though homogenate, broken wall, ultrasonic, microwave abstracting mode are still followed solid---the basic principle of liquid extraction, extraction process has played essential variation, and wherein the most significant variation is to be much higher than traditional extracting mode to being extracted the field of force that material applies.This field of force is under the effect by the multiple physical force that high shear homogeneous dispersion machine, high pressure homogenizer are sheared consumingly, ground, bump and ultrasonic wave, microwave apply strong outfield, huge surface area and very strong selectivity make the stripping in the extremely short or very short time of target solute, in cell a large amount of insoluble matters and more resin, when mucilaginous substance has little time to leach, finished leaching process.After homogeneous dispersion machine and high pressure homogenizer pulverizing, though fineness does not influence extraction rate less than 5 μ m.The broken process for extracting of this micro mist is characterised in that its mass transfer and diffusion velocity are exceedingly fast, do not influence the solute that has dissolved and from the solid interior fluid, be diffused into the surface of solids, also continue to spread the speed that arrives the external solvent main body by liquid film from the surface of solids because of degree of grinding is meticulous, thereby the efficient extra-high-speed.
With the microwave abstracting is example, thereby microwave-assisted extraction technique is to utilize microwave irradiation to come little molecular polarity material is produced the novel technique that the new diffusion admittance of diffusion, change diffusion mechanism or unblank is quickened in useful effect.Microwave action has aggravated molecular activity behind extract, improved the average energy of molecule, has reduced to extract required activation energy, has increased the collision frequency of molecule greatly, thereby has improved the speed of extraction.In the extraction process to plant, microwave is by arriving the inside of extract, because the vascular bundle and the glandular cell system water content height of material so absorb the very fast intensification of microwave energy, increase the pressure of cell interior to the solvent of microwave.When internal pressure surpassed the ability that cell membrane can bear, cell wall rupture freely flowed out so be positioned at intracellular active ingredient, entered solvent and dissolved.Because microwave abstracting can carry out the selectivity heating to one or more components in the system, so target components is directly separated from matrix, and environment on every side is unaffected.Therefore, after solvent and extracting process are determined, influence in the five elements of extraction rate, microwave abstracting is compared with traditional extraction process, and except the common ground that should keep solvent strength difference greatly, other four will have bigger difference.The granularity of raw material can be very thin, and extraction temperature can be a normal temperature, and the time can be very short, and number of times can be seldom, to the speed did not influence of extraction.
(2) having created batch (-type) counter-flow extraction specific practice is, earlier carry out preextraction with the homogenate extraction cells, use broken wall again, ultrasonic, three extraction cells of microwave are extracted around center extractor degree of passing: after 1. extract being cleaned, be crushed to about 40 orders, measure in the material moistening device of packing in accordance with regulations then, add the solvent of the homogenate extract of last consignment of extract again as this batch homogenate extraction, stir earlier and soak into about 20min, mixed material enters high shear homogeneous dispersion machine simultaneously, after the homogenate extraction through 20~30min between material moistening device and the homogeneous dispersion machine, carry out Separation of Solid and Liquid by the filtering type lower discharging centrifuge, this extract is sent into centrifugal station for further processing as final extract, and powder is then got back to the center extractor; 2. add the solvent of the broken wall extract of last consignment of as the wall-breaking abstraction of this batch extraction, behind the wall-breaking abstraction through 10~15min between high pressure homogenizer and the center extractor, carry out Separation of Solid and Liquid, this extract is as the solvent of the extract homogenate extraction of next group, and powder is still got back to the center extractor; 3. use the solvent of the ultrasonic wave extract of last consignment of as this batch ultrasonic extraction, behind the ultrasonic extraction through 5~10min, this extract is as the solvent of next group extract wall-breaking abstraction, and powder returns the center extractor; 4. after carrying out the microwave abstracting of 30~120s with fresh solvent at last, carry out Separation of Solid and Liquid, this extract is as the solution of the ultrasonic extraction of next group extract, and powder returns the center extractor the 4th time, discharges residue behind the precipitation on the spot.5. in leaching process, time of staying in tube extractor of the frequency of steam consumption that can be by center extractor chuck and ultrasonic wave, microwave, intensity, material, the size of chiller water amount are more directly regulated and control, and extraction is carried out continuously.Doing purpose like this is, by the improvement of this method, available 5 head tanks simple in structure, that cost is lower replace the extractor group, realize counter-flow extraction by method of the present invention between center extractor and head tank.Distinguishedly be, the present invention changes the method for common counter-flow extraction " material that surges is motionless ", liquid, material after extracting are shifted out the center extractor and carry out Separation of Solid and Liquid outward at every turn simultaneously, moisture content in the extract next time, the target extractive content that has just been leached by solvent are reduced significantly than common mode, this also means needs the content of the target extract that leaches to reduce significantly than common mode next time, thereby reduced the consumption of solvent, also reduce the treating capacity and the reduction of extract and extracted cost.It is characterized in that changing Continuous Countercurrent Extraction is the batch (-type) counter-flow extraction, has reduced solvent load effectively.
(3) health food of having created the anhydrous extraction of bright product China's exploitation and having produced, enter the second generation and emphasize science and authenticity by first generation nourishing reinforced food, require to confirm that through human body and animal experiment this product has certain neurological progression food phases, and will enter the third generation and not only need to have certain physiological function through human body and animal experiment proof product, and need investigate thoroughly to have this health care function factor, promptly just obtain the stage of remarkable efficacy with the function factor of trace.Third generation health food will be the emphasis of 21 century development.Therefore, research separates and keeps its technology active and stability, comprise and how to remove some harmful, noxious materials in these raw materials, make the quality of health food be tending towards natural, safe, effective, make the technological element of a product height of producing, steady quality, it is most important to the degree of belief of health food to increase people.The extraction major part of traditional approach is an object with the plant dry product, plant in nature or artificial drying process, more and more be subjected in recent years people pay attention to, to cancer and cardiovascular and cerebrovascular disease have the effect materials such as saponin, flavones, phospholipid and unrighted acid of significant curative effect, often lost more than half.Therefore, be that to extract object the same with micron Chinese medicine with the aquatic foods product of plant, obtain increasing expert, scholar, knowledgeable people certainly and pay attention to.This brings new problem to extraction again, wherein importantly under the situation of water content 60~70% even 80%, how to keep higher recovery rate?
The present invention has created bright product does not have water extraction process, reasonable this difficult problem that solved.As everyone knows, contain a large amount of moisture in the cell of fresh plant, under self catharsis of planting trees, do not polluted basically.Most of medicinal plant and most wild plant, agricultural byproducts all use food-grade alcohol as solvent, and the alcohol in 50~95 degree scopes is best to the functional component solubility property in the plant.The tradition extraction method generally is to use the dry product of plant to extract, and concentration 95 degree food-grade alcohol is added the deionized water dilution reach above-mentioned concentration.The present invention utilizes the feature of alcohol strong water absorbent, reaches the purpose of dilution by the moisture in the bright product of absorption plant.Specific practice is that the bright product of plant after directly spending the food-grade alcohol and pulverize with 95 mix, and carry out homogenate, broken wall, ultrasonic and Microwave Extraction respectively.At the beginning, alcohol absorbs the moisture in the plant in a large number, and concentration is diluted to about 55 degree.Along with the increase of extraction time, the moisture in the plant is fewer and feweri, and the concentration of alcohol is more and more higher.When next group extracts, the solvent that extracts at first as this batch with the extract of the least concentration in the last consignment of extract, the solvent that the extract of low concentration extracts for the second time as this batch, by that analogy, the fresh alcohol with 95 degree is that solvent is done last the extraction again.Thisly toward high degree of passing extracting method spirit solvent is remained in 50~95 optimum concentration ranges of spending, in the process of counter-flow extraction, realized anhydrous extraction by low.Except material plant needed the water cleaning, leaching process need not water in whole process of production.One of purpose of doing like this is, because whole leaching process all is to carry out at normal temperatures, thereby has kept the effect nutritional labeling that is extracted plant to greatest extent.It is characterized in that at normal temperatures having reached and extract day with solvent commonly used; Two of purpose is that extraction is by progressively improving the method for alcohol concentration, to degree of the passing extraction effectively of each target extract in the plant.It is characterized in that same solvent realization system by variable concentrations extracts, comprehensive utilization; Three of purpose is that by enforcement of the present invention, the agricultural chemicals in the extract, chemical fertilizer and heavy-metal residual are lower than required standard.It is characterized in that going after profits and advoiding disadvantages by the science innovation.
The solvent of indication of the present invention comprises organic solvent, inorganic solvent and water.
As described above, thisly get the rate height, the time is short, energy consumption is low, solvent load is few, controllability is strong, operating flexibility is big, the Multifunction combined type plant extract technical equipment and the supporting with it process of applied range are the plant extract apparatus and method of not reporting fully in the past.
The invention has the beneficial effects as follows, under purity, the yield of extract are won the prerequisite of similar extraction equipment, extraction time shortens 1/2~2/3, solvent load reduces by 50~70%, energy resource consumption reduces 40~60%, and agricultural chemicals, chemical fertilizer and the heavy-metal residual in the extract is lower than the standing order of developed country.
The present invention is further described below in conjunction with drawings and Examples for description of drawings.
Fig. 1 is a technical equipment process chart of the present invention.
Fig. 2 is a ultrasonic extraction device of the present invention vertical section structural map.
Fig. 3 is a microwave extracter of the present invention vertical section structural map.
Fig. 4 is extractor vertical section, a center of the present invention structural map.
Fig. 5 is the extraction process route map of first embodiment of the invention.
1. homogenate extract head tanks, 2. wall-breaking abstraction liquid head tank, 3. ultrasonic extraction liquid head tank among Fig. 1,4. microwave abstracting liquid head tank, 5. fresh solvent head tank, 6. microwave extracter, 7. ultrasonic extraction device, 8. shell and tube cooler, 9. high pressure homogenizer, 10. high shear homogeneous dispersion machine, 11. center extractors, 12. high-order slurry buckets, 13. filtering type lower discharging centrifuge, 14. reflux condenser, 15. receive flow container, 16. material moistening devices, 17. gas-liquid separator, 18. filter, 19. water-ring vacuum pumps, 20. Pressure gauges, 21. point for measuring temperature, 22. spinner flowmeter, 23. look handleless cup, 24. safety valves.
1. control power cabinets among Fig. 2,2. ultrasonic extraction device, 3. bar type ultrasonic vibrator, 4. extractor top cover, 5. extractor bottom, 6. mixed material inlet, 7. mixed material inlet, 8. cable, 9. support.
1. control power cabinets among Fig. 3,2. microwave source, 3. microwave radial chamber (band chamber door), 4. microwave abstracting pipe, 5. micro-wave screening sleeve pipe, 6. the microwave abstracting pipe is imported and exported flange, 7. mixed material inlet, 8. mixed material outlet, 9. observing and controlling temperature system.
1. motor among Fig. 4,2. reductor, 3. an envelope, 4. frame, 5. material is managed, 6. hand hole, 7. flange, 8. bearing, 9. cylindrical shell, 10. chuck, 11. or the steam inlet, 12. double-deck anchor gate stirrer, 13. the circulation discharging opening, 14. dregs of a decoction outlet quick operating valves, 15. steam condensate (SC) outlets, 16. soup outlet, 17. the shaft support, the ultra-fine filter plate of 18. stainless steels, 19. polyene PVF engineering plastics plates, 20. rivet (double-deck anchor gate stirrer is linked to each other with polyene PVF engineering plastics plate), 21. filter plate screw holes.
List embodiment below the specific embodiment, the present invention will be described in further detail, and the present invention has more than and is limited to these examples.
Embodiment: the system to the radix cynanchi bungei functional component extracts with the utility model, referring to accompanying drawing 1,5.
Radix cynanchi bungei is a kind of Chinese medicine that " Chinese medicinal herbal " (second, the People's Press, 328 pages, 1979) once put down in writing.Its main effect and nutritional labeling are: 1. contain the steroidal ester glucoside of protection human immunity regulatory function, enhancing immunization of cell, wherein C 21The tool activity of steroid glucoside; 2. be rich in phospholipid, wherein higher with lecithin, lipositol and cephalin content; 3. rich nutrient contents is arranged, comprise crude fat, protein, polysaccharide, starch and nine kinds of different vitamins, wherein higher with B family vitamin content; The amino acid that 4. needed by human is arranged, the amino acid content of content and American Ginseng is close, and especially arginine content is the highest, reaches 2.23%; Inorganic salts and trace element that 5. needed by human is arranged, wherein higher with potassium, phosphorus, magnesium, copper equal size; 6. contain prevention the elderly atherosclerotic effect unrighted acid, wherein the highest with linoleic acid content.Confirm that after further research the main pharmacological of radix cynanchi bungei shows as immunological regulation, anti-curing oncoma, promotes effects such as hair growth, protection heart and liver.For hundreds of years, unique product that radix cynanchi bungei is used as food is exactly a radix polygoni multiflori powder, and its production method follows ancient WATER-WASHING METHOD always, causes the very big waste of precious resources in the radix cynanchi bungei.
Designer of the present utility model served as that topic has been declared national patent (number of patent application 03259658.8) with " a kind of processing method that radix cynanchi bungei is fully utilized " once, replace the washing processing method with the homogenate processing method, the productive rate of bright radix cynanchi bungei goods rises to 30% by 16% of WATER-WASHING METHOD.But still there is extraction efficiency is not very high, 3 deficiencies that the agricultural chemicals in the extract, heavy-metal residual severe overweight and dietary fiber are given it up because of coarse mouthfeel.After adopting technical equipment of the present utility model and process, these three problems are all solved satisfactorily.
The concrete operations step is as follows:
When using the present technique equipment first, 1. in fresh solvent head tank (5), add quantitative fresh solvent, measure the bright radix cynanchi bungei that in material moistening device (16), adds after cleaning and crush in accordance with regulations, again fresh solvent is put into the material moistening device, after soaking into stirring 5min, start high shear homogeneous dispersion machine (10), return the material moistening device behind the mixed material process homogeneous dispersion crusher machine pulping, and after the circular flow dynamic formula homogenate preextraction through 10~20min between material moistening device and the homogeneous dispersion machine, with the homogeneous dispersion machine slurry is all squeezed into high-order slurry bucket (12), put into filtering type lower discharging centrifuge (13) again and carry out Separation of Solid and Liquid, extract after the separation is put into homogenate extract head tank (1), and powder is then put into center extractor (11).Before each extraction finishes, in time add quantitative fresh solvent, for extract use next time to the fresh solvent head tank; 2. the quantitative fresh solvent in the fresh solvent head tank is put into the center extractor, mix stirring 5min with powder after, start homogeneous dispersion machine, high pressure homogenizer (9), after the circular flow dynamic formula broken wall extraction through 10~15min between high pressure homogenizer and the center extractor, slurry is squeezed into high-order slurry bucket, put into lower discharging centrifuge and carry out Separation of Solid and Liquid, the extract after the separation is put into broken wall extract head tank (2), and powder is put back to the center extractor; 3. the quantitative fresh solvent in the fresh solvent head tank is put into the center extractor, mix stirring 5min with powder after, start the homogeneous dispersion machine, after the ultrasonic extraction of circular flow dynamic formula through 5~10min between ultrasonic extraction device (7) and the center extractor, slurry is squeezed into high-order slurry bucket, put into lower discharging centrifuge and carry out Separation of Solid and Liquid, ultrasonic wave extract after the separation is put into ultrasonic extraction liquid head tank (3), and powder is still put back to extractor; 4. the quantitative fresh solvent in the fresh solvent head tank is put into the center extractor, mix stirring 5min with powder after, start the homogeneous dispersion machine, after the ripple that declines through circulating of 30~120s between microwave extracter (6) and the center extractor extracts, slurry is squeezed into high-order slurry bucket, put into lower discharging centrifuge and carry out Separation of Solid and Liquid, Microwave Extraction liquid after the separation is put into microwave abstracting liquid head tank (4), and powder is still put back to the center extractor; 5. extract through 4 times, water-soluble, the liposoluble substance in the radix cynanchi bungei carried to the greatest extent already, can be from the color and luster judgement that handleless cup (23) is observed extract of looking in lower discharging centrifuge exit.Chuck to the center extractor feeds steam then, start water-ring vacuum pump (19), under stirring state, make powder negative pressure precipitation on the spot in device, by reflux condenser (14), receive flow containers (15) and reclaim solvent, open the quick operating valve of extractor bottom, center then and discharge powder.The powder of this moment through high shear homogeneous dispersion machine repeatedly repeatedly shearing-crushing and high pressure homogenizer cross fine lapping, the granularity of dietary fiber wherein<5 μ m does not have harsh feeling fully, can directly eat.
When reusing this device, 1. measure the bright radix cynanchi bungei that in material moistening device (16), adds after cleaning and crush in accordance with regulations, last consignment of homogenate extract in the homogenate extract head tank (1) is put into the material moistening device, after soaking into stirring 5min, start high shear homogeneous dispersion machine (10), behind the mixed material process homogeneous dispersion crusher machine pulping, return the material moistening device, and after the circular flow dynamic formula homogenate preextraction through 10~20min between homogeneous dispersion machine and the material moistening device, with the homogeneous dispersion machine slurry is all squeezed into high-order slurry bucket (12), put into filtering type lower discharging centrifuge (13) again and carry out Separation of Solid and Liquid, homogenate extract after the separation is put into homogenate extract head tank (1), send into centrifugal station as final extract and concentrate, powder is then put into center extractor (11); 2. the last consignment of broken wall extract in the wall-breaking abstraction liquid head tank (2) is put into the center extractor, mix stirring 5min with powder after, start homogeneous dispersion machine, high pressure homogenizer (9), after the circular flow dynamic formula broken wall extraction through 10~15min between high pressure homogenizer and the center extractor, slurry is squeezed into high-order slurry bucket, put into lower discharging centrifuge and carry out Separation of Solid and Liquid, extract after the separation is put into wall-breaking abstraction liquid head tank (2), as the solvent of next group homogenate extraction, powder is put back to the center extractor; 3. the last consignment of ultrasonic extraction liquid in the ultrasonic extraction liquid head tank (3) is put into the center extractor, mix stirring 5min with powder after, start the homogeneous dispersion machine, after the ultrasonic extraction of circular flow dynamic formula through 5~10min between ultrasonic extraction device (7) and the center extractor, slurry is squeezed into high-order slurry bucket, put into lower discharging centrifuge and carry out Separation of Solid and Liquid, ultrasonic wave extract after the separation is put into ultrasonic extraction liquid head tank (3), as the solvent of next group wall-breaking abstraction, powder is still put back to extractor; 4. the last consignment of microwave abstracting liquid in the microwave abstracting liquid head tank (4) is put into the center extractor, mix stirring 5min with powder after, start the homogeneous dispersion machine, after the ripple that declines through circulating of 30~120s between microwave extracter (6) and the center extractor extracts, slurry is squeezed into high-order slurry bucket, put into lower discharging centrifuge and carry out Separation of Solid and Liquid, Microwave Extraction liquid after the separation is put into microwave liquid head tank (4), as the solvent of next group ultrasonic extraction, powder is still put back to the center extractor; 5. the quantitative fresh solvent in the fresh solvent head tank is put into the center extractor, mix stirring 5min with powder after, start the homogeneous dispersion machine, after the ripple that declines through circulating of 30~60s once more between microwave extracter (6) and the center extractor extracts, slurry is squeezed into high-order slurry bucket, put into lower discharging centrifuge and carry out Separation of Solid and Liquid, Microwave Extraction liquid after the separation is put into microwave liquid head tank (4), and as the solvent of next group microwave abstracting, powder is still put back to the center extractor; 6. extract through 5 times, water-soluble, the liposoluble substance in the radix cynanchi bungei carried to the greatest extent already, can be from the color and luster judgement that handleless cup (23) is observed extract of looking in lower discharging centrifuge exit.Chuck to the center extractor feeds steam then, start water-ring vacuum pump (19), under stirring state, make powder negative pressure precipitation on the spot in device, by reflux condenser (14), receive flow containers (15) and reclaim solvent, open the quick operating valve of extractor bottom, center then and discharge powder.The powder of this moment through high shear homogeneous dispersion machine repeatedly broken repeatedly and high pressure homogenizer cross fine lapping, do not had harsh feeling, can directly eat; 7. after final extract concentrates, up to standard fully through microwave abstracting and precipitation once more, its agricultural chemicals, heavy-metal residual, for further being processed as medicine, cosmetics and food additives,
Digital proof in table 1~6 effect of the present invention.
The radix cynanchi bungei goods that table 1 different processing methods obtains contain scale (%)
The key technical indexes The bright product content of radix cynanchi bungei Processing method
WATER-WASHING METHOD The homogenate method Processing method of the present invention
Thick general glycoside (pharmaceutical raw material) 1.07 Trace 0.97 1.02
Raw phospholipid (medicine, cosmetics, food additives raw material) 0.28 Trace 0.21 0.24
Polysaccharide (food additives) 4.97 Trace 4.05 4.53
Starch, crude protein; Crude fat etc. 26.34 15.31 20.66 22.37
Dietary fiber 5.67 Do not detect 4.13 4.94
Add up to 38.33 16.00 30.02 33.10
Annotate:, after the data actual measurement, all press the bright product conversion of radix cynanchi bungei in the table for ease of contrast.
The general nutrient composition content (% butt) of the radix polygoni multiflori powder of table 2 distinct methods processing
Moisture Crude protein Crude fat Crude fibre Ash content Starch
Natural dry product ????10.28 ????9.38 ????1.46 ????5.01 ????2.16 ????62.4
The washing processing method ????9.65 ????0.503 ????0.187 Do not measure ????0.595 ????92.1
The homogenate processing method ????9.39 ????9.07 ????1.25 ????5.47 ????2.44 ????56.9
Processing method of the present invention ????8.12 ????9.35 ????0.37 ????6.42 ????0.27 ????71.9
The content (μ g/g) of several human essential elementses in the radix polygoni multiflori powder of table 3 distinct methods processing
Potassium Calcium Magnesium Iron Copper Zinc Manganese Phosphorus
Natural dry product ?11057.6 ????52.3 ??1119 ??20 ????7.1 ????13.7 ????5.2 ????2146
The washing processing method ?202 ????42.6 ??126 ??12 ????2.39 ????5.24 ????1.65 ????179
The homogenate processing method ?10133.3 ????47 ??1143 ??23 ????7.9 ????14.3 ????5.7 ????2040
Processing method of the present invention ?10711.5 ????51.2 ??1102 ??25 ????8.2 ????14.6 ????6.1 ????2207
The content (mg/kg) of harmful material in the radix polygoni multiflori powder of table 4 distinct methods processing
Plumbous (in Pb) Arsenic (in As)
State food health legislation set quota ????≤0.5 ????≤0.2
Natural dry product ????83.23 ????1.15
Homogenate processing method (in the radix polygoni multiflori powder) Do not detect Do not detect
(in the extract concentrate) ????8.46 ????0.74
Processing method of the present invention (in the radix polygoni multiflori powder) Do not detect Do not detect
(in the extract concentrate) ????0.07 ????0.02
Main amino acid content % before and after table 5 processing
The bright product content of radix cynanchi bungei Radix polygoni multiflori powder after the present invention's processing
Valine ????0.17 ????0.24
Leucine ????0.26 ????0.34
Isoleucine ????0.30 ????0.24
Threonine ????0.18 ????0.21
Phenylalanine ????0.34 ????0.30
Methionine ????0.05
Tryptophan ????0.08
Cystine ????0.08 ????0.02
Cruel propylhomoserin ????0.33 ????0.14
Glycine ????0.19 ????0.30
Serine ????0.14 ????0.14
Alanine ????0.22 ????0.32
Glutamic acid ????0.75 ????0.98
Asparatate ????0.64 ????0.78
Proline ????0.31 ????0.20
Lysine ????0.25 ????0.40
Histidine ????0.13 ????0.18
Arginine ????2.23 ????2.28
Add up to ????6.60 ????7.12
Table 6, the main vitamins content mg/kg before and after the processing
The bright product content of radix cynanchi bungei Radix polygoni multiflori powder after the present invention's processing
????B1 ????0.752 ????9.110
????B2 ????0.213 ????19.220
????B6 ????28.300 ????40.760
????PP ????854.680 ????820.560
Add up to ????883.945 ????889.650

Claims (10)

1, a kind of new process equipment and process that is used for plant extract, it is characterized in that by to the improvement of existing homogenate, broken wall, ultrasonic wave, microwave and traditional extraction device or optional can better equipment, form 5 extraction cells, then with the design of having complementary advantages, making overall plans, its organic combination is become to have the technical equipment of original effect, and created that micro mist is broken with growing with each passing hour, new processes such as batch (-type) adverse current and the anhydrous extraction of bright product.
2, new process equipment and the process that is used for plant extract according to claim 1, it is characterized in that in homogenate and wall-breaking abstraction unit, replace existing refiner and disintegrating machine with online high shear homogeneous dispersion machine and the better high pressure homogenizer of performance, provide the mass transfer space that makes solute and solvent obtain huge surface area to reach the condition that helps the effective ingredient stripping most and do not change extract effect characteristic, thereby improved the utilization rate of plant functional component.
3, new process equipment and the process that is used for plant extract according to claim 1 is characterized in that replacing traditional pot type ultrasonic extraction device in the ultrasonic extraction unit with single hose ultrasonic extraction device.This single hose ultrasonic extraction device dead angle simple in structure, no, superior performance, the thickness of chamber wall and container placement location are required also not harsh, and cleaning equipment and change ultrasonic vibrator easily is a kind of novel, ultrasonic wave plant extraction device of not reporting fully in the past.
4, new process equipment and the process that is used for plant extract according to claim 1, it is characterized in that to extract and the microwave irradiation device separates in the microwave abstracting unit, in the microwave irradiation chamber, tube extractor is installed, strengthened controllability, can operation safely under vacuum, normal pressure and pressurized conditions.
5, new process equipment and the process that is used for plant extract according to claim 1, it is characterized in that in the extractor of the center of center extraction cells, being provided with the agitator and the return-flow system of special construction, can carry out the extraction operation of method more than five kinds with same extractor, and extraction and precipitation carry out in the extractor of center, reduce to extract operation operation.
6, new process equipment and the process that is used for plant extract according to claim 1, it is characterized in that with the design of having complementary advantages, making overall plans, allow homogenate, broken wall, ultrasonic, microwave, each doing his best for 5 extraction cells of tradition, maximized favourable factors and minimized unfavourable ones, brought into play the global advantage of technical equipment.These 5 extraction cells both can independent or any series combination, also can extract with wherein a kind of, several a kind of methods of connecting with usual ways such as infiltration, decoction, backflows.And to adopt with high shear homogeneous dispersion machine be the complete alternation extraction mode of power, increased extraction process state, mass flow, and extracting pressure and 4 control devices of extraction environment make extraction more safe and efficient.
7, new process equipment and the process that is used for plant extract according to claim 1, it is characterized in that creating the process of the broken extraction of micro mist, this new process for extracting is characterised in that its mass transfer and diffusion velocity are exceedingly fast, do not influence the solute that has dissolved and from the solid interior fluid, be diffused into the surface of solids, also continue to spread the speed that arrives the external solvent main body by liquid film from the surface of solids because of degree of grinding is meticulous, thereby the efficient extra-high-speed.And the dietary fiber in the plant does not have coarse mouthfeel, can directly eat.
8, new process equipment and the process that is used for plant extract according to claim 1, it is characterized in that creating the process of batch (-type) counter-flow extraction, this new process for extracting is characterised in that equipment simple in structure with several, that cost is lower replaces traditional extractor group, and take liquid, material after each the extraction to shift out extractor simultaneously and carry out Separation of Solid and Liquid outward, reduce the method for target extract moisture content significantly, reduced extraction cost.
9, new process equipment and the process that is used for plant extract according to claim 1, it is characterized in that creating the process of the anhydrous extraction of bright product, this new process for extracting is characterised in that the feature of utilizing the alcohol strong water absorbent, by the moisture that absorbs in the fresh plant alcohol is remained in the best concentration range of solubility property, reach final extraction target with degree of the passing extracting method that progressively improves alcohol concentration.
10, new process equipment and the process that is used for plant extract according to claim 1 is characterized in that the plant of indication of the present invention comprises Chinese herbal medicine, wild plant and agricultural byproducts, and solvent comprises organic solvent, inorganic solvent and water.
CN 03132385 2003-08-17 2003-08-17 New-type technological equipment and method for plant extraction Pending CN1579592A (en)

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CN102350087A (en) * 2011-07-01 2012-02-15 江苏大学 Ultrasonic negative pressure circulating extraction device
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CN104258594A (en) * 2014-10-29 2015-01-07 大闽食品(漳州)有限公司 Method for extracting plant effective constituents efficiently
CN104839615A (en) * 2015-04-29 2015-08-19 潍坊友容实业有限公司 Method for extracting high-calcium low-arsenic plant salt contained in suaeda salsa in saline land
CN108970169B (en) * 2015-09-01 2023-05-02 广州泽力医药科技有限公司 Coupled plant component extraction device and process method
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CN111107917A (en) * 2017-09-21 2020-05-05 惠斯勒科技公司 Apparatus and method for resin extraction
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