CN1292682C - Normal temperature extraction method of plant formulated concentrate - Google Patents
Normal temperature extraction method of plant formulated concentrate Download PDFInfo
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- CN1292682C CN1292682C CNB2003101000123A CN200310100012A CN1292682C CN 1292682 C CN1292682 C CN 1292682C CN B2003101000123 A CNB2003101000123 A CN B2003101000123A CN 200310100012 A CN200310100012 A CN 200310100012A CN 1292682 C CN1292682 C CN 1292682C
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Abstract
The present invention relates to a general technology for extracting, dissolving and separating fresh plants at normal temperature. The technology has three characteristics that the whole working process is carried out at normal temperature, and thus, the basic characteristics of natural substances can be kept at a maximum; most of bacteria can be killed in the extractive process; low-boiling components can be separated out. Experiments prove that the extraction rate of kernel removal fresh fruits with sufficient moisture accounts for 80 to 85% of weight percentage; the extraction rate of fresh alose and onion accounts for 80 to 85% of weight percentage; the extraction rate of garlics and dioscorea zingiberensis accounts for 80 to 85% of weight percentage; the extraction rate of herb or ligneous plants accounts for 30 to 35%. A set of apparatus of the technology can process multiple plant raw materials, and the system is easily washed.
Description
Technical field
The present invention relates to a kind of method of extracting original plant juice, be specifically related to the method that a kind of technological means of utilizing bioengineering to combine with Chemical Engineering is extracted original plant juice at normal temperatures.
Background technology
In the prior art, it generally is the method that adopts squeezing that fresh fruit of vegetables is extracted fruit drink, but for many fruit is 100% fruit juice that can't obtain clarifying with the method for squeezing, such as peach, apricot, mango, tomato, Kiwi berry etc., the above-mentioned five kinds of fruit juice that are commercially available all are muddy basically and can not mark 100% fruit drink (also is false if marked), this be because its pulp and wherein the combination of moisture determine, it can only break into slurry and not add water and be difficult to directly to filter, and therefore conventional processing method can not obtain the fruit juice of business-like 100% clarification of above-mentioned fruit.So because business-like fruit juice must have certain shelf-life must carry out sterilization treatment, general sterilization measure all needs 80 ℃ or higher temperature, therefore fruit drink can not be arranged.Many effective ingredients in fruit juice spatial configuration of molecules under natural situation is left-handed, but has changed through the space structure of molecule after the temperature more than 60 ℃, such as fructose, tartaric acid etc., and has many nutritional labelings destroyed.It is fragrant that some fresh fruit is put, and all can emit the fragrance of its uniqueness when the maturation such as apricot, these fresh fruits of mango, but these precious aromatic substances run off all in conventional process.
In the prior art, the deep processing of Chinese herbal medicine and medicinal nutriment generally is meant the dried raw material of gas of Chinese herbal medicine is processed, conventional method is that water, alcohol, benzinum carry out lixiviate as solvent, use water as solvent general through boiling, evaporation obtains concentrate or spray-drying obtains the former medicine composition of powdery.Make will distilling of solvent or vacuum distillation recovered solvent and obtain medicinal ingredient with alcohol or benzinum.And many fruit classes, piece root class, bulb class Chinese medicine such as the fruit of Chinese magnoliavine, the fruit of Chinese wolfberry, genseng, American Ginseng, the fleece-flower root, aloe, lily, garlic have passed through airing or high-temperature baking in rough machined process, light component in its medicinal ingredient part has run off, baking is dry can to make the space structure of part medicinal ingredient and nutritional labeling destroyed, Ancient Chinese is for the ease of long preservation for being made into gas to fresh Chinese medicine dried, be to come from the preservation technique that does not have other at that time, fresh Chinese medical extract should have better medicinal effects.Many in recent years biotechnologys enterprise is introducing and is developing overcritical high-tech natural colouring matter energetically, the extractive technique of Chinese herbal medicine and health products, data is presented in Beijing, Chengdu, Sichuan is all at the large and super-critical equipment of introducing 1.5 cubic metres * 3,0.3～0.5 cubic metre overcritical equipment of domestic production has had tens covers at home, the investment of each project is up to ten million at least more than one hundred million at most, and the applicant is in organic institute of nineteen ninety and Chinese Academy of Sciences Shanghai, Shanghai spices and Guangxi woods section the begin one's study application of supercritical technology means on Chinese herbal medicine and natural perfume material of relevant expert.But, a kind ofly invest the little method that can reach identical or propinquity effect again and carry out large-scale industrial production so also thinking deeply to have always because the investment of industrialization large-scale plant is huge.
Have existed since ancient times in China to utilize natural perfume plant to extract natural perfume material, be flower, stem, leaf, skin, the fruit that utilizes plant mostly, and also useful its xylem extracts banksia rose type spices, as sweet osmanthus, jasmine, yulan, cypress skin, beautiful osmanthus, anise, fragrant camphor tree.Conventional extracting method generally has two kinds, a kind of be the water steam stripping after, utilize its solubility in water to carry out water-oil separating and obtain thick essential oil, carry out normal pressure or decompression distillation again and obtain essential oil.Another kind method is to be that solvent carries out lixiviate to material with benzinum or alcohol, distills then or decompression distillation obtains essential oil or obtains medicinal extract and reclaim solvent at the bottom of tower from cat head.Concrete which kind of method of using decide on the kind of material and the kind of essential oil, no matter and the temperature of which kind of method distillation or decompression distillation all more than 70 ℃, so the essential oil that obtains or the fragrance of medicinal extract and the fragrance of natural materials have bigger gap.Therefore have only the fragrance of using the essential oil resin that overcritical means extract near the fragrance of natural materials, unique shortcoming is to invest too greatly, and operating cost is too big, and relatively difficulty is accepted in market.
Summary of the invention
Technical problem to be solved by this invention provides and can access 100% clear juice, the active ingredient that can keep Chinese herbal medicine and medicinal nutriment, the natural perfume material that extracts is near the fragrance of natural materials, invest little, operating cost is low, the method for extracting original plant juice at normal temperatures that is received by the market.
The present invention extracts the method for original plant juice at normal temperatures, may further comprise the steps,
(1) clean material, and drain surperficial open fire, roll extrusion destroys eucaryotic cell structure;
(2) at normal temperatures, adopting alcoholic strength is that 65%～100% alcohol carries out extracting as extraction solvent, the stripping clear liquid;
(3) cross cleaner liquid, separate through vacuum distillation at normal temperatures, obtain the component of original plant juice and maintenance material natural characteristic.
The method of extracting original plant juice at normal temperatures of the present invention, some material also need be crushed to the broken particle of 3～8mm after roll extrusion, some band nuclear fresh fruit need carry out twice roll extrusion, adds the stoning operation after the roll extrusion for the first time, carry out the roll extrusion second time then, to prevent that examining interior material pollutes.
The method of extracting original plant juice at normal temperatures of the present invention, because of the high more material of water content, the alcoholic strength of the extraction solvent that needs is high more, so can select the extraction solvent of suitable alcoholic strength for use according to the water content of material, the alcoholic strength control of this available extracting tail washings, the alcoholic strength percent by volume of generally controlling tail washings is between 55%～65%.
The method of extracting original plant juice at normal temperatures of the present invention, described extracting are that quadruple effect or six is imitated or the semicontinuous adverse current extracting of eight effects.
Because nutrition and Chinese medicinal ingredients are extremely complicated, having many is alcohol and water-insoluble, solid portion after the extracting is through after the centrifugation, the solid of gained can also be used for becoming a kind of product separately after the extraction of other active ingredient or the low temperature drying, the liquid filtering of gained, the extract after filtering enters separating technology.
The method of extracting original plant juice at normal temperatures of the present invention, adopt vacuum (distilling) column infinite reflux separating plant stoste and alcohol, the gas phase leadout hole is established on afterbody top at the case partition of reflux condenser, the needs of the light component that separates according to desire, for the material that contains lower boiling light component, then connect light component vacuum packed tower, adopt the light component of-5 ℃～5 ℃ freezing liquid condensation separation, obtain to keep-5～20 ℃ low boiling light component of material natural characteristic at gas phase leadout hole place.
Method that to be extraction solvent at normal temperatures with alcohol carry out the extracting stripping and separate under vacuum the moisture in moisture higher fresh or preserve moisture freezing fruits and vegetables, Chinese herbal medicine and the natural perfume plant and effective ingredient that the present invention is.To air-dry but pulverize moistening plant material again and also can use this method.Can also be except that fresh raw material with bag (food polybag) the freezing long preservation of preserving moisture of preserving moisture of packing into after the fresh raw material cleaning, the reprocessing of thawing during use can not reduce sucrose extraction.The present invention isolated nutriment, medicinal ingredient or aromatic substance must be water-soluble or alcohol is molten, and can be not at normal temperatures and the material of water or alcohol generation chemical reaction.The present invention has three characteristics, first characteristics are that whole process is all carried out at normal temperatures, the fundamental characteristics that therefore can keep natural materials to greatest extent, as natural activity, taste and the smell of nutriment and medical substance all very near natural materials, isolated stoste is if carry out the extract of approaching overcritical means of separator that microwave low-temperature drying obtains, and investment only is 1/10th of the overcritical project of identical scale with operating cost.Second characteristic are that what to take in extractive process is that quadruple effect or six is imitated semicontinuous adverse current extracting stripping, what fresh material contacted is wake flow liquid, about alcoholic strength 65%, can kill most bacteriums, therefore, as long as whole system is not contaminated, the original plant juice that is separated is can directly carry out packing or can through what sterilize, and this sterilization process has still kept the various characteristics of natural materials without crossing high temperature.The 3rd characteristics are that the cooling medium that uses in the afterbody condenser of system is-5～5 ℃ freezing liquid and has connect one-level filler knockout tower,-5～20 ℃ low boiling component can be separated, this part material natural materials often gives out the aromatics or the pungent class material of peculiar fragrance, it is extremely precious essential oil part, when the processing natural perfume material, can become product separately, also can join in the stoste of tower still extraction fragrance and medicinal ingredient when making stoste keep material natural.Through experiment, sucrose extraction for the stoning fresh fruit of moisture content abundance is weight percentage 80～85%, sucrose extraction for the fresh aloe onion is weight percentage 85～90%, reach percentage by weight 65～69% for the sucrose extraction of garlic after supercentrifuge takes off liquid, for the bar of draft and xylophyta and the sucrose extraction about 30～35% of branches and leaves.Technological process of the present invention and equipment thereof can be processed various materials, because the cleaning of system is easy to, for enterprise's meeting the market requirement has been created condition.
Description of drawings
Fig. 1 is an extraction process schematic flow sheet of the present invention
Fig. 2 is a vacuum separation process flow diagram of the present invention
Reference numeral
1-rinse bath, 2-roller press, the 3-electronic chain of leading, 4-head tank, 5-extracting tank, 6-measuring pump, 7-clear liquid storage tank, 8-measuring pump, 9-centrifuge, 10-recovery liquid bath, 11-filter;
A-tower still, b-heater, c-stripping section, d-rectifying section, e-reflux condenser, f-light component packed tower, g-light component condenser, h-alcohol storage tank, i-light component storage tank, j-boilers heated electrically, k-serpentine (trombone) cooler, l-backwater head tank, m-vacuum control jar.
The specific embodiment
1, raw material extraction process flow process
The raw material extraction process be utilize the dehydration property of high neutral spirits and dissolubility with the moisture in the plant and some composition extractings in alcoholic solution.
The extraction process flow process is from equipment 1, equipment 1 is for adopting continuous, semicontinuous or batch (-type) rinse bath, the pollutant on material surface, remains of pesticide, silt etc. are cleaned up and drain surperficial open fire, by roller press 2 roll extrusion materials, press down the eucaryotic cell structure of destroying material and be beneficial to extracting, two pressure rollers of roller press 2 are isometrical, the pressure roller diameter is not less than 300mm surface band anti-slip tank, variable speed, a pressure roller is 40～60 rev/mins, another is 80～120 rev/mins, and the nip drum spacing is adjustable, and power adopts buncher.Some material also need be crushed to the broken particle of 3～8mm after roll extrusion, the band nuclear material must carry out secondary rolled after stoning, to prevent that examining interior material pollutes.The electronic chain 3 of leading is used for cylinder mould and material in the mobile extracting tank.Dress extraction solvent alcohol in the head tank 4, alcoholic strength is selected for use according to the water content of material 65%～100%, and what water content was high more selects for use the solvent liquor precision high more, and with the alcoholic strength control of extracting tail washings, the alcoholic strength of generally controlling tail washings is between 55%～65%.Character according to material, extracting tank group 5 is selected the semicontinuous extracting of four-effect countercurrent extraction for use, select explosion-proof magnetic valve group control for use, single jar structure is two-layer, skin is the cylinder mould of stainless steel structure for the stainless steel outer sleeve internal layer, the content material, cylinder mould can be selected 80～120 purpose stainless steel cloths for use according to the character of material.Supercentrifuge 9, with Separation of Solid and Liquid, reclaim liquid bath 10 withdrawal liquid, because nutrition and Chinese medicinal ingredients are extremely complicated, having many is alcohol and water-insoluble, and the solid portion after the extracting can also be used for becoming a kind of product separately after the extraction of other active ingredient or the low temperature drying.Reclaim liquid and get back to clear liquid storage tank 7 after filtration, because separating technology is continuous, so the volume of clear liquid storage tank 7 should calculate by at least four hours demand.In the filter 11 is two-layer kink, and the kink internal layer is 200 order stainless steel cloths, and skin is 300 order stainless steel cloths, and tail washings filters the alternately cleaning use of two filters from inside to outside.Single jar of tail washings of emptying when measuring pump 6 is used for controlling the tail washings flow and changes material.Measuring pump 8 is used for steady and continuous quantitatively to separating technology conveying clear liquid.
2, vacuum separation technological process
Vacuum separation technology is that alcohol in the alcoholic solution that the raw material extraction process is sent here and water and some component separation come, and obtains the stoste of plant and and keeps the component of material natural characteristic.
Device numbering a, b, c, d are four parts of vacuum (distilling) column, and material is generally used stainless steel, and special material should carry out corrosion resistance test.The temperature of tower still a is 40～45 ℃, vacuum is 17.0～18.0KPa, the outlet of extracting stoste is arranged at tower still a bottom, stoste should be controlled its alcoholic strength less than 0.04%, with fluid level controller control adjustable dosing pump extracting stoste is sent to finished product and handles the workshop, because extracting stoste is 100% the stoste of having sterilized, it can direct packaging or can, also can obtain the product of concentrate or semifluid, solid with the method for microwave low-temperature drying.Heater b adopts the shell and tube thin film evaporator, and the service condition in the pipe is identical with the tower still, adopts 60～65 ℃ water at low temperature steam heated, and temperature is 60～65 ℃ in the chuck, vacuum 20～25KPa.The stripping section c of destilling tower, the actual plate number is 19～21, adopts whole stainless steel metal perforated plate corrugated filler tower, and topmost is equipped with from the next extracting stoste spray thrower of extraction process, and the temperature of stripping section c is 30～40 ℃, and vacuum is 13.0～17.0KPa.The rectifying section d of destilling tower, the actual plate number is 20～22 plates, is filler and float valve mixing column, below 15 plates adopt whole stainless steel metal perforated plate corrugated filler tower, 16～21 plates adopt stainless steel float valve tower, and 16～17 distances between plates are that other distances between plates of 300mm all adopt 200mm.16 plates are that liquid phase solvent reclaims plate, and 95～97% alcohol is drawn the extraction process process of returning from 16 plates, and the alcohol amount of drawing should strictly be controlled flow in order to avoid cause the tower operation unbalance.Smart temperature of slipping section d is 25～30 ℃, and vacuum is 9.5～13.0KPa, and topmost is equipped with the phegma spray thrower.Reflux condenser e adopts Stainless Steel Shell shell and tube condensing mode, adds the multilayer dividing plate in the condensation efficiency housing in order to improve, and lower partition is established pod apertures, and a gas phase export mouth is established on the afterbody top of different with general reflux condenser is housing upper spacer.Reflux condenser e does cooling medium with recirculated water, and cooling water recycles after lowering the temperature with two-stage or three grade cooling towers.The service condition of reflux condenser e is 15～20 ℃ of cooling water temperatures, and vacuum is 9.5KPa in the housing, and the phegma temperature is 20～25 ℃, adopts infinite reflux.For the material that contains the low boiling light component, connect light component vacuum separation tower f at the gas phase leadout hole, adopt 10 plate stainless steel metal perforated plate corrugated filler towers, reflux and establish phegma spray beautiful jade device from the 7th plate, service condition, temperature are 23～25 ℃, and vacuum is 9.0～9.5KPa.Light component condenser g is the Stainless Steel Shell shell and tube, add the multilayer dividing plate in the housing, lower partition is established pod apertures, a vacuum structure is stayed on the afterbody top of dividing plate, the interface regulation and control thus of the vacuum of entire separation system, the cooling medium of light component condenser is a freezing liquid, use floride-free refrigeration modes as far as possible, in order to avoid cause to environment damage, the temperature of freezing liquid is-5～5 ℃, actual conditions according to light component are adjusted, and the temperature in the housing is 0～5 ℃, and vacuum is 8.5～9.0KPa.Except the light component of natural perfume material and some Chinese herbal medicines was many, the content of the light component of ordinary material was micro-, therefore can intermittently extract light component with continuous extraction of big reflux ratio or infinite reflux, and these light components are extremely precious parts.Take turns to discharge the alcohol storage tank h that vacuum is used for two, by flowmeter control discharge, single capacity should satisfy 2～3 hours discharge of technology.Take turns for two to discharge the light component storage tank i that vacuum is used, capacity should satisfy the amount of 8 hours light component of technology.Vacuum control jar m, the vacuum of control and distribution system each several part, vacuum is formed by two-stage or three grades of water stream injection pumps, and vacuum reaches 0.099MPa.Boilers heated electrically j, serpentine (trombone) cooler K and two vacuum backwater high-temperature tank L form electric heating low temperature steam generator system, the temperature of system is 60～65 ℃, vacuum is 20～23KPa, cold 20～25 ℃ of the water temperatures of anhydrating, and smaller system can directly make heat medium with 60-65 ℃ hot water.
3. the calculating of material extraction efficiency
Should carry out the alcohol extraction test so that the basic data of design to be provided for different materials, concrete method is that the fresh material that 1. will use is smashed accurate weighing 100g in sand-ground opening 500ml triangular flask to pieces.2. use edible alcohol and the accurately weighing of 200ml volumetric flask accurate quantification 200ml 95%, and pour the tight bottle stopper of triangular flask middle cover into.3. shook up once every one hour, after four hours clear liquid poured in the 250ml graduated cylinder with alcoholic strength instrumentation amount alcoholic strength and weigh, if alcoholic strength is lower than 80% and should remeasures alcoholic strength by the way of distillation.4. after falling to do bright liquid, residue is carried out weighing, after putting a dried filter paper weighing, centrifuge tube bottom gets residue in the bottle that 10g falls to do bright liquid again, turned round 5-7 minute under 3000-3500 rev/min of condition with centrifuge, residue is taken out the gain in weight of back weighing centrifuge tube with tweezers.5. according to the alcohol of measuring and every data computation sucrose extraction of residue.
What did in the laboratory is the balance extracting, should increase by 3～7% at the actual sucrose extraction of the adverse current extracting of suitability for industrialized production on experience.More than three parallel sample are made in test at every turn, and data have two coincidence data approvals.
Extraction process of the present invention is to have made full use of alcohol to the dissolving of material and two characteristics of dewatering, and separating technology has been used the characteristic of water and the boiling point reduction of alcohol under vacuum.Chemical industry equipment and unit related in the whole technical process can replace reducing operating cost with the efficient that improves operation with equipment that upgrades and unit.Should actively use simultaneously exploitations such as modern new membrane separation technique and post isolation technics to the deep processing of material stoste to improve the technical value added of product.
Separating technology has been used the characteristic of water and the boiling point reduction of alcohol under vacuum.Chemical industry equipment and unit related in the whole technical process can replace reducing operating cost with the efficient that improves operation with equipment that upgrades and unit.Should actively use simultaneously exploitations such as modern new membrane separation technique and post isolation technics to the deep processing of material stoste to improve the technical value added of product.
Claims (8)
1, extract the method for original plant juice at normal temperatures, may further comprise the steps,
(1) clean material, and drain surperficial open fire, roll extrusion destroys eucaryotic cell structure;
(2) at normal temperatures, adopting the alcohol of alcoholic strength 65%～100% is that extraction solvent carries out extracting, the stripping clear liquid;
(3) cross cleaner liquid, separate through vacuum distillation at normal temperatures, obtain original plant juice.
2, the method for extracting original plant juice at normal temperatures according to claim 1 is characterized in that, is crushed to 3～8 millimeters broken particle after the material roll extrusion;
3, the method for extracting original plant juice at normal temperatures according to claim 1 is characterized in that, band nuclear fresh fruit carries out twice roll extrusion, adds the stoning operation after the roll extrusion for the first time, carries out the roll extrusion second time then.
4, the method for extracting original plant juice at normal temperatures according to claim 1 is characterized in that, selects the alcoholic strength of extraction solvent alcohol for use according to the alcoholic strength of extracting tail washings, and the alcoholic strength of control tail washings is in percent by volume 55%～65%.
5, the method for extracting original plant juice at normal temperatures according to claim 1 is characterized in that, described extracting is that quadruple effect or six is imitated or the semicontinuous adverse current extracting of eight effects.
6, the method for extracting original plant juice at normal temperatures according to claim 1 is characterized in that, adopts infinite reflux separating plant stoste and alcohol under the vacuum (distilling) column normal temperature, establishes the gas phase leadout hole on the afterbody top of the case partition of reflux condenser.
7, the method for extracting original plant juice at normal temperatures according to claim 6 is characterized in that, connects low boiling light component vacuum packed tower in the gas phase derivation aperture of described reflux condenser, and normal temperature separates contained low boiling light component down.
8, the method for extracting original plant juice at normal temperatures according to claim 7 is characterized in that, connects low boiling light component vacuum packed tower in the gas phase derivation aperture of described reflux condenser, and normal temperature separates contained low boiling light component down.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2003101000123A CN1292682C (en) | 2003-10-08 | 2003-10-08 | Normal temperature extraction method of plant formulated concentrate |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2003101000123A CN1292682C (en) | 2003-10-08 | 2003-10-08 | Normal temperature extraction method of plant formulated concentrate |
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| CN1605288A CN1605288A (en) | 2005-04-13 |
| CN1292682C true CN1292682C (en) | 2007-01-03 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102061220B (en) * | 2010-12-09 | 2012-10-31 | 江南大学 | Method for preparing onion functional components by using double-stage extraction based on subcritical water and solvent method |
| CN104046514B (en) * | 2013-03-15 | 2016-08-03 | 什邡市恒源油脂有限责任公司 | A kind of Bulbus Allii quintessence oil extracting method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1081069A (en) * | 1992-07-11 | 1994-01-26 | 大连黑米商务会社 | A kind of process of making black rice magma |
| CN1028245C (en) * | 1990-09-08 | 1995-04-19 | 湖北省建始县白肋烟复烤厂 | Technology for extracting essence cream from tobacco bud |
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2003
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1028245C (en) * | 1990-09-08 | 1995-04-19 | 湖北省建始县白肋烟复烤厂 | Technology for extracting essence cream from tobacco bud |
| CN1081069A (en) * | 1992-07-11 | 1994-01-26 | 大连黑米商务会社 | A kind of process of making black rice magma |
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