CN102127129A - Method for extracting stevioside from fresh stevia rebaudiana leaves - Google Patents
Method for extracting stevioside from fresh stevia rebaudiana leaves Download PDFInfo
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Abstract
The invention discloses a method for extracting stevioside from fresh stevia rebaudiana leaves, which comprises: crushing fresh stevia rebaudiana leaves with homogenizing crushing equipment under a condition of water, performing pressure filtration in continuous automatic discharge filtering equipment, subjecting the filtrate to flocculation by mixed flocculating agent; and absorbing by resin, analyzing, desalting and decolorizing by resin, concentrating and spray drying to obtain the stevioside product. In the invention, time and working procedures are saved, a long-distance transport process is avoided, raw material cost is lowered, discharge of waste water is reduced greatly, and clean production can be realized basically.
Description
Technical field
The invention belongs to the technical field that relates to the Steviosides extraction, be specifically related to a kind of method of utilizing fresh stevioside leaf for the raw material extraction of steviosides.
Background technology
Sweet Stevia (stevia rebaudiana) is composite family (Compositae) Stevia plant.Steviosides is commonly called as stevioside (Stevioside), is the smart new type natural sweeting agent of carrying from catananche's sweet Stevia.Sweet Stevia originates in ground such as Paraguay, Brazil, Argentina of South America.China's sweet Stevia be 1976 from Japanese introducing culture success, and extracted Steviosides in 1979.The glucoside mixture that the Steviosides glycoside that to be a class connect different numbers by this tetracyclic diterpene compound of stevia rebaudianum alcohol is formed.That discovers at present has 12 kinds of materials, is approved and did have eight kinds of medical science toxicological experiment by people, and be specially: stevioside (stevioside) (St); Stevia rebaudianum disaccharide glucoside (steviolbioside); Content rebaudioside-A (rebaudioside A) (R-A); Rebaudioside B (rebaudioside B) (R-B); Rebaudioside C (rebaudioside C) (R-C); Rebaudioside D (rebaudioside D) (R-D); Rebaudioside E (rebaudioside E) (R-E); But Dole's glucoside A (dulcoside A) (D-A).
Steviosides is not participated in the metabolism of human body.Safe, reliable, nontoxic, have no side effect.High sugariness, (calorific value be equivalent to sucrose 1/300) low in calories.Sweet taste is similar to sucrose, but the time length is longer than sucrose.Cardiovascular and cerebrovascular disease, obesity, diabetic subject there is the assisting therapy function, the carbohydrate surrogate that more helps to prevent and treat carious tooth and urinate ketosis (PKU) patient as phenylpropyl alcohol.Be to continue outside sucrose, the beet sugar that the third has exploitation to be worth and the natural product of replacing sugar of healthy functions, be described as " trisaccharide source " in the world.Be widely used in varieties of food items, beverage, medicine, the daily use chemicals industrial goods.
China is through the development of three more than ten years, and the sweet Stevia cultivated area has reached more than 50 ten thousand mu, nearly 30 families of manufacturer, and output reaches more than 5000 ton, is maximum in the world sweet Stevia plantation state, also is maximum producing country and export State.
At present, the extraction of Steviosides both at home and abroad all is to be raw material with the sweet Stevia cured leaf, the bright leaf of sweet Stevia through artificial picking leaves, dry or air-dry, be transported to Steviosides factory after the compressed packing and soak extraction.The bright leaf of sweet Stevia is drying takes a lot of work consuming timely, soaks that to extract water consumption big, causes the outer discharge capacity of water big, has increased production cost.
Summary of the invention
It is the method for raw material extraction of steviosides that the present invention discloses the fresh stevioside leaf of a kind of usefulness, and purpose is to provide the Steviosides extracting method that a kind of technology is simple, of reduced contamination and cost reduces.
The present invention implements by the following technical programs:
The method of the fresh stevioside leaf extraction of steviosides of a kind of usefulness is characterized in that: said method comprising the steps of:
(1) Mechanical Crushing: fresh stevioside leaf is put into the homogeneous disintegrating apparatus with water carry out the homogeneous fragmentation, make fresh stevioside leaf be broken into particulate, thereby the cell walls of the bright leaf of sweet Stevia is destroyed, obtain the bright leaf slurries of sweet Stevia;
(2) filter: the bright leaf slurries of the sweet Stevia after the fragmentation are squeezed into continuous automatic unloading material filter plant with pump filter the removal mechanical impurity, obtain filtrate and filter residue;
(3) ultrasonic extraction: with the water of 5-15 times of volume of step (2) gained filter residue adding, filter residue is carried out the first time soak, carry out the extraction first time, 30 minutes time in ultrasonic wave with under stirring then; The general's extracting solution first time is squeezed into continuous automatic unloading material filter plant and is filtered, obtain filtrate for later use, the water that the residue filter residue adds about 5-15 times again carries out the immersion second time, carry out the extraction second time in ultrasonic wave with under stirring, the general's extracting solution second time is squeezed into continuous automatic unloading material filter plant again and is filtered, the gained filtrate recycle is as the water of homogeneous fragmentation, and filter residue is transported outward as fertilizer;
(4) flocculation: standby filtrate merging in the filtrate of step (2) gained and the step (3) is obtained mixed solution, under agitation in mixed solution, add the flocculation agent that accounts for mixed solution weight 0.25% earlier, mixed solution is transferred to liming be pH value 9.5-10 then; Continue to stir after 30 minutes, squeeze into continuous automatic unloading material filter plant and filter, remove materials such as macromolecular protein, colloid, pigment, Mierocrystalline cellulose, obtain filtrate for later use;
(5) resin absorption: the standby filtrate in the step (4) is adsorbed Steviosides by polymeric adsorbent, waste water ultrafiltration membrance filter after the absorption, the gained filtrate recycle is used as fodder additives as the broken water of homogeneous or as the first time or the second time soaking water, making fertilizer after the filter residue outward transport is fermented or directly handle;
(6) resolve: the ethanolic soln that with concentration is 60%-80% carries out wash-out to the Steviosides that is adsorbed on the polymeric adsorbent, and Steviosides is resolved from polymeric adsorbent, forms desorbed solution;
(7) desalination bleaching: allow desorbed solution by desalination resin and decolorizing resin, remove metal-salt and pigment in the desorbed solution;
(8) concentrate: allow the desorbed solution behind the desalination bleaching concentrate, make the concentration of concentrated solution reach spray-dired concentration requirement by nanofiltration membrane.The concentrated solution that is by nanofiltration membrane not; By the penetrating fluid that is of nanofiltration membrane, reuse is as desorbed solution;
(9) spraying drying: concentrated solution is placed spray drying device, obtain the Steviosides product.
Fresh stevioside leaf is put into clarifixator with the water of 5-15 times of volume carry out the homogeneous fragmentation.
Flocculation agent is selected FeSO for use
47H
2O.
It is the ultra-filtration membrane of 5000-10000 that ultra-filtration membrane described in the step (5) adopts molecular weight cut off, moves in the cross-flow mode.
It is the nanofiltration membrane of 270-500 that nanofiltration membrane described in the step (8) adopts molecular weight cut off, moves in the cross-flow mode.
The homogeneous disintegrating apparatus comprises clarifixator, hollander, colloidal mill.
Continuous automatic unloading material filter plant comprises sheet frame, continuous automatic unloading flitch frame pressure filter and continuous automatic unloading material whizzer.
Polymeric adsorbent, desalination resin, decolorizing resin are carried out manipulation of regeneration with acid solution and the alkali lye of 2%-4% respectively, and acid solution after the processing and alkali lye are respectively with utilizing again behind the membrane filtration again.
It is the ultra-filtration membrane of 150-800 that membrane filtration adopts molecular weight cut off, moves in the cross-flow mode.
Major advantage of the present invention:
(1) with the fresh leaf extraction of steviosides of sweet Stevia, reduces the drying process of leaf, saved time and operation, reduced the long-distance transport link, reduced raw materials cost.
(2) compare with existing cured leaf extraction process, saved soak time, need 8 hours, reduce to 2.5 hours, saved the 2-3 time doubly by original immersion.
(3) this technology adopts continuous automatic unloading flitch frame filter first, general flame filter press has been saved the time, has saved the operation and the time of discharging, filter wash cloth.
(4) acid solution of waste water, desorbed solution and the resin regeneration after the absorption and alkali lye have significantly reduced effluxing of waste water through cyclically utilizing behind the membrane filtration, can accomplish clean production substantially.
(5) compare with existing cured leaf extraction process, output is brought up to more than 3 times, has reduced production cost.
Description of drawings:
Fig. 1 is a process flow sheet of the present invention.
Embodiment:
Fig. 1 is a process flow sheet of the present invention, as shown in the figure, the present invention is adding fresh stevioside leaf under the condition of water, with the homogeneous disintegrating apparatus with its fragmentation, with the press filtration of continuous automatic unloading material filter plant, filtrate is flocculated with flocculation agent, again through resin absorption, parsing, resin desalination bleaching, concentrate and the spraying drying operation makes the Steviosides product.
Describe the present invention below in conjunction with specific embodiment.
Embodiment 1:
Get 60kg sweet Stevia fresh leaf, fresh stevioside leaf is carried out the homogeneous fragmentation with the water of 5 times of volumes, obtain the broken slurries of 360kg sweet Stevia with the homogeneous disintegrating apparatus.
The bright leaf slurries of sweet Stevia after the fragmentation are squeezed in the continuous automatic unloading material filter plant with pump carry out press filtration, the water that bright leaf filter residue after filtering is added 8 times of volumes, carry out the extraction first time in ultrasonic wave with under stirring, 30 minutes time, squeeze into continuous automatic unloading material filter plant then and filter, obtain the extracting solution of 480kg.The water that filter residue is added again 8 times of volumes carries out the extraction second time in ultrasonic wave with under stirring, and filters with continuous automatic unloading material filter plant again, and secondary filtrate is as the water of homogeneous fragmentation.
To merge through the filtrate of homogeneous fragmentation and the filtrate of once extracting, under agitation add the FeSO that accounts for merging filtrate weight 0.25% earlier
47H
2O is as flocculation agent, and just 2.1kg is 9.5-10 with liming accent pH value afterwards, and the continuation stirring is squeezed into continuous automatic unloading material filter plant after 30 minutes and filtered.
Filtrate by polymeric adsorbent, is adsorbed Steviosides, the ultrafiltration membrance filter reuse of the waste water after the absorption, it is the ultra-filtration membrane of 5000-10000 that ultra-filtration membrane adopts molecular weight cut off, moves in the cross-flow mode.Ethanol 50kg with concentration 70% carries out wash-out to the Steviosides that is adsorbed on the polymeric adsorbent, obtains the desorbed solution of 35kg.
Allow desorbed solution by desalination resin and decolorizing resin, remove metal-salt and pigment in the desorbed solution.Allow the desorbed solution behind the desalination bleaching concentrate desorbed solution, make the concentration of concentrated solution reach 40% by nanofiltration membrane.Desorbed solution is made in the penetrating fluid reuse that sees through nanofiltration membrane.It is the nanofiltration membrane of 270-500 that nanofiltration membrane adopts molecular weight cut off, moves in the cross-flow mode.
Concentrated solution behind the membrane concentration by spray drying device, is obtained Steviosides product 11.2kg.
After testing, product is up to state standards.
Embodiment 2:
Get 60kg sweet Stevia fresh leaf, fresh stevioside leaf is carried out the homogeneous fragmentation with the water of 10 times of volumes with the homogeneous disintegrating apparatus.Obtain the broken slurries of sweet Stevia of 660kg.
The bright leaf slurries of sweet Stevia after the fragmentation are squeezed in the continuous automatic unloading material filter plant with pump carry out press filtration, the bright leaf filter residue after filtering is added the water of 10 times of volumes, carry out extraction first time, 30 minutes time in ultrasonic wave with under stirring.Squeeze into then in the continuous automatic unloading material filter plant and filter, obtain the extracting solution of 600kg.The water that filter residue is added again 10 times of volumes carries out the extraction second time in ultrasonic wave with under stirring, and filters with continuous automatic unloading material filter plant again, will filter the water of gained filtrate as the homogeneous fragmentation for the second time.
To merge through the filtrate of homogeneous fragmentation and the filtrate of once extracting, under agitation add the FeSO that accounts for merging filtrate weight 0.25% earlier
47H
2O is as flocculation agent, and just 3.15kg is 9.5-10 with liming accent pH value then, continues to stir to squeeze in the continuous automatic unloading material filter plant after 30 minutes and filters.
Filtrate is adsorbed Steviosides by polymeric adsorbent, the ultrafiltration membrance filter reuse of the waste water after the absorption, it is the ultra-filtration membrane of 5000-10000 that ultra-filtration membrane adopts molecular weight cut off, moves in the cross-flow mode.Ethanolic soln 50kg with concentration 70% carries out wash-out to the Steviosides that is adsorbed on the polymeric adsorbent, obtains the desorbed solution of 35kg.
Allow desorbed solution by desalination resin and decolorizing resin, remove metal-salt and pigment in the desorbed solution.Allow the desorbed solution behind the desalination bleaching concentrate desorbed solution, make the concentration of concentrated solution reach 40% by nanofiltration membrane.It is the nanofiltration membrane of 270-500 that nanofiltration membrane adopts molecular weight cut off, moves in the cross-flow mode.Desorbed solution is made in the penetrating fluid reuse that sees through nanofiltration membrane.
Concentrated solution behind the membrane concentration by spray drying device, is obtained Steviosides product 11.5kg.
Embodiment 3:
Get 60kg sweet Stevia fresh leaf, fresh stevioside leaf is carried out the homogeneous fragmentation with the water of 15 times of volumes with the homogeneous disintegrating apparatus.Obtain the bright leaf slurries of sweet Stevia of 960kg.
The bright leaf slurries of sweet Stevia after the fragmentation are squeezed in the continuous automatic unloading material filter plant with pump carry out press filtration, the bright leaf filter residue after filtering is added the water of 15 times of volumes, carry out extraction first time, 30 minutes time in ultrasonic wave with under stirring.Squeeze into then in the continuous automatic unloading material filter plant and filter, obtain the extracting solution of 900kg.The water that filter residue is added again 10 times of volumes carries out the extraction second time in ultrasonic wave with under stirring, and filters with continuous automatic unloading material filter plant again, and filtrate filtered is as the water of homogeneous fragmentation for the second time.
To merge through the filtrate of homogeneous fragmentation and the filtrate of extracting for the first time, under agitation add the FeSO that accounts for merging filtrate weight 0.25% earlier
47H
2O is as flocculation agent, and just 4.65kg is 9.5-10 with liming accent pH value then, and the continuation stirring is squeezed into continuous automatic unloading material filter plant after 30 minutes and filtered.
Filtrate by polymeric adsorbent, is adsorbed Steviosides, the ultrafiltration membrance filter reuse of the waste water after the absorption, it is the ultra-filtration membrane of 5000-10000 that ultra-filtration membrane adopts molecular weight cut off, moves in the cross-flow mode.Ethanol 50kg with concentration 70% carries out wash-out to the Steviosides that is adsorbed on the polymeric adsorbent, obtains the desorbed solution of 35kg.
Allow desorbed solution by desalination resin and decolorizing resin, remove metal-salt and pigment in the desorbed solution.Allow the desorbed solution behind the desalination bleaching concentrate desorbed solution, make the concentration of concentrated solution reach 40% by nanofiltration membrane.Desorbed solution is made in the penetrating fluid reuse that sees through nanofiltration membrane.It is the nanofiltration membrane of 270-500 that nanofiltration membrane adopts molecular weight cut off, moves in the cross-flow mode.
Concentrated solution behind the membrane concentration by spray drying device, is obtained Steviosides product 11.6kg.
Claims (9)
1. method with fresh stevioside leaf extraction of steviosides is characterized in that: said method comprising the steps of:
(1) Mechanical Crushing: fresh stevioside leaf is put into the homogeneous disintegrating apparatus with water carry out the homogeneous fragmentation, make fresh stevioside leaf be broken into particulate, thereby the cell walls of the bright leaf of sweet Stevia is destroyed, obtain the bright leaf slurries of sweet Stevia;
(2) filter: the bright leaf slurries of the sweet Stevia after the fragmentation are squeezed into continuous automatic unloading material filter plant with pump filter the removal mechanical impurity, obtain filtrate and filter residue;
(3) ultrasonic extraction: with the water of 5-15 times of volume of step (2) gained filter residue adding, filter residue is carried out the first time soak, carry out the extraction first time, 30 minutes time in ultrasonic wave with under stirring then; The general's extracting solution first time is squeezed into continuous automatic unloading material filter plant and is filtered, obtain filtrate for later use, the water that the residue filter residue adds about 5-15 times again carries out the immersion second time, carry out the extraction second time in ultrasonic wave with under stirring, the general's extracting solution second time is squeezed into continuous automatic unloading material filter plant again and is filtered, the gained filtrate recycle is as the water of homogeneous fragmentation, and filter residue is transported outward as fertilizer;
(4) flocculation: standby filtrate merging in the filtrate of step (2) gained and the step (3) is obtained mixed solution, under agitation in mixed solution, add the flocculation agent that accounts for mixed solution weight 0.25% earlier, mixed solution is transferred to liming be pH value 9.5-10 then; Continue to stir after 30 minutes, squeeze into continuous automatic unloading material filter plant and filter, remove materials such as macromolecular protein, colloid, pigment, Mierocrystalline cellulose, obtain filtrate for later use;
(5) resin absorption: the standby filtrate in the step (4) is adsorbed Steviosides by polymeric adsorbent, waste water ultrafiltration membrance filter after the absorption, the gained filtrate recycle is used as fodder additives as the broken water of homogeneous or as the first time or the second time soaking water, making fertilizer after the filter residue outward transport is fermented or directly handle;
(6) resolve: the ethanolic soln that with concentration is 60%-80% carries out wash-out to the Steviosides that is adsorbed on the polymeric adsorbent, and Steviosides is resolved from polymeric adsorbent, forms desorbed solution;
(7) desalination bleaching: allow desorbed solution by desalination resin and decolorizing resin, remove metal-salt and pigment in the desorbed solution;
(8) concentrate: allow the desorbed solution behind the desalination bleaching concentrate, make the concentration of concentrated solution reach spray-dired concentration requirement by nanofiltration membrane;
The concentrated solution that is by nanofiltration membrane not; By the penetrating fluid that is of nanofiltration membrane, reuse is as desorbed solution;
(9) spraying drying: concentrated solution is placed spray drying device, obtain the Steviosides product.
2. according to the method for the fresh stevioside leaf extraction of steviosides of the described usefulness of claim 1, it is characterized in that: fresh stevioside leaf is put into clarifixator with the water of 5-15 times of volume carry out the homogeneous fragmentation.
3. according to the method for the fresh stevioside leaf extraction of steviosides of the described usefulness of claim 1, it is characterized in that: flocculation agent is selected FeSO for use
47H
2O.
4. according to the method for the fresh stevioside leaf extraction of steviosides of the described usefulness of claim 1, it is characterized in that: it is the ultra-filtration membrane of 5000-10000 that ultra-filtration membrane described in the step (5) adopts molecular weight cut off, moves in the cross-flow mode.
5. according to the method for the fresh stevioside leaf extraction of steviosides of the described usefulness of claim 1, it is characterized in that: it is the nanofiltration membrane of 270-500 that nanofiltration membrane described in the step (8) adopts molecular weight cut off, moves in the cross-flow mode.
6. according to the method for the fresh stevioside leaf extraction of steviosides of the described usefulness of claim 1, it is characterized in that: the homogeneous disintegrating apparatus comprises clarifixator, hollander, colloidal mill.
7. according to the method for the fresh stevioside leaf extraction of steviosides of the described usefulness of claim 1, it is characterized in that: continuous automatic unloading material filter plant comprises sheet frame, continuous automatic unloading flitch frame pressure filter and continuous automatic unloading material whizzer.
8. according to the method for the fresh stevioside leaf extraction of steviosides of the described usefulness of claim 1, it is characterized in that: polymeric adsorbent, desalination resin, decolorizing resin are carried out manipulation of regeneration with acid solution and the alkali lye of 2%-4% respectively, and acid solution after the processing and alkali lye are respectively with utilizing again behind the membrane filtration again.
9. the method for the fresh stevioside leaf extraction of steviosides of described according to Claim 8 usefulness is characterized in that: it is the ultra-filtration membrane of 150-800 that membrane filtration adopts molecular weight cut off, moves in the cross-flow mode.
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| CN102351923A (en) * | 2011-08-25 | 2012-02-15 | 辽宁千千生物科技有限公司 | Method for extracting stevioside from whole-plant stevia |
| CN102702284A (en) * | 2012-05-23 | 2012-10-03 | 广西甙元植物制品有限公司 | Production process of high-purity sweet tea glycosides |
| CN102796152A (en) * | 2012-09-07 | 2012-11-28 | 谱赛科（江西）生物技术有限公司 | Method for preparing high-Reb-D-content stevioside |
| CN102816192A (en) * | 2012-08-13 | 2012-12-12 | 南通市常海食品添加剂有限公司 | Production technology of high-purity stevioside |
| CN102924544A (en) * | 2012-10-30 | 2013-02-13 | 晨光生物科技集团股份有限公司 | Method for preparing stevioside and chlorogenic acid from stevia step by step |
| CN103570777A (en) * | 2013-11-01 | 2014-02-12 | 湖南科源生物制品有限公司 | Extraction and purification method of stevioside RA |
| CN104163838A (en) * | 2014-04-26 | 2014-11-26 | 陈军 | Method for extracting RA and STV from sweet chrysanthemum leaves |
| WO2015126876A1 (en) | 2014-02-18 | 2015-08-27 | Mcneil Nutritionals, Llc. | Process for separation, isolation and characterization of steviol glycosides |
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| CN102702284A (en) * | 2012-05-23 | 2012-10-03 | 广西甙元植物制品有限公司 | Production process of high-purity sweet tea glycosides |
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