CN101717418B - Technology for separating stevioside in one step with simulated moving bed - Google Patents

Technology for separating stevioside in one step with simulated moving bed Download PDF

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CN101717418B
CN101717418B CN2009103111895A CN200910311189A CN101717418B CN 101717418 B CN101717418 B CN 101717418B CN 2009103111895 A CN2009103111895 A CN 2009103111895A CN 200910311189 A CN200910311189 A CN 200910311189A CN 101717418 B CN101717418 B CN 101717418B
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stevioside
rebaudioside
filtrate
water
flow velocity
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CN101717418A (en
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张丽萍
曹龙奎
冯兴元
李洪飞
张桂芳
王学群
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Heilongjiang Bayi Agricultural University
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AGRI-FOOD PROCESSING AND ENGINEERING TECHNOLOGY RESEARCH CENTER OF HEILONGJIANG PROVINCE
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Abstract

The invention relates to a technology for separating stevioside in one step with a simulated moving bed, comprising the following steps: soaking ground stevia leaves in water for 0.5-1h; guiding ultrasonic waves at the frequency of 90 into the solution; crudely filtering the solution and extracting filtrate; adding KAL(SO4) 2 and CaO to the filtrate to adjust the pH value to 7; standing the filtrate at 50-60 DEG C for 0.5-3.0h; removing the impurities in the filtrate and finely filtering the filtrate; and concentrating, adsorbing, separating and drying the filtrate to obtain stevioside powder. Water is rapidly extracted from the stevioside in the stevia leaves by non-toxic extractant with an ultrasonic extracting device, thus the water extracting time is shortened and the water extracting rate is improved. Crude extract of stevioside is purified and refined with the ion exchange equipment of the simulated moving bed, thus less regenerant is used, less energy is consumed, the recovery rate of the crude extract of stevioside can be about 90 percent and the purity of the crude extract of stevioside can be over 93 percent. The technology for separating stevioside in one step with the simulated moving bed can realize the continuous production and the industrialization easily.

Description

Technology for separating stevioside in one step with simulated moving bed
Technical field
What the present invention relates to is technology for separating stevioside in one step with simulated moving bed, specifically is to utilize supersonic method that the sweet Stevia leaf is extracted, by simulation moving-bed method of the rebaudioside in the crude extract being carried out separation and purification.
Background technology
Sweetleaf Chrysanthemum composite family Stevia per nnial herb, country of origin are in the subtropical zone, South America, and China in 1977 introduces cultivation and succeeds.Sweet Stevia contains 14 kinds of trace elements, 32 kinds of nutritive ingredients, so it is fabulous sugared source, is again good source of nutrition.The rebaudioside is the mixture of the diterpene glucoside that contains 8 kinds of compositions that extracts from the sweet Stevia leaf, according to the division of natural phant chemistry, belongs to the glucoside of tetracyclic diterpene, and it is subjected to people's favor gradually with characteristics such as high sugariness, low in calories, safety non-toxics.In the known 8 kinds of glucosides of stevioside, the content of various compositions, mouthfeel and sugariness have nothing in common with each other, and wherein the content of stevioside (St), content rebaudioside-A (RA), rebaudioside C (RC) is higher, accounts for more than 90% altogether.The RA sugariness is the highest, is equivalent to 450 times of sucrose, and sweet taste characteristic also is close with sucrose, is a kind of new type natural sweeting agent with high sugariness, dissolving low in calories, easy, characteristics such as heat-resisting, stable.Experiment showed, that the rebaudioside has no side effect, non-carcinogenesis, noresidue, safe and reliable, but illnesss such as often edible preventing hypertension, heart trouble, carious tooth are specially adapted to the health care of diabetic subject, phenyl ketonuria patient and obese people.The rebaudioside is that the present world finds, and through the approval of China Ministry of Health, Ministry of Light Industry use near the natural low caloric value sweeting agent of sucrose taste, be to continue to have exploitation to be worth and healthy natural sucrose substitute of praising highly outside sucrose and the beet sugar, be described as " third place in the world sucrose ".
Because good physiological property and the stability of rebaudioside is widely used in industries such as food, beverage, wine brewing, medicine, daily-use chemical industry as a kind of new food additive, not only extraction process reaches its maturity, and extraction yield also improves day by day.The method of extracting the rebaudioside at present from the sweet Stevia leaf mainly contains organic solvent extraction method and water extraction method, and wherein organic solvent extraction method solvent consumption is big, cost is high, practicality is not good enough.The hot water extraction is to use extracting method more widely at present, the general technology flow process of rebaudioside's water extraction is as follows in the industry: stevioside leaf → water logging (8~10h) → coarse filtration → precipitation removal of impurities → essence filter → purifying → decolouring → desalination → concentrate drying, wherein water logging extraction and purifying are the committed step of this technology, using extracting process more widely is 80 ℃ hot water extracted many times, the now resin absorption that adopt of the method for purifying are separated more, and the method for decolouring mainly contains two kinds of activated carbon decolorizing and resin decolorization.The shortcoming of this technology is that extraction time is long, the heat energy consumption height, and High Temperature High Pressure is to operation of equipment security requirement height, and continuity is relatively poor in purifying and the decolorization, and resin and reagent dosage are big simultaneously, and the resin utilization ratio is low, operates length consuming time.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art, developed a kind of ultrasonic wave of utilizing in conjunction with technology for separating stevioside in one step with simulated moving bed, and the rebaudioside is carried out purifying and decolouring by simulation moving-bed ion-exchange unit, shortened rebaudioside's extraction time, step simplifies the operation, reduce the production loss, and can serialization production, production efficiency promoted.
Technology for separating stevioside in one step with simulated moving bed of the present invention, realize as follows:
A, pulverizing: the sweet Stevia leaf is made fine debris;
B, water logging: will be dipped in through the sweet Stevia leaf fragment that a step makes and soak 0.5~1 hour in the water, feeding intake is 1: 15~30 by weight;
C, importing ultrasonic wave: impose ultrasonic wave in the solution of b step, frequency is 50~90khz, the material plant cell wall is broken, the composition stripping;
D, coarse filtration: will carry out 50~200 purpose filter clothes through the mixture of c step process and filter, and remove the defoliation slag;
E, precipitation: extract the d step and make filtrate, add the KAL (SO of leaching liquid weight percent 0.6~1.2% 4) 2With the CaO of leaching liquid weight percent 0.6~1.2%, adjust pH to 7 under the condition of 50~60 ℃ of temperature, left standstill 0.5-3.0 hour, removed impurity;
F, smart filter: the solution that the e step is made filters with the micron order filter, makes clarifying orange-yellow liquid;
G, concentrate: the filtrate that the f step is made contains rebaudioside 8~30% with rising membrane concentrator during rebaudioside's extracting solution is concentrated into every milliliter;
H, fractionation by adsorption: rebaudioside's seminal fluid that the g step is made separates purification continuously with simulation moving-bed again, promptly makes mass percent concentration 20~45%, purity 60~90% rebaudiosides' liquid;
J, concentrate drying: the h step being made rebaudioside's liquid concentrate, is to carry out spraying drying under 180~230 ℃ in temperature, promptly makes rebaudioside's powder.
During simulation moving-bed continuous adsorption of the present invention was separated, sorbent material was any among macroporous adsorbent resin AB-8, ADS-8, D-06, ADS-7 or the ADS-17; The parsing agent is 50%~70% ethanolic soln, and its consumption is 1~4 times of resin volume; Water wash zone is a deionized water; The resin absorption regenerated solvent is 2%~4% NaOH solution; Adsorption zone flow velocity 5~12BV/h; Desorption zone flow velocity 10~25BV/h; Water wash zone flow velocity 8~30BV/h; Breeding blanket flow velocity 4~10BV/h; Be 650~800s switching time; Temperature is controlled at 30~60 ℃; Pressure-controlling is 0.2MPa~1.0MPa.
The present invention adopts and simulation moving-bedly carries out continuous desalination, decolouring and fractionation by adsorption, and a step finish, do not need to establish in addition bleaching process and desalination operation.
The present invention extracts the rebaudioside in the stevioside leaf by supersonic method first, adopts simulation moving-bed continuous chromatography isolation technique single stage method to separate the purification rebaudioside, and purifying, desalination, decolouring are finished by a step operation.
Ultrasonic extraction also is called the ultrasonic wave auxiliary extraction, be the strong cavitation effect, disturbance effect, the high acceleration that utilize the ultrasonic wave radiation pressure to produce, smash and multistage effect such as stirring action, increase molecular motion of material frequency and speed, increase the solvent penetration power, thereby quicken target component and enter solvent, promote the carrying out of extracting.Ultrasonic extraction has thoroughly changed the extracting process of traditional poach alcohol precipitation, compares with the poach alcohol precipitation process, and ultrasonic extraction has following characteristics: normal temperature and pressure, safety are easily gone, omnidistance serialization operation, the production efficiency high energy consumption is low, reduces labor intensity, and the big cost of treatment capacity is low; Supersound extraction time ratio ordinary method has shortened 7~9h, and temperature reduces by 30 ℃~40 ℃, and yield improves 5%~30%; Dynamic countercurrent extracts solvent load and reduces 30%~50%, and yield improves 5%~20%; The automatic discharger of the dregs of a decoction: solved difficult problems such as dangerous in the dregs of a decoction dischargings, trouble, sealing; The dregs of a decoction are extracted, and liquid holdup reaches 50%, reduce wastage of material.
Absorption is a kind of important separation method in the chemical engineering, and it utilizes the difference of each component to be separated partition ratio between moving phase and stationary phase to separate.What adopt at adsorption technology development early stage main is fixed bed, carries out to penetrate the fairly simple like this intermittent mode of regeneration, and this mode is low to the utilization ratio of adsorbent capacity, and is difficult to obtain highly purified product.And solid adsorbent moves and the moving phase counter current contact under action of gravity from top to bottom in the moving-bed adsorption separation process, improved the efficient of process, but it is harsh that this operating method requires the sorbent material wear resistance, and the mobile back-mixing that increased of solid phase, making flows is difficult to keep the ideal plug flow.Simulated moving bed technology causes the relative countercurrent movement of stationary phase and moving phase by the import and export position of each burst of periodic variation moving phase logistics, solve the difficulty that moving bed process ran into dexterously, pushed adsorption technology to a wide development space.The characteristics of separating stevioside in one step with simulated moving bed are: use a kind of resin that original adsorption and desorption by resin, desalination, decolouring three-procedure are separated a step by simulated moving bed chromatography and finish; Resin is big to the pigment adsorptive capacity, high adsorption capacity, and it is more thorough to decolour; Resin utilization ratio height, usage quantity reduces 60%, and eluent saves 70%; But the continuous and automatic operation makes quality product guaranteed, and product purity can reach more than 90%, and yield can improve 1~5%; Labour intensity reduces, and production site significantly reduces; Running cost reduces greatly, has only 25%~40% of other technologies; Can accomplish three-waste free discharge in the whole technology, realize cleaning production.
Technology for separating stevioside in one step with simulated moving bed of the present invention carries out quick water extraction by ultrasonic extraction equipment to the rebaudioside in the sweet Stevia leaf, the extraction agent nontoxicity, shortened extraction time, improved extraction yield, by simulation moving-bed ion-exchange unit rebaudioside's crude extract is purified simultaneously and make with extra care, compare resin demand reduces with fixed bed, regenerant consumption reduces, energy consumption reduces, the rate of recovery is up to about 90%, purity also reaches more than 93%, can realize serialization production, is easy to industrialization.
Embodiment
Embodiment 1
Technology for separating stevioside in one step with simulated moving bed of the present invention is that starting material are realized through the following steps with the sweet Stevia leaf:
A, pulverizing: the sweet Stevia leaf is made fine debris;
B, water logging: will be dipped in through the sweet Stevia leaf fragment that a step makes and soak 0.5~1 hour in the water, feeding intake is 1: 15~30 by weight;
C, importing ultrasonic wave: impose ultrasonic wave in the solution of b step, frequency is 50~90khz, the material plant cell wall is broken, the composition stripping;
D, coarse filtration: will carry out 50~200 purpose filter clothes through the mixture of c step process and filter, and remove the defoliation slag;
E, precipitation: extract the d step and make filtrate, add the KAL (SO of leaching liquid weight percent 0.6~1.2% 4) 2With the CaO of leaching liquid weight percent 0.6-1.2%, add hydrochloric acid, adjust pH to 7 under the condition of 50~60 ℃ of temperature, left standstill 0.5~3.0 hour, removed impurity such as protein, organic acid, pigment, tannin;
F, smart filter: the solution that the e step is made filters with the micron order filter, makes clarifying orange-yellow liquid;
G, concentrate: the filtrate that the f step is made contains rebaudioside 8~30% with rising membrane concentrator during rebaudioside's extracting solution is concentrated into every milliliter;
H, fractionation by adsorption: rebaudioside's seminal fluid that the g step is made separates purification continuously with simulation moving-bed again, promptly makes mass percent concentration 20~45%, purity 60~90% rebaudiosides' liquid;
J, concentrate drying: the h step being made rebaudioside's liquid concentrate, is to carry out spraying drying under 180~230 ℃ in temperature, promptly makes rebaudioside's powder;
Wherein, the h step simulation moving-bed in sorbent material adopt any among macroporous adsorbent resin AB-8, ADS-8, D-06, ADS-7 or the ADS-17; The parsing agent is 50%~70% ethanolic soln, and its consumption is 1~4 times of resin volume; Water wash zone is a deionized water; The resin absorption regenerated solvent is 2%~4% NaOH solution;
Adsorption zone: flow velocity 5~12BV/h; Washing 1 district: flow velocity 8~30BV/h; Desorption zone: flow velocity 10~25BV/h; Breeding blanket: flow velocity 4~10BV/h; Washing 2 districts: flow velocity 8~30BV/h;
Be 650~800s switching time; Pressure-controlling is 0.2MPa~1.0MPa.
Embodiment 2
Technology for separating stevioside in one step with simulated moving bed of the present invention is that starting material are realized through the following steps with the sweet Stevia leaf:
A, pulverizing: the sweet Stevia leaf is made fine debris;
B, water logging: sweet Stevia leaf fragment 100 grams that a step of learning from else's experience makes are dipped in the 1500 gram water and soaked 0.5 hour;
C, importing ultrasonic wave: impose ultrasonic wave in the solution of b step, frequency is 50khz, the material plant cell wall is broken, the composition stripping;
D, coarse filtration: will carry out 50 purpose filter clothes through the mixture of c step process and filter, and remove the defoliation slag;
E, precipitation: extract the d step and make filtrate, add the KAL (SO of 9 grams 4) 2With the CaO of 9 grams, add hydrochloric acid, adjust pH to 7 under the condition of 50~60 ℃ of temperature, left standstill 0.5~3.0 hour, removed impurity such as protein, organic acid, pigment, tannin;
F, smart filter: the solution that the e step is made filters with the micron order filter, makes clarifying orange-yellow liquid;
G, concentrate: the filtrate that the f step is made contains rebaudioside 8~30% with rising membrane concentrator during rebaudioside's extracting solution is concentrated into every milliliter;
H, fractionation by adsorption: rebaudioside's seminal fluid that the g step is made separates purification continuously with simulation moving-bed again, promptly makes mass percent concentration 20~45%, purity 60~90% rebaudiosides' liquid;
J, concentrate drying: the h step being made rebaudioside's liquid concentrate, is to carry out spraying drying under 180~230 ℃ in temperature, promptly makes rebaudioside's powder;
Wherein, the simulation moving-bed middle sorbent material of h step is macroporous adsorbent resin AB-8; The parsing agent is 50%~70% ethanolic soln, and its consumption is 1 times of resin volume; Water wash zone is a deionized water; The resin absorption regenerated solvent is 2%~4% NaOH solution;
Adsorption zone: flow velocity 5BV/h; Washing 1 district: flow velocity 8BV/h; Desorption zone: flow velocity 10BV/h; Breeding blanket: flow velocity 4BV/h; Washing 2 districts: flow velocity 8BV/h;
Be 650s switching time; Pressure-controlling is 0.2MPa.
Embodiment 3
Technology for separating stevioside in one step with simulated moving bed of the present invention is that starting material are realized through the following steps with the sweet Stevia leaf:
A, pulverizing: the sweet Stevia leaf is made fine debris;
B, water logging: sweet Stevia leaf fragment that a step of learning from else's experience makes 100 grams are dipped in that 3000 grams soaked 1 hour in the water;
C, importing ultrasonic wave: impose ultrasonic wave in the solution of b step, frequency is 90khz, the material plant cell wall is broken, the composition stripping;
D, coarse filtration: will carry out 200 purpose filter clothes through the mixture of c step process and filter, and remove the defoliation slag;
E, precipitation: extract the d step and make filtrate, add the KAL (SO of 18 grams 4) 2With the CaO of 18 grams, add hydrochloric acid, adjust pH to 7 under the condition of 50~60 ℃ of temperature, left standstill 0.5~3.0 hour, removed impurity such as protein, organic acid, pigment, tannin;
F, smart filter: the solution that the e step is made filters with the micron order filter, makes clarifying orange-yellow liquid;
G, concentrate: the filtrate that the f step is made contains rebaudioside 8~30% with rising membrane concentrator during rebaudioside's extracting solution is concentrated into every milliliter;
H, fractionation by adsorption: rebaudioside's seminal fluid that the g step is made separates purification continuously with simulation moving-bed again, promptly makes mass percent concentration 20~45%, purity 60~90% rebaudiosides' liquid;
J, concentrate drying: the h step being made rebaudioside's liquid concentrate, is to carry out spraying drying under 180~230 ℃ in temperature, promptly makes rebaudioside's powder;
Wherein, the simulation moving-bed middle sorbent material of h step is macroporous adsorbent resin ADS-8; The parsing agent is 50%~70% ethanolic soln, and its consumption is 4 times of resin volume; Water wash zone is a deionized water; The resin absorption regenerated solvent is 2%~4% NaOH solution;
Adsorption zone: flow velocity 12BV/h; Washing 1 district: flow velocity 30BV/h; Desorption zone: flow velocity 25BV/h; Breeding blanket: flow velocity 10BV/h; Washing 2 districts: flow velocity 30BV/h;
Be 800s switching time; Pressure-controlling is 1.0MPa.
Embodiment 4
Rubble in the sweet Stevia cured leaf of buying is removed, the tiny fragment that cured leaf is ground into pulverizer, preserve in lucifuge, dry place, getting 100 gram sweet Stevia leaf fragments is dipped in the 2500 gram water and soaks after 0.8 hour, in solution, impose ultrasonic wave, ultrasonic frequency is 70khz, causes the material plant cell wall and breaks, the composition stripping; Remove the sweet Stevia residue with 100 purpose filter cloths again, in filtrate, add the KAL (SO of 25 grams again 4) 2With the CaO of 25 grams, add hydrochloric acid, adjust pH to 7 leaves standstill to precipitating fully, and the application flame filter press will precipitate thoroughly to be removed, and obtains clarifying orange-yellow liquid.Utilize again 1 μ m titanium rod further filter, with the filtrate that obtains with rising the seminal fluid that membrane concentrator contains rebaudioside 9% in being concentrated into every milliliter, rebaudioside's seminal fluid is carried out a step with simulation moving-bed or column chromatography separate purification, promptly make the liquid of mass percent concentration 20~45%, purity 60~90% steviosides; Carry out concentrate drying again, promptly make rebaudioside's powder.
Wherein, the simulation moving-bed middle sorbent material of h step is macroporous adsorbent resin D-06; The parsing agent is 50%~70% ethanolic soln, and its consumption is 3 times of resin volume; Water wash zone is a deionized water; The resin absorption regenerated solvent is 2%~4% NaOH solution;
Adsorption zone: flow velocity 10BV/h; Washing 1 district: flow velocity 25BV/h; Desorption zone: flow velocity 20BV/h; Breeding blanket: flow velocity 8BV/h; Washing 2 districts: flow velocity 28BV/h;
Be 750s switching time; Pressure-controlling is 0.8MPa.
Embodiment 5
Rubble in the sweet Stevia cured leaf of buying is removed, with pulverizer cured leaf is crushed to fine debris, preserve in lucifuge, dry place, getting 100 gram sweet Stevia leaf fragments is dipped in the 2000 gram water and soaks after 1 hour, impose ultrasonic wave in solution, ultrasonic frequency is 60khz, filters with 100 order filter clothes again, remove the sweet Stevia residue, in filtrate, add the KAL (SO of 16 grams again 4) 2With the CaO of 20 grams, add hydrochloric acid, adjust pH to 7 under the condition of 50 ℃ of temperature, leaves standstill 2h, removes solid impurity; Use flame filter press again and will precipitate thoroughly removal, obtain clarifying orange-yellow liquid.Utilize again titanium rod further filter, with the filtrate that obtains with rising the seminal fluid that membrane concentrator contains rebaudioside 9% in being concentrated into every milliliter, rebaudioside's seminal fluid is purified with simulation moving-bed carrying out continuous separation the in a step, promptly make mass percent concentration 20~45%, purity 60~90% rebaudiosides' liquid; Carry out concentrate drying again, promptly make rebaudioside's powder;
Wherein, the simulation moving-bed middle sorbent material of h step is macroporous adsorbent resin ADS-7; The parsing agent is 50%~70% ethanolic soln, and its consumption is 2 times of resin volume; Water wash zone is a deionized water; The resin absorption regenerated solvent is 2%~4% NaOH solution;
Adsorption zone: flow velocity 8BV/h; Washing 1 district: flow velocity 15BV/h; Desorption zone: flow velocity 15BV/h; Breeding blanket: flow velocity 6BV/h; Washing 2 districts: flow velocity 15BV/h.
Be 700s switching time; Pressure-controlling is 0.6MPa.
Core technology of the present invention is the application of simulation Slide in the separation and Extraction rebaudioside, except function with traditional analog moving-bed, it also has following characteristics: preparative column number, the preparative column mode of connection that can design compartment model, each district voluntarily, a plurality of opening for feeds and discharge port are arranged, change voluntarily according to arts demand fully.
Simulation moving-bed technical process described in the embodiment 1~5: absorption → washing → desorb → regeneration → washing.

Claims (3)

1. the method for separating stevioside in one step with simulated moving bed is that starting material are realized through the following steps with the sweet Stevia leaf:
A, pulverizing: the sweet Stevia leaf is made fine debris;
B, water logging: will be dipped in through the sweet Stevia leaf fragment that a step makes and soak 0.5~1 hour in the water, and feed intake by weight being 1:15~30;
C, importing ultrasonic wave: impose ultrasonic wave in the solution of b step, frequency is 50~90khz, causes the material plant cell wall and breaks, the composition stripping;
D, coarse filtration: will carry out 50~200 purpose filter clothes through the mixture of c step process and filter, and remove the defoliation slag;
E, precipitation: extract the d step and make filtrate, add the KAL(SO of leaching liquid weight percent 0.6~1.2% 4) 2With the CaO of leaching liquid weight percent 0.6~1.2%, adjust pH to 7 under the condition of 50~60 ℃ of temperature, left standstill 0.5-3.0 hour, removed impurity;
F, smart filter: the solution that the e step is made filters with the micron order filter, makes clarifying orange-yellow liquid;
G, concentrate: the filtrate that the f step is made contains rebaudioside 8~30% with rising membrane concentrator during rebaudioside's extracting solution is concentrated into every milliliter;
H, fractionation by adsorption: rebaudioside's seminal fluid that the g step is made separates purification continuously with simulation moving-bed again, promptly makes mass percent concentration 20~45%, purity 60~90% rebaudiosides' liquid;
J, concentrate drying: the h step being made rebaudioside's liquid concentrate, is to carry out spraying drying under 180~230 ℃ in temperature, promptly makes rebaudioside's powder.
2. the method for separating stevioside in one step with simulated moving bed as claimed in claim 1 is characterized in that simulation moving-bed continuous adsorption is separated in the h step, and sorbent material is a macroporous adsorbent resin; The parsing agent is 50%~70% ethanolic soln, and its consumption is 1~4 times of resin volume; Water wash zone is a deionized water; The resin absorption regenerated solvent is 2%~4% NaOH solution; Adsorption zone flow velocity 5~12BV/h; Desorption zone flow velocity 10~25BV/h; Water wash zone flow velocity 8~30BV/h; Breeding blanket flow velocity 4~10BV/h; Be 650~800s switching time; Temperature is controlled at 30~60 ℃; Pressure-controlling is 0.2MPa~1.0 MPa.
3. as the method for the described separating stevioside in one step with simulated moving bed of claim 2, it is characterized in that macroporous adsorbent resin is any among AB-8, ADS-8, D-06, ADS-7 or the ADS-17.
CN2009103111895A 2009-12-10 2009-12-10 Technology for separating stevioside in one step with simulated moving bed Expired - Fee Related CN101717418B (en)

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