CN101817854A - Method for preparing high-RA stevioside by utilizing macroporous resin - Google Patents
Method for preparing high-RA stevioside by utilizing macroporous resin Download PDFInfo
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- CN101817854A CN101817854A CN201010142785A CN201010142785A CN101817854A CN 101817854 A CN101817854 A CN 101817854A CN 201010142785 A CN201010142785 A CN 201010142785A CN 201010142785 A CN201010142785 A CN 201010142785A CN 101817854 A CN101817854 A CN 101817854A
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- macroporous resin
- stevioside
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Abstract
The invention discloses a method for preparing high-RA stevioside by utilizing macroporous resin, and the preparation method is as follows: injecting water into a steeping tank, pouring stevia rebaudiana into the steeping tank under stirring, extracting at constant temperature, filtering obtained extract liquid for obtaining filtrate, and then injecting the filtrate into a tank filled with the macroporous resin for absorption; injecting effluent sugar solution into a concentration tower for concentration, injecting concentrate into a mixed solvent tank according to the volume ratio when the concentration of the concentrate is more than 46%, and fully stirring solution after mixing; then carrying out vacuum filtration, injecting the filtrate into an alcohol recovery tower, separating mixed solvent in the sugar solution, then flowing by a spray tower, and carrying out spray drying for forming powder; and obtaining the stevioside with the RA content of above 90%. The method can not only effectively separate STV glucoside (or ST glucoside) in the stevioside, but also solve the problems that the technological process of producing the high-quality stevioside needs to carry out desalination and discoloration at one time, thereby saving auxiliary materials and improving yield.
Description
Technical field
The present invention relates to a kind of separation method of liquid mixture, specifically a kind of method of utilizing macroporous resin to prepare high-RA stevioside.
Background technology
Stevioside is the smart new type natural sweeting agent of carrying from catananche's Folium Chrysanthemi.It has the characteristics of high sugariness, low heat energy, and its sugariness is 200～300 times of sucrose, and calorific value only is 1/300 of a sucrose.Experiment showed, that through high amount of drug stevioside has no side effect, no carcinogens, edible safety, but illnesss such as often edible preventing hypertension, diabetes, obesity, heart trouble, carious tooth are very ideal sweeting agents of a kind of alternative sucrose.It is made up of 8 kinds of known glucosides, and wherein, Steviosides (STV), content rebaudioside-A (RA), the content of rebaudioside C (RC) in total reducing sugar are higher, also are the main effective constituent that influences its sweet taste.The sugariness of STV is 270～280 times of sucrose, but that it is flavor speed is slow, has certain unpleasant odor; The sugariness of RC is less than 50 times of sucrose, and stronger back bitter taste and unpleasant odor are arranged; And the stevia sugar RA sugariness to be 300 times of sucrose and flavor matter more approach sucrose, and the pure and fresh no bitter taste of mouthfeel is a kind of ideal natural sweeteners, and is therefore higher to the demand of high-content RA product both at home and abroad.
The method of the present high-end stevioside of domestic production, what generally adopt all is recrystallization method, and this processing method operational path is long, and not only producing large amount of sewage influences environment, and stevioside rate of loss height, and cost of labor is big.
Summary of the invention
Technical assignment of the present invention provides a kind of method of utilizing macroporous resin to prepare high-RA stevioside.
Technical assignment of the present invention is realized in the following manner, this preparation method's process is as follows: will inject water in the steeping tank, be warming up to 40～45 ℃, under this temperature, while stirring Folium Chrysanthemi is poured in the steeping tank, extracting at constant temperature 40～50 minutes, the gained vat liquor by flame filter press filter filtered liquid, filtered liquid is under the pressure of 0.5～1.0MPa, squeeze in the jar that macroporous resin is housed and adsorb, when last volume that exports effusive liquid glucose is 2.5～3 times of the resin volume of adorning when resin container, close outlet valve; Effusive liquid glucose is squeezed into upgrading tower to be concentrated, when the concentration of concentrated solution reaches 46% when above, by volume concentrated solution is squeezed in the mixed solvent jar, mixed solution is warming up to 75～80 ℃, fully stirred 50～60 minutes with the speed of 120～150r/min; Add then and carry out vacuum filtration in the vacuum filtration equipment, filtrate is squeezed into alcohol distillation column, isolate the mixed solvent in the liquid glucose, the spray tower of flowing through then sprays the dried powder that becomes; Can get RA content at the Steviosides more than 90%.
The described gross weight ratio that soaks used Folium Chrysanthemi and water is 1: 10～12.
It is described that to carry out the blended solvent with concentrated solution in the mixed solvent jar be ethanol and methanol mixed solvent.
Described vacuum filtration equipment is the vacuum filtration extrusion machine.
Described macroporous resin is synthetic with following method: in producing jar with 15～20 kilograms of industrial toluene and divinylbenzenes, 1～3 kilogram of methyl methacrylate, 4～5 kilograms of benzoyl peroxides, uniform mixing, add the mixing pore-creating agent alkylbenzene and the whiteruss of 40～60 kilograms of gross weights, wherein the weight ratio of alkylbenzene and paraffin is 4～6: 1; Add the NaCl aqueous solution then, make water oil phase volume ratio be controlled at 4～4.5: 1, and to add the quality percentage composition be that 0.6% Sodium dodecylbenzene sulfonate is as tensio-active agent, start stirring, the control stirring velocity is distributed between 200～250 orders bead particle diameter, speed with 6 ℃/10min at the uniform velocity slowly is warming up to 90 ℃, isothermal reaction 2 hours continues to be warming up to 95 ℃, and isothermal reaction is 2 hours again; Be warming up to 98 ℃ at last and boiled ball 2 hours, make polymerization complete; Gained resin water thorough washing is used ethanol, each extracting of sherwood oil 8 hours respectively after drying, drying under reduced pressure is standby under the room temperature; Got final product with pure water is clean then in 2 hours with 90～95% alcohol immersion before using.
The technical indicator of table 1 macroporous resin
| Project | Technical indicator |
| Water content (%) | ??70％ |
| Specific surface area (m 2/g) | ??≥550 |
| Pore volume: (cm 3/g) | ??1.4～2.2 |
| Mean pore size: (nm) | ??9～12 |
| Polarity | Low-pole |
The invention has the beneficial effects as follows: (1) has carried out reasonable control to the part by weight of Folium Chrysanthemi and water and the temperature of water, not only water saving, and stevioside leaching yield height, and alleviated a macroporous resin absorption pressure and the big difficult problem of quantity of wastewater effluent.(2) utilize macroporous adsorbent resin the stevioside composition to be carried out the principle of selective adsorption: there is the certain selectivity effect in the adsorption molecule of opposed polarity in the process that adsorbent surface is adsorbed, compare with RA, stevioside STV has lacked a hydrophilic grape glucosyl at 13 carbon, therefore its polar phase is to less than the RA glucoside, solubleness in water is also a little less than RA, according to the close principle of polarity, the low-pole resin is higher than RA to the adsorption rate of STV.And, RA in the solution and STV molecule are in close adsorbent surface, and the absorption that also may take place to a certain degree by the polarity selective action between the adsorbate that has been adsorbed is adsorbed with exchange, the absorption exchange interaction may take place with the high polar RA that has been adsorbed in the less STV of free polarity in the ie in solution, STV is adsorbed and RA is free, thereby further improved selectivity, cause spray to do the resulting Steviosides RA content in back and reached more than 90%, satisfied the demand of users at home and abroad high-quality stevioside.(3) owing to adopted vacuum filtration technology and new resin Technology, directly save operations such as flocculation sediment, filtration, decolouring, press filtration, shortened processing link, reduced sugared rate of loss, saved auxiliary material and artificial.
Embodiment
Embodiment 1:
1) 16 kilograms (the two mass ratio is a toluene: divinylbenzene=1: 8) with industrial toluene and divinylbenzene in producing jar, 1 kilogram of methyl methacrylate, 4 kilograms of benzoyl peroxides, uniform mixing, add the mixing pore-creating agent alkylbenzene and the whiteruss of 40 kilograms of gross weights, wherein the weight ratio of alkylbenzene and paraffin is 4: 1; Add the NaCl aqueous solution then, water oil phase volume ratio was controlled at 4: 1, and to add the quality percentage composition be that 0.6% Sodium dodecylbenzene sulfonate is as tensio-active agent, start stirring, the control stirring velocity is distributed between 200～250 orders bead particle diameter, speed with 6 ℃/10min at the uniform velocity slowly is warming up to 90 ℃, isothermal reaction 2 hours continues to be warming up to 95 ℃, isothermal reaction 2 hours; Be warming up to 98 ℃ at last and boiled ball 2 hours, make polymerization complete; Gained macroporous resin water thorough washing is used ethanol, each extracting of sherwood oil 8 hours respectively after drying, drying under reduced pressure is standby under the room temperature.Got final product with pure water is clean then in 2 hours with 90% alcohol immersion before using.
2) with injecting tap water 1000L in the steeping tank, be warming up to 40 ℃, under this temperature, with RA content be 55% while stirring, yield is that 400 kilograms of Folium Chrysanthemis of 10% are poured in the jar extracting at constant temperature 40 minutes into.The mode lixiviate is 4 times successively, and gained 4000L vat liquor filters by flame filter press;
3) with above-mentioned 4000L filtered liquid liquid, under the pressure of 0.7MPa, with filtered liquid squeeze into be equipped with macroporous resin the jar in adsorb.Flowing out liquid glucose with last outlet of resin container begins to calculate, when the volume of effusive liquid glucose is 2.5 times of the macroporous resin volume of adorning, close outlet valve, effluent liquid is squeezed into upgrading tower steam part moisture in the liquid glucose, when concentration reaches 46%, 1: 1 by volume, concentrated solution is squeezed in the jar that holds 49.35L ethanol～methanol mixed solvent, mixed solvent is warming up to 75 ℃, fully stirred 55 minutes with the speed of 140r/min, back vacuum filtration extrusion machine suction filtration, filtrate is squeezed into alcohol distillation column, isolate ethanol and methanol mixed solvent in the liquid glucose, the spray tower of flowing through then, spray the dried powder that becomes, can get RA content 20.5 kilograms of 92% Steviosidess; Suction filtration gained filter cake (high STV content Steviosides crystal) is squeezed in the desorbed solution of handling macroporous resin for 2.2 kilograms.
4) macroporous resin that has adsorbed the stevia rebaudianum liquid glucose is resolved with 70% ethanol, the desorbed solution positively charged ion is returned macroporous resin carry out desalination, then, with desorbed solution distillation, concentrate, decolouring, filter, 18.2 kilograms of Steviosidess that spray can get high STV content after doing.The high-RA stevioside rate of recovery is 51.25%, and the Steviosides total yield is 96.75%.
Embodiment 2:
1) 18 kilograms (the two mass ratio is a toluene: divinylbenzene=1: 9) with industrial toluene and divinylbenzene in producing jar, 1.6 kilograms of methyl methacrylates, 4.4 kilograms of benzoyl peroxides, uniform mixing, add the mixing pore-creating agent alkylbenzene and the whiteruss of gross weight 50 grams, wherein the weight ratio of alkylbenzene and paraffin is 4.5: 1; Add the NaCl aqueous solution then, water oil phase volume ratio was controlled at 4.2: 1, and to add the quality percentage composition be that 0.6% Sodium dodecylbenzene sulfonate is as tensio-active agent, start stirring, the control stirring velocity is distributed between the 200-250 order bead particle diameter, speed with 6 ℃/10min at the uniform velocity slowly is warming up to 90 ℃, isothermal reaction 2 hours continues to be warming up to 95 ℃, isothermal reaction 2 hours; Be warming up to 98 ℃ at last and boiled ball 2 hours, make polymerization complete; Gained macroporous resin water thorough washing is used ethanol, each extracting of sherwood oil 8 hours respectively after drying, drying under reduced pressure is standby under the room temperature.Got final product with pure water is clean then in 2 hours with the 90-95% alcohol immersion before using.
2) with injecting tap water 1200L in the steeping tank, be warming up to 45 ℃, under this temperature, with RA content be 52% while stirring, yield is that 400 kilograms of Folium Chrysanthemis of 10% are poured in the jar extracting at constant temperature 50 minutes into.The mode lixiviate is 4 times according to this.Gained 4800L vat liquor filters by flame filter press.
3) with above-mentioned 4800L filtered liquid liquid, under the pressure of 0.8MPa, with filtered liquid squeeze into be equipped with macroporous resin the jar in adsorb.Flowing out liquid glucose with last outlet of resin container begins to calculate, when the volume of liquid glucose is 3 times of the macroporous resin volume of adorning, close outlet valve, effluent liquid is squeezed into upgrading tower steam part moisture in the liquid glucose, when concentration reaches 47%, 1: 1.5 by volume, concentrated solution is squeezed in the jar that holds 69.89L ethanol～methanol mixed solvent, mixed solvent is warming up to 80 ℃, fully stirred 60 minutes with the speed of 130r/min, back vacuum filtration extrusion machine suction filtration, filtrate is squeezed into alcohol distillation column, isolate ethanol and methanol mixed solvent in the liquid glucose, the spray tower of flowing through then, spray the dried powder that becomes, can get RA content 19.3 kilograms of 90% Steviosidess; Suction filtration gained filter cake (high STV content Steviosides crystal) is squeezed in the desorbed solution of handling macroporous resin for 2.7 kilograms.
4) macroporous resin that has adsorbed the stevia rebaudianum liquid glucose is resolved with 70% ethanol, the desorbed solution positively charged ion is returned macroporous resin carry out desalination, then, with desorbed solution distillation, concentrate, decolouring, filter, 19.1 kilograms of Steviosidess that spray can get high STV content after doing.The high-RA stevioside rate of recovery is 48%, and the Steviosides total yield is 96%.
Embodiment 3:
1) 20 kilograms (the two mass ratio is a toluene: divinylbenzene=1: 10) with industrial toluene and divinylbenzene in producing jar, 3 kilograms of methyl methacrylates, 5 kilograms of benzoyl peroxides, uniform mixing, add the mixing pore-creating agent alkylbenzene and the whiteruss of gross weight 60 grams, wherein the weight ratio of alkylbenzene and paraffin is 6: 1; Add the NaCl aqueous solution then, water oil phase volume ratio was controlled at 4.5: 1, and to add the quality percentage composition be that 0.6% Sodium dodecylbenzene sulfonate is as tensio-active agent, start stirring, the control stirring velocity is distributed between the 200-250 order bead particle diameter, speed with 6 ℃/10min at the uniform velocity slowly is warming up to 90 ℃, isothermal reaction 2 hours continues to be warming up to 95 ℃, isothermal reaction 2 hours; Be warming up to 98 ℃ at last and boiled ball 2 hours, make polymerization complete; Gained macroporous resin water thorough washing is used ethanol, each extracting of sherwood oil 8 hours respectively after drying, drying under reduced pressure is standby under the room temperature.Got final product with pure water is clean then in 2 hours with the 90-95% alcohol immersion before using.
2) with injecting tap water 1000L in the steeping tank, be warming up to 42 ℃, under this temperature, with RA content be 55% while stirring, yield is that 400 kilograms of Folium Chrysanthemis of 10% are poured in the jar extracting at constant temperature 45 minutes into.The mode lixiviate is 4 times successively, and gained 4000L vat liquor filters by flame filter press;
3) with above-mentioned 4000L filtered liquid liquid, under the pressure of 1.0MPa, with filtered liquid squeeze into be equipped with macroporous resin the jar in adsorb.Flowing out liquid glucose with last outlet of resin container begins to calculate, when the volume of effusive liquid glucose is 2.8 times of the macroporous resin volume of adorning, close outlet valve, effluent liquid is squeezed into upgrading tower steam part moisture in the liquid glucose, when concentration reaches 46%, 1: 1.2 by volume, concentrated solution is squeezed in the jar that holds 55.911 ethanol～methanol mixed solvent, mixed solvent is warming up to 77 ℃, fully stirred 50 minutes with the speed of 150r/min, back vacuum filtration extrusion machine suction filtration, filtrate is squeezed into alcohol distillation column, isolate ethanol and methanol mixed solvent in the liquid glucose, the spray tower of flowing through then, spray the dried powder that becomes, can get RA content 19.5 kilograms of 91% Steviosidess; Suction filtration gained filter cake (high STV content Steviosides) is squeezed in the desorbed solution of handling macroporous resin for 2.1 kilograms.
4) macroporous resin that has adsorbed the stevia rebaudianum liquid glucose is resolved with 70% ethanol, the desorbed solution positively charged ion is returned macroporous resin carry out desalination, then, with desorbed solution distillation, concentrate, decolouring, filter, 18.0 kilograms of Steviosidess that spray can get high STV content after doing.The high-RA stevioside rate of recovery is 48.7%, and the Steviosides total yield is 93.75%.
Claims (5)
1. utilize macroporous resin to prepare the method for high-RA stevioside, it is characterized in that the preparation method is as follows: water will be injected in the steeping tank, be warming up to 40～45 ℃, under this temperature, while stirring Folium Chrysanthemi is poured in the steeping tank, extracting at constant temperature 40～50 minutes, the gained vat liquor by flame filter press filter filtered liquid, filtered liquid is under the pressure of 0.5～1.0MPa, squeeze in the jar that macroporous resin is housed and adsorb, when last volume that exports effusive liquid glucose is 2.5～3 times of the resin volume of adorning when resin container, close outlet valve; Effusive liquid glucose is squeezed into upgrading tower to be concentrated, when the concentration of concentrated solution reaches 46% when above, by volume concentrated solution is squeezed in the mixed solvent jar, mixed solution is warming up to 75～80 ℃, fully stirred 50～60 minutes with the speed of 120～150r/min; Add then and carry out vacuum filtration in the vacuum filtration equipment, filtrate is squeezed into alcohol distillation column, isolate the mixed solvent in the liquid glucose, the spray tower of flowing through then sprays the dried powder that becomes; Can get RA content at the Steviosides more than 90%.
2. the method for utilizing macroporous resin to prepare high-RA stevioside according to claim 1 is characterized in that the described gross weight ratio that soaks used Folium Chrysanthemi and water is 1: 10～12.
3. the method for utilizing macroporous resin to prepare high-RA stevioside according to claim 1 is characterized in that described to carry out the blended solvent with concentrated solution in the mixed solvent jar be ethanol and methanol mixed solvent.
4. the method for utilizing macroporous resin to prepare high-RA stevioside according to claim 1 is characterized in that described vacuum filtration equipment is the vacuum filtration extrusion machine.
5. the method for utilizing macroporous resin to prepare high-RA stevioside according to claim 1, it is characterized in that described macroporous resin is synthetic with following method: in producing jar with 15～20 kilograms of industrial toluene and divinylbenzenes, 1～3 kilogram of methyl methacrylate, 4～5 kilograms of benzoyl peroxides, uniform mixing, add the mixing pore-creating agent alkylbenzene and the whiteruss of 40～60 kilograms of gross weights, wherein the weight ratio of alkylbenzene and paraffin is 4～6: 1; Add the NaCl aqueous solution then, make water oil phase volume ratio be controlled at 4～4.5: 1, and to add the quality percentage composition be that 0.6% Sodium dodecylbenzene sulfonate is as tensio-active agent, start stirring, the control stirring velocity is distributed between 200～250 orders bead particle diameter, speed with 6 ℃/10min at the uniform velocity slowly is warming up to 90 ℃, isothermal reaction 2 hours continues to be warming up to 95 ℃, and isothermal reaction is 2 hours again; Be warming up to 98 ℃ at last and boiled ball 2 hours, make polymerization complete; Gained resin water thorough washing is used ethanol, each extracting of sherwood oil 8 hours respectively after drying, drying under reduced pressure is standby under the room temperature; Got final product with pure water is clean then in 2 hours with 90～95% alcohol immersion before using.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093447A (en) * | 2010-12-30 | 2011-06-15 | 青岛润浩甜菊糖高科有限公司 | Purifying method of stevioside RB |
| CN103319550A (en) * | 2013-07-12 | 2013-09-25 | 兰州理工大学 | Method for separating and purifying stevioside in crude stevia rebaudiana |
| CN103951779A (en) * | 2014-05-13 | 2014-07-30 | 安徽三星树脂科技有限公司 | Preparation method of medium polar macroporous adsorption resin |
| CN104262428A (en) * | 2014-10-17 | 2015-01-07 | 南通海天生物科技有限公司 | Method for extracting and separating rebaudioside-A from stevia rebaudian leaves |
| CN110523440A (en) * | 2019-08-28 | 2019-12-03 | 华南理工大学 | A kind of desalination method of purification of water-solubility chitosan derivative |
-
2010
- 2010-04-09 CN CN201010142785A patent/CN101817854A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093447A (en) * | 2010-12-30 | 2011-06-15 | 青岛润浩甜菊糖高科有限公司 | Purifying method of stevioside RB |
| CN102093447B (en) * | 2010-12-30 | 2015-04-08 | 青岛润浩甜菊糖高科有限公司 | Purifying method of stevioside RB |
| CN103319550A (en) * | 2013-07-12 | 2013-09-25 | 兰州理工大学 | Method for separating and purifying stevioside in crude stevia rebaudiana |
| CN103319550B (en) * | 2013-07-12 | 2016-06-29 | 兰州理工大学 | The isolation and purification method of stevioside in Folium Stevlae Rebaudianae crude product |
| CN103951779A (en) * | 2014-05-13 | 2014-07-30 | 安徽三星树脂科技有限公司 | Preparation method of medium polar macroporous adsorption resin |
| CN104262428A (en) * | 2014-10-17 | 2015-01-07 | 南通海天生物科技有限公司 | Method for extracting and separating rebaudioside-A from stevia rebaudian leaves |
| CN110523440A (en) * | 2019-08-28 | 2019-12-03 | 华南理工大学 | A kind of desalination method of purification of water-solubility chitosan derivative |
| CN110523440B (en) * | 2019-08-28 | 2022-04-22 | 华南理工大学 | Desalination purification method of water-soluble chitosan derivative |
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Application publication date: 20100901 |