CN101177716A - Method for separating and purifying glucose, fructose and oligomeric polysaccharide from high fructose syrup - Google Patents
Method for separating and purifying glucose, fructose and oligomeric polysaccharide from high fructose syrup Download PDFInfo
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- CN101177716A CN101177716A CNA2007101912546A CN200710191254A CN101177716A CN 101177716 A CN101177716 A CN 101177716A CN A2007101912546 A CNA2007101912546 A CN A2007101912546A CN 200710191254 A CN200710191254 A CN 200710191254A CN 101177716 A CN101177716 A CN 101177716A
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- fructose
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- oligomeric polysaccharide
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Abstract
The invention discloses a separation and purification method for glucose, fructose and oligomeric polysaccharide from fructose syrup, pertaining to the chromatogram-separation technical field of a simulated moving bed. By synthesizing special resin and utilizing the simulated moving bed technique, the glucose, the fructose and the oligomeric polysaccharide with high purity are separated from the fructose syrup. The invention has preparation method that: first, chelating resin with an acid calcium type is synthesized for specially adsorbing and separating the glucose, the fructose and the oligomeric polysaccharide; the fructose syrup is used as the material and a fixed bed provided with the chelating resin with the acid calcium type is adopted, by adopting the simulated moving bed technique and using water as eluent under the temperature of 60 to 80 DEG C, the glucose, the fructose and the oligomeric polysaccharide are completely separated, and three components which richly contain the glucose, the fructose and the oligomeric polysaccharide are respectively obtained.
Description
Technical field
The present invention relates to from high fructose syrup, separate the method for purify glucose, fructose and oligomeric polysaccharide, specifically, it relates to the ingenious resin dedicated technology of separating preparation high purity glucose, fructose and oligomeric polysaccharide with the simulated moving bed chromatography technology from high fructose syrup of utilizing, and belongs to the simulated moving bed chromatography separation technology field.
Background technology
It is raw material that W-Gum is generally adopted in the manufacturing of fructose, obtains containing fructose 42%, glucose 53%, oligose 5%, and concentration is 70% high fructose syrup.All high fructose syrups all are the industry chromatography techniques that adopts based on separating glucose and fructose two components at present.Because can not the coverlet exclusive effect of oligomeric polysaccharide is separated, so major part all focuses in the glucose component and discharges together, and glucose content is wherein reduced, and generally only reaches about 92%.Therefore influenced the deep application of isolating the glucose component, as producing xylo-oligosaccharide etc.; And oligomeric polysaccharide is the main component of nutrition dietary fiber, can directly use as health care for the aged and diet food, have good using value and market outlook.
Summary of the invention
The object of the present invention is to provide a kind of method of from high fructose syrup, separating purify glucose, fructose and oligomeric polysaccharide, adopt the high efficiency chromatography separation method, to obtain high-quality glucose, fructose and oligomeric polysaccharide product.
Technical scheme of the present invention: a kind of method of from high fructose syrup, separating purify glucose, fructose and oligomeric polysaccharide: a, synthetic resins: the synthetic earlier acid calcium type resin that is used for special fractionation by adsorption glucose, fructose and oligomeric polysaccharide; B, separation are purified: adopt the fixed bed that above-mentioned acid calcium type resin is housed to use simulated moving bed technology, separate purification from high fructose syrup, obtain purified glucose, fructose and oligomeric polysaccharide product solution;
A, synthetic resins:
Acid calcium type resin with acid macroporous resin as carrier, with calcium metal ion on its chelating, utilize the avidity between water-soluble macromolecule metal absorbent and the metal ion, on acid macroporous resin surface, and use linking agent to be fixed on the matrix resin adsorbents adsorb; Used linking agent is 6%~9% of an acid macroporous resin weight;
Metal Ca
2+The ionic type of service is can the corresponding Ca of dissolved under neutrality or alkaline condition
2+Ionic salt or oxide compound, metal Ca
2+The ionic amount is so that the resin chelating reaches 30% saturated amount~complete saturated amount;
B, separation are purified: adopt the fixed bed that above-mentioned acid calcium type resin is housed, use simulated moving bed technology, simulation moving-bed device is to be connected in series by the chromatographic column more than 4 or 4, becomes a loop system that connects from beginning to end; Every post all has discharge port, opening for feed, circulation port, water-in; Whole simulated moving bed chromatography system chuck heat tracing guarantees that bed is between the setting steady temperature; Whole simulated moving bed chromatography system adopts the computer auto-control mode to change the position of discharge port, opening for feed, circulation port, water-in, thereby realizes charging, water inlet, preceding component discharging, the simultaneously continuous operation of back component discharging;
Simulated moving bed chromatography is separated the position according to charging and discharging mouth and circulation port, and all placed in-line chromatographic columns are divided into 5 districts in the system:
The I district: fructose liquid exports to the high fructose syrup opening for feed, is called oligomeric polysaccharide and extracts the district;
The II district: the high fructose syrup opening for feed is called glucose and extracts the district to the Glucose Liquid outlet;
The III district: Glucose Liquid exports to the outlet of oligomeric polysaccharide liquid, is called and resolves the district;
The IV district: oligomeric polysaccharide liquid exports to the eluting water import, is called the fructose enrichment region;
The V district: the eluting water import is called the race way to the outlet of fructose liquid;
Adopting above-mentioned acid calcium type resin in the moving bed imitation chromatogram separation facility is the stationary phase sorbent material, utilizes the avidity difference between macromole metal absorbent and the various sugar alcohol, realizes the separation fully between glucose, fructose and the oligomeric polysaccharide; Employing water is eluent, and separation temperature is 35 ℃~95 ℃, carries out charging, discharging operation continuously, obtains three class discharging components simultaneously, the first kind be glucose purity>95% be rich in the glucose component; Second class be fructose purity>91% be rich in the fructose component; The 3rd class be oligomeric polysaccharide purity>74% be rich in the oligomeric polysaccharide component.
Macroporous resin is acid polystyrene macroporous resin or polymethylmethacrylate class macroporous resin; Linking agent is the polyene-based linking agent: divinylbenzene, triethylene benzene or two propylene benzene.
High fructose syrup directly enters simulation moving-bed separation, obtains glucose, fructose and oligomeric polysaccharide product solution.
Preferred separation temperature is 60 ℃~80 ℃.
The content (W/W) of the used linking agent of this resin in resin is 2%~40%, and the best is 6%~9%.
The resin of the present invention's preparation has higher physical stability than general commercial resin, and mill back rate of small round spheres>99% is applicable to 90 ℃ of left and right sides prolonged operation temperature.This resin has very high resolution to glucose, fructose and oligomeric polysaccharide, generally can reach 20% high concentration glucose liquid, fructose liquid and oligomeric polysaccharide liquid.
Beneficial effect of the present invention: the simulated moving bed chromatography technology that the present invention proposes a kind of pollution-free separation purify glucose, fructose and oligomeric polysaccharide product.High fructose syrup directly enters simulation moving-bed separation,
Obtain glucose, fructose and oligomeric polysaccharide product solution.
The outstanding advantage that has is as follows: 1. glucose, fructose and oligomeric polysaccharide have fabulous adsorption separation performance on this acid calcium type resin, realize the separation fully between glucose, fructose and the oligomeric polysaccharide substantially; 2. adopt the moving-bed continuous chromatography to separate; Resin utilization ratio height; 3. production process full-automation, labour intensity is low, and production site is little; 4. production cost is low, separates every cubic metre of high fructose syrup alcohol liquid, only needs 2 cubic metres~4 cubic metres water and a small amount of; 5. do not use any chemical in the production process, produce without any polluting.
Description of drawings
Fig. 1 high fructose syrup separates the purification preparation technique schema.
The zone chart of Fig. 2 chromatographic column.
Embodiment
Embodiment 1: synthetic resins: the synthetic earlier acid calcium type resin that is used for special fractionation by adsorption glucose, fructose and oligomeric polysaccharide;
Acid calcium type resin with acid macro porous crosslinking resin as carrier, with metal Ca on its chelating
2+Ion utilizes the avidity between water-soluble macromolecule metal absorbent and the metal ion, on acid macroporous resin surface, and uses linking agent to be fixed on the matrix resin adsorbents adsorb; Metal Ca
2+The ionic type of service is can the corresponding Ca of dissolved under neutrality or alkaline condition
2+Ionic salt or oxide compound, metal Ca
2+The ionic amount is so that the resin chelating reaches 30% saturated amount~complete saturated amount;
Utilize various sugar alcohols and metal Ca
2+Avidity between the ion is adsorbed on resin surface with various sugar alcohols.Macroporous resin is acid polystyrene macroporous resin or polymethylmethacrylate class macroporous resin; Linking agent is the polyene-based linking agent, as divinylbenzene or triethylene benzene or two propylene benzene etc.The content of used linking agent in acid macroporous resin is 2%~40%, and the best is 6%~9%.
Embodiment 2: separate and purify: high fructose syrup directly enters simulation moving-bed separation, obtains glucose, fructose and oligomeric polysaccharide product solution.
Simulated moving bed technology: adopting above-mentioned acid calcium type resin in the moving bed imitation chromatogram separation facility is the stationary phase sorbent material, utilize the avidity difference between macromole metal absorbent and the various sugar alcohol, realize the separation fully between glucose, fructose and the oligomeric polysaccharide; Employing water is eluent, and separation temperature is 35 ℃~95 ℃, and the optimal separation temperature is 60 ℃~80 ℃, carries out charging, discharging operation continuously, obtains three class discharging components simultaneously, and the first kind is for being rich in the component of glucose (glucose purity>95%); Second class is for being rich in the component of fructose (fructose purity>91%); The 3rd class is for being rich in the component of oligomeric polysaccharide (oligomeric polysaccharide purity>74%).
High fructose syrup directly enters simulation moving-bed separation, obtains glucose, fructose and oligomeric polysaccharide product solution.
Simulation moving-bedly be connected in series the loop system that becomes head and the tail to connect by the chromatographic column more than 4 or 4; Every root chromatogram column all has discharge port, opening for feed, circulation port, water-in; Adopt the computer auto-control mode to change the position of discharge port, opening for feed, circulation port, water-in, thereby realize charging, water inlet, preceding component discharging, the simultaneously continuous operation of back component discharging.
According to the position of feed inlet and outlet and circulation port, all placed in-line chromatographic columns are divided into 5 districts in the system:
The I district: fructose liquid exports to the high fructose syrup opening for feed, is called oligomeric polysaccharide and extracts the district.
The II district: the high fructose syrup opening for feed is called glucose and extracts the district to the Glucose Liquid outlet.
The III district: Glucose Liquid exports to the outlet of oligomeric polysaccharide liquid, is called and resolves the district.
The IV district: oligomeric polysaccharide liquid exports to the eluting water inlet, is called the fructose enrichment region.
The V district: enter the mouth fructose liquid outlet of eluting water is called the race way.
Next step comes further to introduce technology of the present invention in conjunction with the embodiments.
Feeding liquid is a high fructose syrup, its concentration is about 70%, wherein glucose 52%, fructose 42%, oligomeric polysaccharide 5%, pass through this liquid simulation moving-bed, simulation moving-bed operational condition is as follows: 75 ℃ of separation temperatures, and system pressure 1.1Mpa, the feed liquid inlet amount is 1L/h, the eluting water inlet amount is 3.5L/h, and charging reached balance after 24 hours.The discharging situation that obtains is as follows:
1) glucose moiety: concentration is about 34%, glucose purity 95%, fructose purity 3%, oligomeric polysaccharide purity 2%.
2) fructose part: concentration is about 29%, fructose purity 91%, glucose purity 8%, oligomeric polysaccharide 1%.
3) oligomeric polysaccharide part: concentration is about 14%, oligomeric polysaccharide purity 74%, glucose purity 20%, fructose purity 6%.
Claims (4)
1. a method of separating purify glucose, fructose and oligomeric polysaccharide from high fructose syrup is characterized in that, a, synthetic resins: the synthetic earlier acid calcium type resin that is used for special fractionation by adsorption glucose, fructose and oligomeric polysaccharide; B, separation are purified: adopt the fixed bed that above-mentioned acid calcium type resin is housed to use simulated moving bed technology, separate purification from high fructose syrup, obtain purified glucose, fructose and oligomeric polysaccharide product solution;
A, synthetic resins:
Acid calcium type resin with acid macroporous resin as carrier, with calcium metal ion on its chelating, utilize the avidity between water-soluble macromolecule metal absorbent and the metal ion, on acid macroporous resin surface, and use linking agent to be fixed on the matrix resin adsorbents adsorb; Used linking agent is 6%~9% of an acid macroporous resin weight;
Metal Ca
2+The ionic type of service is can the corresponding Ca of dissolved under neutrality or alkaline condition
2+Ionic salt or oxide compound, metal Ca
2+The ionic amount is so that the resin chelating reaches 30% saturated amount~complete saturated amount;
B, separation are purified: adopt the fixed bed that above-mentioned acid calcium type resin is housed, use simulated moving bed technology, simulation moving-bed device is to be connected in series by the chromatographic column more than 4 or 4, becomes a loop system that connects from beginning to end; Every post all has discharge port, opening for feed, circulation port, water-in; Whole simulated moving bed chromatography system chuck heat tracing guarantees that bed is between the setting steady temperature; Whole simulated moving bed chromatography system adopts the computer auto-control mode to change the position of discharge port, opening for feed, circulation port, water-in, thereby realizes charging, water inlet, preceding component discharging, the simultaneously continuous operation of back component discharging;
Simulated moving bed chromatography is separated the position according to charging and discharging mouth and circulation port, and all placed in-line chromatographic columns are divided into 5 districts in the system:
The I district: fructose liquid exports to the high fructose syrup opening for feed, is called oligomeric polysaccharide and extracts the district;
The II district: the high fructose syrup opening for feed is called glucose and extracts the district to the Glucose Liquid outlet;
The III district: Glucose Liquid exports to the outlet of oligomeric polysaccharide liquid, is called and resolves the district;
The IV district: oligomeric polysaccharide liquid exports to the eluting water import, is called the fructose enrichment region;
The V district: the eluting water import is called the race way to the outlet of fructose liquid;
Adopting above-mentioned acid calcium type resin in the moving bed imitation chromatogram separation facility is the stationary phase sorbent material, utilizes the avidity difference between macromole metal absorbent and the various sugar alcohol, realizes the separation fully between glucose, fructose and the oligomeric polysaccharide; Employing water is eluent, and separation temperature is 35 ℃~95 ℃, carries out charging, discharging operation continuously, obtains three class discharging components simultaneously, the first kind be glucose purity>95% be rich in the glucose component; Second class be fructose purity>91% be rich in the fructose component; The 3rd class be oligomeric polysaccharide purity>74% be rich in the oligomeric polysaccharide component.
2. method according to claim 1 is characterized in that, macroporous resin is acid polystyrene macroporous resin or polymethylmethacrylate class macroporous resin; Linking agent is the polyene-based linking agent: divinylbenzene, triethylene benzene or two propylene benzene.
3. method according to claim 1 is characterized in that high fructose syrup directly enters simulation moving-bed separation, obtains glucose, fructose and oligomeric polysaccharide product solution.
4. method according to claim 1 is characterized in that, separation temperature is 60 ℃~80 ℃.
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CN101928305A (en) * | 2010-05-31 | 2010-12-29 | 黑龙江省农产品加工工程技术研究中心 | Method for purifying xylo-oligosaccharide by adsorption and separation by simulated moving bed |
CN102876817A (en) * | 2012-09-24 | 2013-01-16 | 厦门世达膜科技有限公司 | Method for separating glucose and allulose from high fructose corn syrup |
CN103276116A (en) * | 2013-05-05 | 2013-09-04 | 厦门世达膜科技有限公司 | Method for comprehensively utilizing waste sugar liquid in production process of fructose-glucose syrup |
CN103657152A (en) * | 2013-12-14 | 2014-03-26 | 山东理工大学 | Novel separation system for simulated moving bed chromatography (SMBC) |
CN104611475A (en) * | 2013-11-04 | 2015-05-13 | 南京工业大学 | Fructose separation method |
CN104837376A (en) * | 2012-08-20 | 2015-08-12 | 天然成分有限责任公司 | Method of producing a sugar product from fruit |
CN105194904A (en) * | 2015-09-06 | 2015-12-30 | 中国科学院烟台海岸带研究所 | Continuous chromatographic separation and purification system for separating sugar in inulin |
CN105256079A (en) * | 2015-10-22 | 2016-01-20 | 林树仁 | Purification method for HFCS (high fructose corn syrup) in fructose production process |
CN106831893A (en) * | 2017-02-10 | 2017-06-13 | 广西轻工业科学技术研究院 | A kind of method that utilization molecular sieve Simulation moving bed prepares high-purity fructo oligosaccharides |
CN108251470A (en) * | 2017-11-03 | 2018-07-06 | 毛强平 | A kind of preparation method of fructose syrup |
CN109674843A (en) * | 2019-01-30 | 2019-04-26 | 湖南绿蔓生物科技股份有限公司 | A kind of method for extraction and purification of dried fructus momordicae comprehensive utilization |
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CN101928305A (en) * | 2010-05-31 | 2010-12-29 | 黑龙江省农产品加工工程技术研究中心 | Method for purifying xylo-oligosaccharide by adsorption and separation by simulated moving bed |
CN104837376A (en) * | 2012-08-20 | 2015-08-12 | 天然成分有限责任公司 | Method of producing a sugar product from fruit |
CN102876817A (en) * | 2012-09-24 | 2013-01-16 | 厦门世达膜科技有限公司 | Method for separating glucose and allulose from high fructose corn syrup |
CN102876817B (en) * | 2012-09-24 | 2015-04-01 | 厦门世达膜科技有限公司 | Method for separating glucose and allulose from high fructose corn syrup |
CN103276116A (en) * | 2013-05-05 | 2013-09-04 | 厦门世达膜科技有限公司 | Method for comprehensively utilizing waste sugar liquid in production process of fructose-glucose syrup |
CN103276116B (en) * | 2013-05-05 | 2015-04-01 | 厦门世达膜科技有限公司 | Method for comprehensively utilizing waste sugar liquid in production process of fructose-glucose syrup |
CN104611475B (en) * | 2013-11-04 | 2018-11-20 | 南京工业大学 | A kind of method of fructose separation |
CN104611475A (en) * | 2013-11-04 | 2015-05-13 | 南京工业大学 | Fructose separation method |
CN103657152A (en) * | 2013-12-14 | 2014-03-26 | 山东理工大学 | Novel separation system for simulated moving bed chromatography (SMBC) |
CN103657152B (en) * | 2013-12-14 | 2015-06-17 | 山东理工大学 | Novel separation system for simulated moving bed chromatography (SMBC) |
CN105194904A (en) * | 2015-09-06 | 2015-12-30 | 中国科学院烟台海岸带研究所 | Continuous chromatographic separation and purification system for separating sugar in inulin |
CN105194904B (en) * | 2015-09-06 | 2017-01-25 | 中国科学院烟台海岸带研究所 | Continuous chromatographic separation and purification system for separating sugar in inulin |
CN105256079A (en) * | 2015-10-22 | 2016-01-20 | 林树仁 | Purification method for HFCS (high fructose corn syrup) in fructose production process |
CN106831893A (en) * | 2017-02-10 | 2017-06-13 | 广西轻工业科学技术研究院 | A kind of method that utilization molecular sieve Simulation moving bed prepares high-purity fructo oligosaccharides |
CN108251470A (en) * | 2017-11-03 | 2018-07-06 | 毛强平 | A kind of preparation method of fructose syrup |
WO2020057555A1 (en) * | 2018-09-18 | 2020-03-26 | 上海立足生物科技有限公司 | Method and device for continuous large-scale separation and preparation of d-psicose |
CN109674843A (en) * | 2019-01-30 | 2019-04-26 | 湖南绿蔓生物科技股份有限公司 | A kind of method for extraction and purification of dried fructus momordicae comprehensive utilization |
CN109674843B (en) * | 2019-01-30 | 2022-03-22 | 湖南绿蔓生物科技股份有限公司 | Extraction and purification method for comprehensively utilizing dried momordica grosvenori |
CN114874273A (en) * | 2022-05-16 | 2022-08-09 | 浙江晟格生物科技有限公司 | Preparation method of L-fructose |
CN114874273B (en) * | 2022-05-16 | 2024-03-29 | 浙江晟格生物科技有限公司 | Preparation method of L-fructose |
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