CN1528769A - Process for separating mannitose and glucose by analog moving bed - Google Patents
Process for separating mannitose and glucose by analog moving bed Download PDFInfo
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- CN1528769A CN1528769A CNA031349560A CN03134956A CN1528769A CN 1528769 A CN1528769 A CN 1528769A CN A031349560 A CNA031349560 A CN A031349560A CN 03134956 A CN03134956 A CN 03134956A CN 1528769 A CN1528769 A CN 1528769A
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Abstract
The invention is a technique to separate mannite from glucose by simulated moving bed, using mixed sugar liquor obtained by glucose epimerization reaction as raw material, 12 or 24 columns to simulate moving bed, strong-acid cation exchange resin as sorbent and water as eluent, separating at 40-85 deg.C to obtain mannite-rich after cut, concentration 18-36% and mannite content 75% above; obtaining glucose-rich front cut, concentration 15-30% and mannite content below 8%.
Description
Technical field:
The present invention utilizes simulation moving-bed tripping device to separate the technology of seminose and glucose.Belong to the Separation of Organic Compounds field.
Background technology:
The molecular formula of glucose is C
6H
12O
6, structural formula is
Being human body and the requisite base substance of animals and plants metabolism, also is the component units of starch, extensively exists organism and occurring in nature.
The molecular formula of seminose is C
6H
12O
6, structural formula is
Be the isomers of glucose, both difference only are that institute bonded hydroxyl chirality orientation is just in time opposite on second carbon atom.Seminose exists less at occurring in nature, can be applicable to sweeting agent and biochemistry, pharmaceutical preparation etc.Seminose can all transform generation N.F,USP MANNITOL after hydrogenation reaction, therefore, seminose is one of effective preparation approach of medicine medicine N.F,USP MANNITOL commonly used.With glucose is raw material, can partly transform the generation seminose through behind the epimerization reaction, and hydrogenation generates N.F,USP MANNITOL with high yield.
But the productive rate that the glucose epimerization changes into seminose is lower, is the technology of catalyzer with the molybdate, and the reacted mannose content of one way only reaches 28～33%.Want to improve the productive rate of seminose, seminose is separated with glucose, but the glucose recirculation is carried out epimerization reaction, but and the higher seminose component hydrogenation of separating obtained content generates the seminose product of high level, thereby can prepare N.F,USP MANNITOL with high yield.Can therefore, separate seminose-glucose effectively, becoming glucose be the key that raw material economics ground produces N.F,USP MANNITOL.
Since seminose and glucose for difference to isomers, both character, structure are very similar, general separation method such as crystallization, distillation, extraction etc. are difficult to they separation, perhaps separation costs is too high.Utilize the method for fractionation by adsorption might separate the isomers of this class character fairly similar.The principle of fractionation by adsorption is: select a kind of sorbent material, the intensity that seminose and glucose adsorb on this sorbent material is variant, and seminose is adsorbed more firmly, during with the eluent wash-out, glucose just comes out earlier, and seminose comes out after, and both have just obtained partly separating like this.Fractionation by adsorption is one of effective means that tackles the difficult isolating isomers material of this class, and for example the separation of the separation of fructose-glucose, xylol is exactly the successful example of fractionation by adsorption.Utilize simulation moving-bed fractionation by adsorption now to become one of effective separation method of modern industry.
All there is shortcoming in seminose in the past-glucose separation method.
Patent European Patent Application0074713 has reported the method that adds halide salt of using, cooling is separated out the eutectiferous way of glucose-halide salt and is reached the isolating purpose of part, and this method is resulting to be rich in seminose contained in the seminose component and glucose quality than still reaching 1: 1.Obviously the described separation efficiency of this patent is low, and separate not thorough, moreover that a large amount of halide salts can make from the burden of handing over removal of impurities is very heavy, production cost is very high, this method technology is effectively used industrial being difficult to, and resulting mannitol content is the highest behind the hydrogenation also only reaches 50%.This method is the isolating exemplary of seminose-glucose crystallization.
Patent GB1540556,1977 have reported use calcium type Zeo-karb as sorbent material, use water as eluent, carry out single-column and separate seminose-glucose, seminose goes out after, and glucose goes out earlier, collect the fraction that is come out respectively, the component that can obtain being rich in seminose He be rich in glucose; U.S. Pat P4471114,1984 have also reported the use molecular sieve makes sorbent material, separates seminose and glucose with the single-column partition method.More than two methods only use single-column to separate, be periodical operation, water loss is big, resulting product concentration is very low, for example mannose content reaches 70% when above, concentration is lower than 8%; Glucose content reaches 90% when above, and concentration is lower than 10%, therefore, need expend a large amount of steam and energy and concentrate, and also is not suitable for industrial mass production and uses.But the test of single-column fractionation by adsorption can be simulation moving-bed separation seminose-glucose screening available sorbent material.
Summary of the invention:
The purpose of this invention is to provide a kind of technology of separating seminose and glucose, can realize suitability for industrialized production with simulation moving-bed device.
Because the resulting discharging concentration of single-column fractionation by adsorption seminose glucose is very low, water loss is big, can only periodical operation, and be not suitable for suitability for industrialized production and use; Utilize simulation moving-bed tripping device, can overcome the above-mentioned shortcoming of single-column device, on industrial production, be applied, resulting discharging concentration ratio single-column discharging concentration raises, the continuous charging and discharging operation, easily be automated control, the purity and the quality of resulting discharging component also increase.
The simulation moving-bed example of suitability for industrialized production of having realized has the separation of xylol, the separation of fructose glucose etc., and the large-scale high fructose syrup tripping device of many covers has been built up in the especially separation of fructose glucose in the world, and the production cost of fructose is reduced greatly.Therefore, simulation moving-bed device is to have the operating automation degree height, and process stabilizing is easy to realize computer-controlled separation means.Utilize simulation moving-bed device to can be industrial production separation seminose glucose possibility is provided.
The used raw material of the present invention is to transform the seminose-glucose mixed sugar liquid that generates with glucose epimerization reaction rear section, wherein contains seminose 30%, glucose about 70%, and concentration is 40～70%.
Of the present invention simulation moving-bed be to select for use storng-acid cation exchange resin as sorbent material, be eluent with water, separation temperature is 40～85 ℃, carry out charging, discharging operation continuously, can obtain two kinds of dischargings simultaneously, a kind of for being rich in the component of glucose, be foreshot; Another kind of for being rich in the component of seminose, be after cut.Control well after the operational condition, charging, water inlet, foreshot discharging, after cut discharging can be carried out simultaneously.
Used in the present invention simulation moving-bed be end to end with the individual post in 24 (or 12), each post all is connected to discharge port, opening for feed, circulation port, water-in.Used simulation moving-bed of the present invention is to change the position that opening for feed, discharge port, water-in, circulation are imported and exported with the mode that rotary valve rotates control.According to the position of feed inlet and outlet and circulation port, 24 pillars are divided into 4 zones:
One district (or claiming to extract district or adsorption zone): front-end volatiles are exported to liquor inlet, and 6 posts are arranged;
Two districts (or claiming an enrichment region or a smart district): liquor inlet to after cut exports, and 8 posts are arranged;
Three districts (or claiming desorption zone): after cut is exported to the eluting water inlet, and 6 posts are arranged;
Four districts (or claiming race way or two smart districts): after cut is exported to the eluting water inlet, and 4 posts are arranged.
The simulation moving-bed zoned format of 12 posts is as follows:
One district (or claiming to extract district or adsorption zone): front-end volatiles are exported to liquor inlet, and 3 posts are arranged;
Two districts (or claiming an enrichment region or a smart district): liquor inlet to after cut exports, and 4 posts are arranged;
Three districts (or claiming desorption zone): after cut is exported to the eluting water inlet, and 3 posts are arranged;
Four districts (or claiming race way or two smart districts): after cut is exported to the eluting water inlet, and 2 posts are arranged.
Whole simulated moving bed system is airtight with stay-warm case, loads onto the air blast well heater of 2 2KW, can keep case temperature and be 40～85 ℃ claimed range.Charging, water inlet need just to enter system after the hot water tank preheating.Like this, the separation temperature that can guarantee system is controlled to be claimed range.
The foreshot discharge port is loaded onto the pressure automatically controlled valve, guarantees that the pressure at foreshot discharge port place is constant value, thereby effectively keeps the stable of system's internal pressure; The after cut discharging is manually controlled by valve.Accumulative total volume numerical value according to the discharging of forward and backward fraction per hour, flooding quantity, inlet amount makes the material of system reach balance.
After input and output material reaches balance, detect the material concentration of discharge port, the discharging concentration of regulating foreshot is 15～30%, and after cut discharging concentration is 18～36% scopes, can obtain satisfied separating effect.
During normal running, top pressure is 0.5～1.5Mpa in the simulated moving bed system, the pump flow registration is 25～35 liters/hour, liquid glucose inlet amount 3.5～4.2L/h, eluting water inlet amount 5.8～6.4L/h pulls 2～12 minutes valve time, and charging is after 48 hours, after system reached steady state operation, resulting discharging situation was as follows:
| Material | ??Bx20℃ | Mannose content |
| Be rich in the foreshot of glucose | 15％～30％ | Be lower than 8% |
| Be rich in the after cut of seminose | 18％～36％ | Be higher than 75% |
Outstanding advantage of the present invention is as follows: (1) operational condition is reliable and stable, is easy to realize suitability for industrialized production and adopts automatic control device; (2) the concentration ratio single-column fractionation by adsorption situation of resulting forward and backward fraction greatly improves, and helps to reduce material and concentrates spent a large amount of steam and energy; (3) quality product of forward and backward fraction also increases, and can steady running long-time.In a word, utilize simulation moving-bed device to carry out seminose-glucose and separate, separate seminose-glucose for suitability for industrialized production and created good condition.
Embodiment:
Below, come further to introduce technology of the present invention in conjunction with the embodiments.
Embodiment 1: charging is to transform the seminose-glucose mixed sugar liquid that generates with glucose epimerization reaction rear section, wherein contains seminose 30%, glucose 70%, and concentration is 50%.Simulation moving-bed operational condition is as follows: 58 ℃ of separation temperatures, top pressure 0.6Mpa, pump flow meter registration is 28 liters/hour, 3.75 liters/hour of liquid glucose feed rates, 6.11 liters/hour of eluting water flooding velocity, pulling the valve step duration is 6 minutes, with 12 cylindricality formulas, make sorbent material with calcium type Zeo-karb, with water eluent, after the steady running 48 hours, resulting discharging situation is as follows:
| Material | Bx20℃ | Mannose content | Discharging flow |
| Be rich in the foreshot of glucose | 21.65％ | ????7.5％ | 7.16 rise/hour |
| Be rich in the after cut of seminose | 30.04％ | ????78.86％ | 2.68 rise/hour |
Embodiment 2: charging is to transform the seminose-glucose mixed sugar liquid that generates with glucose epimerization reaction rear section, wherein contains seminose 30%, glucose 70%, and concentration is 55%.Simulation moving-bed operational condition is as follows: 50 ℃ of separation temperatures, top pressure 0.75Mpa, pump flow meter registration is 32 liters/hour, 3.7 liters/hour of liquid glucose feed rates, 6.3 liters/hour of eluting water flooding velocity, pulling the valve step duration is 5 minutes and 30 seconds, with 24 cylindricality formulas, make sorbent material with calcium type Zeo-karb, with water eluent, after 60 hours, resulting discharging situation is as follows through steady running:
| Material | ????Bx20℃ | Mannose content | Discharging flow |
| Be rich in the foreshot of glucose | ????20.58％ | ????1.82％ | 7.92 rise/hour |
| Be rich in the after cut of seminose | ????33.66％ | ????88.80％ | 1.93 rise/hour |
Claims (10)
1, the technology of a kind of simulation moving-bed separation seminose and glucose, it is characterized in that: the mixed sugar liquid behind the glucose epimerization reaction is after simulation moving-bed separating treatment, obtain two kinds of dischargings: foreshot is for being rich in the glucose component, and concentration 15～30% contains seminose and is lower than 8%; After cut is for being rich in the seminose component, and concentration 18～36% contains seminose and is higher than 75%.
2, the technology of simulation moving-bed separation seminose according to claim 1 and glucose, it is characterized in that: described simulation moving-bed device is to make sorbent material with storng-acid cation exchange resin, is eluent with water.
3, the technology of simulation moving-bed separation seminose according to claim 1 and glucose, it is characterized in that: described simulation moving-bed device has 12 posts and 24 cylindricality formulas, and the mode of rotating with rotary valve changes the position that opening for feed, discharge port, water-in and circulation are imported and exported.
4, the technology of simulation moving-bed separation seminose according to claim 1 and glucose, it is characterized in that: simulation moving-bed operational condition is as follows: 40～85 ℃ of separation temperatures, top pressure 0.5～1.5Mpa, 25～35 liters/hour of pump flow registrations, 3.5～4.2 liters/hour of liquid glucose feed rates, 5.8～6.4 liters/hour of eluting water flooding velocity, pulling the valve step duration is 2～12 minutes
5, the technology of simulation moving-bed separation seminose according to claim 1 and glucose, it is characterized in that: simulation moving-bed charging is that glucose epimerization reaction rear section transforms the seminose-glucose mixed sugar liquid that generates, wherein contain seminose 30%, about glucose 70%, concentration is 40～70%.
6, the technology of simulation moving-bed separation seminose according to claim 1 and glucose, it is characterized in that: after the simulated moving bed system input and output material reaches balance, detect the material concentration of discharge port, the discharging concentration of regulating foreshot is 15～30%, after cut discharging concentration is 18～36% scopes, can obtain satisfied separating effect.
7, the technology of simulation moving-bed separation seminose according to claim 1 and glucose, it is characterized in that: the foreshot discharge port is loaded onto the pressure automatically controlled valve, the pressure that can guarantee foreshot discharge port place is constant value, thereby effectively keeps the stable of system's internal pressure; The after cut discharging is manually controlled by valve; Accumulative total volume numerical value according to the discharging of forward and backward fraction per hour, flooding quantity, inlet amount makes the material of system reach balance.
8, the technology of simulation moving-bed separation seminose according to claim 1 and glucose is characterized in that: simulated moving bed system is according to the position of feed inlet and outlet and circulation port, and 24 pillars are divided into 4 zones:
One district or title extract district or adsorption zone: front-end volatiles are exported to liquor inlet, and 6 posts are arranged;
Two districts or title enrichment region or a smart district: liquor inlet to after cut exports, and 8 posts are arranged;
Three districts or title desorption zone: after cut is exported to the eluting water inlet, and 6 posts are arranged;
Four districts or title race way or two smart districts: after cut is exported to the eluting water inlet, and 4 posts are arranged.
9, the technology of simulation moving-bed separation seminose according to claim 1 and glucose is characterized in that: simulated moving bed system is according to the position of feed inlet and outlet and circulation port, and 12 pillars are divided into 4 zones:
One district or title extract district or adsorption zone: front-end volatiles are exported to liquor inlet, and 3 posts are arranged;
Two districts or title enrichment region or a smart district: liquor inlet to after cut exports, and 4 posts are arranged;
Three districts or title desorption zone: after cut is exported to the eluting water inlet, and 3 posts are arranged;
Four districts or title race way or two smart districts: after cut is exported to the eluting water inlet, and 2 posts are arranged.
10, the technology of simulation moving-bed separation seminose according to claim 1 and glucose, it is characterized in that: whole simulated moving bed system is airtight with stay-warm case, load onto the air blast well heater, can keep case temperature and be 40～85 ℃ claimed range, charging, water inlet need just to enter system after the hot water tank preheating, guarantee that the separation temperature of system is controlled to be claimed range.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA031349560A CN1528769A (en) | 2003-09-28 | 2003-09-28 | Process for separating mannitose and glucose by analog moving bed |
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| CNA031349560A CN1528769A (en) | 2003-09-28 | 2003-09-28 | Process for separating mannitose and glucose by analog moving bed |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1301334C (en) * | 2005-07-01 | 2007-02-21 | 江南大学 | Method for extracting high purity glucose and functional oligose from crystalline glucose mother liquid |
| CN101367843B (en) * | 2008-09-17 | 2010-10-06 | 无锡绿色分离应用技术研究所有限公司 | Method for separating heteroside from tea saponin liquid to purify glucose and triterpene |
| CN101554540B (en) * | 2009-04-22 | 2011-04-20 | 南京凯通粮食生化研究设计有限公司 | Method for separating glucose, seminose and oligosaccharide by simulated moving bed |
| CN101538291B (en) * | 2009-04-22 | 2011-12-21 | 南京凯通粮食生化研究设计有限公司 | Method for using a simulated movable bed to separate and prepare high-content soybean oligosaccharide |
| CN102329340A (en) * | 2011-11-01 | 2012-01-25 | 青岛明月海藻集团有限公司 | Method for preparing D-mannose |
| CN104744524A (en) * | 2013-12-26 | 2015-07-01 | 天津大学 | Method for preparation of D-fructose and D-mannose by simulated moving bed reactor |
| CN105906475A (en) * | 2016-05-09 | 2016-08-31 | 河北乐开节能科技股份有限公司 | Production method and production device of crystal mannite |
| CN107406893A (en) * | 2015-02-02 | 2017-11-28 | 瑞典酒精化工集团电子技术公司 | Soft wood material pretreatment control |
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2003
- 2003-09-28 CN CNA031349560A patent/CN1528769A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1301334C (en) * | 2005-07-01 | 2007-02-21 | 江南大学 | Method for extracting high purity glucose and functional oligose from crystalline glucose mother liquid |
| CN101367843B (en) * | 2008-09-17 | 2010-10-06 | 无锡绿色分离应用技术研究所有限公司 | Method for separating heteroside from tea saponin liquid to purify glucose and triterpene |
| CN101554540B (en) * | 2009-04-22 | 2011-04-20 | 南京凯通粮食生化研究设计有限公司 | Method for separating glucose, seminose and oligosaccharide by simulated moving bed |
| CN101538291B (en) * | 2009-04-22 | 2011-12-21 | 南京凯通粮食生化研究设计有限公司 | Method for using a simulated movable bed to separate and prepare high-content soybean oligosaccharide |
| CN102329340A (en) * | 2011-11-01 | 2012-01-25 | 青岛明月海藻集团有限公司 | Method for preparing D-mannose |
| CN104744524A (en) * | 2013-12-26 | 2015-07-01 | 天津大学 | Method for preparation of D-fructose and D-mannose by simulated moving bed reactor |
| CN104744524B (en) * | 2013-12-26 | 2017-05-24 | 天津大学 | Method for preparation of D-fructose and D-mannose by simulated moving bed reactor |
| CN107406893A (en) * | 2015-02-02 | 2017-11-28 | 瑞典酒精化工集团电子技术公司 | Soft wood material pretreatment control |
| CN107406893B (en) * | 2015-02-02 | 2020-12-25 | 瑞典酒精化工集团电子技术公司 | Cork raw material pretreatment control |
| CN105906475A (en) * | 2016-05-09 | 2016-08-31 | 河北乐开节能科技股份有限公司 | Production method and production device of crystal mannite |
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