CN101899486B - Method for separating and purifying oligo-xylose by using simulated moving bed - Google Patents
Method for separating and purifying oligo-xylose by using simulated moving bed Download PDFInfo
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- CN101899486B CN101899486B CN201010231823A CN201010231823A CN101899486B CN 101899486 B CN101899486 B CN 101899486B CN 201010231823 A CN201010231823 A CN 201010231823A CN 201010231823 A CN201010231823 A CN 201010231823A CN 101899486 B CN101899486 B CN 101899486B
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Abstract
The invention relates to a method for separating and purifying oligo-xylose by using a simulated moving bed. The method comprises the following steps of: performing preprocessing such as decolorization, deinoning, condensation and the like on feed liquor obtained by performing enzyme hydrolysis on feed solution, namely hemicellulose; filtering and deoxidizing the preprocessed hemicellulose hydrolysis liquid with high purity water for later use; feeding the preprocessed hemicellulose hydrolysis liquid into a chromatographic separation device of the simulated moving bed to perform separation so as to obtain oligo-xylose crude liquor which is rich in oligo-xylose components; and performing reduced pressure evaporation concentration or excipient spray drying on the oligo-xylose crude liquor obtained by the separation to obtain oligo-xylose syrup or powder. In the method, the chromatographic separation device of the simulated moving bed (SMB) is used to extract the oligo-xylose, a plurality of adsorption posts is connected in series to form a closed loop, the positions of the inlet and outlet of each strand of materials are changed by continuously switching valves, and the relative movement of solid and liquid phases is realized, so that different components are separated and extracted. The method not only has the advantage of simple absorption operation of a fixed bed but also has the continuous operation capability of the moving bed, so that the method is suitable for large-scaled industrialized production.
Description
Technical field
The invention belongs to the SMBC separation technology field, especially a kind of method of utilizing simulation moving-bed separating and purifying oligo-xylose.
Background technology
Semicellulose is one of important composition composition of vegetable matter; Account for 15%～35%; It is the heterogeneous polymer that is made up of several kinds of dissimilar monose; Wherein mainly be five-carbon sugar, pre-treatment is after mainly contain the glucose of xylooligosaccharides, a spot of wood sugar, pectinose and trace in the mother liquor of xylanase hydrolysis.Xylooligosaccharides is with β-1 by 2～7 wood sugar molecules; 4 glycosidic link be combined intos; And be the mixture of staple with xylo-bioses, xylotriose, Xylotetrose, also claim wood oligose, its sugariness is about 40% of sucrose; Be a kind of good propagation bifidus bacillus, improve the food function factor of intestinal flora environment, it separates, and to purify be one of gordian technique.
In the separation and purification of carbohydrate, method commonly used has column chromatography, membrane separation process, enzyme partition method and microbe fermentation method etc.The membrane sepn process be the size according to the filter membrane aperture make material through or be retained in the purpose that film reaches separating substances.All be to adopt ultrafiltration to separate the xylooligosaccharides for preparing with nanofiltration in Chinese patent 200710054198.1 and the Chinese patent 200410013840.8; Because the restriction of masking technique; The aperture of holding back of film is not absolute, but the MV of a scope, the concentration of adding separated liquid glucose is higher; Therefore will reach higher separating size often needs long post film length, makes sepn process become uneconomical.Enzyme partition method and microbe fermentation method all are the removals to a certain in the liquid glucose or several kinds of compositions, and process is difficult to effective control, and use cost is high, has influenced suitability for industrialized production.
Chromatographic separation is a kind of widely applied unit operation in carbohydrate and verivate production thereof, and it is to utilize the difference of certain sorbent material to the matrix absorption property, through the process of absorption-wash-out, makes several kinds of very close separating substances of character.The continuous chromatography system is to be the unit with the chromatography, mechanism such as the adverse current in the introducing chemical industry, backflow, so the general bed technology of separation efficiency exceeds a lot.In addition, the continuous chromatography process can effectively utilize the weighting agent bed, and the product of constant mass is provided, and is particularly suitable among the production of carbohydrate.It is to be a kind of liquid chromatography stripping technique of stationary phase with the ionite that ion-exchange chromatography separates; Its ultimate principle is different according to various separated components and ionite absorption property, utilizes the balance of IX absorption or wash-out effect to reach the purpose of separating substances.
Summary of the invention
The objective of the invention is to overcome the weak point of prior art, provide a kind of can operate continuously, extraction effect is good, cost the is low method of utilizing simulation moving-bed separating and purifying oligo-xylose.
The present invention realizes through following technical scheme:
A kind of method of utilizing simulation moving-bed separating and purifying oligo-xylose, step is following:
(1) with the liquid stock feed liquid that to be semicellulose obtain through enzymic hydrolysis through pre-treatment, high purity water filters, deoxidation is subsequent use;
(2) start column oven and water bath switch, make it rise to design temperature 60-80 ℃, with high purity water as eluent; Pretreated liquid stock is got into moving bed imitation chromatogram separation facility separate, processing condition are following: keep pressure≤0.5Mpa, separation temperature 60-80 ℃; Feeding liquid flow 40～80ml/min; Inlet 60～the 160ml/min of eluent high purity water, valve switching time is 280～420s, under the booster action of recycle pump; 3-6 all after date of operation reaches balance, obtains being rich in the thick liquid of xylooligosaccharides of xylooligosaccharides component;
(3) the thick liquid of xylooligosaccharides that separation is obtained concentrates through reduction vaporization and obtains the xylooligosaccharides syrup, or obtains the xylooligosaccharides pulvis after adding the vehicle spraying drying.
And said pre-treatment comprises that activated carbon decolorizing, IX removal of impurities, membrane filtration concentrate.
And the separating medium that the chromatographic column of said moving bed imitation chromatogram separation facility is filled is sodium type, potassium type Zeo-karb or sodium type, potassium type cationic molecule sieve.
And used linking agent is a divinylbenzene when said sodium type, the polymerization of potassium type Zeo-karb, degree of crosslinking 4%-10%.
And used excipient is W-Gum, maltodextrin or beta-cyclodextrin during the thick liquid spraying drying of said step (3) xylooligosaccharides.
Advantage of the present invention and positively effect are:
1, the present invention adopts moving bed imitation chromatogram separation facility (SMB) system to extract xylooligosaccharides; A plurality of adsorption columns are connected into closed circuit,, realize relatively moving of solid, liquid two-phase through the import and export position of continuous each strand of switch valve change material; Carry out the separation and Extraction of different components; The advantage that existing ADSORPTION IN A FIXED BED is simple to operate has the ability of moving-bed operate continuously again, is fit to large-scale industrial production.
2, that the total post that the present invention relates to is imitated is high, the moving phase consumption is few, can realize operating serialization, can access the higher xylooligosaccharides of purity, has improved raw material availability, reduction production cost, increased economic benefit.
Description of drawings
Fig. 1 is the technological process of production figure of separating and purifying oligo-xylose of the present invention;
Fig. 2 is a SMBC lock out operation synoptic diagram of the present invention, wherein:
The I district: for allowing solid phase regeneration, its function is from the strong absorbed component B of solid phase desorb between elutriant and extracting solution;
II district: be the desorption zone of weak absorbed component A between extracting solution and feeding liquid;
III district: be the adsorption zone of strong absorbed component B between feeding liquid and raffinate;
The IV district: the function between raffinate and elutriant is the weak component A of absorption, regenerative elution liquid.
The moving bed imitation chromatogram separation facility of Fig. 3 for using among the present invention.
Embodiment
Below in conjunction with embodiment, the present invention is further specified, following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
The moving bed imitation chromatogram separation facility that relates in following examples is the device that relates in the patent 200820218308.3; Moving bed imitation chromatogram separation facility; Be to connect and compose by drive system, transmission system, rotary distributor and chromatographic column and pipeline; It is characterized in that drive system is to be made up of electromagnetic braking motor (1); Transmission system is that electromagnetic braking motor axle (2) links with wheel casing (3); The bottom of wheel casing (3) fixes with the stator discs (6) of rotary distributor and connects; The transmission shaft (4) of wheel casing (3) fixes with the rotor disk (5) of rotary distributor and connects, and rotary distributor all has the conduit (7,8) of linking up mutually by rotor disk (5) and stator discs (6) face exposure phase movingly in stator discs (6) and rotor disk (5); Stator discs (6) is provided with material import and export a, the b that is connected with conduit (7), and rotor disk (5) ring is provided with the pipe connecting (10) of chromatographic column (9) one ends that are connected with conduit (8) week, the lower plane of rotor disk is provided with chromatographic column (9) the other end pipe connecting (11) that is connected with conduit (8); Transmission shaft (4) lower end and support shaft (12) are connected and fixed, and support shaft (12) lower end is upright with top, support seat (13) location, and concrete structure is as shown in Figure 3.
In the simulation moving-bed synoptic diagram of four plot structures as shown in Figure 2; In the I district, the net flow of strong absorbed component B must move right, and the net flow of the weak absorbed component A in II district must move right; The net flow of the strong absorbed component B in III district must be moved to the left, and the net flow of the weak absorbed component A of IV must be moved to the left.
Embodiment 1
A kind of method of utilizing simulation moving-bed separating and purifying oligo-xylose, step is following:
(1) feed liquid that semicellulose is obtained through enzymic hydrolysis is through pre-treatment such as activated carbon decolorizing, IX removal of impurities, membrane filtration concentrate, and recording solid content is 54.25%; Its each component content detects through performance liquid chromatography, xylooligosaccharides content 68.4%, and assorted sugared content such as wood sugar, pectinose are 31.5%; High purity water filters, deoxidation is subsequent use.
(2) start column oven and water bath switch, make it rise to 70 ℃ of design temperatures, pretreated liquid stock is got into moving bed imitation chromatogram separation facility separate; Processing condition are following: keep pressure≤0.4Mpa, 70 ℃ of separation temperatures, feeding liquid flow 60ml/min; The inlet 90ml/min of eluent high purity water; Valve switching time is 303s, under the booster action of recycle pump, moves 5 all after dates and reaches balance.The xylooligosaccharides out-feed liquid that obtains is through detecting purity 91.25%.
(3) out-feed liquid is under 75 ℃ of conditions, concentrates through reduction vaporization that to obtain solid content be 70% xylooligosaccharides syrup.
A kind of method of utilizing simulation moving-bed separating and purifying oligo-xylose, step is following:
(1) feed liquid that semicellulose is obtained through enzymic hydrolysis is through pre-treatment such as activated carbon decolorizing, IX removal of impurities, membrane filtration concentrate, and recording solid content is 43.75%; Its each component content detects through performance liquid chromatography, xylooligosaccharides content 72.3%, and assorted sugared content such as wood sugar, pectinose are 26.7%; High purity water filters, deoxidation is subsequent use.
(2) start column oven and water bath switch, make it rise to 75 ℃ of design temperatures, pretreated liquid stock is got into moving bed imitation chromatogram separation facility separate; Processing condition are following: keep pressure≤0.5Mpa, 75 ℃ of separation temperatures, feeding liquid flow 50ml/min; The inlet 80ml/min of eluent high purity water; Valve switching time is 300s, under the booster action of recycle pump, moves 5 all after dates and reaches balance.The xylooligosaccharides out-feed liquid that obtains is through detecting purity 93.2%
(3) out-feed liquid is under 75 ℃ of conditions, concentrates through reduction vaporization that to obtain solid content be 45% xylooligosaccharides syrup, and to be 98% maltodextrin with content carry out spraying drying as vehicle, and to obtain content be 30% xylooligosaccharides pulvis.
Embodiment 3
A kind of method of utilizing simulation moving-bed separating and purifying oligo-xylose, step is following:
(1) feed liquid that semicellulose is obtained through enzymic hydrolysis is through pre-treatment such as activated carbon decolorizing, IX removal of impurities, membrane filtration concentrate, and recording solid content is 31.5%; Its each component content detects through performance liquid chromatography, xylooligosaccharides content 70.36%, and assorted sugared content such as wood sugar, pectinose are 29.1%; High purity water filters, deoxidation is subsequent use.
(2) start column oven and water bath switch, make it rise to 70 ℃ of design temperatures, pretreated liquid stock is got into moving bed imitation chromatogram separation facility separate; Processing condition are following: keep pressure≤0.4Mpa, 70 ℃ of separation temperatures, feeding liquid flow 40ml/min; The inlet 60ml/min of eluent high purity water; Valve switching time is 295s, under the booster action of recycle pump, moves 5 all after dates and reaches balance.The xylooligosaccharides out-feed liquid that obtains is through detecting purity 90.64%.
(3) out-feed liquid is under 75 ℃ of conditions, concentrates through reduction vaporization that to obtain solid content be 65% xylooligosaccharides syrup.
Claims (4)
1. method of utilizing simulation moving-bed separating and purifying oligo-xylose is characterized in that step is following:
(1) with the liquid stock feed liquid that to be semicellulose obtain through enzymic hydrolysis through pre-treatment, high purity water filters, deoxidation is subsequent use;
(2) start column oven and water bath switch, make it rise to design temperature 60-80 ℃, with high purity water as eluent; Pretreated liquid stock is got into moving bed imitation chromatogram separation facility separate, processing condition are following: keep pressure≤0.5Mpa, separation temperature 60-80 ℃; Feeding liquid flow 40～80ml/min; Inlet 60～the 160ml/min of eluent high purity water, valve switching time is 280～420s, under the booster action of recycle pump; 3-6 all after date of operation reaches balance, obtains being rich in the thick liquid of xylooligosaccharides of xylooligosaccharides component;
(3) the thick liquid of xylooligosaccharides that separation is obtained concentrates through reduction vaporization and obtains the xylooligosaccharides syrup, or obtains the xylooligosaccharides pulvis after adding the vehicle spraying drying;
The separating medium that the chromatographic column of said moving bed imitation chromatogram separation facility is filled is sodium type, potassium type Zeo-karb or sodium type, potassium type cationic molecule sieve.
2. the method for utilizing simulation moving-bed separating and purifying oligo-xylose according to claim 1 is characterized in that: said pre-treatment comprises that activated carbon decolorizing, IX removal of impurities, membrane filtration concentrate.
3. the method for utilizing simulation moving-bed separating and purifying oligo-xylose according to claim 1 is characterized in that: used linking agent is a divinylbenzene when said sodium type, the polymerization of potassium type Zeo-karb, degree of crosslinking 4%-10%.
4. the method for utilizing simulation moving-bed separating and purifying oligo-xylose according to claim 1 is characterized in that: used excipient is W-Gum, maltodextrin or beta-cyclodextrin during the thick liquid spraying drying of said step (3) xylooligosaccharides.
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| NZ743055A (en) * | 2013-03-08 | 2020-03-27 | Xyleco Inc | Equipment protecting enclosures |
| CN105255965B (en) * | 2015-10-14 | 2023-04-25 | 山东龙力生物科技股份有限公司 | Method for preparing high-purity xylo-oligosaccharide by using cotton seed hulls as raw materials |
| CN106831893B (en) * | 2017-02-10 | 2019-04-23 | 广西轻工业科学技术研究院有限公司 | A method of high-purity fructo oligosaccharides are prepared using molecular sieve-Simulation moving bed |
| CN107142337B (en) * | 2017-05-19 | 2020-06-19 | 南京凯通粮食生化研究设计有限公司 | Method for preparing xylose and arabinose by taking bagasse as raw material |
| CN110465114B (en) * | 2019-08-23 | 2021-08-20 | 内蒙古金达威药业有限公司 | Simulated moving bed continuous chromatography chromatographic system, application thereof and method for purifying coenzyme Q10 |
| CN111705168A (en) * | 2020-07-08 | 2020-09-25 | 江南大学 | Method for purifying xylose hydrolysate by desalting with three zones with simulated moving bed |
Citations (3)
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|---|---|---|---|---|
| US6548662B1 (en) * | 1999-01-14 | 2003-04-15 | Sanwa Kosan Kabushiki Kaisha | Method for purification of saccharide |
| CN201283233Y (en) * | 2008-09-28 | 2009-08-05 | 王学群 | Separation device of simulated moving bed chromatography |
| CN101597628A (en) * | 2009-07-03 | 2009-12-09 | 天津科技大学 | The method of preparing xylo-oligosaccharide by corn husk enzymatic hydrolysis |
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| FI962204A0 (en) * | 1996-05-24 | 1996-05-24 | Cultor Oy | Foerfarande Foer fractionation av en loesning |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6548662B1 (en) * | 1999-01-14 | 2003-04-15 | Sanwa Kosan Kabushiki Kaisha | Method for purification of saccharide |
| CN201283233Y (en) * | 2008-09-28 | 2009-08-05 | 王学群 | Separation device of simulated moving bed chromatography |
| CN101597628A (en) * | 2009-07-03 | 2009-12-09 | 天津科技大学 | The method of preparing xylo-oligosaccharide by corn husk enzymatic hydrolysis |
Non-Patent Citations (3)
| Title |
|---|
| Andre´ |
| Andre´s Moure等.Advances in the manufacture, purification and applications of xylo-oligosaccharides as food additives and nutraceuticals.<Process Biochemistry>.2006,第41卷1913–1923. * |
| sMoure等.Advancesinthemanufacture purification and applications of xylo-oligosaccharides as food additives and nutraceuticals.<Process Biochemistry>.2006 |
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