CN102952165A - Method for extracting L-arabinose from xylose mother liquid - Google Patents
Method for extracting L-arabinose from xylose mother liquid Download PDFInfo
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- CN102952165A CN102952165A CN2011102432434A CN201110243243A CN102952165A CN 102952165 A CN102952165 A CN 102952165A CN 2011102432434 A CN2011102432434 A CN 2011102432434A CN 201110243243 A CN201110243243 A CN 201110243243A CN 102952165 A CN102952165 A CN 102952165A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
- C07H3/02—Monosaccharides
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Abstract
The invention provides a method for extracting L-arabinose from a xylose mother liquid. The method comprises the following processes: fermenting the xylose mother liquid, purifying the xylose mother liquid, concentrating the xylose mother liquid, crystallizing the concentrated xylose mother liquid, carrying out particle grading of the obtained crystal particles, and collecting small-granule crystals to obtain the L-arabinose. The method realizes the separation of the xylose and the L-arabinose through simple particle grading, and lays a foundation for the large-scale production of the L-arabinose.
Description
Technical field
The present invention relates to chemical field, particularly, relate to a kind of method of from xylose mother liquid, extracting L-arabinose.
Background technology
L-arabinose is a kind of broad-spectrum five-carbon sugar, and mainly the form with polymkeric substance is present in the hemicellulose of plant.Generally contain 20~35% the hemicellulose of having an appointment in the dry-matter of higher plant, and hemicellulose is comprised of wood sugar and L-arabinose mainly.In addition, L-arabinose also is present in the plant colloids such as gum arabic in large quantities.Because the output of hemicellulose is huge, therefore can prepare in a large number wood sugar and L-arabinose by the hemicellulose in the hydrolysis higher plant.
Contain multiple monose in the hemicellulose hydrolysate, take wood sugar as main, and glucose, L-arabinose, semi-lactosi etc.Because the monose overwhelming majority in the hemicellulose hydrolysate is wood sugar, so can at first separate xylose crystalline by the method for crystallization, until wood sugar can't recrystallize, the mother liquor of remainder is called xylose mother liquid.According to liquid-phase chromatographic analysis (Agriculture of Anhui science, 2009,37 (5): 1881-1882, " the PHLC method is measured the composition of xylose mother liquid "), contain 38.10% wood sugar in the xylose mother liquid, the 23.70%L-pectinose, 13.80% glucose, 9.89% semi-lactosi.Present separation and Extraction L-arabinose from xylose mother liquid generally is to adopt the simulated moving bed chromatography isolation technique, because this investment in machinery and equipment is large, but production capacity is little, makes the demand that L-arabinose can't satisfying the market.
L-arabinose is except mainly from hydrolysis of hemicellulose preparation, can also contain the vegetable jelly of L-arabinose such as the gum arabic from some to prepare.According to analysis, the monomer composition of gum arabic is: semi-lactosi 42%, L-arabinose 31%, rhamnosyl 13%, glucuronic acid 13%, 4-O-methyl glucoside aldehydic acid 1%.Disclose a kind of method of extracting L-arabinose with gum arabic such as Chinese patent 02116353.7, still needed to separate by two column chromatographies and obtain L-arabinose but mix monose, be difficult to industrialization.Paper " Crystallization Separation L-arabinose from the gum arabic hydrolyzed solution " (chemical industry and engineering, 2007,24 (5): the separation method of 398-400) describing is: the hydrolyzed solution after the hydrolysis of gum arabic dilute sulphuric acid and the neutralization is removed semi-lactosi through fermentation, then Crystallization Separation makes thick L-arabinose in methyl alcohol, then adds ethanol in the thick L-arabinose aqueous solution and crystallization obtains 97.5% L-arabinose.The method is because the L-arabinose in methanol crystallization mother liquor and the alcohol crystal mother liquor can't Separation and Recovery, so yield is not high, the highest only have 50% of theoretical yield, thereby cost is higher.
Not only output is little but also cost high owing to adopting existing method to produce L-arabinose, thereby has limited this universal use that possesses the functional sugar of good nourishing function.For this reason, the large scale production method that needs the exploitation L-arabinose.
Summary of the invention
In order to overcome above-mentioned shortcoming, the invention provides a kind of method of from xylose mother liquid, extracting L-arabinose, just realized separating of wood sugar and L-arabinose by simple gradation, for the scale operation L-arabinose is laid a good foundation.
Utilize xylose mother liquid to prepare L-arabinose, whole glucose is removed in general at first fermentation, and perhaps then all or part of semi-lactosi of removing of while purifies, separates.The crystallization property of the xylose mother liquid after the applicant purifies by research is found, two kinds of crystallizations can appear during the xylose mother liquid crystallization, the first crystallization at first occurs, become at last the larger crystallization of diameter (abbreviation large particle crystal), the second crystallization then occurs later, and its diameter is than the first much smaller (being called for short the small-particle crystallization); Then the inventor further mode by gradation large particle crystal and small-particle Crystallization Separation out measures its composition, finds that surprisingly large particle crystal is essentially wood sugar, and the small-particle crystallization then is essentially L-arabinose.Obviously, on the basis of above-mentioned discovery, by simple gradation, just can obtain the higher thick L-arabinose of purity to the crystallization that forms in the xylose mother liquid, just can obtain pure L-arabinose by recrystallization again.
Technical scheme of the present invention is as follows: a kind of method of extracting L-arabinose from xylose mother liquid, the method comprises fermentation, purification, the concentration process of xylose mother liquid, with the xylose mother liquid crystallization after concentrated, form to the magma have the large particle crystal and small-particle crystallization of large and small difference after, crystal grain is carried out gradation, collect the small-particle crystallization, namely obtain L-arabinose.
The fermentation of described xylose mother liquid is inoculation yeast bacterium fermentation in xylose mother liquid, removes glucose and all or part of semi-lactosi of removing.
The purification of described xylose mother liquid comprise with the fermentation after xylose mother liquid remove ion with activated carbon decolorizing and/or spent ion exchange resin.
The concentrated of described xylose mother liquid is that the xylose mother liquid after purifying is obtained the syrup that the refractive power pol is 80-86% through underpressure distillation.
Add crystal seed before the described xylose mother liquid crystallization.
Described gradation is the method for the two class Crystallization Separation with large and small difference that form in the same crystallizer, comprises screening, centrifugal settling or gravity settling method.
After the described xylose mother liquid crystallization, when magma removes crystalline mother solution, carry out simultaneously gradation, perhaps from magma, collect the gradation that carries out again crystallization after the crystallization;
Behind the described gradation, collect large particle crystal, be thick wood sugar, carry out recrystallization again and obtain pure wood sugar.
The crystalline mother solution that separates gained after the crystallization in the magma repeats fermentation, purifies, concentrated, crystallization and gradation process, until complete L-arabinose extraction wherein.
The L-arabinose that obtains is carried out recrystallization, obtain pure L-arabinose.
A kind of method of from xylose mother liquid, extracting L-arabinose of the present invention, on the basis of this discovery xylose mother liquid crystallization new features, adopt simple gradation method, can from xylose mother liquid, extract and obtain pure L-arabinose, the method process is simple, output is large, need not to adopt traditional chromatographic separation technology, and the applying of rare functional sugar that has special healthy functions for L-arabinose is this laid a good foundation.
Embodiment
Embodiment 1
Access brewer's dried yeasts after the xylose mother liquid dilution, until the whole fermentation finished thoroughly1s of glucose, remove the yeast thalline with the butterfly centrifugal machine, be heated to 60 ℃ with activated carbon decolorizing 45 minutes, use again pressure filter removal activity charcoal, it is 82% syrup that the gained liquid glucose is condensed into the refractive power pol with the method for underpressure distillation, syrup delivery to crystallizer and access crystal seed, crystallisation by cooling then.Microscopy is carried out in sampling in the crystallisation process, the crystallization initial stage only has very uniformly crystal of a kind of size, new crystal appearred again after for some time, when the degree of supersaturation of syrup approach run out of full-time, form two very large class crystalline particles of size differences, i.e. large particle crystal and small-particle crystallization in the magma.Magma is added in the three-column settle centrifuge, and first low speed settles down large particle crystal and collects, and is thick wood sugar, and purity is 82%; Then improve centrifuge speed and the small-particle crystallization is settled down and collect, be thick L-arabinose, purity is 61%; Large particle crystal water recrystallization is obtained pure wood sugar, small-particle crystallization water recrystallization is obtained pure L-arabinose.
Embodiment 2
The centrifugal gained crystalline mother solution of magma among the embodiment 1 is re-started underpressure distillation, obtains the refractive power pol and be 85% syrup, syrup delivery to crystallizer and access crystal seed, crystallisation by cooling then.Microscopy is carried out in sampling in the crystallisation process, the crystallization initial stage only has very uniformly crystal of a kind of size, new crystal appearred again after for some time, when the degree of supersaturation of syrup approach run out of full-time, form two larger class crystalline particles of size differences, i.e. large particle crystal and small-particle crystallization in the magma.Filtering out crystalline mother solution in the magma adding filtering centrifuge, obtain containing the mixed crystallization powder of large particle crystal and small-particle crystallization.
Getting this mixed crystallization powder mixes with 10 times 95% ethanol and stirs, add continuously in the horizontal spiral discharge sedimentation centrifuge, adjusting rotary speed and flow, the solid phase that obtains is large particle crystal, be thick wood sugar, purity is 85%, and liquid phase enters and removes ethanol in the filtering centrifuge and obtain the small-particle crystallization, be thick L-arabinose, purity is 63%; Obtaining pure wood sugar behind the large particle crystal water recrystallization, obtaining pure L-arabinose behind the small-particle crystallization water recrystallization.
Embodiment 3
The mixed crystallization powder of getting embodiment 2 centrifugal gained mixes with 5 times dehydrated alcohol and stirs, add continuously in the cross-current type grading machine, flow media also is dehydrated alcohol, collect respectively large particle crystal and small-particle crystallization, wherein the thick wood sugar purity of large particle crystal is 87%, and the thick L-arabinose purity of small-particle crystallization is 68%; Again large particle crystal and small-particle crystallization respectively water carry out recrystallization, obtain respectively pure wood sugar and pure L-arabinose.
Embodiment 4
Be the centrifugal crystalline mother solution out of magma among the embodiment 2 rear simmer down to refractive power pol of again decolouring 86% syrup, syrup delivery to crystallizer and access crystal seed, crystallisation by cooling then.Microscopy is carried out in sampling in the crystallisation process, the crystallization initial stage only has very uniformly crystal of a kind of size, new crystal appearred again after for some time, when the degree of supersaturation of syrup approach run out of full-time, form two larger class crystalline particles of size differences, i.e. large particle crystal and small-particle crystallization in the magma.Filtering out crystalline mother solution in the magma adding filtering centrifuge, obtain containing the mixed crystallization powder of large particle crystal and small-particle crystallization.
The mixed crystallization powder of gained is mixed with 10 times 95% ethanol and stir, then add and eluriate in the grading machine, collect respectively large particle crystal and small-particle crystallization; Follow-up same adding 95% ethanol is eluriated for eluriating liquid and repeating, and the wood sugar purity of gained large particle crystal is 91%, and the L-arabinose purity of small-particle crystallization is 76%; Again large particle crystal and small-particle crystallization respectively water carry out recrystallization, obtain respectively pure wood sugar and pure L-arabinose.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that implementation of the present invention is confined to these explanations.For the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, its framework form can be flexible and changeable, can the subseries product.Just make some simple deduction or replace, all should be considered as belonging to the scope of patent protection that the present invention is determined by claims of submitting to.
Claims (10)
1. method of from xylose mother liquid, extracting L-arabinose, the method comprises fermentation, purification, the concentration process of xylose mother liquid, it is characterized in that: the xylose mother liquid crystallization after will concentrating, form to the magma have the large particle crystal and small-particle crystallization of large and small difference after, crystal grain is carried out gradation, collect the small-particle crystallization, namely obtain L-arabinose.
2. the method for extracting L-arabinose from xylose mother liquid as claimed in claim 1 is characterized in that, the fermentation of described xylose mother liquid is inoculation yeast bacterium fermentation in xylose mother liquid, removes glucose and all or part of semi-lactosi of removing.
3. the method for extracting L-arabinose from xylose mother liquid as claimed in claim 1 is characterized in that, the purification of described xylose mother liquid comprises the xylose mother liquid after the fermentation is removed ion with activated carbon decolorizing and/or spent ion exchange resin.
4. the method for extracting L-arabinose from xylose mother liquid as claimed in claim 1 is characterized in that, the concentrated of described xylose mother liquid is that the xylose mother liquid after purifying is obtained the syrup that the refractive power pol is 80-86% through underpressure distillation.
5. the method for extracting L-arabinose from xylose mother liquid as claimed in claim 1 is characterized in that, adds crystal seed before the crystallization of described xylose mother liquid.
6. the method for from xylose mother liquid, extracting L-arabinose as claimed in claim 1, it is characterized in that, described gradation is the method for the two class Crystallization Separation with large and small difference that form in the same crystallizer, comprises screening, centrifugal settling or gravity settling method.
7. the method for from xylose mother liquid, extracting L-arabinose as claimed in claim 1, it is characterized in that, after the described xylose mother liquid crystallization, when magma removes crystalline mother solution, carry out simultaneously gradation, perhaps from magma, collect the gradation that carries out again crystallization after the crystallization.
8. the method for extracting L-arabinose from xylose mother liquid as claimed in claim 1 is characterized in that, behind the described gradation, collects large particle crystal, is thick wood sugar, carries out recrystallization again and obtains pure wood sugar.
9. the method for from xylose mother liquid, extracting L-arabinose as claimed in claim 1, it is characterized in that, separate the xylose mother liquid after the crystallization obtain, repeat fermentation, purify, concentrated, crystallization and gradation process, until complete L-arabinose extraction wherein.
10. the method for extracting L-arabinose from xylose mother liquid as claimed in claim 1 is characterized in that, the L-arabinose that obtains that obtains is carried out recrystallization, obtains pure L-arabinose.
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CN201110243243.4A CN102952165B (en) | 2011-08-23 | 2011-08-23 | A kind of method extracting L-arabinose from xylose mother liquid |
PCT/CN2012/072423 WO2013026275A1 (en) | 2011-08-23 | 2012-03-16 | Process for extracting l-arabinose from xylose mother liquid |
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CN201110243243.4A CN102952165B (en) | 2011-08-23 | 2011-08-23 | A kind of method extracting L-arabinose from xylose mother liquid |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103610020A (en) * | 2013-11-25 | 2014-03-05 | 通辽梅花生物科技有限公司 | Sieving type monosodium glutamate crystallization and separation process and equipment |
CN106350613A (en) * | 2016-08-31 | 2017-01-25 | 广西农垦糖业集团昌菱制糖有限公司 | Crystalline sugar mother liquor purifying recycling method |
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CN114181268B (en) | 2021-12-26 | 2023-08-11 | 浙江华康药业股份有限公司 | Method for co-producing erythritol and arabinose by xylose mother liquor |
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US4857642A (en) * | 1986-12-31 | 1989-08-15 | Uop | Process for separating arabinose from a mixture of other aldoses |
JP2004261039A (en) * | 2003-02-28 | 2004-09-24 | Unitika Ltd | L-arabinose-containing crystalline powder sugar composition and method for producing the same |
CN101659681A (en) * | 2009-09-30 | 2010-03-03 | 济南圣泉集团股份有限公司 | Method for producing wood sugar product |
CN101880329A (en) * | 2009-05-04 | 2010-11-10 | 陈培豪 | Method for preparing plant hemicellulose hydrolysis liquid and method for extracting xylose and gum sugar |
CN101921810A (en) * | 2010-06-11 | 2010-12-22 | 广西民族大学 | Method for preparing xylitol and L-arabinose mixed crystal from xylose mother liquid |
CN102093435A (en) * | 2009-12-09 | 2011-06-15 | 陈培豪 | Method for extracting arabinose from arabinose-containing mixed sugar |
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US7498430B2 (en) * | 2004-11-09 | 2009-03-03 | Board Of Trustees Of Michigan State University | Process for the preparation and separation of arabinose and xylose from a mixture of saccharides |
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US4857642A (en) * | 1986-12-31 | 1989-08-15 | Uop | Process for separating arabinose from a mixture of other aldoses |
JP2004261039A (en) * | 2003-02-28 | 2004-09-24 | Unitika Ltd | L-arabinose-containing crystalline powder sugar composition and method for producing the same |
CN101880329A (en) * | 2009-05-04 | 2010-11-10 | 陈培豪 | Method for preparing plant hemicellulose hydrolysis liquid and method for extracting xylose and gum sugar |
CN101659681A (en) * | 2009-09-30 | 2010-03-03 | 济南圣泉集团股份有限公司 | Method for producing wood sugar product |
CN102093435A (en) * | 2009-12-09 | 2011-06-15 | 陈培豪 | Method for extracting arabinose from arabinose-containing mixed sugar |
CN101921810A (en) * | 2010-06-11 | 2010-12-22 | 广西民族大学 | Method for preparing xylitol and L-arabinose mixed crystal from xylose mother liquid |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103610020A (en) * | 2013-11-25 | 2014-03-05 | 通辽梅花生物科技有限公司 | Sieving type monosodium glutamate crystallization and separation process and equipment |
CN106350613A (en) * | 2016-08-31 | 2017-01-25 | 广西农垦糖业集团昌菱制糖有限公司 | Crystalline sugar mother liquor purifying recycling method |
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Application publication date: 20130306 Assignee: Song Huaying Assignor: Chen Peihao Contract record no.: X2021210000012 Denomination of invention: A method of extracting L-arabinose from xylose mother liquor Granted publication date: 20160120 License type: Common License Record date: 20210323 |
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