CN102952165B - A kind of method extracting L-arabinose from xylose mother liquid - Google Patents
A kind of method extracting L-arabinose from xylose mother liquid Download PDFInfo
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- CN102952165B CN102952165B CN201110243243.4A CN201110243243A CN102952165B CN 102952165 B CN102952165 B CN 102952165B CN 201110243243 A CN201110243243 A CN 201110243243A CN 102952165 B CN102952165 B CN 102952165B
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- 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
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Abstract
The invention provides a kind of method extracting L-arabinose from xylose mother liquid, the method comprises the fermentation of xylose mother liquid, purification, concentration process, crystal grain is carried out gradation by xylose mother liquid crystallization after concentrated again, collects small-particle crystallization, obtains L-arabinose.The method just achieves being separated, for scale operation L-arabinose is laid a good foundation of wood sugar and L-arabinose by simple gradation.
Description
Technical field
The present invention relates to chemical field, particularly, relate to a kind of method extracting L-arabinose from xylose mother liquid.
Background technology
L-arabinose is a kind of broad-spectrum five-carbon sugar, is mainly present in polymer form in the hemicellulose of plant.In the dry-matter of higher plant generally containing have an appointment 20 ~ 35% hemicellulose, and hemicellulose is primarily of wood sugar and L-arabinose composition.In addition, L-arabinose is also present in the plant colloids such as gum arabic in large quantities.Because the output of hemicellulose is huge, therefore wood sugar and L-arabinose can be prepared in a large number by the hemicellulose in hydrolysis higher plant.
Containing multiple monose in hemicellulose hydrolysate, based on wood sugar, and glucose, L-arabinose, semi-lactosi etc.Because the monose overwhelming majority in hemicellulose hydrolysate is wood sugar, so first xylose crystalline can be separated by the method for crystallization, until wood sugar cannot recrystallize, remaining mother liquor is called xylose mother liquid.According to liquid-phase chromatographic analysis (Agriculture of Anhui science, 2009,37 (5): 1881-1882, " PHLC method measures the composition of xylose mother liquid "), containing 38.10% wood sugar in xylose mother liquid, 23.70%L-pectinose, 13.80% glucose, 9.89% semi-lactosi.Separation and Extraction L-arabinose from xylose mother liquid is at present generally adopt simulated moving bed chromatography isolation technique, and because this investment in machinery and equipment is large, but production capacity is little, makes L-arabinose cannot meet the demand in market.
L-arabinose, except mainly from hydrolysis of hemicellulose preparation, can also contain the vegetable jelly of L-arabinose as prepared gum arabic from some.According to analysis, the set of monomers of gum arabic becomes: semi-lactosi 42%, L-arabinose 31%, rhamnosyl 13%, glucuronic acid 13%, 4-O-methyl glucose uronic acid 1%.As Chinese patent 02116353.7 discloses a kind of method that gum arabic extracts L-arabinose, but mixing monose still needs could be separated by two column chromatographies to obtain L-arabinose, is difficult to industrialization.Paper " from gum arabic hydrolyzed solution Crystallization Separation L-arabinose " (chemical industry and engineering, 2007,24 (5): 398-400) separation method described is: gum arabic dilute sulphuric acid be hydrolyzed and hydrolyzed solution after neutralizing through fermentation removing semi-lactosi, then in methyl alcohol, Crystallization Separation obtains thick L-arabinose, in the thick L-arabinose aqueous solution, then add ethanol and crystallization obtain 97.5% L-arabinose.The method due to the L-arabinose in methanol crystallization mother liquor and alcohol crystal mother liquor cannot Separation and Recovery, so yield is not high, the highest only have 50% of theoretical yield, thus cost is higher.
Owing to adopting existing method to produce L-arabinose, not only output is little but also cost remains high, thus limits this universal use possessing the functional sugar of good nourishing function.For this reason, the large scale production method developing L-arabinose is needed.
Summary of the invention
In order to overcome above-mentioned shortcoming, the invention provides a kind of method extracting L-arabinose from xylose mother liquid, just achieving being separated, for scale operation L-arabinose is laid a good foundation of wood sugar and L-arabinose by simple gradation.
Xylose mother liquid is utilized to prepare L-arabinose, generally the first whole glucose of fermentation removing, or all or part of removing semi-lactosi simultaneously, then purify, be separated.The applicant is found by the crystallization property of the xylose mother liquid after research purification, there will be two kinds of crystallizations during xylose mother liquid crystallization, first the first crystallization occurs, finally become the larger crystallization of diameter (abbreviation large particle crystal), the second crystallization then occurs later, its diameter more much smaller than the first (being called for short small-particle crystallization); The present inventor further by gradation mode large particle crystal and small-particle Crystallization Separation out, then measure its composition, find that large particle crystal is essentially wood sugar surprisingly, small-particle crystallization is then essentially L-arabinose.Obviously, on the basis of above-mentioned discovery, the crystallization formed in xylose mother liquid by simple gradation, just can obtain the thick L-arabinose that purity is higher, more just can obtain pure L-arabinose by recrystallization.
Technical scheme of the present invention is as follows: a kind of method extracting L-arabinose from xylose mother liquid, the method comprises the fermentation of xylose mother liquid, purification, concentration process, by the xylose mother liquid crystallization after concentrated, form the large particle crystal with large and small difference and small-particle crystallization to magma after, crystal grain is carried out gradation, collect small-particle crystallization, namely obtain L-arabinose.
The fermentation of described xylose mother liquid is inoculation yeast bacterium fermentation in xylose mother liquid, removing glucose and all or part of removing semi-lactosi.
The purification of described xylose mother liquid comprises the xylose mother liquid activated carbon decolorizing after by fermentation and/or spent ion exchange resin removes ion.
Described xylose mother liquid concentrated be by purification after xylose mother liquid obtain through underpressure distillation the syrup that refractive power pol is 80-86%.
Crystal seed is added before described xylose mother liquid crystallization.
Described gradation, being the method with two class Crystallization Separation of large and small difference being formed in same crystallizer, comprising screening, centrifugal settling or gravity settling method.
After described xylose mother liquid crystallization, carry out gradation when magma removes crystalline mother solution simultaneously, or carry out the gradation of crystallization again collect crystallization from magma after;
After described gradation, collect large particle crystal, be thick wood sugar, then carry out recrystallization and obtain pure wood sugar.
Be separated the crystalline mother solution of gained after the crystallization in magma, repeat fermentation, purification, concentrated, crystallization and gradation process, until L-arabinose is wherein extracted complete.
The L-arabinose obtained is carried out recrystallization, obtains pure L-arabinose.
A kind of method extracting L-arabinose from xylose mother liquid of the present invention, on the basis of this discovery xylose mother liquid crystallization new features, adopt simple gradation method, can extract from xylose mother liquid and obtain pure L-arabinose, the method process is simple, output is large, and without the need to adopting traditional chromatographic separation technology, the applying of rare functional sugar for L-arabinose is this with special healthy functions is laid a good foundation.
Embodiment
Embodiment 1
Brewer's dried yeasts is accessed after xylose mother liquid dilution, until glucose is all fermented completely, yeast thalline is removed with butterfly centrifugal machine, be heated to 60 DEG C with activated carbon decolorizing 45 minutes, use pressure filter removal activity charcoal again, the method of gained liquid glucose underpressure distillation is condensed into the syrup that refractive power pol is 82%, and syrup delivery is accessed crystal seed, then crystallisation by cooling to crystallizer.In crystallisation process, microscopy is carried out in sampling, the crystallization initial stage only has the very uniform crystal of a kind of size, new crystal is there is again after for some time, when the degree of supersaturation of syrup is full-time close to ruing out of, the two class crystalline particles that size differences is very large are formed, i.e. large particle crystal and small-particle crystallization in magma.Magma is added in 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 small-particle crystallization is settled down and collects, 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
Centrifugal for magma in embodiment 1 gained crystalline mother solution is re-started underpressure distillation, obtain the syrup that refractive power pol is 85%, syrup delivery is accessed crystal seed, then crystallisation by cooling to crystallizer.In crystallisation process, microscopy is carried out in sampling, the crystallization initial stage only has the very uniform crystal of a kind of size, new crystal is there is again after for some time, when the degree of supersaturation of syrup is full-time close to ruing out of, the two class crystalline particles that size differences is larger are formed, i.e. large particle crystal and small-particle crystallization in magma.Magma is added in filtering centrifuge and filters out crystalline mother solution, obtain the mixed crystallization powder containing large particle crystal and small-particle crystallization.
Get this mixed crystallization powder mix with 95% ethanol of 10 times and stir, add continuously in horizontal spiral discharge sedimentation centrifuge, adjusting rotary speed and flow, the solid phase obtained is large particle crystal, be thick wood sugar, purity is 85%, and liquid phase enters and removes ethanol in filtering centrifuge and obtain small-particle crystallization, be thick L-arabinose, purity is 63%; Obtain pure wood sugar after large particle crystal water recrystallization, obtain pure L-arabinose after small-particle crystallization water recrystallization.
Embodiment 3
The mixed crystallization powder of the centrifugal gained of Example 2 mixes with the dehydrated alcohol of 5 times and stirs, add in cross-current type grading machine continuously, flow media is also dehydrated alcohol, collect large particle crystal and small-particle crystallization respectively, wherein the thick xylose 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 are carried out recrystallization with water respectively, obtain pure wood sugar and pure L-arabinose respectively.
Embodiment 4
After centrifugal for magma in embodiment 2 crystalline mother solution is out decoloured again, simmer down to refractive power pol is the syrup of 86%, and syrup delivery is accessed crystal seed, then crystallisation by cooling to crystallizer.In crystallisation process, microscopy is carried out in sampling, the crystallization initial stage only has the very uniform crystal of a kind of size, new crystal is there is again after for some time, when the degree of supersaturation of syrup is full-time close to ruing out of, the two class crystalline particles that size differences is larger are formed, i.e. large particle crystal and small-particle crystallization in magma.Magma is added in filtering centrifuge and filters out crystalline mother solution, obtain the mixed crystallization powder containing large particle crystal and small-particle crystallization.
95% ethanol of the mixed crystallization powder of gained with 10 times is mixed and stirred, then adds and eluriate in grading machine, collect large particle crystal and small-particle crystallization respectively; Follow-up 95% ethanol that adds equally is for eluriating liquid and carrying out repeating to eluriate, and the xylose 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 are carried out recrystallization with water respectively, obtain pure wood sugar and pure L-arabinose respectively.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For 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 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 submitted to claims.
Claims (7)
1. one kind is extracted the method for L-arabinose from xylose mother liquid, the method comprises the fermentation of xylose mother liquid, purification, concentration process, it is characterized in that: by the xylose mother liquid crystallization after concentrated, form the large particle crystal with large and small difference and small-particle crystallization to magma after, crystal grain is carried out gradation, collect small-particle crystallization, namely obtain L-arabinose;
Wherein, the fermentation of described xylose mother liquid is inoculation yeast bacterium fermentation in xylose mother liquid, removing glucose and all or part of removing semi-lactosi; The purification of described xylose mother liquid comprises the xylose mother liquid activated carbon decolorizing after by fermentation and/or spent ion exchange resin removes ion; Described xylose mother liquid concentrated be by purification after xylose mother liquid obtain through underpressure distillation the syrup that refractive power pol is 80-86%.
2. from xylose mother liquid, extract the method for L-arabinose as claimed in claim 1, it is characterized in that, before the crystallization of described xylose mother liquid, add crystal seed.
3. from xylose mother liquid, extract the method for L-arabinose as claimed in claim 1, it is characterized in that, described gradation, being the method with two class Crystallization Separation of large and small difference being formed in same crystallizer, comprising screening, centrifugal settling or gravity settling method.
4. from xylose mother liquid, extract the method for L-arabinose as claimed in claim 1, it is characterized in that, after described xylose mother liquid crystallization, carry out gradation when magma removes crystalline mother solution simultaneously, or carry out the gradation of crystallization again collect crystallization from magma after.
5. from xylose mother liquid, extract the method for L-arabinose as claimed in claim 1, it is characterized in that, after described gradation, collect large particle crystal, be thick wood sugar, then carry out recrystallization and obtain pure wood sugar.
6. from xylose mother liquid, extract the method for L-arabinose as claimed in claim 1, it is characterized in that, be separated the xylose mother liquid after the crystallization that obtains, repeat fermentation, purification, concentrated, crystallization and gradation process, until L-arabinose is wherein extracted complete.
7. from xylose mother liquid, extract the method for L-arabinose as claimed in claim 1, it is characterized in that, the L-arabinose that obtains obtained is carried out recrystallization, obtains pure L-arabinose.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| CN102952165A CN102952165A (en) | 2013-03-06 |
| CN102952165B true CN102952165B (en) | 2016-01-20 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023116302A1 (en) | 2021-12-26 | 2023-06-29 | 浙江华康药业股份有限公司 | Method for co-producing erythritol and arabinose from xylose mother liquor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103610020B (en) * | 2013-11-25 | 2015-05-13 | 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 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4857642A (en) * | 1986-12-31 | 1989-08-15 | Uop | Process for separating arabinose from a mixture of other aldoses |
| 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 |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004261039A (en) * | 2003-02-28 | 2004-09-24 | Unitika Ltd | L-arabinose-containing crystalline powder sugar composition and method for producing the same |
| 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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2011
- 2011-08-23 CN CN201110243243.4A patent/CN102952165B/en active Active
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- 2012-03-16 WO PCT/CN2012/072423 patent/WO2013026275A1/en active Application Filing
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4857642A (en) * | 1986-12-31 | 1989-08-15 | Uop | Process for separating arabinose from a mixture of other aldoses |
| 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023116302A1 (en) | 2021-12-26 | 2023-06-29 | 浙江华康药业股份有限公司 | Method for co-producing erythritol and arabinose from xylose mother liquor |
| US11866756B2 (en) | 2021-12-26 | 2024-01-09 | Zhejiang Huakang Pharmaceutical Co., Ltd. | Methods for co-producing erythritol and arabinose by using xylose mother liquor |
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| CN102952165A (en) | 2013-03-06 |
| WO2013026275A1 (en) | 2013-02-28 |
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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 |