CN102924538A - Method for extracting xylose, arabinose and galactose from xylose fermentation broth or xylose mother liquor - Google Patents
Method for extracting xylose, arabinose and galactose from xylose fermentation broth or xylose mother liquor Download PDFInfo
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- CN102924538A CN102924538A CN 201210427569 CN201210427569A CN102924538A CN 102924538 A CN102924538 A CN 102924538A CN 201210427569 CN201210427569 CN 201210427569 CN 201210427569 A CN201210427569 A CN 201210427569A CN 102924538 A CN102924538 A CN 102924538A
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Abstract
The invention provides a method for extracting xylose, arabinose and galactose from xylose fermentation broth or xylose mother liquor. According to the method, a simulated moving bed chromatographic separation device of sugar alcohol separating resin special for filling is adopted, water serves as an eluent, the separation temperature is 30-90DEG C, the flow rate of feed liquid is controlled at 2-50cm/min, continuous separation and purification of the xylose, the arabinose and the galactose in the xylose fermentation broth or the xylose mother liquor is achieved, and high-purity xylose, arabinose and galactose products are obtained through concentration and crystallization. The method has the advantages of being wide in application range, good in separation effect, high in product purity, environment-friendly and the like.
Description
Technical field
The present invention relates to a kind of from wood-sugar fermentation liquid or xylose mother liquid the method for separation and Extraction wood sugar, pectinose and semi-lactosi, belong to the simulated moving bed chromatography separation technology field.
Background technology
Wood-sugar fermentation liquid refers to that the agricultural byproducts such as corn cob, stalk and bagasse pass through first dilute acid hydrolysis again by the rare thick liquid that obtains behind the microbial fermentation, contain a large amount of wood sugars and a small amount of pectinose and semi-lactosi etc. in the fermented liquid.Mother liquor is to be rich in the dark colour thick liquid that the wood sugar of high density and pectinose solution produce after by twice crystallization, because the assorted sugar such as semi-lactosi and glucose increases through the ratio in mother liquor after the crystallization, traditional crystallization processes can't continue to extract wood sugar and pectinose.Chinese patent 200510040433.0 discloses a kind ofly removes first glucose in xylose hydrolysis fluid or the xylose mother liquid by yeast saccharomyces cerevisiae, the recycling simulated moving bed technology extracts wood sugar or the Xylitol in the solution, the method can not be extracted pectinose and the semi-lactosi with high added value, therefore can only process with 10% price as assorted liquid glucose, greatly reduce the productivity effect of enterprise.Chinese patent 200710014175.8 discloses a kind of xylose solution that utilizes the method acquisition higher degree of complicated sequential simulated moving bed device purifying xylose mother liquor, but the pectinose of high added value and semi-lactosi do not obtain effective separation yet, have significantly reduced the utility value of xylose mother liquid.Chinese patent 200910014319.9 discloses a kind of remover of introducing and has removed wherein glucose in xylose mother liquid, although the method has obtained the pectinose of high added value, its pre-treatment is complicated, and fails wood sugar and semi-lactosi in the effective separation mother liquor.Chinese patent CN102344467A discloses a kind of method of utilizing xylose mother liquid to produce wood sugar and pectinose, it is lower that the method is not only separated the wood sugar and the pectinose solution purity that obtain, and fail to extract semi-lactosi in the xylose mother liquid, the assorted sugar such as semi-lactosi has significantly reduced the crystallization yield of wood sugar and pectinose in the condensing crystal process, has caused the huge loss of resource and the energy.
Because the existing simulated moving bed process of employing can not effectively extract the semi-lactosi in wood-sugar fermentation liquid or the xylose mother liquid, it is generally lower to cause separating the wood sugar and the pectinose product purity that obtain, greatly reduce the yield of product in the follow-up crystallisation process, and be accompanied by and produced a large amount of crystalline mother solutions.In order to take full advantage of the effective constituent in wood-sugar fermentation liquid or the xylose mother liquid, improve the productive rate of crystalline xylose, pectinose and semi-lactosi, need exploitation badly and have the technology of wood sugar, semi-lactosi and pectinose in high efficiency separation wood-sugar fermentation liquid or the xylose mother liquid.
Summary of the invention
For the deficiency that prior art exists, the invention provides a kind of method of from wood-sugar fermentation liquid or xylose mother liquid, extracting wood sugar, pectinose and semi-lactosi of suitable industrial scale production.The method application simulation mobile bed chromatic isolation technique can realize high efficiency separation and the automatic production of three kinds of sugars in the wood-sugar fermentation liquid, and obtains highly purified wood sugar, pectinose and semi-lactosi product.
A kind of main technical schemes of extracting wood sugar in the wood-sugar fermentation liquid, pectinose and semi-lactosi method of the present invention comprises:
1) moving bed imitation chromatogram separation facility is the loop system that the six roots of sensation or the above chromatographic column of the six roots of sensation are formed by connecting from beginning to end.The sugar alcohol separating specific resin of chromatographic column filling independent research, Chinese patent 200510040433.0 is open, utilizes this resin to the difference of the absorption avidity of various sugar alcohols, can realize the separation of multiple sugar in the wood-sugar fermentation liquid.Every root chromatogram column all has one group of pneumatic self control valve, every group of internally piloted valve advances Material valve by one, a water intaking valve, one goes out to be rich in the valve of wood sugar component, a valve that goes out to be rich in the pectinose component, valve and a feed liquid recycle valve composition that goes out to be rich in the valve of semi-lactosi component, the sugar that goes out to contain to mix.The chromatographic column of complete assembly and pipeline are all used the chuck heat tracing, guarantee that the temperature of the interior resin of chromatographic column and solution can the constant temperature of setting.Simulated moving bed chromatography system is according to the unlatching of PLC time variable control pneumatic self control valve, thereby continuous operation when realizing charging and discharging, the direction of district III-district, II-district, I-district V-district, IV-district VI is the liquid flow path direction, and district IV-district, V-district, VI-district II-district, III-district I is the switching direction of chromatographic column.
2) after the xylose hydrolysis fluid fermenting process finished, the disclosed any method in employing this area was removed the macromolecular substance in the fermented liquid;
3) wood-sugar fermentation liquid removes clear liquid that salinity obtains again through vacuum-concentrcted through ion-exchange, and the refractive power concentration of the wood-sugar fermentation clear liquid after control is concentrated is more than 30%; Perhaps do not concentrate after the fermentation clear liquid desalination and directly separate;
4) wood-sugar fermentation liquid or xylose mother liquid or the two mixed solution are adjusted to charging and inflow temperature, namely 30~90 ℃, enter again 1) in simulated movable bed chromatography device separate, the flow rate control of whole system liquid is at 2~50cm/min; Carry out continuously charging and discharging operation, can obtain four class discharging components simultaneously.The first kind is for being rich in wood sugar (wood sugar purity 84%~95%, generally greater than 90%) component, Equations of The Second Kind is for being rich in pectinose (pectinose purity 73~89%, generally greater than 82%) component, the 3rd class is for being rich in the component of semi-lactosi (semi-lactosi purity 55~68% is generally greater than 60%).The component that is rich in wood sugar, pectinose and semi-lactosi is through further obtaining highly purified three kinds of products after concentrated, the crystallization, and assorted sugar component continues to return fermentation system.
Compared with prior art, advantage of the present invention:
1, applied widely, workable, can be applicable to the separating-purifying of wood-sugar fermentation liquid, xylose mother liquid and the two mixed solution;
2, adopt simulation moving-bed separating fully of substantially realizing wood sugar, pectinose and semi-lactosi, obtain highly purified wood sugar and pectinose solution, also can obtain the galactose solution of higher degree simultaneously;
3, processing condition are ripe, environmental protection, and the eluent of production process take water as resin, with low cost, and realized the zero release of pollutent.
Description of drawings
Fig. 1 is wood sugar, pectinose and semi-lactosi production technique
Fig. 2 is the simulated moving bed chromatography zone chart
Embodiment
[embodiment 1]
After the hydrolyzed solution fermentation ends, filter to remove the impurity such as albumen, yeast, ion-exchange removes the salinity in the fermented liquid, obtains refractive power concentration after further concentrated again and be 56% wood-sugar fermentation concentrated solution (wood sugar~60% wherein; Semi-lactosi~12%, pectinose~21%), this solution is entered simulation moving-bed separation, separation condition is as follows: separation temperature is controlled to be 70 ℃, the charging flow velocity of fermented liquid is 5cm/min, the flow velocity of eluting water is 20cm/min, and system reached balance after charging moved 24 hours, and the discharging situation of three components is as follows:
1) wood sugar part: refractive power concentration 27% (volume is 2 times of feeding liquid); Xylose from solutions purity 91%, semi-lactosi purity 3%, pectinose purity 1%;
2) galactose moiety: refractive power concentration is 7% (volume is 1.5 times of feeding liquid); Xylose from solutions purity 25%, semi-lactosi purity 62%, pectinose purity 7%;
3) pectinose part: refractive power concentration is 11% (volume is 1.5 times of feeding liquid); Xylose from solutions purity 4%, semi-lactosi purity 4%, pectinose purity 85%.
Wherein the yield of wood sugar, pectinose and semi-lactosi is respectively 90%, 86% and 80%.
[embodiment 2]
Refractive power concentration (wood sugar~62% wherein that is 68% after the crystalline mother solution of wood sugar, pectinose and semi-lactosi mixes; Semi-lactosi~10%, pectinose~20%) enters simulation moving-bed separation, separation condition is as follows: separation temperature is controlled to be 75 ℃, the charging flow velocity of crystalline mother solution is 3cm/min, the flow velocity of eluting water is 12cm/min, charging operation 24 as a child system reaches balance, and the discharging situation of three components is as follows:
1) wood sugar part: refractive power concentration 32% (volume is 2 times of feeding liquid); Xylose from solutions purity 93%, semi-lactosi purity 2%, pectinose purity 1%;
2) galactose moiety: refractive power concentration is 5% (volume is 1.5 times of feeding liquid); Xylose from solutions purity 24%, semi-lactosi purity 65%, pectinose purity 5%;
3) pectinose part: refractive power concentration is 11% (volume is 1.5 times of feeding liquid); Xylose from solutions purity 7%, semi-lactosi purity 3%, pectinose purity 83%.
Wherein the yield of wood sugar, pectinose and semi-lactosi is respectively 91%, 87% and 89%.
[embodiment 3]
Fermented Condensed liquid and crystalline mother solution are that 3: 1 ratio is mixed according to volume ratio respectively, the refractive power concentration of mixed solution~60% (wood sugar~60% wherein; Semi-lactosi~11%, pectinose~22%) enter simulation moving-bed, separation condition is as follows: separation temperature is controlled to be 70 ℃, the charging flow velocity of crystalline mother solution is 4cm/min, the flow velocity of eluting water is 16cm/min, charging operation 24 as a child system reaches balance, and the discharging situation of three components is as follows:
1) wood sugar part: refractive power concentration 30% (volume is 2 times of feeding liquid); Xylose from solutions purity 90%, semi-lactosi purity 3%, pectinose purity 2%;
2) galactose moiety: refractive power concentration is 6% (volume is 1.5 times of feeding liquid); Xylose from solutions purity 22%, semi-lactosi purity 67%, pectinose purity 4%;
3) pectinose part: refractive power concentration is 11% (volume is 1.5 times of feeding liquid); Xylose from solutions purity 8%, semi-lactosi purity 3%, pectinose purity 83%.
Wherein the yield of wood sugar, pectinose and semi-lactosi is respectively 90%, 85% and 81%.
Although the present invention with preferred embodiment openly as above; but they are not to limit the scope of application of the present invention; any scientific research or staff who is familiar with this technology; without departing from the spirit and scope of the invention; from when can doing various variations or retouching, so being as the criterion of should being defined with the application's claim protection domain of the protection domain of Ben Fanming.
Claims (5)
1. method of from wood-sugar fermentation liquid or xylose mother liquid, extracting wood sugar, pectinose and semi-lactosi, it is characterized in that pretreated wood-sugar fermentation liquid or xylose mother liquid are introduced moving bed imitation chromatogram separation facility, take water as eluent, separation temperature is 30~90 ℃, feed velocity is controlled at 2~50cm/min, has realized the continuous separation and purification of wood sugar, pectinose and semi-lactosi in wood-sugar fermentation liquid or the xylose mother liquid.
2. the method for from wood-sugar fermentation liquid or xylose mother liquid, extracting wood sugar, pectinose and semi-lactosi according to claim 1, it is characterized in that described pretreated wood-sugar fermentation liquid must after filtration except macromolecular substance such as Deproteinizations, remove salinity with ion-exchange again.
3. the method for extracting wood sugar, pectinose and semi-lactosi from wood-sugar fermentation liquid or xylose mother liquid according to claim 1 is characterized in that described moving bed imitation chromatogram separation facility is the loop system that the six roots of sensation or the above chromatographic column of the six roots of sensation are formed by connecting from beginning to end; The resin of chromatographic column filling is sugar alcohol dedicated separation Special Resin; The chromatographic column of complete assembly and pipeline are all used the chuck heat tracing, system is according to the unlatching of PLC time variable control pneumatic self control valve, thereby continuous operation when realizing charging and discharging, the direction of district III-district, II-district, I-district V-district, IV-district VI is the liquid flow path direction, and district IV-district, V-district, VI-district II-district, III-district I is the chromatographic column switching direction.
4. moving bed imitation chromatogram separation facility according to claim 1, it is characterized in that take water as eluent, separation temperature is 30~90 ℃, flow rate control is at 2~50cm/min, can obtain simultaneously four class discharging components after continuously feeding and the discharging, the first kind is that wood sugar purity reaches 84%~95% component, and Equations of The Second Kind pectinose purity reaches 73%~87% component, the 3rd class is that semi-lactosi purity reaches 55%~68%, and the 4th class is assorted sugar component.
5. simulated moving bed chromatography separator column according to claim 3, it is characterized in that described chromatographic column all has one group of pneumatic self control valve, every group of internally piloted valve advances Material valve by one, a water intaking valve, one goes out to be rich in the valve of wood sugar component, a valve that goes out to be rich in the pectinose component, valve and a feed liquid recycle valve composition that goes out to be rich in the valve of semi-lactosi component, the sugar that goes out to contain to mix.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103657152A (en) * | 2013-12-14 | 2014-03-26 | 山东理工大学 | Novel separation system for simulated moving bed chromatography (SMBC) |
CN104611476A (en) * | 2013-11-04 | 2015-05-13 | 南京工业大学 | Xylose and arabinose separating method |
CN105001272A (en) * | 2015-06-24 | 2015-10-28 | 济南圣泉集团股份有限公司 | Treating method for xylose mother liquor |
CN106589010A (en) * | 2016-12-16 | 2017-04-26 | 南京凯通粮食生化研究设计有限公司 | Method for simultaneously producing L-arabinose and D-galactose |
CN111747997A (en) * | 2020-07-08 | 2020-10-09 | 江南大学 | Method for simultaneously preparing xylose, arabinose and galactose by using intermittent simulated moving bed chromatography |
CN112079886A (en) * | 2020-09-17 | 2020-12-15 | 甘肃赫原生物制品有限公司 | Method for improving purity of xylose and arabinose by chromatographic separation |
-
2012
- 2012-10-31 CN CN 201210427569 patent/CN102924538A/en active Pending
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104611476A (en) * | 2013-11-04 | 2015-05-13 | 南京工业大学 | Xylose and arabinose separating method |
CN104611476B (en) * | 2013-11-04 | 2018-04-27 | 南京工业大学 | A kind of xylose method separated with arabinose |
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) |
CN105001272A (en) * | 2015-06-24 | 2015-10-28 | 济南圣泉集团股份有限公司 | Treating method for xylose mother liquor |
CN106589010A (en) * | 2016-12-16 | 2017-04-26 | 南京凯通粮食生化研究设计有限公司 | Method for simultaneously producing L-arabinose and D-galactose |
CN106589010B (en) * | 2016-12-16 | 2019-07-19 | 南京凯通粮食生化研究设计有限公司 | Method that is a kind of while producing L-arabinose and D- galactolipin |
CN111747997A (en) * | 2020-07-08 | 2020-10-09 | 江南大学 | Method for simultaneously preparing xylose, arabinose and galactose by using intermittent simulated moving bed chromatography |
CN111747997B (en) * | 2020-07-08 | 2022-02-01 | 江南大学 | Method for simultaneously preparing xylose, arabinose and galactose by using intermittent simulated moving bed chromatography |
CN112079886A (en) * | 2020-09-17 | 2020-12-15 | 甘肃赫原生物制品有限公司 | Method for improving purity of xylose and arabinose by chromatographic separation |
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Application publication date: 20130213 |