CN104611476B - A kind of xylose method separated with arabinose - Google Patents
A kind of xylose method separated with arabinose Download PDFInfo
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- CN104611476B CN104611476B CN201310539010.8A CN201310539010A CN104611476B CN 104611476 B CN104611476 B CN 104611476B CN 201310539010 A CN201310539010 A CN 201310539010A CN 104611476 B CN104611476 B CN 104611476B
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- xylose
- ion
- exchange
- arabinose
- mother liquor
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- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K13/00—Sugars not otherwise provided for in this class
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/36—Selective adsorption, e.g. chromatography characterised by the separation mechanism involving ionic interaction
- B01D15/361—Ion-exchange
- B01D15/362—Cation-exchange
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K13/00—Sugars not otherwise provided for in this class
- C13K13/002—Xylose
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K13/00—Sugars not otherwise provided for in this class
- C13K13/007—Separation of sugars provided for in subclass C13K
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
It is used for xylose method separated with arabinose as chromatograph packing material the present invention relates to a kind of ion-exchange fibre, using ion-exchange fibre as chromatographic isolation filler, for the method that separation prepares high-purity xylose and arabinose in xylose crystallization mother liquor；The ion-exchange fibre is strong acidic ion-exchange fiber, a diameter of 8~170 μm under drying regime, cation exchange capacity is 2.0~4.3mmol/g, before being separated for xylose crystallization mother liquor, the displacement of progress calcium ion in advance is needed, completes the conversion from Hydrogen to calcium type.Compared with ion-exchange particles resin chromatography column, strong acidic ion-exchange fiber shows the production efficiency of more excellent separation accuracy and higher.
Description
Technical field
The present invention relates to one kind to use strong acidic ion-exchange fiber as chromatography new packing, from xylose crystallization mother liquor
The process of high-purity xylose and arabinose is separated, belongs to technical field of chromatography separation.
Background technology
Country's xylose production process is to obtain Xylose under acid hydrolysis conditions with corncob or bagasse at present, in xylose
In crystallization process, since miscellaneous sugar content is high, a large amount of xyloses in crystalline mother solution are difficult to crystallize out, and final xylose crystallization mother liquor is big
Part is used as pigment raw material and handles at a low price, and utility value is very low.Due to several monose physical chemistry in xylose crystallization mother liquor
Matter is very close, therefore it is larger to isolate and purify difficulty.Monose process for separation and purification common at present mainly has：Chemical method, film point
From method, biological fermentation process and chromatography.Chemical method can efficiently separate xylose and arabinose, but due to needs pair
Monose performs the derivatization reaction, and technique is cumbersome, and needs to add substantial amounts of organic solvent in mother liquor, is not suitable for food-grade carbohydrate
Production.Membrane separation process separates monose using the selective penetrated property of film, suitable for the liquid glucose system that molecular weight difference is larger.
In xylose crystallization mother liquor, glucose and galactolipin are aldohexose, and xylose and arabinose are aldopentose, and molecular weight difference is little,
Although therefore having certain enrichment to pentose using UF membrane, it is completely separated, is still needed to permeate it can be difficult to realizing
It is further separated.Microbial method is the direction of current green chemistry, but microorganism and the on the high side of enzyme are always
The important restriction factor that this method is promoted.At present in medicine and food-grade carbohydrate industrial production, using chromatographic separation technology, from xylose
Separating xylose in crystalline mother solution.Used special chromatograph packing material is mainly from Europe, the U.S. and Japanese import.
Spheric granules resin since its material specific surface area and adsorption capacity are limited, generally deposit by the chromatographic column in industrial production
It is big in loadings and material containing amount is small, the absorb-elute cycle is long, cylinder draw ratio requires the shortcomings of high, and then cause process units such as
The inefficient and flow of Simulation moving bed is complicated.On the other hand, compared with spheric granules ion exchange resin, ion-exchange fiber
Many advantages obtained being widely recognized as scientific research technical staff, including specific surface area is big, and adsorption capacity is big, exchange velocity and
Elution speed is fast, easily regeneration, and it is more preferable etc. to fill out the bed body uniformity and Flow Field Distribution after column.But up to the present, use ion
Exchange fiber is used for xylose technology application separated with arabinose as chromatograph packing material, still without disclosed document and patent report
Road.
The content of the invention
It is an object of the present invention to provide a kind of new chromatographic isolation to produce xylose and arabinose method, especially
Using ion-exchange fibre as chromatographic isolation filler, separation preparation high-purity xylose and arabinose from xylose crystallization mother liquor
Method.
The described separated ion-exchange fibre of xylose crystallization mother liquor that is used for is highly acid, exchange capacity for 2.0~
4.3mmol/g, a diameter of 8~170 μm in the dry state of fiber.
The ion-exchange fibre can be the short fine form that length is 5~100mm as filler, can also in advance into
Type is non-woven fabrics or felt form of the bulk density in 100~500g/mL.
The ion-exchange fibre is as filler, it is necessary to carry out calcium in advance before being separated for xylose crystallization mother liquor
The displacement of ion, completes the conversion from Hydrogen to calcium type.
It is provided by the invention using xylose crystallization mother liquor separation method of the ion-exchange fibre as chromatograph packing material, its feature
It is that implementation process includes following key step：
a）Ion-exchange fibre column loads：Above-mentioned short fine or non-woven fabrics form the ion-exchange for having been converted into calcium type is fine
Dimension, uses column length compress mode to fill column with after pure water complete wetting.Loading density is 200~600g/L, and filling blade diameter length ratio is
1:5~70.
b）Material containing is adsorbed：By xylose crystallization mother liquor with 2.2~8% volumes of packing volume, constant separation temperature is maintained
Degree, by 0.35~2.5BV/h flow velocitys, injects water-filled chromatographic column from cylinder feed inlet constant speed.
c）Elution：Stop injection liquid glucose after, immediately cylinder charging saliva do mobile phase, according to packing volume 0.5~
1.3 times of waters, 0.35~3.5BV/h flow velocitys elute filler, obtain rich in Xylose and rich in Arabic liquid glucose.
d）Above-mentioned steps a)~c) it is that a material containing elutes the cycle, calculated in one cycle according to area-method, take me
When the sugared purity 61% of uncle is as cut-point, the rate of recovery of arabinose is 70~85%, and the purity rich in xylose in Xylose is 86
~95%, the rate of recovery is 85~92%.
Above-mentioned steps a)~c provided by the invention), it can continuously be run by the way of multicolumn connection in series-parallel combination, also may be used
Continuously run in a manner of using Simulation moving bed.
Loading density in preferred steps a) is 250~550g/L.
Separation temperature in preferred steps b) is 35~60 DEG C.
Elution speed in preferred steps c) is 0.5~1.5BV/h.
Beneficial effects of the present invention：Compared with ion-exchange resins method, ion-exchange fibre method proposes first, can be substantially improved
The efficiency of the separated production of sugar, processing load is under the same conditions, it is possible to reduce chromatographic bed packing volume, reduces equipment manufacturing cost；
Under the conditions of identical bed body size and technological process, treating capacity can be improved, product purity is more preferable.Limited in particular by the present invention
Fixed process conditions are wider, and service life is obviously prolonged, and effect is more preferable.
Embodiment
Embodiment given below is not to form limitation to scope of the invention as claimed, but to the present invention into advancing one
The description of step.
Embodiment 1
1）Ion-exchange fibre prepares：Select under drying regime a diameter of 33~40 μm, exchange capacity be 3.3mmol/g
Strong acidic ion-exchange fiber, is cut into the short fibre of 3~10mm or so, with pure water saturates.It is allowed to put using excessive calcium ion
Change, complete the conversion from Hydrogen to calcium type.The polystyrene-based place proposed in particular by Chinese patent 201310533240.3
Functional fibre base material after reason, ion-exchange fibre is prepared by cross-linking reaction and functional modification, if other reach this
Functional fibre material also may be used.Processing procedure may be referred to the prior art, and typical reference is such as：F. and J.Homogeneous and Heterogeneous Sulfonation of Polymers:A
Review.Polym.Eng.Sci.1998,38(5),783-792。
2）Ion-exchange fibre loads：The ion-exchange fibre of calcium type is had been converted into pure water immersion, using column length
Compress mode fills column, fiber packing density 500g/L, and filling blade diameter length ratio is 1:70.
3）Xylose mother liquid separates：The concentration of the xylose mother liquid of 60 ° of Bx, wherein xylose and arabinose be respectively 31.1% and
14.1%.The liquid glucose of packing volume 2.2% is taken, is adsorbed with flow velocity 1BV/h by 26 DEG C of ion-exchange fibre columns, immediately with sugar
The water elution of 17 times of volumes of liquid.Treat that elution samples are collected in liquid glucose outflow, formed with HPLC analysis eluents.Obtain being rich in Xylose
With rich in Arabic liquid glucose, separating degree 0.76, when taking arabinose purity 61% as cut-point, the rate of recovery of arabinose
For 76%, the purity rich in xylose in Xylose is 93%, the rate of recovery 86%.
4）With the contrast of spheric granules resin：Fiberfill in chromatographic column is changed to the calcium type particle tree of same volume
Fat, resin average diameter are about 300 μm, exchange capacity 1.5mol/L, wet method dress post after being soaked with pure water.Resin loading density is
790g/L, filling blade diameter length ratio are 1:70.Under conditions of parameters are identical with filling ion-exchange fibre, water is eluted
For 23 times of liquid glucose volume, formed with HPLC analysis eluents.Obtain being rich in Xylose and be rich in Arabic liquid glucose, separating degree
0.49, when taking arabinose purity 61% as cut-point, the rate of recovery of arabinose is 46%, and the purity of xylose is 81%, xylose
The rate of recovery be 88%.
Embodiment 2
1）Ion-exchange fibre prepares：Select under drying regime a diameter of 33~40 μm, exchange capacity be 3.3mmol/g
Strong acidic ion-exchange fiber, is cut into the short fibre of 3~10mm or so, with pure water saturates.It is allowed to put using excessive calcium ion
Change, complete the conversion from Hydrogen to calcium type.Using 1 ion exchange fiber material of embodiment.
2）Ion-exchange fibre loads：The ion-exchange fibre of calcium type is had been converted into pure water immersion, using column length
Compress mode fills column, fiber packing density 500g/L, and filling blade diameter length ratio is 1:70.
3）Xylose mother liquid separates：The concentration of the xylose mother liquid of 60 ° of Bx, wherein xylose and arabinose be respectively 31.1% and
14.1%.The liquid glucose of packing volume 3.5% is taken, is adsorbed with flow velocity 1BV/h by 26 DEG C of ion-exchange fibre columns, immediately with sugar
The water elution of 12.5 times of volumes of liquid.Treat that elution samples are collected in liquid glucose outflow, formed with HPLC analysis eluents.Obtain xylose and Ah
It is 0.67 to draw the sugared separating degree of uncle, and when taking arabinose purity 61% as cut-point, the rate of recovery of arabinose is 72%, rich in wood
The purity of xylose is 87% in liquid glucose, the rate of recovery 80%.
4）With the contrast of spheric granules resin：Fiberfill in chromatographic column is changed to the calcium type particle tree of same volume
Fat, resin average diameter are about 300 μm, exchange capacity 1.5mol/L, wet method dress post after being soaked with pure water.Resin loading density is
790g/L, filling blade diameter length ratio are 1:70.Under conditions of parameters are identical with filling ion-exchange fibre, water is eluted
For 15 times of liquid glucose volume, formed with HPLC analysis eluents.Obtain being rich in Xylose and be rich in Arabic liquid glucose, separating degree
0.52, when taking arabinose purity 61% as cut-point, the rate of recovery of arabinose is 43%, and the purity of xylose is 79%, xylose
The rate of recovery be 89%.
5）By the comparative analysis to result, in order to obtain identical separating effect, particulate resin filler is used for xylose knot
The chromatographic isolation of brilliant mother liquor is, it is necessary to the draw ratio of bigger and slower elution speed.As it can be seen that using ion-exchange fibre as color
Filler is composed, the separation accuracy of higher can be obtained in xylose crystallization mother liquor separation, and the separative efficiency under the same terms is remote
Higher than particulate resin filler.
Although the present invention is disclosed above with preferred embodiment, so it is not limited to the present invention.Skill belonging to the present invention
Has usually intellectual in art field, without departing from the spirit and scope of the present invention, when can be used for a variety of modifications and variations.Cause
This, the scope of protection of the present invention is defined by those of the claims.
Claims (2)
1. ion-exchange fibre is used for xylose method separated with arabinose as chromatograph packing material, it is characterized in that being handed over using ion
Fiber is changed as chromatographic isolation filler, for the method that separation prepares high-purity xylose and arabinose in xylose crystallization mother liquor；
The ion-exchange fibre is strong acidic ion-exchange fiber, a diameter of 8 ~ 170 μm under drying regime, cation exchange capacity
For 2.0 ~ 4.3 mmol/g, it is necessary to carry out the displacement of calcium ion in advance before being separated for xylose crystallization mother liquor, complete from hydrogen
Conversion of the type to calcium type；
Use length to be loaded for the short fine form of 5 ~ 100 mm, or use and be pre-formed as bulk density in 100 ~ 500 g/L
Non-woven fabrics or felt form, then loaded；
Step is as follows：
a）Ion-exchange fibre column loads：By described short fine or non-woven fabrics form ion-exchange fiber, with pure water complete wetting
Afterwards using column length compress mode dress column；Loading density is 200 ~ 600 g/L, and filling blade diameter length ratio is 1:5~70；
b）Material containing is adsorbed：By above-mentioned 25 ~ 60 °C of xylose crystallization mother liquor with 2.2 ~ 8 % volumes of packing volume, by 0.35 ~
2.5 BV/h flow velocitys, inject water-filled chromatographic column from cylinder feed inlet constant speed；
c）Elution：After stopping injection liquid glucose, mobile phase is done with water in cylinder feed inlet immediately, according to the 0.5 ~ 1.3 of packing volume
Times water, 1 ~ 2BV/h flow velocitys elute filler, obtain rich in Xylose and rich in Arabic liquid glucose；
d）Above-mentioned steps a) ~ c) it is that a material containing elutes the cycle, calculated in one cycle according to area-method, take Arab
When sugared purity 61% is as cut-point, the rate of recovery of arabinose is 70 ~ 85 %, and the purity rich in xylose in Xylose is 86 ~ 95
%, the rate of recovery are 85 ~ 92 %；
Step a) ~ c) continuously run by the way of multicolumn connection in series-parallel combination or continuously run using Simulation moving bed mode.
2. ion-exchange fibre as claimed in claim 1 is used for xylose method separated with arabinose as chromatograph packing material,
It is characterized in that the loading density in step a) is 250 ~ 550 g/L.
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| CN201310539010.8A CN104611476B (en) | 2013-11-04 | 2013-11-04 | A kind of xylose method separated with arabinose |
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| CN104611476B true CN104611476B (en) | 2018-04-27 |
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| JP6732017B2 (en) * | 2015-07-24 | 2020-07-29 | アニッキ ゲーエムベーハーＡｎｎｉｋｋｉ Ｇｍｂｈ | Method for obtaining oxidation and reduction products from sugar mixtures |
| MY186792A (en) | 2016-02-04 | 2021-08-20 | Ind Tech Res Inst | Method for separating hydrolysis product of biomass |
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