CN104611475B - A kind of method of fructose separation - Google Patents
A kind of method of fructose separation Download PDFInfo
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- CN104611475B CN104611475B CN201310538665.3A CN201310538665A CN104611475B CN 104611475 B CN104611475 B CN 104611475B CN 201310538665 A CN201310538665 A CN 201310538665A CN 104611475 B CN104611475 B CN 104611475B
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- ion
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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
- C13K11/00—Fructose
-
- 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
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- 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
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Organic Chemistry (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
A kind of method the present invention relates to ion-exchange fibre as chromatograph packing material for fructose separation prepares high-purity fructose for separation in the mixed sugar liquids such as fructose syrup using ion-exchange fibre as chromatographic isolation filler；The mixed sugar liquid is the mixed liquor of the fructose comprising fructose syrup F42 or other concentration；The ion-exchange fibre is a kind of strong acidic ion-exchange fiber, and diameter is 8~170 μm under drying regime, cation exchange capacity is 2.0~4.3mmol/g, before for fructose separation, needs to carry out the displacement of calcium ion in advance, complete from Hydrogen to the conversion of calcium type.Compared with ion-exchange particles resin chromatography column, strong acidic ion-exchange fiber shows superior separation accuracy and higher production efficiency.
Description
Technical field
It uses strong acidic ion-exchange fiber as chromatography new packing the present invention relates to a kind of, is separated from fructose syrup
The process of high-purity fructose, belongs to technical field of chromatography separation.
Background technique
Fructose have sugariness is high, in good taste, anti-caries tooth, eat after do not cause the good characteristics such as blood glucose fluctuation, largely answered
In production for food, drug and health care product, the market demand increasingly increases.Since fructose and glucose are isomers,
Physicochemical property is close, and separation is extremely difficult, how to realize that fructose and efficiently separating for glucose are urgent need to resolve in fructose production
The problem of.The separation method of fructose and glucose mainly has crystallisation, double salt method, chromatography, fractionation, reverse osmosis
Method, liquid~liquid extraction separation method and Exchange Resin by Adsorption etc., most enterprises are mainly divided using chromatography both at home and abroad at present
From method, uses spherical calcium type ion exchange resin as chromatograph packing material, fructose is isolated from fructose syrup.
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 period is long, cylinder draw ratio requires the disadvantages of high, and then lead to process units such as
The inefficient and process 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 large specific surface area, adsorption capacity is big, exchange velocity and
Elution speed is fast, easily regenerates, and it is more preferable etc. to fill out the bed body uniformity and Flow Field Distribution after column.But up to the present, ion is used
Exchange fiber is used for the technical application of fructose separation as chromatograph packing material, still without disclosed document and patent report.
Summary of the invention
The object of the present invention is to provide a kind of novel chromatographic isolations to produce fructose method, hands in particular by ion
Fiber is changed as chromatographic isolation filler, the method for preparing high-purity fructose for separation in the mixed sugar liquids such as fructose syrup.
The technical scheme is that：A kind of chromatographic isolation fructose method, using ion-exchange fibre as chromatographic isolation
Filler, the method for preparing high-purity fructose for separation in the mixed sugar liquids such as fructose syrup.The mixed sugar liquid is comprising fruit Portugal
The mixed liquor of syrup F42 or the fructose of other concentration；The ion-exchange fibre, it is characterized in that a kind of strong acidic ion exchanges
Fiber, diameter is 8~170 μm under drying regime, and cation exchange capacity is 2.0~4.3mmol/g, is separating it for fructose
Before, it needs to carry out the displacement of calcium ion in advance, completes from Hydrogen to the conversion of calcium type.
Fructose separation method provided by the invention using ion-exchange fibre as chromatograph packing material, implementation process include
Following key step：
a）The filling of ion-exchange fibre column：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 diameter height, which compares, is
1:5~70.
b）Material containing absorption：By above-mentioned mixed sugar liquid with 0.1~0.4 times of amount of packing volume, constant separation temperature is maintained,
By 0.35~2.5BV/h flow velocity, water-filled chromatographic column is injected from cylinder feed inlet constant speed.
c）Elution：After stopping injection liquid glucose, mobile phase is done in cylinder charging saliva immediately, according to 4~8 times of liquid glucose volume
Water, 0.35~3.5BV/h flow velocity elute filler.
d）Above-mentioned steps a)~c) it is that a material containing elutes the period, it is calculated in one cycle according to area-method, fructose is pure
When spending 90%, the rate of recovery of fructose is 40~70%.
Above-mentioned steps a)~c), can in such a way that multicolumn combines in series and parallel continuous operation, can also using simulation move
Dynamic bed mode continuous operation.
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 1~2BV/h.
Beneficial effects of the present invention：Implementation through the invention separates the color of high-purity fructose from fructose syrup
Spectrum separation, compared with ion-exchange resins method, ion-exchange fibre method is put forward for the first time, and is in particular, provided and is exchanged using strong acidic ion
The efficiency of the production of fructose and glucose separation, the identical condition of processing load can be substantially improved as chromatograph packing material in fiber
Under, it is possible to reduce chromatographic bed packing volume reduces equipment manufacturing cost；Under the conditions of identical bed body size and process flow, Ke Yiti
Format high throughput, product purity are more preferable.Fructose syrup injection is transformed into the cation exchange fibre chromatographic column of calcium type, is washed with water
It is de-, it can be used for producing the fructose that purity is 90% or more.Process conditions of the invention are wider, and service life extends, and effect is more
It is good.
Specific embodiment
Embodiment given below is not the limitation constituted to scope of the invention as claimed, but carries out the present invention into one
The description of step.
Embodiment 1
1）Ion-exchange fibre prepares：Diameter is 33~40 μm under selection drying regime, exchange capacity is 3.3mmol/g's
Strong acidic ion-exchange fiber is cut into the short fibre of 3~10mm or so, with pure water saturates.It is allowed to set using excessive calcium ion
It changes, completes from Hydrogen to the conversion of calcium type.The polystyrene-based place proposed in particular by Chinese patent 201310533240.3
Functional fibre substrate after reason, is prepared ion-exchange fibre by cross-linking reaction and functional modification, if other reach this
Functional fibre material also may be used.Treatment process can refer 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 filling：The ion-exchange fibre for having been converted into calcium type is impregnated with pure water, using column length
Compress mode fills column, and fiber packing density 500g/L, it is 1 that filling diameter height, which compares,:70.
3）Fructose syrup separation：Fructose syrup total sugar concentration is 50%, fructose content 42%, glucose content 58%.Take filler
The liquid glucose of volume 8.5% is adsorbed with flow velocity 0.5BV/h by 26 DEG C of ion-exchange fibre columns, uses 5.8 times of bodies of liquid glucose immediately
Long-pending water elution.It is flowed out to liquid glucose and collects elution samples, with HPLC analysis eluent composition.Fructose and glucose separating degree are
0.89, when fructose purity 90%, the rate of recovery of fructose is 67%.
4）Above-mentioned steps 3）Be adsorbed in elution process, can be carried out continuously in such a way that multicolumn combines in series and parallel,
It can be carried out continuously using Simulation moving bed mode.
Embodiment 2
1）Ion-exchange fibre prepares：Diameter is 33~40 μm under selection drying regime, exchange capacity is 3.3mmol/g's
Strong acidic ion-exchange fiber is cut into the short fibre of 3~10mm or so, with pure water saturates.It is allowed to set using excessive calcium ion
It changes, completes from Hydrogen to the conversion of calcium type.Using 1 ion exchange fiber material of embodiment.
2）Ion-exchange fibre filling：The ion-exchange fibre for having been converted into calcium type is impregnated with pure water, using column length
Compress mode fills column, and fiber packing density 500g/L, it is 1 that filling diameter height, which compares,:70.
3）Fructose syrup separation：Fructose syrup total sugar concentration is 50%, fructose content 42%, glucose content 58%.Take filler
The liquid glucose of volume 8.5% is adsorbed with flow velocity 1.5BV/h by 26 DEG C of ion-exchange fibre columns, uses 6.7 times of liquid glucose immediately
The water elution of volume.It is flowed out to liquid glucose and collects elution samples, with HPLC analysis eluent composition.Fructose and glucose separating degree are
0.91, when fructose purity 90%, the rate of recovery of fructose is 53%.
4）Above-mentioned steps 3）Be adsorbed in elution process, can be carried out continuously in such a way that multicolumn combines in series and parallel,
It can be carried out continuously using Simulation moving bed mode.
Embodiment 3
1）Ion-exchange fibre prepares：Diameter is 33~40 μm under selection drying regime, exchange capacity is 3.3mmol/g's
Strong acidic ion-exchange fiber is cut into the short fibre of 3~10mm or so, with pure water saturates.It is allowed to set using excessive calcium ion
It changes, completes from Hydrogen to the conversion of calcium type.Using 1 ion exchange fiber material of embodiment.
2）Ion-exchange fibre filling：The ion-exchange fibre for having been converted into calcium type is impregnated with pure water, using column length
Compress mode fills column, and fiber packing density 500g/L, it is 1 that filling diameter height, which compares,:70.
3）Fructose syrup separation：The commodity F42 fructose syrup for being diluted to total sugar concentration 50% is taken, volume is filling body accumulated amount
8.5%, it is adsorbed with flow velocity 1.5BV/h by 26 DEG C of ion-exchange fibre columns, uses the water elution of 7.2 times of volumes of liquid glucose immediately.
It is flowed out to liquid glucose and collects elution samples, with HPLC analysis eluent composition.Fructose and glucose separating degree are 0.88, fructose purity
When 90%, the rate of recovery of fructose is 61%.
4）With the comparison of spheric granules resin：Fiberfill in chromatographic column is changed to the calcium type particle tree of same volume
Rouge, resin average diameter are about 300 μm, exchange capacity 1.5mol/L, wet method dress post after being impregnated with pure water.Resin loading density is
790g/L, it is 1 that filling diameter height, which compares,:70.Under conditions of parameters are identical with filling ion-exchange fibre, water is eluted
It is 8 times of liquid glucose volume.With HPLC analysis eluent composition.Fructose and glucose separating degree are 0.52, when fructose purity 90%,
The rate of recovery of fructose is 23%.
By the comparative analysis of the particulate resin separating resulting to ion-exchange fiber it can be found that in order to obtain identical separation
Effect, particulate resin filler are used for the chromatographic isolation of fructose, need bigger draw ratio and slower elution speed.And use from
Sub- exchange fiber can obtain higher separation accuracy in fructose separation as chromatograph packing material, and point under the same terms
It is much higher than particulate resin filler from efficiency.
Although the present invention has been disclosed as a preferred embodiment, however, it is not to limit the 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 (5)
1. a kind of method that ion-exchange fibre is used for fructose separation as chromatograph packing material, it is characterized in that using ion-exchange fibre
As chromatographic isolation filler, high-purity fructose is prepared for separation in fructose syrup mixed sugar liquid；The mixed sugar liquid is to include
The mixed liquor of fructose syrup F42；The ion-exchange fibre, is a kind of strong acidic ion-exchange fiber, straight under drying regime
Diameter is 8 ~ 170 μm, and cation exchange capacity is 2.0 ~ 4.3 mmol/g, before for fructose separation, needs to carry out calcium in advance
The displacement of ion is completed from Hydrogen to the conversion of calcium type；
Ion-exchange fibre is as filler, and ion-exchange fibre uses length to be loaded for the short fine form of 5 ~ 100 mm, so
Laggard luggage is filled out；
Steps are as follows：
a）The filling of ion-exchange fibre column：By short fine or non-woven fabrics form the ion-exchange fiber, with pure water complete wetting
Column is filled using column length compress mode afterwards；Loading density is 200 ~ 600 g/L, and it is 1 that filling diameter height, which compares,:5~70；
b）Material containing absorption：By above-mentioned 25 ~ 60 °C of mixed sugar liquid with 0.1 ~ 0.4 times of amount of packing volume, by 0.35 ~ 2.5 BV/
H flow velocity injects 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 4 ~ 8 times of water of liquid glucose volume
Amount, 0.35 ~ 3.5 BV/h flow velocity elute filler.
2. the method that ion-exchange fibre as described in claim 1 is used for fructose separation as chromatograph packing material, it is characterised in that
Above-mentioned steps a) ~ c) continuous operation in such a way that multicolumn combines in series and parallel, or use Simulation moving bed mode continuous operation.
3. the method that ion-exchange fibre as described in claim 1 is used for fructose separation as chromatograph packing material, it is characterised in that
Loading density in step a) is 250 ~ 550 g/L.
4. the method that ion-exchange fibre as described in claim 1 is used for fructose separation as chromatograph packing material, it is characterised in that
Separation temperature in step b) is 35 ~ 60 °C.
5. the method that ion-exchange fibre as described in claim 1 is used for fructose separation as chromatograph packing material, it is characterised in that
Elution speed in step c) is 1 ~ 2 BV/h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310538665.3A CN104611475B (en) | 2013-11-04 | 2013-11-04 | A kind of method of fructose separation |
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| CN201310538665.3A CN104611475B (en) | 2013-11-04 | 2013-11-04 | A kind of method of fructose separation |
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| CN104611475A CN104611475A (en) | 2015-05-13 |
| CN104611475B true CN104611475B (en) | 2018-11-20 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3560571B1 (en) * | 2018-04-23 | 2023-12-13 | Novasep Process Solutions | Method for purifying fructose |
| CN111346622B (en) * | 2018-12-24 | 2023-05-09 | 内蒙古蒙牛乳业（集团）股份有限公司 | Chromatographic packing and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1753952A (en) * | 2003-02-24 | 2006-03-29 | 兰爱克谢斯德国有限责任公司 | Mixture |
| CN101177716A (en) * | 2007-12-12 | 2008-05-14 | 江南大学 | Method for separating and purifying glucose, fructose and oligomeric polysaccharide from high fructose syrup |
| CN101766289A (en) * | 2010-01-29 | 2010-07-07 | 安徽丰原发酵技术工程研究有限公司 | Method for preparing high fructose corn syrup |
| CN102205039A (en) * | 2011-05-25 | 2011-10-05 | 北京服装学院 | Method for extracting purified saponin with ion exchange fiber |
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- 2013-11-04 CN CN201310538665.3A patent/CN104611475B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1753952A (en) * | 2003-02-24 | 2006-03-29 | 兰爱克谢斯德国有限责任公司 | Mixture |
| CN101177716A (en) * | 2007-12-12 | 2008-05-14 | 江南大学 | Method for separating and purifying glucose, fructose and oligomeric polysaccharide from high fructose syrup |
| CN101766289A (en) * | 2010-01-29 | 2010-07-07 | 安徽丰原发酵技术工程研究有限公司 | Method for preparing high fructose corn syrup |
| CN102205039A (en) * | 2011-05-25 | 2011-10-05 | 北京服装学院 | Method for extracting purified saponin with ion exchange fiber |
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