CN104611475B - Fructose separation method - Google Patents

Fructose separation method Download PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
fructose
ion
exchange
separation
exchange fibre
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201310538665.3A
Other languages
Chinese (zh)
Other versions
CN104611475A (en
Inventor
林晓
陆剑鸣
张丽方
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nanjing Tech University
Original Assignee
Nanjing Tech University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanjing Tech University filed Critical Nanjing Tech University
Priority to CN201310538665.3A priority Critical patent/CN104611475B/en
Publication of CN104611475A publication Critical patent/CN104611475A/en
Application granted granted Critical
Publication of CN104611475B publication Critical patent/CN104611475B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C13SUGAR INDUSTRY
    • C13KSACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K11/00Fructose
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/26Selective adsorption, e.g. chromatography characterised by the separation mechanism
    • B01D15/36Selective adsorption, e.g. chromatography characterised by the separation mechanism involving ionic interaction
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/26Selective adsorption, e.g. chromatography characterised by the separation mechanism
    • B01D15/36Selective adsorption, e.g. chromatography characterised by the separation mechanism involving ionic interaction
    • B01D15/361Ion-exchange

Landscapes

  • 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

The invention relates to a method for separating fructose by taking ion exchange fiber as chromatographic packing, which adopts the ion exchange fiber as the chromatographic packing and is used for separating and preparing high-purity fructose from mixed sugar liquid such as fructose-glucose syrup and the like; the mixed sugar solution is a mixed solution containing fructose glucose syrup F42 or fructose with other concentration; the ion exchange fiber is a strong acid ion exchange fiber, the diameter of the ion exchange fiber is 8-170 mu m in a dry state, the cation exchange capacity is 2.0-4.3 mmol/g, and calcium ions need to be replaced in advance before the ion exchange fiber is used for fructose separation, so that the conversion from a hydrogen type to a calcium type is completed. Compared with ion exchange particle resin chromatographic columns, the strong acid ion exchange fibers show more excellent separation precision and higher production efficiency.

Description

A kind of method of fructose separation
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.
CN201310538665.3A 2013-11-04 2013-11-04 Fructose separation method Active CN104611475B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310538665.3A CN104611475B (en) 2013-11-04 2013-11-04 Fructose separation method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310538665.3A CN104611475B (en) 2013-11-04 2013-11-04 Fructose separation method

Publications (2)

Publication Number Publication Date
CN104611475A CN104611475A (en) 2015-05-13
CN104611475B true CN104611475B (en) 2018-11-20

Family

ID=53146122

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310538665.3A Active CN104611475B (en) 2013-11-04 2013-11-04 Fructose separation method

Country Status (1)

Country Link
CN (1) CN104611475B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
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

Also Published As

Publication number Publication date
CN104611475A (en) 2015-05-13

Similar Documents

Publication Publication Date Title
CN1267185C (en) Paraxylene sorbent and its preparing method
CN102145256B (en) Method for separating boron isotopes by simulated moving bed chromatography
CN101274217A (en) Technique for separating boron isotope with boron specific resin ion-exchange chromatography
CN109646998B (en) Simulated moving bed and method for separating saccharides
CN101177716A (en) Method for separating and purifying glucose, fructose and oligomeric polysaccharide from high fructose syrup
CN101721979B (en) Method for preparing macroporous adsorbent resin special for separating valine
CN104611475B (en) Fructose separation method
CN101570497A (en) Method for purifying high-purity organic solvent acetonitrile for research
CN102093160B (en) Method for preparing chromatographically-pure trichloromethane
CN101940289B (en) Method for separating discolored chili extract from chili pigment in crude products of chili extract
CN102417441A (en) Method for purifying chromatographic grade organic solvent methyl tertiary butyl ether
CN102675379B (en) A kind of method of Hydrolysis kinetics hydroxyl radical carthamin yellow carthamus A from safflower
CN104611476B (en) Method for separating xylose and arabinose
CN103962091A (en) Method for separating EPA (eicosapentaenoic acid) and DHA (docosahexaenoic acid) by using silver ion modified amino silica gel
CN101928305A (en) Method for purifying xylo-oligosaccharide by adsorption and separation by simulated moving bed
CN108084007A (en) A kind of method of Simulated Moving Bed Chromatography separation Co-Q10 and CoQ1 1
CN102432428A (en) Method for purifying chromatographically pure organic solvent tert-butyl alcohol
CN100534996C (en) Preparation of dulcose crystal
CN109646999A (en) It is a kind of for separating the Simulation moving bed and method of glucide
CN109836479A (en) The method that application simulation thermopnore isolates and purifies FMD inactivation of viruses antigen
CN104557542B (en) A kind of Supercritical fluid chromatography prepares the method for high purity EPA ester and DHA ester monomer
Gillarová et al. Chromatographic separation of mannitol from mixtures of other carbohydrates in aqueous solutions.
CN108623649B (en) Method for separating and purifying notoginsenoside Fc from total saponins of panax notoginseng leaves
CN103803588A (en) Preparation method of potassium nitrate
CN102030758A (en) Preparation method of chalepensin

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant