CN109053823A - A method of isolating and purifying glucose from glucose syrup - Google Patents

A method of isolating and purifying glucose from glucose syrup Download PDF

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Publication number
CN109053823A
CN109053823A CN201810909021.3A CN201810909021A CN109053823A CN 109053823 A CN109053823 A CN 109053823A CN 201810909021 A CN201810909021 A CN 201810909021A CN 109053823 A CN109053823 A CN 109053823A
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Prior art keywords
glucose
zsm
molecular sieve
glucose syrup
ultrafiltration membrane
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CN201810909021.3A
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Chinese (zh)
Inventor
王永旗
王伟
吕明
李定发
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TAICANG HUSHI REAGENT CO Ltd
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TAICANG HUSHI REAGENT CO Ltd
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Priority to CN201810909021.3A priority Critical patent/CN109053823A/en
Publication of CN109053823A publication Critical patent/CN109053823A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00Processes for the preparation of sugar derivatives
    • C07H1/06Separation; Purification
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H3/00Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
    • C07H3/02Monosaccharides

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Biotechnology (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Molecular Biology (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The method that the invention discloses a kind of to isolate and purify glucose from glucose syrup.The method that the present invention isolates and purifies glucose from glucose syrup, firstly, by glucose syrup by ZSM-5 molecular sieve, ZSM-5 molecular sieve can preferably adsorb inorganic salt impurities ion contained by glucose syrup;Pass through the ultrafiltration membrane in 8~12 angstroms of apertures again, the specific aperture of the ultrafiltration membrane can penetrate glucose molecule and retain the polysaccharide molecules such as maltose, maltotriose, maltotetraose and tetrose, preferably realize the separation of glucose homopolysaccharide molecule.

Description

A method of isolating and purifying glucose from glucose syrup
Technical field
The present invention relates to the technical fields of glucose purification, more particularly to one kind, and glucose is isolated and purified from glucose syrup Method.
Background technique
Glucose is the raw material of a kind of important monosaccharide and important Essential Chemistry pharmaceuticals and multiple compounds.Portugal The production of grape sugar experienced the development processes such as acid system, acid-enzyme hydrolysis method and two enzymes method.
Glucose is the raw material of a kind of important monosaccharide and important Essential Chemistry pharmaceuticals and multiple compounds.Portugal The production of grape sugar experienced the development processes such as acid system, acid-enzyme hydrolysis method and two enzymes method.The production technology for producing glucose is as follows: to form sediment Powder is raw material, by liquefying under the action of enzyme re-liquefied after sizing mixing, then forms glucose syrup through saccharification enzyme effect saccharification again. The main ingredient of glucose syrup is glucose, maltose, maltotriose, maltotetraose and tetrose or more.
In the prior art, glucose is isolated from glucose syrup generally use fixed bed ion-exchange process, it is mainly sharp With the salinity in a large amount of anion-cation exchange resin removing liquid glucose.There are following drawbacks for this production technology: firstly, resin Regeneration needs to consume a large amount of soda acid and water, while it is seriously polluted to generate a large amount of acidic and alkaline waste water;Importantly, separated The purity of the glucose of extraction is lower.
Summary of the invention
In view of this, the present invention provides a kind of purification process of electron level n-hexane, the purification obtained through the purification process The purity of product is higher.
A method of isolating and purifying glucose from glucose syrup, comprising the following steps:
(1) by glucose syrup by ZSM-5 molecular sieve, reservation passes through liquid;
(2) by the ultrafiltration membrane for passing through 8~12 angstroms of apertures by liquid, retain permeate.
The above-mentioned method that glucose is isolated and purified from glucose syrup of the invention, firstly, glucose syrup is passed through ZSM-5 Molecular sieve, ZSM-5 molecular sieve can preferably adsorb inorganic salt impurities ion contained by glucose syrup;Pass through 8~12 angstroms of holes again The ultrafiltration membrane of diameter, the specific aperture of the ultrafiltration membrane can penetrate glucose molecule and retain maltose, maltotriose, malt four The polysaccharide molecules such as sugar and tetrose, preferably realize the separation of glucose homopolysaccharide molecule.
ZSM-5 molecular sieve
ZSM-5 molecular sieve, that is, ZSM-5 zeolite is that Mobile oil company of the U.S. is synthesized in eighties of last century the late sixties A kind of New-type Zeolite Molecular Sieves containing organic amine cation.The chemical composition of its ZSM-5 zeolite can use the molar ratio table of oxide Be shown as: 0.9 ± 0.2M2/nO:Al2O3:5---100SiO2:ZH2O, M is cationic (alkali metallic sodium ion and organic amine in formula Ion);N is the valence mumber of cation;Z is from 0 to 40.
Based on the consideration improved to the adsorptivity of inorganic ion, the silica alumina ratio of ZSM-5 molecular sieve can be preferably 20~ 40, such as 20,22,25,30,34,38 or 40 etc..
It can be the Simulated Moving Bed Chromatography dress that ZSM-5 molecular sieve is stationary phase as the installation form of ZSM-5 molecular sieve It sets, naturally it is also possible to be cylindricality.Herein, simulated movable bed chromatography device is equipment well known in the art.For example, Simulation moving bed Chromatogram arrangement can be connected by the Coupled columns of 4 or more (being free of 4), at the closed system of a head and the tail connection;Every color Spectrum column has discharge port, feed inlet, circulation port, water inlet;Change discharge port, charging by the way of computer automatic control The position of mouth, circulation port, water inlet, to realize charging, water inlet, the discharging of preceding component, the discharging of rear component continuous operation behaviour simultaneously Make.
In the case where simulated movable bed chromatography device form, by the temperature of ZSM-5 molecular sieve be more suitably 40~ 60℃.In this embodiment, the inlet amount by ZSM-5 molecular sieve is 1~5L/h.
Ultrafiltration membrane
Ultrafiltration is the membrane separation technique using pressure as motive force, for the purpose of macromolecular and separation of small molecuies, membrane aperture 20~ 1000 angstroms.Since glucose sugar is unimolecule, molecular size is about 0.75 angstrom, and the above glycan molecule of the binary such as maltose is greatly as low as It is less 15 angstroms, thus 8~12 angstroms of aperture possessed by ultrafiltration membrane can preferably allow glucose sugar to penetrate and retain polysaccharide point Son.
It more preferably, is 25~40 DEG C by the temperature of ultrafiltration membrane.In this embodiment, pass through the pressure of ultrafiltration membrane For 10~20bar.
As used herein, above-mentioned term:
"one", "an" and " described " be used interchangeably and refer to one or more.
"and/or" is used to indicate that one of illustrated situation or both may to occur, for example, A and/or B includes (A And B) and (A or B).
In addition, herein by endpoint state range include included within the scope of this all numerical value (for example, 1 to 10 packet Include 1.4,1.9,2.33,5.75,9.98 etc.).
In addition, the statement of "at least one" herein is including one or more all number (for example, at least two, at least 4, at least six, at least eight, at least ten, at least 25, at least 50, at least 100 etc.).
The above-mentioned method that glucose is isolated and purified from glucose syrup of the invention, firstly, glucose syrup is passed through ZSM-5 Molecular sieve, ZSM-5 molecular sieve can preferably adsorb inorganic salt impurities ion contained by glucose syrup;Pass through 8~12 angstroms of holes again The ultrafiltration membrane of diameter, the specific aperture of the ultrafiltration membrane can penetrate glucose molecule and retain maltose, maltotriose, malt four The polysaccharide molecules such as sugar and tetrose, preferably realize the separation of glucose homopolysaccharide molecule.
Specific embodiment
Below with reference to embodiment to further illustrate the technical scheme of the present invention.
Embodiment 1
Firstly, being packed into the ZSM-5 molecular sieve of silica alumina ratio 20 as stationary phase on simulated movable bed chromatography device bed.By glucose Slurry controls through the temperature of simulated movable bed chromatography device by above-mentioned simulated movable bed chromatography device ZSM-5 molecular sieve and is 40 DEG C, inlet amount 1L/h, collection passes through liquid.
Then, the ultrafiltration membrane in 8 angstroms of apertures will be passed through above by liquid.25 DEG C of ultrafiltration are controlled, permeate is retained.This example is received The purity for collecting glucose is 99.25%.
Embodiment 2
Firstly, being packed into the ZSM-5 molecular sieve of silica alumina ratio 40 as stationary phase on simulated movable bed chromatography device bed.By glucose Slurry controls through the temperature of simulated movable bed chromatography device by above-mentioned simulated movable bed chromatography device ZSM-5 molecular sieve and is 60 DEG C, inlet amount 1L/h, collection passes through liquid.
Then, the ultrafiltration membrane in 8~12 angstroms of apertures will be passed through above by liquid.25~40 DEG C of ultrafiltration are controlled, retains and penetrates The purity of liquid is 99.30%.
Embodiment 3
Firstly, being packed into the ZSM-5 molecular sieve of silica alumina ratio 28 as stationary phase on simulated movable bed chromatography device bed.By glucose Slurry controls through the temperature of simulated movable bed chromatography device by above-mentioned simulated movable bed chromatography device ZSM-5 molecular sieve and is 50 DEG C, inlet amount 5L/h, collection passes through liquid.
Then, the ultrafiltration membrane in 10 angstroms of apertures will be passed through above by liquid.30 DEG C of ultrafiltration are controlled, the purity of permeate is retained It is 99.42%.
Embodiment 4
Firstly, being packed into the ZSM-5 molecular sieve of silica alumina ratio 28 as stationary phase on simulated movable bed chromatography device bed.By glucose Slurry controls through the temperature of simulated movable bed chromatography device by above-mentioned simulated movable bed chromatography device ZSM-5 molecular sieve and is 50 DEG C, inlet amount 5L/h, collection passes through liquid.
Then, the ultrafiltration membrane in 10 angstroms of apertures will be passed through above by liquid.30 DEG C of ultrafiltration are controlled, the purity of permeate is retained It is 99.47%.
Embodiment 5
Firstly, being packed into the ZSM-5 molecular sieve of silica alumina ratio 28 as stationary phase on simulated movable bed chromatography device bed.By glucose Slurry controls through the temperature of simulated movable bed chromatography device by above-mentioned simulated movable bed chromatography device ZSM-5 molecular sieve and is 50 DEG C, inlet amount 3L/h, collection passes through liquid.
Then, the ultrafiltration membrane in 9 angstroms of apertures will be passed through above by liquid.30 DEG C of ultrafiltration are controlled, the purity of permeate is retained It is 99.55%.
The numberical range of each technological parameter as involved in the present invention can not all embody in the above-described embodiments, As long as but those skilled in the art's envisioned any numerical value fallen into the above-mentioned numberical range completely can be implemented this Invention also includes any combination of occurrence in several numberical ranges certainly.Herein, due to space considerations, be omitted to Out in certain one or more numberical range occurrence embodiment, this disclosure for being not to be construed as technical solution of the present invention do not fill Point.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention, But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention, Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention Within protection scope and the open scope.

Claims (6)

1. a kind of method for isolating and purifying glucose from glucose syrup, which comprises the following steps:
(1) by glucose syrup by ZSM-5 molecular sieve, reservation passes through liquid;
(2) by the ultrafiltration membrane for passing through 8~12 angstroms of apertures by liquid, retain permeate.
2. the method for glucose is isolated and purified from glucose syrup according to claim 1, which is characterized in that the ZSM-5 The form of molecular sieve is using ZSM-5 molecular sieve as the simulated movable bed chromatography device of stationary phase.
3. the method for glucose is isolated and purified from glucose syrup according to claim 2, which is characterized in that pass through ZSM-5 The temperature of molecular sieve is 40~60 DEG C.
4. the method for glucose is isolated and purified from glucose syrup according to claim 2, which is characterized in that pass through ZSM-5 The inlet amount of molecular sieve is 1~5L/h.
5. the method for glucose is isolated and purified from glucose syrup according to claim 2, which is characterized in that pass through ultrafiltration membrane Temperature be 25~40 DEG C.
6. the method for glucose is isolated and purified from glucose syrup according to claim 1, which is characterized in that pass through ultrafiltration membrane Pressure be 10~20bar.
CN201810909021.3A 2018-08-10 2018-08-10 A method of isolating and purifying glucose from glucose syrup Pending CN109053823A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5548400A (en) * 1978-10-04 1980-04-07 Mitsubishi Chem Ind Removing of oligosaccharide
CN1222869A (en) * 1996-05-24 1999-07-14 库尔特公司 Method for fractionation of solution by chromatographic simulated moving bed process
CN1928121A (en) * 2006-09-20 2007-03-14 山东西王糖业有限公司 Method of extracting high-purity glucose from saccharified glucose syrup
CN102492782A (en) * 2011-12-16 2012-06-13 长春大成新资源集团有限公司 Desalting method for syrup and production method for glucose syrup
CN102559940A (en) * 2011-12-31 2012-07-11 三达膜科技(厦门)有限公司 Separation and purification method of glucose
CN103179866A (en) * 2010-10-08 2013-06-26 罗盖特兄弟公司 Method for manufacturing high-purity sorbitol syrups from sucrose and uses thereof
CN104593447A (en) * 2014-12-24 2015-05-06 山东龙力生物科技股份有限公司 Energy-saving preparation technology of high-quality glucose powder

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5548400A (en) * 1978-10-04 1980-04-07 Mitsubishi Chem Ind Removing of oligosaccharide
CN1222869A (en) * 1996-05-24 1999-07-14 库尔特公司 Method for fractionation of solution by chromatographic simulated moving bed process
CN1928121A (en) * 2006-09-20 2007-03-14 山东西王糖业有限公司 Method of extracting high-purity glucose from saccharified glucose syrup
CN103179866A (en) * 2010-10-08 2013-06-26 罗盖特兄弟公司 Method for manufacturing high-purity sorbitol syrups from sucrose and uses thereof
CN102492782A (en) * 2011-12-16 2012-06-13 长春大成新资源集团有限公司 Desalting method for syrup and production method for glucose syrup
CN102559940A (en) * 2011-12-31 2012-07-11 三达膜科技(厦门)有限公司 Separation and purification method of glucose
CN104593447A (en) * 2014-12-24 2015-05-06 山东龙力生物科技股份有限公司 Energy-saving preparation technology of high-quality glucose powder

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
朱洪法 主编: "《催化剂手册》", 31 August 2008, 金盾出版社 *
李万才 主编: "《生物分离技术》", 31 August 2009, 中国轻工业出版社 *

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