CN105483182A - Production technique of fiber oligosaccharide - Google Patents
Production technique of fiber oligosaccharide Download PDFInfo
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- CN105483182A CN105483182A CN201511005042.5A CN201511005042A CN105483182A CN 105483182 A CN105483182 A CN 105483182A CN 201511005042 A CN201511005042 A CN 201511005042A CN 105483182 A CN105483182 A CN 105483182A
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- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
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Abstract
The invention discloses a production technique of fiber oligosaccharide, which comprises the following steps: putting cellulose-containing biomass into a selective plant glycosidic bond high-energy blasting machine, keeping the temperature under the pressure of 1.5-2.0 MPa for 5-7 minutes, and instantaneously relieving pressure within 0.02-0.5 second; and after blasting, adding water, extracting to obtain an extracting solution, adding an oriented cellulose endoenzyme into the extracting solution to perform enzymolysis to obtain an enzymolysis solution, sequentially carrying out decolorization, ultrafiltration, ion exchange desalting and nanofiltration refinement on the enzymolysis solution to obtain a refined solution, and concentrating or drying the refined solution to obtain the fiber oligosaccharide syrup or fiber oligosaccharide solid powder. The method solves the problem that the molecular weight can not be artificially controlled by single biodegradation at some stage. Thus, the fiber oligosaccharide can be prepared from the cellulose-rich biomass raw material in industry. The method has actual and practical meanings in industrial scale production.
Description
Technical field
The invention belongs to oligosaccharides preparing technical field, be specifically related to a kind of production technique of cell-oligosaccharide.
Background technology
Prepare at present cell-oligosaccharide mainly from the biomass material containing vegetable fibre through fiber composite enzyme liberating Mierocrystalline cellulose, propose through being separated again, Chinese cell-oligosaccharide, English name cello-oligosaccharide, by less than 10 glucose molecules by β-1, the oligosaccharides that 4-glycosidic link is formed by connecting is the product in cellulose degradation process.Because molecular weight cellulose arrives hundreds of thousands of tens0000, glycosidic link bond energy is higher, be difficult to control the oligosaccharides that glucose molecule is formed by connecting by β-Isosorbide-5-Nitrae-glycosidic link below 10 by fiber composite enzyme liberating, both having made oligosaccharides generate does not have industrial production meaning because content is too low yet.
Summary of the invention
For problems of the prior art, the invention provides a kind of production technique of cell-oligosaccharide, directly glycosidic link molecular structure in cellulose macromolecule chain is brokenly interrupted the low molecule compounding substances forming fibrous polysaccharaide, low sugar and monose through high energy is quick-fried by the plant material of rich cellulose, then the cell-oligosaccharide product concentrating or be dried to different content is refined through extracting and developing, the oligosaccharides that the method obtains is controlled, can realize suitability for industrialized production.
For achieving the above object, the present invention is by the following technical solutions:
A kind of production technique of cell-oligosaccharide, by the biomass of cellulose, put into the quick-fried broken then extracting in water of selective vegetable glycosidic link high energy puffing machine and obtain extracting solution, in extracting solution, add directional fiber element restriction endonuclease enzymolysis obtain enzymolysis solution, enzymolysis solution obtains refined liquid through decolouring, ultrafiltration, ion-exchange desalination and nanofiltration successively, carries out concentrating or drying obtains cell-oligosaccharide syrup or cell-oligosaccharide solid powder to refined liquid.
The quick-fried broken service temperature of described high energy is 150 ~ 195 DEG C, and working pressure is 1.5 ~ 2.0Mpa, and venting duration was at 0.02 ~ 0.5 second.
The pH of described Extracting temperature 40-80 DEG C extracting solution is 4 ~ 8.
The operation steps of described enzymolysis is: be under the condition of 45 ~ 55 DEG C in temperature, adds directional fiber element restriction endonuclease 40,000 units/gram butt substrate, enzymolysis 40min ~ 30 hour in extracting solution.
The biomass of described cellulose are at least one in the fibrous residue after corn cob, maize straw, cotton straws, extraction wood oligose or the bagasse after extracting wood oligose.
Enzymolysis solution decolouring adopts food and activated carbon decolorizing temperature to be not less than 95 DEG C, filtered while hot. and removing gac, obtains destainer.Ultrafiltration employing aperture is the hollow fiber ultrafiltration membrane of 3000 ~ 5000 molecular weight, what ion-exchange desalination adopted is that food grade macroporous adsorbent resin carries out degree of depth decolouring desalination and removes the fibrous polysaccharaide of more than 1800 molecular weight, and the polysulfones nanofiltration membrane of to be aperture be 300 ~ 500 molecular weight of nanofiltration employing deviates from moisture content and monose.Obtain the refined liquid of main fibre-bearing oligosaccharides.
Under 40 ~ 70 DEG C of conditions, being concentrated into mass concentration to refined liquid concentrated employing MVR thickening equipment is 65 ~ 75%, obtains faint yellow food-grade cellulose oligosaccharides syrup.
Spray-dired mode is adopted to obtain cell-oligosaccharide solid powder at 80--185 DEG C to refined liquid drying.
Beneficial effect of the present invention: cellulosic biomass material will be rich in (as maize straw by the quick-fried broken equipment of high energy glycosidic link, the maize straw waste residue of rich cellulose after extraction xylo-oligosaccharide, cellulose is 40 ~ 60%, and cotton stalk, loads the quick-fried broken equipment of high energy glycosidic link.Under the pressure of 1.5---2Mpa, keep certain hour, carry out moment pressure release and material was produced at 0.02-0.5 second.Broken into pieces by cellulose glycosidic bonds, these fragments can with 50 DEG C of hot water strippings.The soluble fiber polysaccharide of 1800 molecular weight of such formation, solubility rate 30% ~ 47%.Solve so pure by biological degradation can not manual control molecular weight in the problem of certain one-phase.So industrially utilize cellulosic biomass feedstock to prepare oligosaccharides and become possibility.After the fibrous polysaccharaide of solubility is dissolved, the more special Mierocrystalline cellulose restriction endonuclease adding 40,000 units/gram substrates is to soluble fiber polysaccharide, directed inscribe enzymolysis, thus prepares containing pol at the extracting solution of 4 ~ 5.5% fibre-bearing oligosaccharides water solubility rates more than 40%.Extracting solution is again through activated carbon decolorizing, and ultrafiltration removes the fibrous polysaccharaide Zulkovsky starch etc. of part macromolecule, then through the refining purification of ion-exchange nanofiltration, produces cell-oligosaccharide syrupy product and cell-oligosaccharide powder after cryoconcentration drying.The method has reality and practical significance in industrial-scale production.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Embodiment 1
Get the corn cob residue after extracting xylo-oligosaccharide, 150 kilograms, containing dry-matter 39.6%, moisture content 61.4%; Cellulose 47% in dry-matter, loads glycosidic link high energy puffing machine and boosts to 1.7Mpa pressurize 7 minutes, pressure release immediately.Quick-fried broken material is added 1000 liters of deionized waters to extract, extracting solution adds Mierocrystalline cellulose restriction endonuclease 40,000 units/gram substrate, filters, survey extracting solution total reducing sugar 13.44 kilograms in 50 DEG C of enzymolysis to 30 hour.Solubility rate 30.29%.In extracting solution, cell-oligosaccharide content reaches 21.974% monose 62% soluble fiber polysaccharide 15%.Through decolouring, ultrafiltration, ion-exchange, after nanofiltration is refining, cryoconcentration obtains 70% cell-oligosaccharide concentrated solution 4.03 kilograms.
Embodiment 2
The production technique of the cell-oligosaccharide of the present embodiment, step is as follows:
Maize straw is put into selective vegetable glycosidic link high energy puffing machine quick-fried broken, the quick-fried broken service temperature of high energy is 150 DEG C, and working pressure is 2.0Mpa, and venting duration is less than 0.02 second, then extracting in water obtains extracting solution, the pH of extracting solution is 4, under the condition of 45 DEG C, the add-on adding directional fiber element restriction endonuclease is 40,000 units/gram butts, enzymolysis 40min obtains enzymolysis solution, enzymolysis solution is successively through decolouring, ultrafiltration, ion-exchange desalination and nanofiltration obtain refined liquid, wherein, enzymolysis solution decolouring adopts food and gac, ultrafiltration employing aperture is the hollow fiber ultrafiltration membrane of 3000 ~ 5000 molecular weight, what ion-exchange desalination adopted is that food grade macroporous adsorbent resin carries out degree of depth decolouring desalination and removes the fibrous polysaccharaide of more than 1800 molecular weight, the polysulfones nanofiltration membrane of to be aperture be 300 ~ 500 molecular weight that nanofiltration adopts, adopt MVR thickening equipment under 40 DEG C of conditions, be concentrated into mass concentration to refined liquid to be 65%, to obtain faint yellow food-grade cellulose oligosaccharides syrup.
Embodiment 3
The production technique of the cell-oligosaccharide of the present embodiment, step is as follows:
Maize straw and cotton straws are put into selective vegetable glycosidic link high energy puffing machine quick-fried broken, the quick-fried broken service temperature of high energy is 195 DEG C, and working pressure is 1.8Mpa, and venting duration is less than 0.5 second, then extracting in water obtains extracting solution, the pH of extracting solution is 8, under the condition of 55 DEG C, the add-on adding directional fiber element restriction endonuclease is 40,000 units/gram butts, enzymolysis obtains enzymolysis solution in 30 hours, enzymolysis solution is successively through decolouring, ultrafiltration, ion-exchange desalination and nanofiltration obtain refined liquid, wherein, enzymolysis solution decolouring adopts food and gac, ultrafiltration employing aperture is the hollow fiber ultrafiltration membrane of 3000 ~ 5000 molecular weight, what ion-exchange desalination adopted is that food grade macroporous adsorbent resin carries out degree of depth decolouring desalination and removes the fibrous polysaccharaide of more than 1800 molecular weight, the polysulfones nanofiltration membrane of to be aperture be 300 ~ 500 molecular weight that nanofiltration adopts, adopt MVR thickening equipment under 70 DEG C of conditions, be concentrated into mass concentration to refined liquid to be 75%, to obtain faint yellow food-grade cellulose oligosaccharides syrup.
Embodiment 4
The production technique of the cell-oligosaccharide of the present embodiment, step is as follows:
Fibrous residue after extraction wood oligose is put into selective vegetable glycosidic link high energy puffing machine quick-fried broken, the quick-fried broken service temperature of high energy is 160 DEG C, and working pressure is 1.5Mpa, and venting duration is less than 0.2 second, then extracting in water obtains extracting solution, the pH of extracting solution is 5, under the condition of 50 DEG C, the add-on adding directional fiber element restriction endonuclease is 40,000 units/gram butts, enzymolysis obtains enzymolysis solution in 10 hours, enzymolysis solution is successively through decolouring, ultrafiltration, ion-exchange desalination and nanofiltration obtain refined liquid, wherein, enzymolysis solution decolouring adopts food and gac, ultrafiltration employing aperture is the hollow fiber ultrafiltration membrane of 3000 ~ 5000 molecular weight, what ion-exchange desalination adopted is that food grade macroporous adsorbent resin carries out degree of depth decolouring desalination and removes the fibrous polysaccharaide of more than 1800 molecular weight, the polysulfones nanofiltration membrane of to be aperture be 300 ~ 500 molecular weight that nanofiltration adopts, spray-dired mode is adopted to obtain cell-oligosaccharide solid powder to refined liquid.
Embodiment 5
The production technique of the cell-oligosaccharide of the present embodiment, step is as follows:
Cotton straws and the bagasse after extracting wood oligose are put into selective vegetable glycosidic link high energy puffing machine quick-fried broken, the quick-fried broken service temperature of high energy is 170 DEG C, and working pressure is 1.6Mpa, and venting duration is less than 0.3 second, then extracting in water obtains extracting solution, the pH of extracting solution is 6, under the condition of 48 DEG C, the add-on adding directional fiber element restriction endonuclease is 40,000 units/gram butts, enzymolysis obtains enzymolysis solution in 20 hours, enzymolysis solution is successively through decolouring, ultrafiltration, ion-exchange desalination and nanofiltration obtain refined liquid, wherein, enzymolysis solution decolouring adopts food and gac, ultrafiltration employing aperture is the hollow fiber ultrafiltration membrane of 3000 ~ 5000 molecular weight, what ion-exchange desalination adopted is that food grade macroporous adsorbent resin carries out degree of depth decolouring desalination and removes the fibrous polysaccharaide of more than 1800 molecular weight, the polysulfones nanofiltration membrane of to be aperture be 300 ~ 500 molecular weight that nanofiltration adopts, spray-dired mode is adopted to obtain cell-oligosaccharide solid powder to refined liquid.
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (8)
1. the production technique of a cell-oligosaccharide, it is characterized in that: by the biomass of cellulose, put into the quick-fried broken then extracting in water of selective vegetable glycosidic link high energy puffing machine and obtain extracting solution, in extracting solution, add directional fiber element restriction endonuclease enzymolysis obtain enzymolysis solution, enzymolysis solution obtains refined liquid through decolouring, ultrafiltration, ion-exchange desalination and nanofiltration successively, carries out concentrating or drying obtains cell-oligosaccharide syrup or cell-oligosaccharide solid powder to refined liquid.
2. the production technique of cell-oligosaccharide according to claim 1, is characterized in that: the quick-fried broken service temperature of described high energy is 150 ~ 195 DEG C, and working pressure is 1.5 ~ 2.0Mpa, and venting duration is less than 0.02 ~ 0.5 second.
3. the production technique of cell-oligosaccharide according to claim 1, is characterized in that: the Extracting temperature of described water is 40---80 DEG C of 30-40 minutes extraction time, and the pH of extracting solution is 4 ~ 8.
4. the production technique of cell-oligosaccharide according to claim 1, it is characterized in that: the operation steps of described enzymolysis is: be preferably at 48---50 DEG C in temperature under the condition of 45 ~ 55 DEG C, directional fiber element restriction endonuclease 40,000 units/gram butt is added, enzymolysis 40min ~ 30 hour in extracting solution.
5. the production technique of cell-oligosaccharide according to claim 1, is characterized in that: the biomass of described cellulose are at least one in the fibrous residue after corn cob, maize straw, cotton straws, extraction wood oligose or the bagasse after extracting wood oligose.
6. the production technique of cell-oligosaccharide according to claim 1, it is characterized in that: enzymolysis solution decolouring adopts food grade active charcoal, ultrafiltration employing aperture is the hollow fiber ultrafiltration membrane of 3000 ~ 5000 molecular weight, what ion-exchange desalination adopted is that food grade macroporous adsorbent resin carries out degree of depth decolouring desalination and removes the fibrous polysaccharaide of more than 1800 molecular weight, the polysulfones nanofiltration membrane of to be aperture be 300 ~ 500 molecular weight that nanofiltration adopts removes water and monose, and cell-oligosaccharide initial concentration is reached 9%--20% to pol.
7. the production technique of cell-oligosaccharide according to claim 1, is characterized in that: under 40 ~ 70 DEG C of conditions, being concentrated into pol to refined liquid concentrated employing MVR thickening equipment is 65 ~ 75%, obtains faint yellow food-grade cellulose oligosaccharides syrup.
8. the production technique of cell-oligosaccharide according to claim 1, is characterized in that: be that spraying dry obtains cell-oligosaccharide solid powder under 80 ~ 185 DEG C of conditions to refined liquid drying.
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| CN201511005042.5A CN105483182A (en) | 2015-12-29 | 2015-12-29 | Production technique of fiber oligosaccharide |
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| CN201511005042.5A CN105483182A (en) | 2015-12-29 | 2015-12-29 | Production technique of fiber oligosaccharide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106244735A (en) * | 2016-07-29 | 2016-12-21 | 中国科学院过程工程研究所 | A kind of production technology of cell-oligosaccharide |
| CN115181137A (en) * | 2021-04-01 | 2022-10-14 | 李来锁 | Process for producing xylooligosaccharide by adopting physical bursting method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115181137A (en) * | 2021-04-01 | 2022-10-14 | 李来锁 | Process for producing xylooligosaccharide by adopting physical bursting method |
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