CN104593446A - Preparation method of pure xylooligosaccharide powder - Google Patents
Preparation method of pure xylooligosaccharide powder Download PDFInfo
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- CN104593446A CN104593446A CN201410819669.3A CN201410819669A CN104593446A CN 104593446 A CN104593446 A CN 104593446A CN 201410819669 A CN201410819669 A CN 201410819669A CN 104593446 A CN104593446 A CN 104593446A
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- xylo
- zytase
- oligosaccharide
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- xylan
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- HEBKCHPVOIAQTA-NGQZWQHPSA-N d-xylitol Chemical compound OC[C@H](O)C(O)[C@H](O)CO HEBKCHPVOIAQTA-NGQZWQHPSA-N 0.000 title claims abstract description 75
- 239000000843 powder Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 37
- 229920001221 xylan Polymers 0.000 claims abstract description 34
- 150000004823 xylans Chemical class 0.000 claims abstract description 34
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 26
- 239000012528 membrane Substances 0.000 claims abstract description 18
- 239000006188 syrup Substances 0.000 claims abstract description 10
- 235000020357 syrup Nutrition 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 19
- 239000007864 aqueous solution Substances 0.000 claims description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000004880 explosion Methods 0.000 claims description 10
- 238000000926 separation method Methods 0.000 claims description 10
- 230000000694 effects Effects 0.000 claims description 9
- 238000004064 recycling Methods 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 7
- 235000008504 concentrate Nutrition 0.000 claims description 7
- 239000012141 concentrate Substances 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 240000008042 Zea mays Species 0.000 claims description 6
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 6
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 235000005822 corn Nutrition 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 5
- 239000000049 pigment Substances 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 239000003456 ion exchange resin Substances 0.000 claims description 2
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 2
- 235000012054 meals Nutrition 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 229920001542 oligosaccharide Polymers 0.000 abstract description 3
- 238000007670 refining Methods 0.000 abstract description 2
- 101710121765 Endo-1,4-beta-xylanase Proteins 0.000 abstract 4
- 101710101928 Endo-1,4-beta-xylanase 2 Proteins 0.000 abstract 2
- 230000002255 enzymatic effect Effects 0.000 abstract 2
- 239000000413 hydrolysate Substances 0.000 abstract 2
- 150000002482 oligosaccharides Chemical class 0.000 abstract 2
- 101710101929 Endo-1,4-beta-xylanase 3 Proteins 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 abstract 1
- 230000035943 smell Effects 0.000 description 10
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 238000005342 ion exchange Methods 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- 229920001353 Dextrin Polymers 0.000 description 3
- 239000004375 Dextrin Substances 0.000 description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 3
- 235000011130 ammonium sulphate Nutrition 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000004061 bleaching Methods 0.000 description 3
- 235000019425 dextrin Nutrition 0.000 description 3
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- -1 polyoxyethylene Polymers 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 240000007594 Oryza sativa Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 239000010903 husk Substances 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- JCSJTDYCNQHPRJ-UHFFFAOYSA-N 20-hydroxyecdysone 2,3-acetonide Natural products OC1C(O)C(O)COC1OC1C(O)C(O)C(OC2C(C(O)C(O)OC2)O)OC1 JCSJTDYCNQHPRJ-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- JVZHSOSUTPAVII-UHFFFAOYSA-N Xylotetraose Natural products OCC(OC1OCC(OC2OCC(OC3OCC(O)C(O)C3O)C(O)C2O)C(O)C1O)C(O)C(O)C=O JVZHSOSUTPAVII-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000001166 ammonium sulphate Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- JCSJTDYCNQHPRJ-FDVJSPBESA-N beta-D-Xylp-(1->4)-beta-D-Xylp-(1->4)-D-Xylp Chemical compound O[C@@H]1[C@@H](O)[C@H](O)CO[C@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O)C(O)OC2)O)OC1 JCSJTDYCNQHPRJ-FDVJSPBESA-N 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 230000000378 dietary effect Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000005846 sugar alcohols Chemical class 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 150000003740 xylobioses Chemical class 0.000 description 1
- ABKNGTPZXRUSOI-UHFFFAOYSA-N xylotriose Natural products OCC(OC1OCC(OC2OCC(O)C(O)C2O)C(O)C1O)C(O)C(O)C=O ABKNGTPZXRUSOI-UHFFFAOYSA-N 0.000 description 1
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- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Saccharide Compounds (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a preparation method of pure xylooligosaccharide powder. The preparation method comprises the following steps: adjusting the pH value of a xylan solution to 3.0-6.0, and adding xylanase to perform enzymolysis to obtain xylan enzymatic hydrolysate containing xylanase; filtering the xylan enzymatic hydrolysate with an ultrafiltration membrane to obtain a coarse xylooligosaccharide liquid 1, recycled xylanase 2 and a macromolecular oligosaccharide mixed liquid respectively, introducing the xylanase 2 and the mixed liquid into a saccharifying tank, meanwhile adding new xylanase, using the recycled xylanase repeatedly, and performing saccharification and enzymolysis on macromolecular oligosaccharide repeatedly to prepare a coarse xylooligosaccharide liquid 2 and recycled xylanase 3, wherein the molecular weight cut-off of the ultrafiltration membrane is 1000-1500Da, the pressure before the ultrafiltration membrane is 0.5-0.7MPa, and the pressure behind the ultrafiltration membrane is 0.3-0.5MPa; combining the obtained coarse xylooligosaccharide liquids, and refining to obtain xylooligosaccharide syrup; and performing vacuum belt type concentration or scraper evaporator concentration to obtain the pure xylooligosaccharide powder. According to the preparation method, the production cost is reduced, the utilization efficiency of raw materials and the product quality are improved, and a favorable market prospect is achieved.
Description
Technical field
The present invention relates to a kind of preparation method of pure xylo-oligosaccharide powder, belong to technical field of functional sugar alcohol production.
Background technology
Xylo-oligosaccharide is the one of oligose, be by β-Isosorbide-5-Nitrae-endo-xylanase take xylan as substrate, the polymerization degree that formed of the hydrolysis β-Isosorbide-5-Nitrae glycosidic link oligose that is 2-7.Xylo-oligosaccharide can improve organism (humans and animals) archenteric flora balance, the growth of promoting digestion road beneficial bacteria, suppresses harmful microbe breeding, promotes dietetic alimentation, improve immunity of organisms.
A kind of method hemicellulose in corn cob being converted into xylan therefrom purifying oligo-xylose is described in the preparation method (patent No. ZL 200410023875.X) of the patent xylo-oligosaccharide now announced, but this method shortcoming is: zytase only utilizes once just by enzyme-deactivating, do not recycle, the utilization ratio of enzyme is very low, zytase is expensive, causes product cost higher; In xylo-oligosaccharide concentration process, employing conventional vacuum concentrates, high temperature concentration time is long, cause product color dark, in powder preparing processes, (as content 20% ~ 70%) must add a certain amount of vehicle such as dextrin, starch etc., then carries out spraying dry, owing to there is vehicle, cause xylo-oligosaccharide powder solubility property to reduce, be mingled with the problems such as other smells and affect its result of use and scope.
Describe a kind of zytase in patent " a kind of method of producing low polyxylose with dual-aqueous phase hydrolyzation system " (CN101294175B) and repeat to recycle the method preparing xylo-oligosaccharide, xylo-oligosaccharide is prepared by two-phase separation system is integrated in the method, enzymolysis solution leaves standstill in distribution trough, zytase is distributed in phase polyethylene glycol system, in recovery, phase system realizes the recycling of zytase, xylo-oligosaccharide is distributed in lower phase ammonium sulphate system, residual oligose and polyoxyethylene glycol recycling is reclaimed by ultra-filtration membrane, this method has the following disadvantages: 1) fusing point of polyoxyethylene glycol is 64 DEG C ~ 66 DEG C, existing zytase peak enzymolysis-ability temperature is 50 DEG C ~ 60 DEG C, therefore, at peak enzymolysis-ability temperature, polyoxyethylene glycol may exist with solid state and impact uses, 2) there is hazardness to HUMAN HEALTH in the ammonium sulfate added in diphasic system, is not suitable in the xylooligosaccharides production used as foodstuff additive, and meanwhile, ammonium sulfate adds the pressure that subsequent ion exchanges operation desalination.
In patent " a kind of preparation method of rice husk xylo-oligosaccharides " (CN101381753B), xylo-oligosaccharide liquid glucose prepared by rice husk adopts conventional vacuum drying mode directly to prepare xylo-oligosaccharide finished product, it is not containing vehicle, but in the method, liquid glucose is at 40 ~ 60 DEG C, the vacuum concentration time is 15 ~ 20h, and xylo-oligosaccharide liquid glucose can cause color and luster to deepen under long-time high temperature, and the method cannot obtain high-purity xylo-oligosaccharide powder.
Summary of the invention
For above-mentioned prior art, the object of this invention is to provide a kind of preparation method of pure xylo-oligosaccharide powder, zytase is reclaimed in the pre-treatment of employing steam explosion, ultra-filtration membrane continuously and macromolecular oligo sugar repeats enzymolysis, refining, the liquid glucose of enzymolysis solution rapidly and efficiently concentrate, the preparation of the technique such as cooling, pulverizing, containing high-purity xylo-oligosaccharide powder of vehicle, solves that the solubility property that xylo-oligosaccharide powder causes due to adding of vehicle reduces, adulterate other smell and long-time high temperature concentrate the problems such as the product color intensification caused.
For achieving the above object, the present invention adopts following technical proposals:
A preparation method for pure xylo-oligosaccharide powder, comprises the following steps:
(1) pH value adjusting the xylan aqueous solution is 3.0-6.0, adds zytase and carries out enzymolysis, obtain the xylan enzymolysis solution containing zytase;
(2) the xylan enzymolysis solution of step (1) is carried out ultrafiltration membrance filter, the molecular weight cut-off of ultra-filtration membrane is 1000 ~ 1500Da, pressure 0.5 ~ 0.7MPa before ultra-filtration membrane, 0.3 ~ 0.5MPa is pressed after film, obtain xylo-oligosaccharide raw sugar liquid 1 respectively, and the mixed solution of the zytase 2 reclaimed and macromolecular oligo sugar, the mixed solution of zytase 2 and macromolecular oligo sugar is squeezed into saccharifying tank, add new zytase simultaneously, the zytase recycling of reclaiming, macromolecular oligo sugar repeats saccharification, enzymolysis, the zytase 3 prepared xylo-oligosaccharide raw sugar liquid 2 and reclaim, zytase like this reuses,
(3) the xylo-oligosaccharide raw sugar liquid obtained in combining step (2), and refine, obtain xylo-oligosaccharide syrup;
(4) by the xylo-oligosaccharide syrup of step (3), through vacuum belt, concentrated or scraper evaporator concentrates, and by cooling, pulverizes to obtain high-purity xylo-oligosaccharide powder.
In step (1), the preparation method of the described xylan aqueous solution is: be that raw material is through solvent pre-treatment with corn cob meal, solid-liquid separation removes the pretreated water solution containing pigment, the filter residue obtained and process water be made into liquid to be blasted that solid-to-liquid ratio is 1:2-6 (g/mL), pressure 1.5-2.5MPa, treatment time be 120s-240s, under diluted acid catalyzer accounts for explosion liquid total mass 0.1%-1.5% condition, carry out continuous steam explosion treatment, solid-liquid separation, collects the aqueous solution being rich in xylan.
The mass concentration of the xylan aqueous solution of preparation is 1%-8%.
Described diluted acid catalyzer is sulfuric acid, acetic acid, formic acid, citric acid.
The add-on of zytase is: the zytase of 30-50UI units activity in every gram of xylan; Be preferably 40UI.
In step (2), new zytase add-on is: the zytase of 5-20UI units activity in every gram of xylan; Be preferably 10UI.
In step (3), the process for purification of xylo-oligosaccharide raw sugar liquid comprises activated carbon decolorizing and ion exchange resin removal of impurities.
In step (4), it be vacuum tightness is-80 ~-120KPa that vacuum belt concentrates parameter, one section of Heating temperature 95 ~ 130 DEG C, two sections of Heating temperatures 95 ~ 130 DEG C, and three sections of Heating temperatures are 60 ~ 90 DEG C, and cooling temperature is 20 ~ 40 DEG C; Scraper plate evaporation concentration parameter is that temperature controls at 115 DEG C ~ 130 DEG C, and evaporating pressure is-0.08 ~-0.098MPa, and drop temperature controls at 105 DEG C ~ 120 DEG C, and scraper plate rotating speed controls at 3 ~ 5m/s, and cooling temperature is 20 ~ 40 DEG C.
Beneficial effect of the present invention:
(1) zytase of the present invention can realize recycling and reusing by ultra-filtration membrane, reduce the production cost of xylo-oligosaccharide, macromole glycan after enzymolysis in enzymolysis solution, after ultrafiltration membrance filter, can repeat enzyme-squash techniqued xylo-oligosaccharide, improves the utilising efficiency of raw material.
(2) syrup of the present invention through rapidly and efficiently concentrated, dry, cooling, pulverize and prepare xylo-oligosaccharide powder, long owing to avoiding high temperature concentration time, adding of vehicle (dextrin etc.), make product water-soluble, smell, color and luster etc. be improved significantly.
(3) present invention reduces production cost, improve raw material utilization efficiency, improve product quality, there are good market outlook.
Accompanying drawing explanation
Fig. 1 is process flow sheet prepared by pure xylo-oligosaccharide powder.
Embodiment
Below by specific examples, the present invention will be further elaborated, should be noted that following explanation is only to explain the present invention, not limiting its content.
Embodiment 1:
1) corn cob raw material is through pulverizing, hot-water pretreatment, solid-liquid separation removes the pretreated water solution containing pigment, the filter residue obtained and process water are made into the liquid to be blasted that solid-to-liquid ratio is 1:2, pressure 1.5MPa, treatment time be 220s, under diluted acid catalyzer accounts for explosion liquid total mass 0.8% condition, carry out continuous steam explosion treatment, solid-liquid separation, collects the aqueous solution being rich in xylan;
2) pH value adjusting the xylan aqueous solution is 6.0, and the ratio adding 40UI units activity according to every gram of xylan in the aqueous solution of xylan adds zytase, and enzymic hydrolysis temperature is 50 DEG C, and the enzymatic hydrolysis reaction time is 7.0h, obtains xylo-oligosaccharide enzymolysis solution;
3) enzymolysis solution carries out ultrafiltration membrance filter, and the molecular weight cut-off of ultra-filtration membrane is 1200Da, pressure 0.5MPa before ultra-filtration membrane, press 0.3MPa after film, reclaim zytase and macromolecular oligo sugar, squeeze into saccharifying tank, zytase reuses, and macromolecular oligo sugar is through repeating saccharification enzymolysis;
4) filtered solution is through activated carbon decolorizing, and activated carbon decolorizing temperature is 80 DEG C, and the per-cent that gac addition accounts for liquid glucose weight is 0.4%, and bleaching time is 30min, by ion-exchange removal of impurities, and flow velocity 9m
3/ h;
5) drying of xylo-oligosaccharide syrup is by scraper evaporator evaporation concentration, scraper plate evaporation drying parameter is that temperature controls at 115 DEG C, and evaporating pressure is-0.085MPa, and drop temperature controls at 105 DEG C, it is 25 DEG C that scraper plate rotating speed controls at 3.5m/s cooling temperature, pulverizes the pure xylo-oligosaccharide powder of preparation.
Embodiment 2:
1) corn cob raw material is through pulverizing, hot-water pretreatment, solid-liquid separation removes the pretreated water solution containing pigment, the filter residue obtained and process water are made into the liquid to be blasted that solid-to-liquid ratio is 1:4, pressure 1.8MPa, treatment time be 200s, under diluted acid catalyzer accounts for explosion liquid total mass 0.6% condition, carry out continuous steam explosion treatment, solid-liquid separation, collects the aqueous solution being rich in xylan;
2) pH value adjusting the xylan aqueous solution is 4.0, the zytase recycling that ultrafiltration in embodiment 1 is reclaimed is added in the aqueous solution of xylan, add new zytase in the ratio of every gram of xylan 10UI units activity simultaneously, enzymic hydrolysis temperature is 45 DEG C, the enzymatic hydrolysis reaction time is 8.0h, obtains xylo-oligosaccharide enzymolysis solution;
3) enzymolysis solution carries out ultrafiltration membrance filter, and the molecular weight cut-off of ultra-filtration membrane is 1200Da, pressure 0.65MPa before ultra-filtration membrane, press 0.45MPa after film, reclaim zytase and macromolecular oligo sugar, squeeze into saccharifying tank, zytase reuses, and macromolecular oligo sugar is through repeating saccharification enzymolysis;
4) filtered solution is through activated carbon decolorizing, and activated carbon decolorizing temperature is 70 DEG C, and the per-cent that gac addition accounts for liquid glucose weight is 0.6%, and bleaching time is 50min, by ion-exchange removal of impurities, and flow velocity 12m
3/ h;
5) xylo-oligosaccharide syrup is dry is concentrated by vacuum belt, and vacuum tightness is-90KPa, one section of Heating temperature 115 DEG C, two sections of Heating temperatures 105 DEG C, and three sections of Heating temperatures are 85 DEG C, and cooling temperature is 30 DEG C, pulverize to obtain pure xylo-oligosaccharide powder;
Embodiment 3:
1) corn cob raw material is through pulverizing, hot-water pretreatment, solid-liquid separation removes the pretreated water solution containing pigment, the filter residue obtained and process water are made into the liquid to be blasted that solid-to-liquid ratio is 1:6, pressure 2.0MPa, treatment time be 150s, under diluted acid catalyzer accounts for explosion liquid total mass 0.2% condition, carry out continuous steam explosion treatment, solid-liquid separation, collects the aqueous solution being rich in xylan;
2) pH value adjusting the xylan aqueous solution is 5.0, add ultrafiltration in embodiment 2 in the aqueous solution of xylan and reclaim zytase recycling, add new zytase in the ratio of every gram of xylan 8UI units activity simultaneously, enzymic hydrolysis temperature is 55 DEG C, the enzymatic hydrolysis reaction time is 5.5h, obtains xylo-oligosaccharide enzymolysis solution;
3) enzymolysis solution carries out ultrafiltration membrance filter, and the molecular weight cut-off of ultra-filtration membrane is 1200Da, pressure 0.7MPa before ultra-filtration membrane, press 0.5MPa after film, reclaim zytase and macromolecular oligo sugar, squeeze into saccharifying tank, zytase reuses, and macromolecular oligo sugar is through repeating saccharification enzymolysis;
4) filtered solution is through activated carbon decolorizing, and activated carbon decolorizing temperature is 90 DEG C, and the per-cent that gac addition accounts for liquid glucose weight is 0.2%, and bleaching time is 20min, by ion-exchange removal of impurities, and flow velocity 7m
3/ h;
5) drying of xylo-oligosaccharide syrup is by vacuum belt drying, and vacuum tightness is-110KPa, one section of Heating temperature 105 DEG C, and two sections of Heating temperatures 95 DEG C, three sections of Heating temperatures are 75 DEG C, and cooling temperature is 25 DEG C, pulverize to obtain pure xylo-oligosaccharide powder.
Pure xylo-oligosaccharide powder prepared by embodiment 1 ~ 3 is carried out compound mensuration, as described in Table 1:
Table 1: embodiment 1 ~ 3 xylo-oligosaccharide product component situation (mass percentage)
| Project | Xylo-bioses | Xylotriose | Xylotetrose | Wood pentasaccharides ~ wood seven sugar | Xylo-oligosaccharide content amounts to |
| Embodiment 1 | 31.32％ | 20.12％ | 11.06％ | 14.05％ | 76.55％ |
| Embodiment 2 | 31.45％ | 19.98％ | 11.34％ | 13.87％ | 76.64％ |
| Embodiment 3 | 31.21％ | 20.04％ | 11.28％ | 13.99％ | 76.52％ |
As shown in Table 1: reclaim zytase recycling by ultra-filtration membrane, xylo-oligosaccharide product component can not be affected.
Table 2: embodiment 1 ~ 3 compares with traditional technology xylo-oligosaccharide powder solubility property, mobility, smell aspect
| Project | Solubility property | Mobility | Smell |
| Embodiment 1 xylo-oligosaccharide powder | 5.2s | 3.9s | Without other smells |
| Embodiment 2 xylo-oligosaccharide powder | 5.5s | 3.7s | Without other smells |
| Embodiment 3 xylo-oligosaccharide powder | 5.6s | 3.8s | Without other smells |
| Traditional technology xylo-oligosaccharide powder | 9.6s | 5s | Be mingled with dextrin smell |
Found out by table 2: syrup through convection drying, cooling, pulverize compared with xylo-oligosaccharide powder obtains Icing Sugar with traditional technology, in solubility property, mobility, smell etc. be improved significantly, there is good beneficial effect.
Table 3 embodiment 1-3 and traditional technology often prepare the cost compare of 1 ton of xylo-oligosaccharide powder zytase used
As shown in Table 3: the average cost of embodiment 1-3 xylo-oligosaccharide powder per ton zytase used is in about 300 units, and traditional technology zytase cost is at about 900 yuan, by recycling zytase, the effect reducing xylo-oligosaccharide product cost can be reached.
Claims (10)
1. a preparation method for pure xylo-oligosaccharide powder, is characterized in that, comprises the following steps:
(1) pH value adjusting the xylan aqueous solution is 3.0-6.0, adds zytase and carries out enzymolysis, obtain the xylan enzymolysis solution containing zytase;
(2) the xylan enzymolysis solution of step (1) is carried out ultrafiltration membrance filter, the molecular weight cut-off of ultra-filtration membrane is 1000 ~ 1500Da, pressure 0.5 ~ 0.7MPa before ultra-filtration membrane, 0.3 ~ 0.5MPa is pressed after film, obtain xylo-oligosaccharide raw sugar liquid 1 respectively, and the mixed solution of the zytase 2 reclaimed and macromolecular oligo sugar, the mixed solution of zytase 2 and macromolecular oligo sugar is squeezed into saccharifying tank, add new zytase simultaneously, the zytase recycling of reclaiming, macromolecular oligo sugar repeats saccharification, enzymolysis, the zytase 3 prepared xylo-oligosaccharide raw sugar liquid 2 and reclaim, zytase like this reuses,
(3) the xylo-oligosaccharide raw sugar liquid obtained in combining step (2), and refine, obtain xylo-oligosaccharide syrup;
(4) by the xylo-oligosaccharide syrup of step (3), through vacuum belt, concentrated or scraper evaporator concentrates, and by cooling, pulverizes to obtain pure xylo-oligosaccharide powder.
2. the preparation method of pure xylo-oligosaccharide powder according to claim 1, it is characterized in that, in step (1), the preparation method of the described xylan aqueous solution is: be that raw material is through solvent pre-treatment with corn cob meal, solid-liquid separation removes the pretreated water solution containing pigment, the filter residue obtained and process water be made into liquid to be blasted that solid-to-liquid ratio is 1:2-6, be 120s-240s, diluted acid catalyzer 0.1%-1.5% condition in pressure 1.5-2.5MPa, treatment time under, carry out continuous steam explosion treatment, solid-liquid separation, collects the aqueous solution being rich in xylan.
3. the preparation method of pure xylo-oligosaccharide powder according to claim 1 and 2, is characterized in that, in step (1), the mass concentration of the xylan aqueous solution of preparation is 1%-8%.
4. the preparation method of pure xylo-oligosaccharide powder according to claim 2, is characterized in that, in step (1), described diluted acid catalyzer is sulfuric acid, acetic acid, formic acid, citric acid.
5. the preparation method of pure xylo-oligosaccharide powder according to claim 1, is characterized in that, in step (1), the add-on of zytase is: the zytase of 30-50UI units activity in every gram of xylan.
6. the preparation method of pure xylo-oligosaccharide powder according to claim 1, is characterized in that, in step (2), new zytase add-on is: the zytase of 5-20UI units activity in every gram of xylan.
7. the preparation method of pure xylo-oligosaccharide powder according to claim 6, is characterized in that, in step (2), the add-on of new zytase is: the zytase of 5-20UI units activity in every gram of xylan.
8. the preparation method of pure xylo-oligosaccharide powder according to claim 1, is characterized in that, in step (3), the process for purification of xylo-oligosaccharide raw sugar liquid comprises activated carbon decolorizing and ion exchange resin removal of impurities.
9. the preparation method of pure xylo-oligosaccharide powder according to claim 1, it is characterized in that, in step (4), it be vacuum tightness is-80 ~-120KPa that vacuum belt concentrates parameter, one section of Heating temperature 95 ~ 130 DEG C, two sections of Heating temperatures 95 ~ 130 DEG C, three sections of Heating temperatures are 60 ~ 90 DEG C, and cooling temperature is 20 ~ 40 DEG C.
10. the preparation method of high-purity xylo-oligosaccharide powder according to claim 1, it is characterized in that, in step (4), scraper plate evaporation concentration parameter is that temperature controls at 115 DEG C ~ 130 DEG C, evaporating pressure is-0.08 ~-0.098MPa, drop temperature controls at 105 DEG C ~ 120 DEG C, and scraper plate rotating speed controls at 3 ~ 5m/s, and cooling temperature is 20 ~ 40 DEG C.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106636256A (en) * | 2016-12-28 | 2017-05-10 | 山东龙力生物科技股份有限公司 | Xylooligosaccharide with low DP (degree of polymerization) as well as preparation method and application of xylooligosaccharide |
| CN106636254A (en) * | 2016-12-28 | 2017-05-10 | 山东龙力生物科技股份有限公司 | Process for preparing high-purity xylooligosaccharide |
| WO2017107527A1 (en) * | 2015-12-25 | 2017-06-29 | 山东龙力生物科技股份有限公司 | Soluble dietary fiber and preparation method thereof |
| CN112458125A (en) * | 2020-10-30 | 2021-03-09 | 济南茂腾生物科技有限公司 | Method for preparing xylo-oligosaccharide from corncob powder |
| CN112458133A (en) * | 2020-10-30 | 2021-03-09 | 济南茂腾生物科技有限公司 | Method for preparing xylo-oligosaccharide from corn bran |
| CN112481331A (en) * | 2020-10-30 | 2021-03-12 | 济南茂腾生物科技有限公司 | Method for preparing xylooligosaccharide from hemicellulose |
| CN113261678A (en) * | 2021-04-15 | 2021-08-17 | 山东卫康生物医药科技有限公司 | Preparation process of natto xylooligosaccharide powder suitable for people with low immunity |
| CN114350723A (en) * | 2021-12-27 | 2022-04-15 | 海南拉风农业科技有限公司 | Method for preparing xylooligosaccharide by using black corncobs |
| CN114457059A (en) * | 2022-01-21 | 2022-05-10 | 青岛尚德生物技术有限公司 | Xylanase-containing enzyme preparation and application thereof in production of xylooligosaccharide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101294175A (en) * | 2008-06-20 | 2008-10-29 | 南京林业大学 | Method for producing low polyxylose with dual-aqueous phase hydrolyzation system |
-
2014
- 2014-12-25 CN CN201410819669.3A patent/CN104593446B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101294175A (en) * | 2008-06-20 | 2008-10-29 | 南京林业大学 | Method for producing low polyxylose with dual-aqueous phase hydrolyzation system |
Non-Patent Citations (1)
| Title |
|---|
| 杨富国等: "膜分离技术在低聚木糖制备及乙醇发酵中的应用", 《林产化学与工业》 * |
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