CN1680415A - Preparation of oligo-wood sugar - Google Patents
Preparation of oligo-wood sugar Download PDFInfo
- Publication number
- CN1680415A CN1680415A CNA200410023875XA CN200410023875A CN1680415A CN 1680415 A CN1680415 A CN 1680415A CN A200410023875X A CNA200410023875X A CN A200410023875XA CN 200410023875 A CN200410023875 A CN 200410023875A CN 1680415 A CN1680415 A CN 1680415A
- Authority
- CN
- China
- Prior art keywords
- xylo
- oligosaccharide
- xylan
- liquid glucose
- corn cob
- 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.)
- Granted
Links
- 238000002360 preparation method Methods 0.000 title claims description 6
- 229960003487 xylose Drugs 0.000 title 1
- 239000012528 membrane Substances 0.000 claims abstract description 36
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 21
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 21
- 239000011734 sodium Substances 0.000 claims abstract description 21
- 229920001221 xylan Polymers 0.000 claims abstract description 21
- 150000004823 xylans Chemical class 0.000 claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005336 cracking Methods 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 239000011347 resin Substances 0.000 claims abstract description 6
- 229920005989 resin Polymers 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005507 spraying Methods 0.000 claims abstract description 5
- 230000001105 regulatory effect Effects 0.000 claims abstract 2
- HEBKCHPVOIAQTA-NGQZWQHPSA-N d-xylitol Chemical compound OC[C@H](O)C(O)[C@H](O)CO HEBKCHPVOIAQTA-NGQZWQHPSA-N 0.000 claims description 69
- 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 claims description 45
- 238000000034 method Methods 0.000 claims description 30
- 240000008042 Zea mays Species 0.000 claims description 29
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 29
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 29
- 235000005822 corn Nutrition 0.000 claims description 29
- 239000006188 syrup Substances 0.000 claims description 25
- 235000020357 syrup Nutrition 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 20
- 235000000346 sugar Nutrition 0.000 claims description 17
- 235000012054 meals Nutrition 0.000 claims description 15
- 230000000694 effects Effects 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000004042 decolorization Methods 0.000 claims description 7
- 238000010612 desalination reaction Methods 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- 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 6
- LPQOADBMXVRBNX-UHFFFAOYSA-N ac1ldcw0 Chemical compound Cl.C1CN(C)CCN1C1=C(F)C=C2C(=O)C(C(O)=O)=CN3CCSC1=C32 LPQOADBMXVRBNX-UHFFFAOYSA-N 0.000 claims description 6
- 238000009835 boiling Methods 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
- 239000003456 ion exchange resin Substances 0.000 claims description 6
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 6
- 238000001976 enzyme digestion Methods 0.000 claims description 5
- 238000004061 bleaching Methods 0.000 claims description 4
- 230000009849 deactivation Effects 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 239000005913 Maltodextrin Substances 0.000 claims description 3
- 229920002774 Maltodextrin Polymers 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 229940035034 maltodextrin Drugs 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical group CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- 229920000858 Cyclodextrin Polymers 0.000 claims description 2
- 239000001116 FEMA 4028 Substances 0.000 claims description 2
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 2
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 2
- 229960004853 betadex Drugs 0.000 claims description 2
- 230000008719 thickening Effects 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims 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 1
- 238000010411 cooking Methods 0.000 claims 1
- 238000000855 fermentation Methods 0.000 claims 1
- 230000004151 fermentation Effects 0.000 claims 1
- 235000019253 formic acid Nutrition 0.000 claims 1
- 101710121765 Endo-1,4-beta-xylanase Proteins 0.000 abstract description 5
- 235000013305 food Nutrition 0.000 abstract description 4
- 239000000843 powder Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
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- 239000003814 drug Substances 0.000 abstract description 2
- 238000005342 ion exchange Methods 0.000 abstract description 2
- 239000003377 acid catalyst Substances 0.000 abstract 1
- 238000004040 coloring Methods 0.000 abstract 1
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- 238000009776 industrial production Methods 0.000 abstract 1
- 239000000546 pharmaceutical excipient Substances 0.000 abstract 1
- 239000002893 slag Substances 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 102000004190 Enzymes Human genes 0.000 description 7
- 108090000790 Enzymes Proteins 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000001728 nano-filtration Methods 0.000 description 5
- 230000001580 bacterial effect Effects 0.000 description 4
- 235000008504 concentrate Nutrition 0.000 description 4
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- 241000193830 Bacillus <bacterium> Species 0.000 description 3
- 229920002488 Hemicellulose Polymers 0.000 description 3
- 235000008429 bread Nutrition 0.000 description 3
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- 230000001143 conditioned effect Effects 0.000 description 3
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- 239000002994 raw material Substances 0.000 description 3
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- 239000002023 wood Substances 0.000 description 3
- 206010020772 Hypertension Diseases 0.000 description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 2
- 229930006000 Sucrose Natural products 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 235000021552 granulated sugar Nutrition 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000005720 sucrose Substances 0.000 description 2
- 230000004083 survival effect Effects 0.000 description 2
- 206010010774 Constipation Diseases 0.000 description 1
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- 206010012735 Diarrhoea Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229930091371 Fructose Natural products 0.000 description 1
- 239000005715 Fructose Substances 0.000 description 1
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 1
- 241000186660 Lactobacillus Species 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 208000008589 Obesity Diseases 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 241001655322 Streptomycetales Species 0.000 description 1
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- 150000001413 amino acids Chemical class 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
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- 235000009508 confectionery Nutrition 0.000 description 1
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- 230000001804 emulsifying effect Effects 0.000 description 1
- 239000002158 endotoxin Substances 0.000 description 1
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- 239000008103 glucose Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 230000001631 hypertensive effect Effects 0.000 description 1
- 230000003053 immunization Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 229940039696 lactobacillus Drugs 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 230000002062 proliferating effect Effects 0.000 description 1
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- 235000009566 rice Nutrition 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
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- 150000008163 sugars Chemical class 0.000 description 1
- 235000012976 tarts Nutrition 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
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- A61F7/00—Heating or cooling appliances for medical or therapeutic treatment of the human body
- A61F7/007—Heating or cooling appliances for medical or therapeutic treatment of the human body characterised by electric heating
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- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
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Abstract
Production of oligoxylose is carried out by mixing corncob powder with water, adding weak acid catalyst, cracking, dissolving out xylan of corncob, regulating pH of xylan solution to 5.0-6.0, adding xylanase, enzymolyzing, inactivating for xylanase at high-temperature, filtering and removing out slag of corncob power, removing impurity and de-coloring for xylan solution by active carbon and ion exchanging resin, trapping macromolecular xylan with macromolecular trapping membrane, filtering out oligoxylose solution, concentrating and desalting by sodium filtering membrane, vacuum concentrating for oligoxylose to be light yellow thick treacle, directly spraying and drying by excipient, and obtaining oligoxylose powdery. It achieves simple operation, industrial production and high purity. It can be used for food, health-care products and medicine additive.
Description
Technical field
The present invention relates to a kind of method for preparing lower polyxylose, be specifically related to a kind of hemicellulose in the corn cob is converted into the xylan and the method for purifying oligo-xylose therefrom.
Background technology
Xylo-oligosaccharide also claims wood oligose (xylooligosaccharides), and with β-1,4-xyloside bond is closed and formed by 2～7 D-wood sugars, is an important member in the functional oligose family.Its sweetness ratio sucrose and glucose are all low, are about 40% of sucrose.Xylo-oligosaccharide is better to the stability of pH value and heat, even also do not decompose substantially in acidic conditions (pH=2.5～7) heating, is suitable in the acidic drinks such as sour milk, lactobacillus drink and soda pop.Figure below is the main component and the chemical structure of xylo-oligosaccharide.
Survival rate height in the xylo-oligosaccharide absorption extremely difficult to digest, enteron aisle has fabulous bifidus bacillus proliferative, and it selects usability to be higher than other functional oligose.The physiological function of having studied at present the xylo-oligosaccharide of affirmation already mainly comprises the following aspects:
(1) provides lower energy, satisfy the requirement that happiness food sweets is worried the person of getting fat again, also can supply diabetics, adiposis patient and hypertensive patient edible;
(2) bifidus bacillus and promote its propagation in the activation enteron aisle suppresses pathogenic bacteria, prevents diarrhoea;
(3) prevent constipation;
(4) reduce cholesterol in serum content, bring high blood pressure down, generate nutritive substance, enhancing body immunizing power and opposing tumour;
5) can not cause carious tooth, help oral Health;
(6) remove enterogenous endotoxin.
The special physiological properties that xylo-oligosaccharide has has determined that its application mainly is to utilize its effect that can give bifidus bacillus selection proliferation activity in the enteron aisle, and secondly, because its stability is strong, mouthfeel is good, is applied on the food.Studies show that, add xylo-oligosaccharide in beverage, even 25 ℃ were preserved 8 months down, 99% the survival rate of still having an appointment shows that xylo-oligosaccharide has satisfactory stability.When xylo-oligosaccharide is added in the cream, be replaced by xylo-oligosaccharide, the good result of the product emulsifying property that can be improved as if 15～50% of the granulated sugar that will cooperate ratio usually.And in jelly, even xylo-oligosaccharide and granulated sugar are changed in 30～50% ratio, the hobby of its product is also no problem, also has tasty and refreshing effect simultaneously.Under the amino acid concurrent conditions, when being heated, xylo-oligosaccharide has than the easy painted characteristics of fructose, use it for the central discovery of baking of bread, in bread, add an amount of xylo-oligosaccharide, can obtain to be easy to give the good color and luster of bread, to tart up, to avoid mildewing and to control easily effects such as moisture.
Xylo-oligosaccharide generally is to be rich in the plant resources of xylan, is raw material as wood chip, corn cob, cotton seed hulls, rice husk and vegetable seed shell etc., after the internal cutting type xylanase hydrolysis, separates again, makes with extra care and make.
Summary of the invention
The objective of the invention is to realize that hemicellulose in the corn cob is converted into the industrialized preparing process of high-quality xylo-oligosaccharide.This method is simple, is with in suitability for industrialized production, the xylo-oligosaccharide purity height that obtains, and look shallow, can be widely used in various food, healthcare products, the medicine as additive.This purpose can by concrete selection to pre-treatment, the explosion of directly-heated vapour of corn cob raw material separate, processing condition, especially the zytase selection and the preparation technology of process such as enzyme digestion reaction, decolouring and removal of impurities and the explosion of directly-heated vapour separate that the selection of catalyzer and reaction conditions realizes in the process.
The invention discloses a kind of means that combine with enzyme process and physical chemistry makes hemicellulose in the corn cob meal change into the method for xylo-oligosaccharide.With corn cob meal and water is 1: 6～10 to mix by weight, and to add the corn cob weight percent be 0.2～1.5% weak acid catalyzer, carries out cracking at 155 ℃～180 ℃ boiling 30min～120min, with the xylan stripping in the corn cob; With the corn cob meal mixture of directly-heated cracking gained in 45～60 ℃ of temperature under the effect of zytase liquid, reaction 4h～10h is warming up to 90～105 ℃ then, insulation 10min～30min; Take off assorted by activated carbon decolorizing and Zeo-karb such as E306FG and anionite-exchange resin such as D001 gained xylo-oligosaccharide liquid glucose, use the xylo-oligosaccharide of macromole mwco membrane molecular weight cut-off more than 1200 and carry out enzymolysis once more, the xylo-oligosaccharide of molecular weight below 1200 passes through mwco membrane, through the concentrated film ratio of desalinization of sodium filter is 70% of stoste, and enrichment factor is 5-6 a times of stoste.Vacuum concentration is 55%～75% liquid glucose again, is vehicle with maltodextrin, beta-cyclodextrin or W-Gum, and spray-dried total sugar content is 20%～70% xylo-oligosaccharide pulvis; Or after the sodium filter membrane separated monose, the purity of xylo-oligosaccharide reached 70%～98% syrup, and spray-dried total reducing sugar is 70%～98% xylo-oligosaccharide pulvis.
The sodium filter membrane is that a kind of molecular weight of liquid that utilizes varies in size isolating a kind of high-end technology in the prior art, is used to make high-purity oligoxylose in this technology, and purity can reach more than 95%.The macromole filtering membrane also is a kind of of sodium filter membrane, is used to hold back the halfway macromolecular xylo-oligosaccharide of enzymolysis in this technology, and enzymolysis has guaranteed quality product once more.
Individual in the aforesaid method, usually the corn cob meal as raw material is carried out pre-treatment, method is at 50 ℃～80 ℃ insulation 30min～120min.
Consider in the xylanase hydrolysis process, the excessive interpolation of enzyme can cause increasing of production cost, therefore to take the zytase crude enzyme liquid and the ratio of corn cob meal be 1ml/12g～1ml/16g in the present invention, zytase crude enzyme liquid enzymic activity is 800UI/ml～1000UI/ml, adds 50～85UI units activity zytase in promptly every gram xylan.
The zytase liquid that the present invention adopts is to be made through liquid fermenting by streptomycete sp.E-86 bacterial strain.
Conventional decoloring method is adopted in the decolouring of xylo-oligosaccharide liquid glucose, it is the decolouring of activated carbon and ion column, for better removing the color of gained xylo-oligosaccharide liquid glucose, activated carbon decolorizing of the present invention can be repeatedly, be generally twice, bleaching temperature can be adjusted as required, is generally 80 ℃, the gac addition is 0.5%～1.5% of a liquid glucose amount, bleaching time 25min～40min.
Ion exchange resin removal of impurities process of the present invention is positive and negative, Zeo-karb, and xylo-oligosaccharide liquid glucose temperature is less than 45 ℃, and per hour xylo-oligosaccharide liquid glucose flow velocity is 1～2 times of resin volume, and the specific conductivity of gained liquid glucose is less than 50VS/cm, and pH is 4.5～6.0.
Employing vacuum of the present invention concentrates the xylan liquid glucose, thickening temperature is 60～80 ℃, and filter concentrated film by sodium and carry out desalination and concentrated, the sodium filter membrane concentrates and can carry out at normal temperatures, usually about 15～30 ℃, 20 ℃ of temperature are best, usually the vacuum concentration mode is the economic benefits and social benefits vacuum concentration, and concentration process can adopt repeatedly mode, as adopts mode twice, simmer down to sodium filter membrane concentrates for the first time, the xylo-oligosaccharide liquid glucose is concentrated to the syrup of total sugar content 8%～12%; For the second time under 75 ℃ of the simmer down tos, the xylo-oligosaccharide liquid glucose is concentrated to the syrup of total sugar content 55%～75%.In the technique scheme, the economic benefits and social benefits vacuum concentration equipment is a kind of facility that utilizes the cryogenic vacuum transpiring moisture to reach concentrated liquid in the prior art.
According to drying means of the present invention, the inlet temperature of hot blast is 130 ℃～160 ℃ during vacuum-drying, and temperature out is 65 ℃～85 ℃, and mass flow is 0.8～1.2m
310 seconds～20 seconds residence time in the/h, tower.
Description of drawings
Fig. 1 is a method for preparing lower polyxylose embodiment process flow sheet.
Embodiment
The technical process of method for preparing lower polyxylose can illustrate by Fig. 1:
Fig. 1 provides the method for preparing xylo-oligosaccharide in corn cob, comprises following sequential steps, and 1, select corn cob; 2, removal of impurities; 3, corn cob is pulverized; 4, to the corn cob pre-treatment; 5, high temperature steaming cracking; 6, xylanase hydrolysis; 7, filter cleaner; 8, activated carbon decolorizing; 9, nanofiltration membrane separation macromole; 10, nanofiltration membrane concentrating and desalinating; 11, ion-exchange purifies; 12, vacuum concentration; 13, nanofiltration membrane separation is purified; 14, add the vehicle spraying drying; 15, light yellow thick xylo-oligosaccharide syrup; 16, vacuum concentration; 17, nanofiltration membrane concentrates; 18, xylo-oligosaccharide pulvis, 19, light yellow thick xylo-oligosaccharide syrup; 20, assorted sugar reclaims.
The concrete grammar of preparation xylo-oligosaccharide is referring to following embodiment in corn cob.
Embodiment 1
Take by weighing 40 orders～60 purpose corn cob meal 500kg, add 4000kg, pure water is mixed well, and heats up 80 ℃ to add 2.5kg acetate, behind 160 ℃ of following boiling cracking 2h, enters enzymatic vessel through vapour liquid separator, is cooled to 55 ℃.Use the pH to 5.5 of the sodium hydroxide solution conditioned reaction liquid of 1mol/ml hydrochloric acid soln and 1mol/ml respectively, adding the enzymic activity that is made by liquid fermenting by the sp.E-86 bacterial strain by the amount of 1ml enzyme liquid/14.5g corn cob meal is the zytase liquid of 900UI/ml, behind the enzyme digestion reaction 8h, at 90 ℃ of insulation deactivation 15min, be cooled to 60 ℃ and carry out Plate Filtration and obtain liquid glucose.The activity charcoal powder that in liquid glucose, adds cumulative volume 1%, 80 ℃ are stirred decolouring 30min, filter, with liquid glucose simmer down to total sugar content 15% xylo-oligosaccharide syrup at 75 ℃.15% syrup is carried out secondary decolourization, and decolorization condition is with for the first time identical.Then will be through ion exchange resin column on the syrup of twice decolouring, decolour assorted according to positive negative and positive mode, use the xylo-oligosaccharide of macromole mwco membrane molecular weight cut-off more than 1000 and carry out enzymolysis once more, the xylo-oligosaccharide of molecular weight below 1000 passes through mwco membrane, through the desalination of sodium filter membrane, ratio of desalinization is 70% of a stoste, and concentrated solution is 5-6 a times of stoste.Vacuum concentration is 55%～75% liquid glucose again, and the liquid glucose specific conductivity is less than 50VS/cm, pH5.0.At last under 75 ℃, be 70% light yellow thick xylo-oligosaccharide syrup with liquid glucose through vacuum concentration to total sugar content, or xylo-oligosaccharide content reach 95% after extracting monose through the sodium filter membrane, the liquid glucose specific conductivity is less than 50VS/cm, pH5.0.At last under 75 ℃, it is 70% light yellow thick xylo-oligosaccharide syrup that liquid glucose is concentrated into total sugar content, yield 8.8%.
Embodiment 2
Take by weighing 40～60 purpose corn cob meal 480kg, add the 4000kg pure water and mix well, add the 2.0kg citric acid, behind 170 ℃ of following boiling cracking 100min, enter enzymatic vessel, be cooled to 55 ℃ through vapour liquid separator.Use the pH to 5.5 of the sodium hydroxide solution conditioned reaction liquid of 1mol/ml hydrochloric acid soln and 1mol/ml respectively, adding the enzymic activity that is made by liquid fermenting by the sp.E-86 bacterial strain by the amount of 1ml enzyme liquid/1.3g corn cob meal is the zytase liquid of 70UI/ml, behind the enzyme digestion reaction 6h, at 100 ℃ of insulation deactivation 13min, be cooled to 60 ℃ and carry out Plate Filtration.The activity charcoal powder that in liquid glucose, adds cumulative volume 1%, 80 ℃ are stirred decolouring 30min, filter, with liquid glucose simmer down to total sugar content 20% xylo-oligosaccharide syrup at 75 ℃.15% syrup is carried out secondary decolourization, and decolorization condition is with for the first time identical.To decolour assorted through ion exchange resin column on the syrup of twice decolouring then, use the xylo-oligosaccharide of macromole mwco membrane molecular weight cut-off more than 1000 and carry out enzymolysis once more, the xylo-oligosaccharide of molecular weight below 1000 passes through mwco membrane, pass through the desalination of sodium filter membrane again, ratio of desalinization is 70% of a stoste, and concentrated solution is 5-6 a times of stoste.Vacuum concentration is 55%～75% liquid glucose, and the liquid glucose specific conductivity is less than 50VS/cm, pH5.0.At last under 75 ℃, it is 70% light yellow thick xylo-oligosaccharide syrup that liquid glucose is concentrated into total sugar content, yield 8.5%; Or xylo-oligosaccharide content reaches 95% after extracting monose through the sodium filter membrane, and the liquid glucose specific conductivity is less than 50VS/cm, pH5.0.At last under 75 ℃, it is 70% light yellow thick xylo-oligosaccharide syrup that liquid glucose is concentrated into total sugar content, yield 8.5%
Take by weighing 40 orders～60 purpose corn cob meal 500kg, add 3800kg, pure water is mixed well, and behind 165 ℃ of following boiling cracking 2h, enters enzymatic vessel through vapour liquid separator, is cooled to 55 ℃.Use the pH to 5.5 of the sodium hydroxide solution conditioned reaction liquid of 1mol/ml hydrochloric acid soln and 1mol/ml respectively, adding the enzymic activity that is made by liquid fermenting by the sp.E-86 bacterial strain by the amount of 1ml enzyme liquid/1.45g corn cob meal is the zytase liquid of 60UI/ml, behind the enzyme digestion reaction 8h, at 90 ℃ of insulation deactivation 15min, be cooled to 60 ℃ and carry out Plate Filtration.The activity charcoal powder that in liquid glucose, adds cumulative volume 1%, 80 ℃ are stirred decolouring 30min, filter, with liquid glucose simmer down to total sugar content 15% xylo-oligosaccharide syrup at 75 ℃.15% syrup is carried out secondary decolourization, and decolorization condition is with for the first time identical.To decolour assorted through ion exchange resin column on the syrup of twice decolouring then, sugar is used the xylo-oligosaccharide of macromole mwco membrane molecular weight cut-off more than 1000 and is carried out enzymolysis once more, the xylo-oligosaccharide of molecular weight below 1000 passes through mwco membrane, through the desalination of sodium filter membrane, ratio of desalinization is 70% of a stoste, and concentrated solution is 5-6 a times of stoste.Vacuum concentration is 55%～75% liquid glucose again, and the liquid glucose specific conductivity is less than 50VS/cm, pH5.0.At last under 75 ℃, it is 70% light yellow thick xylo-oligosaccharide syrup that liquid glucose is concentrated into total sugar content, yield 7.6% or extract monose through the sodium filter membrane after xylo-oligosaccharide content reach 95%, the liquid glucose specific conductivity is less than 50VS/cm, pH5.0.At last under 75 ℃, it is 70% light yellow thick xylo-oligosaccharide syrup that liquid glucose is concentrated into total sugar content, yield 7.6%
Embodiment 4
Condition and step by in the embodiment 1 through the desalination of sodium filter membrane, make the xylo-oligosaccharide syrup of 100kg40%, and adding purity is 98% maltodextrin 120kg, 145 ℃ of inlet temperatures, and 85 ℃ of temperature outs, mass flow is 1.0m
3Carry out spraying drying under the/h condition, obtain the xylo-oligosaccharide powdery product of content 25%.
By condition and the step in the embodiment 1, behind desalination of sodium filter membrane and vacuum concentration, make the xylo-oligosaccharide of 100kg40% concentration, through nanofiltration membrane separation purification syrup, 145 ℃ of inlet temperatures, 85 ℃ of temperature outs, mass flow is 1.0m
3Carry out spraying drying under the/h condition, obtain the xylo-oligosaccharide powdery product of content 95%.
Claims (11)
1, a kind of method for preparing lower polyxylose comprises the following order step:
(1) be 1: 6～10 to mix by weight with corn cob meal and water, and to add the corn cob weight percent is 0.2～1.5% weak acid catalyzer, carries out cracking at 155 ℃～180 ℃ boiling 30min～120min, the xylan stripping in the corn cob;
(2) regulating the xylan aqueous ph value is 5.0～6.0, the ratio that adds 50～85UI units activity zytase according to every gram xylan adds zytase, carry out enzymolysis at 45～60 ℃ of enzyme digestion reaction 4h～10h, be warming up to 90 ℃～105 ℃, insulation 10min～30min carries out deactivation to zytase;
(3) filtering corn cob meal obtains the xylan liquid glucose:
(4) the xylan liquid glucose is carried out gac and ion exchange resin removal of impurities decolouring;
(5) hold back the macromole xylan by the macromole mwco membrane, filter out the xylo-oligosaccharide liquid glucose; Macromole is continued enzymolysis.
(6) the xylo-oligosaccharide liquid glucose is carried out sodium filter membrane concentrating and desalinating, and further process according to the following step (7), step (8), step (9) or (10) the xylan liquid glucose after to sodium filter membrane concentrating and desalinating;
(7) vacuum concentration is light yellow thick xylo-oligosaccharide syrup;
(8) vacuum concentration is 55%～75% liquid glucose, is vehicle with maltodextrin, beta-cyclodextrin or W-Gum, and spray-dried xylo-oligosaccharide weight percent is 20%～50% xylo-oligosaccharide pulvis;
(9) the sodium filter membrane separates monose, and vacuum concentration is faint yellow thickness transparence xylo-oligosaccharide syrup;
(10) the sodium filter membrane separates monose, and vacuum concentration is the syrup of xylo-oligosaccharide weight percent 55%～75%, and spray-dried total reducing sugar is 70%～98% xylo-oligosaccharide pulvis.
2, the preparation method of low xylan according to claim 1 is characterized in that:
In the step (1) during corn cob meal boiling cracking temperature be 160～170 ℃, cooking time 80～120min.
3, the preparation method of low xylan according to claim 1 is characterized in that:
The xylo-oligosaccharide molecular weight of holding back out by the macromole mwco membrane in the step (5) is less than 1000 molecular weight, 18 ℃～28 ℃ of separation temperatures, and the macromole xylan of holding back out comes back in the step (2) and carries out enzymolysis.
4, the preparation method of low xylan according to claim 1 is characterized in that: during look, per hour xylo-oligosaccharide liquid glucose flow velocity is 1～2 times of resin volume.
5, method for preparing lower polyxylose according to claim 1 is characterized in that:
Zytase in the described step (2) makes by the fermentation of sp.E-86 strain liquid.
6, method for preparing lower polyxylose according to claim 1 is characterized in that: described weak acid catalyzer is acetate, formic acid, citric acid, and adding the corn cob weight percent is 0.5～1.2%.
7, method for preparing lower polyxylose according to claim 1 is characterized in that:
Corn cob meal in the step (1) is carried out pre-treatment at 50 ℃～80 ℃ insulation 30min～120min.
8, method for preparing lower polyxylose according to claim 1 is characterized in that:
Activated carbon decolorizing is for repeatedly, and it is 0.5%～1.5% that 70～85 ℃ of bleaching temperatures, gac addition account for the liquid glucose weight percent, bleaching time 25min～40min.
9, method for preparing lower polyxylose according to claim 1 is characterized in that:
In the step (4), ion exchange resin removal of impurities decolorization is passed through Zeo-karb, anionite-exchange resin and Zeo-karb respectively for making the xylan liquid glucose, xylo-oligosaccharide liquid glucose temperature is less than 45 ℃, and per hour xylo-oligosaccharide liquid glucose flow velocity is 1～2 times of resin volume.
10, method for preparing lower polyxylose according to claim 1 is characterized in that:
Vacuum concentration mode in step (7), (8), (9) and (10) is the economic benefits and social benefits vacuum concentration, and thickening temperature is 60～80 ℃; The inlet temperature of the spraying drying hot blast in step (8) and the step (10) is 130 ℃～160 ℃, and temperature out is 65 ℃～85 ℃, and mass flow is 0.8～1.2m
310 seconds～20 seconds residence time in the/h, tower.
11, method for preparing lower polyxylose according to claim 1 is characterized in that:
In the described step (6), the temperature of sodium filter membrane desalination and concentration is 15～30 ℃.
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| CNB200410023875XA CN1303091C (en) | 2004-04-05 | 2004-04-05 | Preparation of oligo-wood sugar |
| KR1020040030170A KR100653748B1 (en) | 2004-04-05 | 2004-04-29 | Method for preparing xylooligosaccharide |
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| CNB200410023875XA CN1303091C (en) | 2004-04-05 | 2004-04-05 | Preparation of oligo-wood sugar |
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| CN112458133B (en) * | 2020-10-30 | 2023-01-10 | 济南茂腾生物科技有限公司 | Method for preparing xylo-oligosaccharide from corn bran |
| CN113151614A (en) * | 2021-03-17 | 2021-07-23 | 南京林业大学 | Method for preparing xylooligosaccharide from agricultural and forestry waste through two-step acetic acid hydrolysis |
| CN114539332A (en) * | 2022-01-10 | 2022-05-27 | 长沙绿叶生物科技有限公司 | Method for preparing xylooligosaccharide by using biomass raw material and application of xylooligosaccharide in preparation of feed additive |
| CN114539332B (en) * | 2022-01-10 | 2023-01-06 | 长沙绿叶生物科技有限公司 | Method for preparing xylooligosaccharide by using biomass raw material and application of xylooligosaccharide in preparation of feed additive |
| CN114836584A (en) * | 2022-05-23 | 2022-08-02 | 南京林业大学 | Method for producing xylooligosaccharide with assistance of amino acid |
| CN114836584B (en) * | 2022-05-23 | 2023-12-01 | 南京林业大学 | Method for producing xylo-oligosaccharide with assistance of amino acid |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20050097878A (en) | 2005-10-10 |
| CN1303091C (en) | 2007-03-07 |
| KR100653748B1 (en) | 2006-12-05 |
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