CN107267688B - Method for preparing xylooligosaccharide or xylose by using disc mill grinding hydrolysis - Google Patents
Method for preparing xylooligosaccharide or xylose by using disc mill grinding hydrolysis Download PDFInfo
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- CN107267688B CN107267688B CN201710533426.7A CN201710533426A CN107267688B CN 107267688 B CN107267688 B CN 107267688B CN 201710533426 A CN201710533426 A CN 201710533426A CN 107267688 B CN107267688 B CN 107267688B
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- xylose
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- oligosaccharide
- xylo
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- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 title claims abstract description 68
- 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 40
- 238000000227 grinding Methods 0.000 title claims abstract description 37
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 title claims abstract description 34
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 30
- 230000007062 hydrolysis Effects 0.000 title description 3
- 238000006460 hydrolysis reaction Methods 0.000 title description 3
- 239000007788 liquid Substances 0.000 claims abstract description 53
- 239000002253 acid Substances 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000002791 soaking Methods 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 37
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 9
- 239000002023 wood Substances 0.000 claims description 9
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims description 8
- 239000010902 straw Substances 0.000 claims description 8
- 241000609240 Ambelania acida Species 0.000 claims description 7
- 239000010905 bagasse Substances 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- 241001520808 Panicum virgatum Species 0.000 claims description 4
- 241000209140 Triticum Species 0.000 claims description 4
- 235000021307 Triticum Nutrition 0.000 claims description 4
- 240000008042 Zea mays Species 0.000 claims description 4
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 claims description 4
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 4
- 235000009973 maize Nutrition 0.000 claims description 4
- 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 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 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 1
- 235000009508 confectionery Nutrition 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 238000003801 milling Methods 0.000 abstract 2
- 238000013341 scale-up Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 description 11
- 239000002994 raw material Substances 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000000428 dust Substances 0.000 description 5
- 239000000049 pigment Substances 0.000 description 5
- LGQKSQQRKHFMLI-SJYYZXOBSA-N (2s,3r,4s,5r)-2-[(3r,4r,5r,6r)-4,5,6-trihydroxyoxan-3-yl]oxyoxane-3,4,5-triol 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)OC1 LGQKSQQRKHFMLI-SJYYZXOBSA-N 0.000 description 4
- LGQKSQQRKHFMLI-UHFFFAOYSA-N 4-O-beta-D-xylopyranosyl-beta-D-xylopyranose Natural products OC1C(O)C(O)COC1OC1C(O)C(O)C(O)OC1 LGQKSQQRKHFMLI-UHFFFAOYSA-N 0.000 description 4
- SQNRKWHRVIAKLP-UHFFFAOYSA-N D-xylobiose Natural products O=CC(O)C(O)C(CO)OC1OCC(O)C(O)C1O SQNRKWHRVIAKLP-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000005903 acid hydrolysis reaction Methods 0.000 description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 4
- 235000011054 acetic acid Nutrition 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- 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 2
- 239000003513 alkali Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000004310 lactic acid Substances 0.000 description 2
- 235000014655 lactic acid Nutrition 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 229920001221 xylan Polymers 0.000 description 2
- 150000004823 xylans Chemical class 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
- 241000186000 Bifidobacterium Species 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 241000193403 Clostridium Species 0.000 description 1
- 206010009944 Colon cancer Diseases 0.000 description 1
- 206010010774 Constipation Diseases 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 244000052616 bacterial pathogen Species 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
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 208000029742 colonic neoplasm Diseases 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000001079 digestive effect Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229930182478 glucoside Natural products 0.000 description 1
- 150000008131 glucosides Chemical class 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000000968 intestinal effect Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 210000002429 large intestine Anatomy 0.000 description 1
- 230000037356 lipid metabolism Effects 0.000 description 1
- 230000002503 metabolic effect Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000006041 probiotic Substances 0.000 description 1
- 230000000529 probiotic effect Effects 0.000 description 1
- 235000018291 probiotics Nutrition 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 235000021391 short chain fatty acids Nutrition 0.000 description 1
- 150000004666 short chain fatty acids Chemical class 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 150000003742 xyloses 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K13/00—Sugars not otherwise provided for in this class
- C13K13/002—Xylose
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Organic Chemistry (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Health & Medical Sciences (AREA)
- Sustainable Development (AREA)
- Saccharide Compounds (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a method for preparing xylo-oligosaccharide or xylose by using disc grinding and milling, which comprises the following steps: (1) soaking the primary lignocellulose in water or acid solution, and performing solid-liquid separation after soaking; (2) grinding the material obtained in the step (1) by using a disc grinder under the conditions of introducing steam, heating and pressurizing, obtaining xylo-oligosaccharide feed liquid or xylose feed liquid after grinding, soaking the raw lignocellulose in the step (1) in water to obtain the xylo-oligosaccharide feed liquid in the step (2), soaking the raw lignocellulose in the step (1) in an acid solution to obtain the xylose feed liquid in the step (2); (3) and (3) carrying out solid-liquid separation on the feed liquid obtained in the step (2) to obtain xylo-oligosaccharide liquid or xylose liquid. Compared with the traditional acid method process, the production period is shortened by adopting disc grinding and milling, the corrosion to equipment is reduced, the scale-up production can be realized, the materials are not heated together with a large amount of acid liquor in the steam heating and pressurizing process, the steam consumption is reduced, and the energy is saved.
Description
Technical field
The invention belongs to technical field of biochemical industry, and in particular to a kind of to prepare xylo-oligosaccharide or xylose using mill grinding
Method.
Background technology
Xylo-oligosaccharide is also known as wood oligose, is formed by 2~10 xyloses with β-(1 → 4) glucosides key connection.Xylo-oligosaccharide because
It is difficult to large intestine is directly entered by the digestive ferment system decomposition in human body, probiotic bifidobacteria and lactic acid in a large amount of enteron aisles that rise in value
On the one hand bacterium, tunning short chain fatty acids such as lactic acid, acetic acid, propionic acid, butyric acid can reduce the pH value in enteron aisle, so as to
Promote function of intestinal canal, lipid metabolism and prevents colon cancer at the absorption of calcium and minerals；On the other hand, these tunning energy
Inhibit the growth of the pathogenic bacteria such as clostridium, prevent diarrhea and than constipation, reduce the generation of toxic metabolic products.Therefore, in food, system
Medicine and animal feed etc. have important application.
The existing preparation method of xylo-oligosaccharide mainly has：Direct enzymatic isolation method, acid-hydrolysis method, hydro-thermal method and chemistry-enzyme process.
Acid-hydrolysis method directly serves as raw material with acid and prepares xylo-oligosaccharide comparing with other methods, and acid-hydrolysis method is because of yield height, reproducibility
It is good to be commonly used to do dynamic analysis and research.But traditional acid system prepares xylo-oligosaccharide, entire technical process water, acid, alkali
And the treating capacity of high-salt wastewater is big, needs acidproof, pressure-resistant, heat-resisting equipment, investment is big and environmental pressure is larger；Temperature need to reach
100 DEG C or so, time 1.5h or so, the period is longer and less efficient, simultaneously because acid solution and material will be same during hydrolysis heating
Shi Shengwen, therefore steam consumption is very high, energy consumption is big；Sour hydrolysis rate is fast, it is difficult to stop reaction in xylo-oligosaccharide level, and
Acid hydrolytic reaction can be generated with nuisance；Neutralizing zone needs alkali to neutralize acid, has fouling generation, while N-process part
The excessively high quality that xylo-oligosaccharide can be caused further to be hydrolyzed to monosaccharide, influence product of pH.
Mill technology is combined with acid system and prepares xylo-oligosaccharide or xylose and is not reported both at home and abroad so far.
Invention content
Goal of the invention：The defects of present invention prepares xylo-oligosaccharide for classical acid hydrolysis provides a kind of mill pressurization
Method prepares xylo-oligosaccharide or xylose, and the advantage is that reduces energy consumption, water consumption and production cost, improves xylo-oligosaccharide or xylose
Quality and yield.
Technical solution：
A kind of method that xylo-oligosaccharide or xylose are prepared using mill grinding, is included the following steps：
(1) primary lignocellulosic water or acid solution are impregnated, separation of solid and liquid after the completion of immersion；
(2) material that step (1) obtains is utilized into mill grinding under conditions of steam heating, pressurization is passed through, grinding is complete
Into obtaining xylo-oligosaccharide feed liquid or xylose feed liquid,
When primary lignocellulosic is soaked in water in step (1), step (2) obtains xylo-oligosaccharide feed liquid,
When primary lignocellulosic is impregnated with acid solution in step (1), step (2) obtains xylose feed liquid；
(3) feed liquid that step (2) obtains is subjected to separation of solid and liquid and obtains xylo-oligosaccharide liquid or Xylose.
Before the primary lignocellulosic of step (1) impregnates, first washing removal dust, sundries and pigment etc..
The primary lignocellulosic of the step (1) is corncob, bagasse, wheat straw bar, maize straw or switchgrass.
The primary lignocellulosic of the step (1) and the mass ratio of water or acid solution are 1:1.5~10.
Step (1) acid solution is the aqueous solution of acetic acid, sulfuric acid, nitric acid, hydrochloric acid, formic acid or trifluoroacetic acid.
Sour mass fraction is 0.1%~5% in step (1) acid solution.
Step (1) soaking temperature is 20 DEG C~80 DEG C, and soaking time is 0.3h~20h.
The pretreated primary lignocellulosic water content that the step (1) obtains for dry weight 30%~
70%.
The pressure of step (2) steam is 0.01~0.8MPa.
Step (2) the grinding speed is 1000~4000r/min, and the grinding time is 2~10min.
The feed liquid that the step (3) obtains carries out separation of solid and liquid, carries out separation of solid and liquid again after filter residue washing, carries out 2~5
Whole filtrate is collected after secondary washing and separation of solid and liquid, obtains xylo-oligosaccharide liquid or Xylose.
Separation of solid and liquid is by the way of press filtration in the step (3).
Advantageous effect：After to primary lignocellulosic tentatively pre-process, using mill pressurization grinding technique substitution
Material of traditional acid system technique productions rich in xylo-oligosaccharide or xylose, the xylo-oligosaccharide of high concentration is obtained by multiple filter-press dehydration
Or xylose solution.Compared with traditional acid technological process, the condition of mill pressurization grinding is more mild, and grinding only needs 2~10min, greatly
The production cycle is shortened greatly, reduces the corrosion to equipment, realizes amplification production；Steam heating pressure process material not with it is a large amount of
Acid solution heats together, greatly reduces the consumption of steam, energy saving, but also the investment of power plant reduces；Xylo-oligosaccharide
Without acid in liquid, it can prevent xylo-oligosaccharide from further degrading and reduce the cost of acid-base neutralization；Acid content is extremely low in Xylose,
Reduce the cost of later stage acid-base neutralization.
Description of the drawings
Fig. 1 is the process flow chart that xylo-oligosaccharide is prepared using mill grinding；
Fig. 2 is the process flow chart that mill grinding prepares xylose.
Specific embodiment
According to following embodiments, the present invention may be better understood.It is however, as it will be easily appreciated by one skilled in the art that real
It applies the described content of example and is merely to illustrate the present invention, without sheet described in detail in claims should will not be limited
Invention.
The pressure high-density paste mill used in embodiment, product type are φ 300, and mill φ 300, manufacturer is Shandong
The morning bell machinery limited company.
Embodiment 1
(1) corncob 200kg, washing raw material removal dust, sundries and pigment etc. are taken, then by raw material soaking in 0.8m3
Water in, soaking temperature be 50 DEG C, soaking time 8h；Next time will be recycled after reaching setting soaking time without absorbed water
It is continuing with, obtains the pretreatment corncob that water content is dry weight 39%；
(2) it will be delivered in pressure high-density paste mill by the corncob of pretreatment, material, which enters, to be detained in cylinder, closes
Feed inlet is heated using steam, and the steam pressure of 0.1MPa is passed through demurrage cylinder, and grinding processing time is 5min, and grinding is fast
It spends for 3000r/min, after grinding to predetermined time, opens pneumatic ball valve, pressure is down to an atmospheric pressure, is obtained containing oligomeric wood
The feed liquid of sugar；
(3) feed liquid containing xylo-oligosaccharide is subjected to press filtration, obtains first time extracting solution, 1m is added in filter residue3Deionized water,
20min is extracted, then press filtration obtains second of extracting solution；Obtained filter residue adds in 0.8m3Then deionized water carries out third time
Press filtration obtains third time extracting solution, collects whole extracting solutions and obtains thick xylo-oligosaccharide liquid.It is obtained by liquid chromatogram measuring low
Xylan conversion ratio is 30%.Wherein xylo-oligosaccharide is distributed in xylobiose to seven sugar of wood, xylobiose quality accounting 10%, xylotriose
Quality accounting 15%, Xylotetrose quality accounting 20%, wooden pentasaccharides quality accounting 23%, wooden six saccharic amount accountings 21%.Seven sugar of wood
Quality accounting 11%.
Wherein, xylo-oligosaccharide conversion ratio is calculated as follows：
Embodiment 2
(1) corncob 200kg, washing raw material removal dust, sundries and pigment etc. are taken, then by raw material soaking in 0.8m3
Water in, soaking temperature be 50 DEG C, soaking time 8h；Next time will be recycled after reaching setting soaking time without absorbed water
It is continuing with, obtains the pretreatment corncob that water content is dry weight 39%；
(2) it will be delivered in pressure high-density paste mill by the corncob of pretreatment, material, which enters, to be detained in cylinder, closes
Feed inlet is heated using steam, and the steam pressure of 0.4MPa is passed through demurrage cylinder, and grinding processing time is 5min, and grinding is fast
It spends for 3000r/min, after grinding to predetermined time, opens pneumatic ball valve, pressure is down to an atmospheric pressure, is obtained containing oligomeric wood
The feed liquid of sugar；
(3) feed liquid containing xylo-oligosaccharide is subjected to press filtration, obtains first time extracting solution, 1m is added in filter residue3Deionized water,
20min is extracted, then press filtration obtains second of extracting solution；Obtained filter residue adds in 0.8m3Then deionized water carries out third time
Press filtration obtains third time extracting solution, collects whole extracting solutions and obtains thick xylo-oligosaccharide liquid.It is obtained by liquid chromatogram measuring low
Xylan conversion ratio is 50%.Wherein xylo-oligosaccharide is distributed in xylobiose to seven sugar of wood, and xylobiose accounts for quality accounting 27%, wood three
Saccharic amount accounting 22%, Xylotetrose quality accounting 19%, wooden pentasaccharides quality accounting 15%, wooden six saccharic amount accountings 10%, wood seven
Saccharic amount accounting 7%.
Embodiment 3
For preparation process with embodiment 1, other conditions are as shown in table 1：
Table 1 prepares the process optimization of xylo-oligosaccharide using mill pressurization grinding
| Primary lignocellulosic | Solid-to-liquid ratio (mass ratio) | Pretreatment condition | Grinding condition |
| Wheat straw bar | 1:1.5 | 80 DEG C, 0.3h | 0.01MPa, 4000r/min, 10min |
| Maize straw | 1:3 | 20 DEG C, 20h | 0.8MPa, 1000r/min, 2min |
| Switchgrass | 1:5 | 50 DEG C, 10h | 0.5MPa, 3000r/min, 5min |
| Corncob | 1:8 | 50 DEG C, 8h | 0.1MPa, 3000r/min, 5min |
| Bagasse | 1:10 | 30 DEG C, 8h | 0.3MPa, 3000r/min, 10min |
Embodiment 4
(1) corncob 200kg, washing raw material removal dust, sundries and pigment etc. are taken, then by raw material soaking in 0.8m3
Mass fraction is in 0.35% trifluoroacetic acid solution, and soaking temperature is 30 DEG C, soaking time 8h；Reach setting soaking time
After will without absorbed acid solution recycling next time be continuing with, obtain water content be dry weight 39% pretreatment corncob；
(2) pretreated corncob is delivered in pressure high-density paste mill, material enter be detained cylinder in, close into
Material mouth is heated using steam, and the steam pressure of 0.2MPa is passed through demurrage cylinder, and grinding processing time is 10min, grinding speed
For 3000r/min, after grinding to predetermined time, pneumatic ball valve is opened, pressure is down to an atmospheric pressure, obtains the material containing xylose
Liquid；
(3) feed liquid containing xylose is subjected to press filtration, obtains first time extracting solution, 1m is added in filter residue3Deionized water, extraction
20min, then press filtration obtain second of extracting solution；Obtained filter residue adds in 0.8m3Then deionized water carries out third time pressure
Filter, obtains third time extracting solution, collects whole extracting solutions and obtain crude xylose solution.Xylose is obtained by liquid chromatogram measuring
Rate is 50%.
Wherein, xylose rate is calculated as follows：
Embodiment 5
(1) bagasse 200kg, washing raw material removal dust, sundries and pigment etc. are taken, then by raw material soaking in 0.8m3
Mass fraction is in 0.35% trifluoroacetic acid solution, and soaking temperature is 50 DEG C, soaking time 8h；Reach setting soaking time
After will without absorbed acid solution recycling next time be continuing with, obtain water content be dry weight 33% pretreatment bagasse；
(2) pretreated bagasse is delivered in pressure high-density paste mill, material enter be detained cylinder in, close into
Material mouth is heated using steam, and the steam pressure of 0.3MPa is passed through demurrage cylinder, and grinding processing time is 10min, grinding speed
For 3000r/min, after grinding to predetermined time, pneumatic ball valve is opened, pressure is down to an atmospheric pressure, obtains the material containing xylose
Liquid；
(3) feed liquid containing xylose is subjected to press filtration, obtains first time extracting solution, 1m is added in filter residue3Deionized water, extraction
20min, then press filtration obtain second of extracting solution；Obtained filter residue adds in 0.8m3Then deionized water carries out third time pressure
Filter, obtains third time extracting solution, collects whole extracting solutions and obtain crude xylose solution.Xylose is obtained by liquid chromatogram measuring
Rate is 70%.
Embodiment 6
For preparation process with embodiment 4, other conditions are as shown in table 2：
Table 2 prepares the process optimization of xylose using mill pressurization grinding
| Primary lignocellulosic | Acid solution | Solid-to-liquid ratio (kg：L) | Pretreatment condition | Grinding condition |
| Wheat straw bar | 2.5% acetic acid | 1:1.5 | 80 DEG C, 0.3h | 0.01MPa, 4000r/min, 10min |
| Maize straw | 5% formic acid | 1:3 | 20 DEG C, 20h | 0.8MPa, 1000r/min, 2min |
| Switchgrass | 1% hydrochloric acid | 1:5 | 50 DEG C, 10h | 0.5MPa, 3000r/min, 5min |
| Corncob | 0.5% nitric acid | 1:8 | 50 DEG C, 8h | 0.2MPa, 3000r/min, 5min |
| Bagasse | 3% sulfuric acid | 1:10 | 30 DEG C, 8h | 0.3MPa, 3000r/min, 10min |
Claims (7)
- A kind of 1. method that xylo-oligosaccharide or xylose are prepared using mill grinding, which is characterized in that include the following steps：（1）Primary lignocellulosic water or acid solution are impregnated, separation of solid and liquid after the completion of immersion；（2）By step（1）Obtained material is completed under conditions of steam heating, pressurization is passed through using mill grinding, grinding To xylo-oligosaccharide feed liquid or xylose feed liquid, the pressure of steam is 0.2~0.8MPa, and grinding speed is 1000~4000r/min, is ground The solution time is 2~10min；Work as step（1）In primary lignocellulosic be soaked in water, step（2）Xylo-oligosaccharide feed liquid is obtained,Work as step（1）In primary lignocellulosic impregnated with acid solution, step（2）Obtain xylose feed liquid；（3）By step（2）Obtained feed liquid carries out separation of solid and liquid and obtains xylo-oligosaccharide liquid or Xylose.
- 2. the according to the method described in claim 1, it is characterized in that, step（1）Primary lignocellulosic is corncob, sweet Bagasse, wheat straw bar, maize straw or switchgrass.
- 3. the according to the method described in claim 1, it is characterized in that, step（1）Primary lignocellulosic and water or acid are molten The mass ratio of liquid is 1:1.5~10.
- 4. the according to the method described in claim 1, it is characterized in that, step（1）Soaking temperature is 20 DEG C~80 DEG C, is impregnated Time is 0.3h~20h.
- 5. the according to the method described in claim 1, it is characterized in that, step（1）Acid solution is acetic acid, sulfuric acid, nitric acid, salt The aqueous solution of acid, formic acid or trifluoroacetic acid.
- 6. the according to the method described in claim 5, it is characterized in that, step（1）Sour mass fraction is in acid solution 0.1%~5%.
- 7. the according to the method described in claim 1, it is characterized in that, step（3）Obtained feed liquid carries out separation of solid and liquid, filter Pulp water carries out separation of solid and liquid again after washing, collect whole filtrate after carrying out 2~5 washings and separation of solid and liquid, obtain oligomeric wood Liquid glucose or Xylose.
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| CN102268490A (en) * | 2011-06-16 | 2011-12-07 | 北京化工大学 | Clean technique for co-producing xylose, xylitol and arabinose from agricultural and forestal waste |
| CN104762419A (en) * | 2015-03-31 | 2015-07-08 | 华南理工大学 | Method for preparing xylooligosaccharide from corncobs through microwave-assisted hydrothermal treatment |
| CN104946803A (en) * | 2015-05-27 | 2015-09-30 | 华南理工大学 | Method for preparing xylose hydrolysis fluid by utilizing oxalic acid mixed ball milling pretreated corncob |
| CN105625075A (en) * | 2016-03-09 | 2016-06-01 | 中国科学院青岛生物能源与过程研究所 | Method for pretreatment and separation of lignocellulose biomass |
| CN105695536A (en) * | 2016-04-07 | 2016-06-22 | 天津科技大学 | Pretreatment method of capable of implementing high-efficiency enzymolysis and saccharification on deciduous wood crotches |
| CN105777674A (en) * | 2016-04-14 | 2016-07-20 | 南京工业大学 | Method for preparing furfural, hydroxymethyl furfural and levulinic acid by using microchannel reaction device |
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| CN102268490A (en) * | 2011-06-16 | 2011-12-07 | 北京化工大学 | Clean technique for co-producing xylose, xylitol and arabinose from agricultural and forestal waste |
| CN104762419A (en) * | 2015-03-31 | 2015-07-08 | 华南理工大学 | Method for preparing xylooligosaccharide from corncobs through microwave-assisted hydrothermal treatment |
| CN104946803A (en) * | 2015-05-27 | 2015-09-30 | 华南理工大学 | Method for preparing xylose hydrolysis fluid by utilizing oxalic acid mixed ball milling pretreated corncob |
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