CN108623710A - A kind of method of microwave-enzyme assisted extraction bagasse hemicellulose - Google Patents
A kind of method of microwave-enzyme assisted extraction bagasse hemicellulose Download PDFInfo
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- 241000609240 Ambelania acida Species 0.000 title claims abstract description 102
- 239000010905 bagasse Substances 0.000 title claims abstract description 101
- 229920002488 Hemicellulose Polymers 0.000 title claims abstract description 75
- 238000000605 extraction Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 37
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 112
- 239000000203 mixture Substances 0.000 claims abstract description 84
- 239000006228 supernatant Substances 0.000 claims abstract description 59
- 239000002244 precipitate Substances 0.000 claims abstract description 47
- 108090000790 Enzymes Proteins 0.000 claims abstract description 39
- 102000004190 Enzymes Human genes 0.000 claims abstract description 39
- 235000019441 ethanol Nutrition 0.000 claims abstract description 38
- 238000001816 cooling Methods 0.000 claims abstract description 30
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 claims abstract description 24
- 108010029541 Laccase Proteins 0.000 claims abstract description 23
- 238000000874 microwave-assisted extraction Methods 0.000 claims abstract description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000005457 ice water Substances 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000007864 aqueous solution Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000001110 calcium chloride Substances 0.000 claims description 18
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 240000000111 Saccharum officinarum Species 0.000 claims description 2
- 235000007201 Saccharum officinarum Nutrition 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000002893 slag Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 21
- 229920005610 lignin Polymers 0.000 description 11
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 7
- 239000001632 sodium acetate Substances 0.000 description 7
- 235000017281 sodium acetate Nutrition 0.000 description 7
- 238000005406 washing Methods 0.000 description 7
- 239000003513 alkali Substances 0.000 description 6
- 229920002678 cellulose Polymers 0.000 description 5
- 239000001913 cellulose Substances 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 4
- 239000000284 extract Substances 0.000 description 3
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 description 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 101100136092 Drosophila melanogaster peng gene Proteins 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 229920002522 Wood fibre Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
Classifications
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- 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
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Sustainable Development (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The present invention relates to a kind of methods of microwave enzyme assisted extraction bagasse hemicellulose, belong to biorefinery extractive technique field.Laccase and water is added in the present invention in bagasse, is 30 ~ 65 DEG C, under stirring condition in temperature, is passed through air and pre-processes 4 ~ 12 h up to enzyme pretreatment bagasse mixture；Then 20 ~ 40 min of cooling treatment under the conditions of ice-water bath；KOH CaCl are added in the enzyme pretreatment bagasse mixture of cooling treatment2Mixture is 65 ~ 85 DEG C, carries out 20 ~ 60 min of microwave reinforced extraction under stirring condition and obtain Microwave Extraction mixture in temperature；Microwave Extraction mixture centrifugal treating is obtained into supernatant A and precipitate A, uses acetic acid sodium acetate aqueous solution to adjust the pH of supernatant A as 2 ~ 5, centrifugal treating obtains supernatant B and precipitate B；Ethyl alcohol and 1 ~ 3 h of cooling and standings processing under the conditions of ice-water bath are added in supernatant B, supernatant C and precipitate C are centrifugally separating to obtain under the conditions of temperature is 5 ~ 0 DEG C, precipitate C uses absolute ethyl alcohol, acetone to wash to neutrality, drying hemicellulose successively.
Description
Technical field
The present invention relates to a kind of methods of microwave-enzyme assisted extraction bagasse hemicellulose, belong to biorefinery extraction skill
Art field.
Background technology
Resource and environmental problem have become one of an important factor for limitation Economic Development, and the day of fossil resource fades
Consumption and environmental pollution caused by it, cause concern of the people to biomass resource, by taking bagasse as an example, the whole world generates every year
Several hundred million tons of bagasse, only a small number of bagasses are applied to paper industry, most of directly to be burnt, this not only causes resource unrestrained
Take, also pollutes the environment.But also only cellulose is utilized in paper industry, and content accounts for 20%- in bagasse
30% hemicellulose is seldom utilized.As comprehensive organism matter refines the proposition of concept, become how to efficiently use hemicellulose
The hot spot of domestic and international research.Hemicellulose is made of D- xyloses for sugar unit as a kind of branched polymer, main chain, and
With a plurality of side chain, there is complicated structure, research to find that hemicellulose can be used for producing such as bio-ethanol, furfural, xylose
The high value-added products such as alcohol.
The technology of traditional alkalinity extraction bagasse hemicellulose excessively falls behind, and alkali consumption is high, the reaction time is long, this is not only
The problems such as molecular structure for destroying hemicellulose, makes hemicellulose degradation, and hemicellulose yield is caused to decline, poor quality, simultaneously
Extraction cost is high, it is difficult to industrialize.For example, Zhou Jinghui et al. extracts Technique of Hemicellulose from Cornstalk using alkaline cooking, can make
Hemicellulose more dissolves out, but it the problem is that alkali consumption is high, cost is higher.
Peng forms etc. using soda acid extracting corncob hemicellulose is carried out under microwave radiation technology, and the diluted alkaline under the conditions of microwave radiation technology is taken out
It carries and shortens the reaction time, and within identical extraction time, the yield of hemicellulose is apparently higher than conventional diluted alkaline extracting, but it is anti-
Hemicellulose goes out compared with indissoluble during answering.
Invention content
The problem of existing for the above-mentioned prior art and deficiency, a kind of microwave-enzyme assisted extraction bagasse of present invention offer half
The method of cellulose, the method for the present invention pre-process bagasse using laccase, reuse multistage microwave amplifier hemicellulose, effectively
Reduction hemicellulose extraction process alkali charge, shorten the reaction time, and can guarantee the molecular weight of hemicellulose, half can be solved
The low problem of cellulose poor quality, yield.
A kind of method of microwave-enzyme assisted extraction bagasse hemicellulose, is as follows：
（1）Bagasse is added in reaction kettle, laccase and water is then added, is 30 ~ 65 DEG C, under stirring condition in temperature, is passed through
Air simultaneously pre-processes 4 ~ 12 h up to enzyme pretreatment bagasse mixture；
（2）Under the conditions of ice-water bath, by step（1）20 ~ 40 min of gained enzyme pretreatment bagasse mixture cooling treatment；
（3）By step（2）The enzyme pretreatment bagasse mixture of cooling treatment is transferred in microwave reactor, and KOH-CaCl is added2
Mixture is 65 ~ 85 DEG C, carries out 20 ~ 60 min of microwave reinforced extraction under stirring condition and obtain Microwave Extraction mixture in temperature；
（4）By step（3）Gained Microwave Extraction mixture centrifugal treating obtains supernatant A and precipitate A, using Acetic acid-sodium acetate
The pH that aqueous solution adjusts supernatant A is 2 ~ 5, and centrifugal treating obtains supernatant B and precipitate B；
（5）In step（4）Hydrous ethanol and 1 ~ 3 h of cooling and standings processing under the conditions of ice-water bath are added in gained supernatant B,
Temperature is centrifugally separating to obtain supernatant C and precipitate C under the conditions of being -5 ~ 0 DEG C, precipitate C use successively absolute ethyl alcohol, acetone wash to
Cleaning solution is neutrality, drying hemicellulose；
In terms of bagasse per ton, the step（1）The addition of middle laccase is 900 ~ 1800 kU, and the liquid of water and bagasse consolidates mass ratio
For (15 ~ 5):1；
The step（3）Middle KOH-CaCl2KOH and CaCl in mixture2Molar ratio be (5 ~ 2):1, KOH-CaCl2Mixture
Mass ratio with enzyme pretreatment bagasse mixture is (2 ~ 8):100；
The step（3）Middle microwave power is 600 ~ 1200 W；
The step（5）The volume ratio of middle hydrous ethanol and supernatant B are (3 ~ 5):1, the mass concentration of ethyl alcohol in hydrous ethanol
It is 60 ~ 95%；
The molecular weight of hemicellulose obtained by the method for the present invention is 6000 ~ 8000 g/mol, the yield of bagasse hemicellulose is 80 ~
90%。
The present invention pre-processes bagasse using laccase, interrupts the chemical bond of hemicellulose and lignin, loose wooden fibre
The structure of dimension improves porosity, specific surface area；Bagasse hemicellulose is extracted using microwave again, microwave energy is for biology
The difference of hemicellulose and cellulose and the dielectric constant of lignin in matter, the knot of less damage hemicellulose in extraction process
Structure ensures the structure of hemicellulose, realizes the high-efficiency low-damage extraction of hemicellulose, can shorten the reaction time, improve hemicellulose
The extraction efficiency of element.
The beneficial effects of the invention are as follows：
（1）The method of the present invention pre-processes bagasse using laccase, interrupts the chemical bond of hemicellulose and lignin, changes bagasse
Internal structure, keep wood fibre overall structure loose, improve porosity, promote microwave to the extraction efficiency of hemicellulose, drop
Low consumption alkali number, and solve the problems, such as that hemicellulose poor quality that high alkali charge is brought and yield are low；
（2）The method of the present invention extracts hemicellulose using the microwave combined facture of laccase-, and laccase dissolves out hemicellulose and lignin,
The overall structure for destroying bagasse can reduce the resistance of Microwave Extraction side cellulose, under conditions of the low alkali dense of microwave, extract sugarcane
Slag hemicellulose is heated evenly in extraction process, and heating is very fast, and the time is short, efficient, and the quality of hemicellulose is preferable.
Description of the drawings
Fig. 1 is the molecule spirogram of 1 hemicellulose of embodiment.
Specific implementation mode
With reference to embodiment, the invention will be further described.
Embodiment 1：A kind of method of microwave-enzyme assisted extraction bagasse hemicellulose, is as follows：
（1）Bagasse is added in reaction kettle, laccase and water is then added, wherein in terms of bagasse per ton, the addition of laccase is
It is 15 that the liquid of 900 kU, water and bagasse, which consolidates mass ratio,:1；It is 45 DEG C, under stirring condition in temperature, is passed through air and pre-processes 4 h
Up to enzyme pretreatment bagasse mixture；
（2）Under the conditions of ice-water bath, by step（1）40 min of gained enzyme pretreatment bagasse mixture cooling treatment；
（3）By step（2）The enzyme pretreatment bagasse mixture of cooling treatment is transferred in microwave reactor, and KOH-CaCl is added2
Mixture, wherein KOH-CaCl2KOH and CaCl in mixture2Molar ratio be 2:1, KOH-CaCl2Mixture and enzyme pretreatment
The mass ratio of bagasse mixture is 4:100；Temperature be 85 DEG C, carry out 20 min of microwave reinforced extraction under stirring condition and obtain it is micro-
Wave extraction mixture；Wherein microwave power is 800 W；
（4）By step（3）Gained Microwave Extraction mixture centrifugal treating obtains supernatant A and precipitate A, using Acetic acid-sodium acetate
The pH that aqueous solution adjusts supernatant A is 2, and the total concentration of Acetic acid-sodium acetate is 2 mol/L wherein in Acetic acid-sodium acetate aqueous solution,
The molar ratio of acetic acid and sodium acetate is 2:1；Centrifugal treating obtains supernatant B and precipitate B；Precipitate B is lignin；
（5）In step（4）Hydrous ethanol and 3 h of cooling and standings processing under the conditions of ice-water bath are added in gained supernatant B, in temperature
Degree is centrifugally separating to obtain supernatant C and precipitate C under the conditions of being -5 DEG C, precipitate C uses absolute ethyl alcohol, acetone to wash to washing successively
Liquid is neutrality, drying hemicellulose；The volume ratio of wherein hydrous ethanol and supernatant B is 4:1, ethyl alcohol in hydrous ethanol
Mass concentration be 95%；
The molecule spirogram of the present embodiment hemicellulose is as shown in Figure 1, from fig. 1, it can be seen that the molecular weight of hemicellulose is 6958 g/
The yield of mol, bagasse hemicellulose are 80.6%.
Embodiment 2：A kind of method of microwave-enzyme assisted extraction bagasse hemicellulose, is as follows：
（1）Bagasse is added in reaction kettle, laccase and water is then added, wherein in terms of bagasse per ton, the addition of laccase is
It is 12 that the liquid of 1800 kU, water and bagasse, which consolidates mass ratio,:1；It is 55 DEG C, under stirring condition in temperature, is passed through air and pre-processes 6
H is up to enzyme pretreatment bagasse mixture；
（2）Under the conditions of ice-water bath, by step（1）Gained enzyme pretreatment bagasse mixture cooling treatment 30min；
（3）By step（2）The enzyme pretreatment bagasse mixture of cooling treatment is transferred in microwave reactor, and KOH-CaCl is added2
Mixture, wherein KOH-CaCl2KOH and CaCl in mixture2Molar ratio be 4:1, KOH-CaCl2Mixture and enzyme pretreatment
The mass ratio of bagasse mixture is 6:100；Temperature be 75 DEG C, carry out 30 min of microwave reinforced extraction under stirring condition and obtain it is micro-
Wave extraction mixture；Wherein microwave power is 1200 W；
（4）By step（3）Gained Microwave Extraction mixture centrifugal treating obtains supernatant A and precipitate A, using Acetic acid-sodium acetate
The pH that aqueous solution adjusts supernatant A is 3, and the total concentration of Acetic acid-sodium acetate is 2 mol/L wherein in Acetic acid-sodium acetate aqueous solution,
The molar ratio of acetic acid and sodium acetate is 3:1；Centrifugal treating obtains supernatant B and precipitate B；Precipitate B is lignin；
（5）In step（4）Hydrous ethanol and 1.5 h of cooling and standings processing under the conditions of ice-water bath are added in gained supernatant B,
Temperature is centrifugally separating to obtain supernatant C and precipitate C under the conditions of being -3 DEG C, and precipitate C uses absolute ethyl alcohol, acetone to wash to washing successively
It is neutrality, drying hemicellulose to wash liquid；The volume ratio of wherein hydrous ethanol and supernatant B is 3:1, second in hydrous ethanol
The mass concentration of alcohol is 95%.
The molecular weight of the present embodiment hemicellulose is 7965g/mol, and the yield of bagasse hemicellulose is 82.3%.
Embodiment 3：A kind of method of microwave-enzyme assisted extraction bagasse hemicellulose, is as follows：
（1）Bagasse is added in reaction kettle, laccase and water is then added, wherein in terms of bagasse per ton, the addition of laccase is
It is 10 that the liquid of 1400 kU, water and bagasse, which consolidates mass ratio,:1；It is 50 DEG C, under stirring condition in temperature, is passed through air and pre-processes 8h
Up to enzyme pretreatment bagasse mixture；
（2）Under the conditions of ice-water bath, by step（1）Gained enzyme pretreatment bagasse mixture cooling treatment 20min；
（3）By step（2）The enzyme pretreatment bagasse mixture of cooling treatment is transferred in microwave reactor, and KOH-CaCl is added2
Mixture, wherein KOH-CaCl2KOH and CaCl in mixture2Molar ratio be 3:1, KOH-CaCl2Mixture and enzyme pretreatment
The mass ratio of bagasse mixture is 7:100；Temperature be 80 DEG C, carry out 40 min of microwave reinforced extraction under stirring condition and obtain it is micro-
Wave extraction mixture；Wherein microwave power is 1000 W；
（4）By step（3）Gained Microwave Extraction mixture centrifugal treating obtains supernatant A and precipitate A, using Acetic acid-sodium acetate
The pH that aqueous solution adjusts supernatant A is 4, and the total concentration of Acetic acid-sodium acetate is 2mol/L wherein in Acetic acid-sodium acetate aqueous solution,
The molar ratio of acetic acid and sodium acetate is 2.5:1；Centrifugal treating obtains supernatant B and precipitate B；Precipitate B is lignin；
（5）In step（4）Hydrous ethanol and 2 h of cooling and standings processing under the conditions of ice-water bath are added in gained supernatant B, in temperature
Degree is centrifugally separating to obtain supernatant C and precipitate C under the conditions of being -2 DEG C, precipitate C uses absolute ethyl alcohol, acetone to wash to washing successively
Liquid is neutrality, drying hemicellulose；The volume ratio of wherein hydrous ethanol and supernatant B is 5:1, ethyl alcohol in hydrous ethanol
Mass concentration is 75%.
The molecular weight of the present embodiment hemicellulose is 6293g/mol, and the yield of bagasse hemicellulose is 81.4%.
Embodiment 4：A kind of method of microwave-enzyme assisted extraction bagasse hemicellulose, is as follows：
（1）Bagasse is added in reaction kettle, laccase and water is then added, wherein in terms of bagasse per ton, the addition of laccase is
It is 8 that the liquid of 1200 kU, water and bagasse, which consolidates mass ratio,:1；It is 50 DEG C, under stirring condition in temperature, is passed through air and pre-processes 10h
Up to enzyme pretreatment bagasse mixture；
（2）Under the conditions of ice-water bath, by step（1）Gained enzyme pretreatment bagasse mixture cooling treatment 20min；
（3）By step（2）The enzyme pretreatment bagasse mixture of cooling treatment is transferred in microwave reactor, and KOH-CaCl is added2
Mixture, wherein KOH-CaCl2KOH and CaCl in mixture2Molar ratio be 2:1, KOH-CaCl2Mixture and enzyme pretreatment
The mass ratio of bagasse mixture is 6:100；Temperature be 85 DEG C, carry out 50 min of microwave reinforced extraction under stirring condition and obtain it is micro-
Wave extraction mixture；Wherein microwave power is 1000 W；
（4）By step（3）Gained Microwave Extraction mixture centrifugal treating obtains supernatant A and precipitate A, using Acetic acid-sodium acetate
The pH that aqueous solution adjusts supernatant A is 5, and the total concentration of Acetic acid-sodium acetate is 2mol/L wherein in Acetic acid-sodium acetate aqueous solution,
The molar ratio of acetic acid and sodium acetate is 3.5:1；Centrifugal treating obtains supernatant B and precipitate B；Precipitate B is lignin；
（5）In step（4）Hydrous ethanol and 2.5 h of cooling and standings processing under the conditions of ice-water bath are added in gained supernatant B,
Temperature is centrifugally separating to obtain supernatant C and precipitate C under the conditions of being 0 DEG C, and precipitate C uses absolute ethyl alcohol, acetone to wash to washing successively
It is neutrality, drying hemicellulose to wash liquid；The volume ratio of wherein hydrous ethanol and supernatant B is 4.5:1, in hydrous ethanol
The mass concentration of ethyl alcohol is 80%.
The molecular weight of the present embodiment hemicellulose is 7728 g/mol, and the yield of bagasse hemicellulose is 86.7%.
Embodiment 5：A kind of method of microwave-enzyme assisted extraction bagasse hemicellulose, is as follows：
（1）Bagasse is added in reaction kettle, laccase and water is then added, wherein in terms of bagasse per ton, the addition of laccase is
It is 5 that the liquid of 1600 kU, water and bagasse, which consolidates mass ratio,:1；It is 50 DEG C, under stirring condition in temperature, is passed through air and pre-processes 8h
Up to enzyme pretreatment bagasse mixture；
（2）Under the conditions of ice-water bath, by step（1）Gained enzyme pretreatment bagasse mixture cooling treatment 40min；
（3）By step（2）The enzyme pretreatment bagasse mixture of cooling treatment is transferred in microwave reactor, and KOH-CaCl is added2
Mixture, wherein KOH-CaCl2KOH and CaCl in mixture2Molar ratio be 2.5:1, KOH-CaCl2Mixture is located in advance with enzyme
The mass ratio for managing bagasse mixture is 5:100；It is 65 DEG C, carries out 60 min of microwave reinforced extraction under stirring condition and obtain in temperature
Microwave Extraction mixture；Wherein microwave power is 1100 W；
（4）By step（3）Gained Microwave Extraction mixture centrifugal treating obtains supernatant A and precipitate A, using Acetic acid-sodium acetate
The pH that aqueous solution adjusts supernatant A is 2.5, and the total concentration of Acetic acid-sodium acetate is 2 mol/ wherein in Acetic acid-sodium acetate aqueous solution
The molar ratio of L, acetic acid and sodium acetate is 4:1；Centrifugal treating obtains supernatant B and precipitate B；Precipitate B is lignin；
（5）In step（4）Hydrous ethanol and 1.2 h of cooling and standings processing under the conditions of ice-water bath are added in gained supernatant B,
Temperature is centrifugally separating to obtain supernatant C and precipitate C under the conditions of being -4 DEG C, and precipitate C uses absolute ethyl alcohol, acetone to wash to washing successively
It is neutrality, drying hemicellulose to wash liquid；The volume ratio of wherein hydrous ethanol and supernatant B is 3.5:1, in hydrous ethanol
The mass concentration of ethyl alcohol is 80%.
The molecular weight of the present embodiment hemicellulose is 7134g/mol, and the yield of bagasse hemicellulose is 82.5%.
Embodiment 6：A kind of method of microwave-enzyme assisted extraction bagasse hemicellulose, is as follows：
（1）Bagasse is added in reaction kettle, laccase and water is then added, wherein in terms of bagasse per ton, the addition of laccase is
It is 5 that the liquid of 1400 kU, water and bagasse, which consolidates mass ratio,:1；It is 65 DEG C, under stirring condition in temperature, is passed through air and pre-processes 12h
Up to enzyme pretreatment bagasse mixture；
（2）Under the conditions of ice-water bath, by step（1）At gained enzyme pretreatment bagasse mixture cooling:60min；
（3）By step（2）The enzyme pretreatment bagasse mixture of cooling treatment is transferred in microwave reactor, and KOH-CaCl is added2
Mixture, wherein KOH-CaCl2KOH and CaCl in mixture2Molar ratio be 3.5:1, KOH-CaCl2Mixture is located in advance with enzyme
The mass ratio for managing bagasse mixture is 2:100；It is 75 DEG C, carries out 60 min of microwave reinforced extraction under stirring condition and obtain in temperature
Microwave Extraction mixture；Wherein microwave power is 1100 W；
（4）By step（3）Gained Microwave Extraction mixture centrifugal treating obtains supernatant A and precipitate A, using Acetic acid-sodium acetate
The pH that aqueous solution adjusts supernatant A is 2.5, and the total concentration of Acetic acid-sodium acetate is 2 mol/ wherein in Acetic acid-sodium acetate aqueous solution
The molar ratio of L, acetic acid and sodium acetate is 3.5:1；Centrifugal treating obtains supernatant B and precipitate B；Precipitate B is lignin；
（5）In step（4）Hydrous ethanol and 1.8 h of cooling and standings processing under the conditions of ice-water bath are added in gained supernatant B,
Temperature is centrifugally separating to obtain supernatant C and precipitate C under the conditions of being -5 DEG C, and precipitate C uses absolute ethyl alcohol, acetone to wash to washing successively
It is neutrality, drying hemicellulose to wash liquid；The volume ratio of wherein hydrous ethanol and supernatant B is 4.5:1, in hydrous ethanol
The mass concentration of ethyl alcohol is 80%.
The molecular weight of the present embodiment hemicellulose is 7581 g/mol, and the yield of bagasse hemicellulose is 80.7%.
Embodiment 7：A kind of method of microwave-enzyme assisted extraction bagasse hemicellulose, is as follows：
（1）Bagasse is added in reaction kettle, laccase and water is then added, wherein in terms of bagasse per ton, the addition of laccase is
It is 5 that the liquid of 900 kU, water and bagasse, which consolidates mass ratio,:1；It is 30 DEG C, under stirring condition in temperature, is passed through air and pre-processes 4 h
Up to enzyme pretreatment bagasse mixture；
（2）Under the conditions of ice-water bath, by step（1）At gained enzyme pretreatment bagasse mixture cooling:60min；
（3）By step（2）The enzyme pretreatment bagasse mixture of cooling treatment is transferred in microwave reactor, and KOH-CaCl is added2
Mixture, wherein KOH-CaCl2KOH and CaCl in mixture2Molar ratio be 2:1, KOH-CaCl2Mixture and enzyme pretreatment
The mass ratio of bagasse mixture is 2:100；Temperature be 65 DEG C, carry out 20 min of microwave reinforced extraction under stirring condition and obtain it is micro-
Wave extraction mixture；Wherein microwave power is 1100 W；
（4）By step（3）Gained Microwave Extraction mixture centrifugal treating obtains supernatant A and precipitate A, using Acetic acid-sodium acetate
The pH that aqueous solution adjusts supernatant A is 2, and the total concentration of Acetic acid-sodium acetate is 2 mol/L wherein in Acetic acid-sodium acetate aqueous solution,
The molar ratio of acetic acid and sodium acetate is 2:1；Centrifugal treating obtains supernatant B and precipitate B；Precipitate B is lignin；
（5）In step（4）Hydrous ethanol and 1 h of cooling and standings processing under the conditions of ice-water bath are added in gained supernatant B, in temperature
Degree is centrifugally separating to obtain supernatant C and precipitate C under the conditions of being -5 DEG C, precipitate C uses absolute ethyl alcohol, acetone to wash to washing successively
Liquid is neutrality, drying hemicellulose；The volume ratio of wherein hydrous ethanol and supernatant B is 3:1, ethyl alcohol in hydrous ethanol
Mass concentration be 95%.
The molecular weight of the present embodiment hemicellulose is 6995 g/mol, and the yield of bagasse hemicellulose is 81.5%.
The specific implementation mode of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party
Formula can also be made without departing from the purpose of the present invention within the knowledge of a person skilled in the art
Go out various change.
Claims (5)
1. a kind of method of microwave-enzyme assisted extraction bagasse hemicellulose, which is characterized in that be as follows：
（1）Bagasse is added in reaction kettle, laccase and water is then added, is 30 ~ 65 DEG C, under stirring condition in temperature, is passed through
Air simultaneously pre-processes 4 ~ 12 h up to enzyme pretreatment bagasse mixture；
（2）Under the conditions of ice-water bath, by step（1）20 ~ 40 min of gained enzyme pretreatment bagasse mixture cooling treatment；
（3）By step（2）The enzyme pretreatment bagasse mixture of cooling treatment is transferred in microwave reactor, and KOH-CaCl is added2It is mixed
Object is closed, is 65 ~ 85 DEG C, carries out 20 ~ 60 min of microwave reinforced extraction under stirring condition and obtain Microwave Extraction mixture in temperature；
（4）By step（3）Gained Microwave Extraction mixture centrifugal treating obtains supernatant A and precipitate A, using Acetic acid-sodium acetate
The pH that aqueous solution adjusts supernatant A is 2 ~ 5, and centrifugal treating obtains supernatant B and precipitate B；
（5）In step（4）Hydrous ethanol and 1 ~ 3 h of cooling and standings processing under the conditions of ice-water bath are added in gained supernatant B,
Temperature is centrifugally separating to obtain supernatant C and precipitate C under the conditions of being -5 ~ 0 DEG C, precipitate C use successively absolute ethyl alcohol, acetone wash to
Cleaning solution is neutrality, drying hemicellulose.
2. the method for microwave-enzyme assisted extraction bagasse hemicellulose according to claim 1, it is characterised in that：With sugarcane per ton
Slag meter, step（1）The addition of middle laccase is 900 ~ 1800 kU, and the liquid of water and bagasse consolidate mass ratio as (15 ~ 5):1.
3. the method for microwave-enzyme assisted extraction bagasse hemicellulose according to claim 1, it is characterised in that：Step（3）In
KOH-CaCl2KOH and CaCl in mixture2Molar ratio be (5 ~ 2):1, KOH-CaCl2Mixture is mixed with enzyme pretreatment bagasse
The mass ratio of object is (2 ~ 8):100.
4. the method for microwave-enzyme assisted extraction bagasse hemicellulose according to claim 1, it is characterised in that：Step（3）In
Microwave power is 600 ~ 1200 W.
5. the method for microwave-enzyme assisted extraction bagasse hemicellulose according to claim 1, it is characterised in that：Step（5）In
The volume ratio of hydrous ethanol and supernatant B are (3 ~ 5):1, the mass concentration of ethyl alcohol is 60 ~ 95% in hydrous ethanol.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110981993A (en) * | 2019-11-21 | 2020-04-10 | 昆明理工大学 | Integrated treatment equipment and method for extracting and separating hemicellulose from grass raw materials |
| CN116042731A (en) * | 2023-02-21 | 2023-05-02 | 四川大学 | Method for producing 1, 3-propylene glycol by using distillers' grains enzymolysis liquid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105440149A (en) * | 2015-12-14 | 2016-03-30 | 陈燕妮 | Process for producing astragalus polysaccharide by using enzymolysis and microwave technology |
| CN106519066A (en) * | 2016-09-27 | 2017-03-22 | 济南米铎碳新能源科技有限公司 | Method for production of dietary fiber and combined production of pectin by utilizing fruit branches and fruit peels (residues) |
-
2018
- 2018-05-03 CN CN201810414669.3A patent/CN108623710A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105440149A (en) * | 2015-12-14 | 2016-03-30 | 陈燕妮 | Process for producing astragalus polysaccharide by using enzymolysis and microwave technology |
| CN106519066A (en) * | 2016-09-27 | 2017-03-22 | 济南米铎碳新能源科技有限公司 | Method for production of dietary fiber and combined production of pectin by utilizing fruit branches and fruit peels (residues) |
Non-Patent Citations (1)
| Title |
|---|
| 李娇阳 等: "漆酶预处理前后蔗渣半纤维素的提取及性质研究", 《林产化学与工业》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110981993A (en) * | 2019-11-21 | 2020-04-10 | 昆明理工大学 | Integrated treatment equipment and method for extracting and separating hemicellulose from grass raw materials |
| CN116042731A (en) * | 2023-02-21 | 2023-05-02 | 四川大学 | Method for producing 1, 3-propylene glycol by using distillers' grains enzymolysis liquid |
| CN116042731B (en) * | 2023-02-21 | 2024-01-30 | 四川大学 | Method for producing 1, 3-propylene glycol by using distillers' grains enzymolysis liquid |
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