CN105568729B - A kind of method that cellulose, hemicellulose and lignin are extracted from Jujun grasses - Google Patents
A kind of method that cellulose, hemicellulose and lignin are extracted from Jujun grasses Download PDFInfo
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- CN105568729B CN105568729B CN201510975275.1A CN201510975275A CN105568729B CN 105568729 B CN105568729 B CN 105568729B CN 201510975275 A CN201510975275 A CN 201510975275A CN 105568729 B CN105568729 B CN 105568729B
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- cellulose
- hemicellulose
- jujun grasses
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- ethanol
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
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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
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
Abstract
The invention discloses a kind of method that cellulose, hemicellulose and lignin are extracted from Jujun grasses, step is as follows:(1) to adding benzene alcohol mixed liquor to be dewaxed in Jujun grasses, to water is added in the Jujun grasses after dewaxing, extract, filtration is dried, and obtains final product pretreated Jujun grasses;(2) to sequentially adding NaOH H in pretreated Jujun grasses2O2Mixed solution and tetraacetyl ethylene diamine, 55 95 DEG C of 1 4h for the treatment of, filtering, as filter residue and drying, cellulose;(3) pH to 5.0 5.5 of filtrate after cellulose is extracted in regulation, adds ethanol, is settled out hemicellulose, and centrifugation obtains hemicellulose;(4) pH to 1.5 2.5 of raffinate after ethanol is reclaimed in the ethanol in the supernatant after recycling step (3) centrifugation, regulation, and centrifugation obtains lignin.Cellulose, hemicellulose and lignin can effectively be extracted successively in same process using the method for the present invention, recovery rate is high, improve the higher value application to wood fibre in Jujun grasses.
Description
Technical field
The present invention relates to a kind of method that cellulose, hemicellulose and lignin are extracted from Jujun grasses, belong to biomass
Convert and utilize field.
Background technology
Jujun grasses also known as imperatoria, hybrid giant napier, huge napier grass, also referred to as generate electricity grass, energy grass, with strong adaptability, growth
Hurry up, the characteristics of yield is high.After testing, growth period can reach 25-43%, half fiber in Jujun grasses content of cellulose more than half a year
Cellulose content, up to 20-32%, content of lignin 10-13%, is a kind of excellent fiber biomass.
At present, Jujun grasses be mainly used as culture medium of mushroom, cattle and sheep feed, biomass fuel generate electricity or for fiberboard system
Make, its abundant wood fibre does not obtain higher value application.Therefore, it is necessary to develop one kind can be by fiber in Jujun grasses
The extracting method that element, hemicellulose and the big component of lignin three are efficiently separated, realizes the height to this biomass resource of Jujun grasses
Value, green utilization.
The content of the invention
For above-mentioned prior art, cellulose, hemicellulose are extracted from Jujun grasses it is an object of the invention to provide one kind
With the method for lignin.Using microwave-alkali -ol method by the cellulose in Jujun grasses, hemicellulose and lignin in same process
In effectively extract successively, recovery rate is high, improves the higher value application to wood fibre in Jujun grasses.
To achieve the above object, the present invention uses following technical proposals:
A kind of method that cellulose, hemicellulose and lignin are extracted from Jujun grasses, step is as follows:
(1) pretreatment of raw material:To adding benzene -ol mixed liquor extracting 5-7h to be dewaxed in Jujun grasses, to huge after dewaxing
In mass ratio it is 1 in Juncao:(20-30) adds water, 80-90 DEG C of extraction 2-4h further to remove protein and fruit in Jujun grasses
The materials such as glue, filtration is dried, and obtains final product pretreated Jujun grasses.Jujun grasses raw material by after pretreatment, most of wax, egg
White matter and pectin etc. are removed, and remaining material is mainly cellulose, hemicellulose and lignin;
(2) cellulose is extracted:To sequentially adding NaOH-H in pretreated Jujun grasses2O2Mixed solution and four acetyl second
Diamines, heating using microwave to 55-95 DEG C, isothermal holding 1-4h, filtering, as filter residue and drying, cellulose.In microwave heating process,
Microwave produced by reactor causes the polar substances in plant cell to absorb microwave energy, produces amount of heat, makes cell
Interior temperature rises rapidly, and the pressure that liquid water vapor is produced breaks through cell membrane and cell membrane, forms small cavity;Further
Heating, causes cell interior and cell membrane moisture to reduce, and crackle occurs in cellular contraction, surface.The presence of hole and crackle makes born of the same parents
Outer reagent easily enters to accelerate reaction in people's cell, meanwhile, the actual amount of organic solvent is reduced by microwave treatment;
(3) hemicellulose is extracted:The pH to 5.0-5.5 of filtrate after cellulose is extracted in regulation, adds ethanol, is settled out half fine
Dimension element, centrifugation obtains hemicellulose;
(4) lignin extraction:The ethanol in supernatant after recycling step (3) centrifugation, raffinate after regulation recovery ethanol
PH to 1.5-2.5, centrifugation obtains lignin.
Preferably, in step (1), the benzene -ol mixed liquor is that toluene and ethanol are by volume (1.5-3):1 mixing
Solution;It is further preferred that it is by volume 2 that the benzene -ol mixed liquor is toluene and ethanol:The solution of 1 mixing.
Due to, containing materials such as more wax, protein and pectin, being unfavorable for cellulose, half fiber in Jujun grasses raw material
The extraction of element and lignin, and for how while the material such as the wax in removing Jujun grasses, protein and pectin, and
The extraction of cellulose, hemicellulose and lignin is not influenceed, this is not on the books in the prior art, the present invention is in process of the test
It is middle attempted various various combinations, the reagent of different ratio carries out dewaxing treatment to Jujun grasses, as a result find, with toluene and ethanol
It is by volume (1.5-3):1 is mixed, and Jujun grasses raw material is dewaxed, and its dewaxing effect is best;Further, to de-
Jujun grasses after Lasaxing Oilfield, carry out water extraction treatment, can preferably remove the material such as protein and pectin in Jujun grasses.
In step (2), the NaOH-H2O2In mixed solution, the mass concentration of NaOH is 1-4%, H2O2Mass concentration
It is 0.1-0.5%.
In step (2), NaOH-H2O2Mixed solution is (15-25) ml with the ratio of pretreated Jujun grasses addition:1g.
In step (2), the addition of tetraacetyl ethylene diamine is the quality of Jujun grasses powder (over dry) after 1-3% pretreatments.
In step (3), before ethanol is added, first filtrate is concentrated, be concentrated into the 1/2-1/3 of former filtrate volume;To dense
Ethanol is added in filtrate after contracting, the addition of ethanol is 3-4 times of filtrate volume after concentration.
In step (3) and step (4), using the HCl regulation pH value of 6mol/L.
In step (3) and step (4), centrifugal speed is 7000-8000r/min, and centrifugation time is 15-20min.
Can realize the separation successively of cellulose, hemicellulose and lignin using this technology, the cellulose isolated,
Hemicellulose and lignin yield and purity are high.
Cellulose, hemicellulose and lignin prepared by the above method is in production lactic acid, xylitol, vanillic aldehyde and/or work
Application in property charcoal is also protection scope of the present invention.
Beneficial effects of the present invention:
(1) can be by the cellulose in Jujun grasses, hemicellulose and lignin same using extracting method of the invention
During effectively extract successively, recovery rate is high, and Jujun grasses cellulose, hemicellulose, the yield of lignin are respectively:
0.37-0.41g/g Jujun grasses, 0.19-0.28g/g Jujun grasses, 0.09-0.11g/g Jujun grasses, improve to wooden in Jujun grasses
The higher value application of fiber.
(2) cellulose, hemicellulose and the lignin purity that present invention extraction is obtained are high, and the purity of the cellulose of extraction is
85.7-89.3%, the purity of hemicellulose is 87.1-92.2%, and the purity of lignin is 86.4-93.3%, can be used as production
The raw material of high added value derived product.Such as:Lactic acid is produced with cellulose fermentation, hemicellulose xylitol zymolysis production is used, with wood
Quality prepares vanillic aldehyde, activated carbon etc..So as to realize high-valued, the green utilization of this biomass resource of Jujun grasses.
(3) cellulose, hemicellulose and lignin are in itself the macromolecular compounds with Complicated Spatial Structure, in day
In right cellulosic material, they are polymerized to an entirety, form complicated super molecular compound.Wherein, lignin major part is deposited
In being intercellular layer, and hemicellulose forms strong bonded layer, and covering protection effect is formed to cellulose.Therefore, for fiber
The separation sequence of element, hemicellulose and lignin needs to carry out reasonable arrangement, and the present invention uses benzene -ol, hot-water extraction pair first
Jujun grasses are pre-processed, the material such as wax, protein and pectin in removing Jujun grasses;Again using microwave-alkali -ol method difference
Extract Jujun grasses cellulose, hemicellulose and lignin, wherein, by microwave-alkali process, destroy lignin and polysaccharide it
Between chemical bonds, make cellulose and lignin separation, cellulose is separated from lignin and hemicellulose, then lead to
Alcohol deposition method is crossed, hemicellulose, further centrifugal treating, isolated lignin is isolated.
Specific embodiment
Below by instantiation, the present invention will be further elaborated, it should explanation, the description below be only for
The present invention is explained, its content is not defined.
Used raw material, reagent are conventional chemical products in the embodiment of the present invention, can be purchased by commercial channel
Can buy.
Embodiment 1:
Pretreatment of raw material:Air-dried Jujun grasses are crushed, the grass meal of 40-60 mesh is obtained through sub-sieve screening.By gained grass meal
With benzene -ol mixed liquor (toluene:Ethanol v/v=2:1) extracting dewaxes for 6 hours, and the addition ratio of grass meal and benzene -ol mixed liquor is
1g:15ml.Grass meal after dewaxing is according to solid-to-liquid ratio 1:25 add deionized water, and 85 DEG C of stirrings are extracted 3 hours, vacuum filtration, institute
60 DEG C of drying of grass meal are obtained, sealed storage is standby.
5g Jujun grasses raw materials after pretreatment are weighed, by liquid ratio 20:1(ml:G) add and fill NaOH-H2O2Mixing is molten
Liquid (NaOH concentration 4%, H2O2Concentration is 0.5%) flat there-necked flask, adds tetraacetyl ethylene diamine (addition is 0.2%).
Microwave chemical reaction generator is used, 75 DEG C are heated to, insulated and stirred is processed 3 hours.After reaction terminating, vacuum filter, gained is residual
60 DEG C of drying of slag, obtain cellulose 2.05g.
Filtrate pH to 5.0-5.5 is adjusted with the HCl of 6mol/L, (i.e. concentrate is former filtrate volume to be concentrated by evaporation about 3 times
1/3) 3 times of 95% ethanol of volume, are added, hemicellulose is settled out, with supercentrifuge, centrifugation (7500r/min,
15min), precipitation is washed with 70% ethanol, is centrifuged 2-3 times again, and 60 DEG C of drying obtain hemicellulose 1.2g.
Gained supernatant will be centrifuged, low pressure rotary evaporation reclaims ethanol, and the ethanol of recovery is recycled.Raffinate 6mol/L
HCl regulation filtrate pH to 2.0, with supercentrifuge, supernatant is poured out in centrifugation (7500r/min, 15min), and gained is residual
60 DEG C of drying of slag, obtain lignin 0.5g.
Cellulose, hemicellulose and lignin purity testing:According to Van Soest methods, the method is by determining neutral detergent
Fiber (NDF), acid detergent fiber (ADF), acidic cleaning lignin (ADL), the content of ash content (S) calculate in plant each
The content of main component.By methods pair such as inherent viscosity, molecular weight, FT-IR, CP-MAS 13C-NMR and thermodynamic analysis
Cellulose, hemicellulose and the lignin isolated carry out purity testing.
In the present embodiment, the purity of the cellulose separated is 89.3%, and the purity of hemicellulose is 92.2%, wooden
The purity of element is 93.3%.
Embodiment 2:
The pretreatment of raw material is with embodiment 1.
The pretreated Jujun grasses raw materials of 5g are weighed, by liquid ratio 25:1(ml:G) add and fill NaOH-H2O2Mixed solution
(NaOH concentration 4%, H2O2Concentration is 0.5%) flat there-necked flask, adds tetraacetyl ethylene diamine (addition is 0.2%).With
Microwave chemical reaction generator, is heated to 75 DEG C, and insulated and stirred is processed 4 hours.After reaction terminating, vacuum filter is residue obtained
60 DEG C of drying, obtain cellulose 1.95g.Filtrate pH to 5.0-5.5 is adjusted with the HCl of 6mol/L, about 3 times are concentrated by evaporation, 3 are added
95% ethanol of times volume, is settled out hemicellulose, and with supercentrifuge, centrifugation (7500r/min, 15min), precipitation is again
Washed with 70% ethanol, be centrifuged 2-3 times, 60 DEG C of drying obtain hemicellulose 1.32g.Will centrifugation gained supernatant, low pressure rotation
Turn evaporation and reclaim ethanol, the ethanol of recovery is recycled.Raffinate adjusts filtrate pH to 2.0 with the HCl of 6mol/L, uses high speed centrifugation
Supernatant is poured out in machine, centrifugation (7500r/min, 15min), and residue obtained 60 DEG C of drying obtain lignin 0.55g.
In the present embodiment, the purity of the cellulose isolated is 88.7%, and the purity of hemicellulose is 90.1%, lignin
Purity be 91.6%.
Comparative example 1:
Jujun grasses raw material is not preprocessed, after convection drying is crushed, 5g is weighed, by liquid ratio 20:1(ml:G) add and contain
There is NaOH-H2O2Mixed solution (NaOH concentration 4%, H2O2Concentration is 0.5%) flat there-necked flask, adds four acetyl second two
Amine (addition is 0.2%).Microwave chemical reaction generator is used, 75 DEG C are heated to, insulated and stirred is processed 3 hours.Reaction terminating
Afterwards, vacuum filter, residue obtained 60 DEG C of drying, obtains cellulose 1.45g.
Filtrate pH to 5.0-5.5 is adjusted with the HCl of 6mol/L, about 3 times are concentrated by evaporation, 3 times of 95% ethanol of volume are added,
Hemicellulose is settled out, with supercentrifuge, centrifugation (7500r/min, 15min), precipitation washed with 70% ethanol again,
Centrifugation 2-3 times, 60 DEG C of drying obtain hemicellulose 0.7g.
Gained supernatant will be centrifuged, low pressure rotary evaporation reclaims ethanol, and the ethanol of recovery is recycled.Raffinate 6mol/L
HCl regulation filtrate pH to 2.0, with supercentrifuge, supernatant is poured out in centrifugation (7500r/min, 15min), and gained is residual
60 DEG C of drying of slag, obtain lignin 0.2g.
The purity of the cellulose isolated is 83.7%, and the purity of hemicellulose is 82.1%, and the purity of lignin is
81.6%.
Comparative example 2:
Jujun grasses raw material is not preprocessed, after convection drying is crushed, 5g is weighed, by liquid ratio 25:1(ml:G) add and contain
There is NaOH-H2O2Mixed solution (NaOH concentration 4%, H2O2Concentration is 0.5%) flat there-necked flask, adds four acetyl second two
Amine (addition is 0.2%).Microwave chemical reaction generator is used, 75 DEG C are heated to, insulated and stirred is processed 4 hours.Reaction terminating
Afterwards, vacuum filter, residue obtained 60 DEG C of drying, obtains cellulose 1.35g.Filtrate pH to 5.0- is adjusted with the HCl of 6mol/L
5.5, about 3 times are concentrated by evaporation, 3 times of 95% ethanol of volume are added, hemicellulose is settled out, with supercentrifuge, centrifugation
(7500r/min, 15min), precipitation is washed with 70% ethanol, is centrifuged 2-3 times again, and 60 DEG C of drying obtain hemicellulose 0.82g.
Gained supernatant will be centrifuged, low pressure rotary evaporation reclaims ethanol, and the ethanol of recovery is recycled.Raffinate is adjusted with the HCl of 6mol/L
Section filtrate pH to 2.0, with supercentrifuge, supernatant, residue obtained 60 DEG C are poured out in centrifugation (7500r/min, 15min)
Drying, obtains lignin 0.25g.
The purity of the cellulose isolated is 84.7%, and the purity of hemicellulose is 83.5%, and the purity of lignin is
85.6%.
Be can be seen that by embodiment 1-2, comparative example 1-2 and pre-processed by Jujun grasses raw material, can significantly improved
The recovery rate of cellulose, hemicellulose and lignin.
Comparative example 3:
Pretreatment of raw material:Air-dried Jujun grasses are crushed, the grass meal of 40-60 mesh is obtained through sub-sieve screening.By gained grass meal
With benzene-methanol solution (benzene:Methyl alcohol v/v=2:1) extract 6 hours and dewax, the addition ratio of grass meal and benzene -ol mixed liquor is 1g:
15ml.Grass meal after dewaxing is according to solid-to-liquid ratio 1:25 add deionized water, and 85 DEG C of stirrings are extracted 3 hours, vacuum filtration, gained grass
60 DEG C of drying of powder, sealed storage is standby.
5g Jujun grasses raw materials after pretreatment are weighed, the separation of cellulose, hemicellulose and lignin, separation side is carried out
Method with embodiment 1, as a result isolated cellulose 1.58g, hemicellulose 0.98g, lignin 0.32g.
The purity of the cellulose isolated is 87.7%, and the purity of hemicellulose is 86.4%, and the purity of lignin is
88.2%.
Comparative example 4:
Pretreatment of raw material:Air-dried Jujun grasses are crushed, the grass meal of 40-60 mesh is obtained through sub-sieve screening.By gained grass meal
With benzene -ol mixed liquor (toluene:Ethanol v/v=4:1) extract 6 hours and dewax, the addition ratio of grass meal and benzene -ol mixed liquor is
1g:15ml.Grass meal after dewaxing is according to solid-to-liquid ratio 1:25 add deionized water, and 85 DEG C of stirrings are extracted 3 hours, vacuum filtration, institute
60 DEG C of drying of grass meal are obtained, sealed storage is standby.
5g Jujun grasses raw materials after pretreatment are weighed, the separation of cellulose, hemicellulose and lignin, separation side is carried out
Method with embodiment 1, as a result isolated cellulose 1.62g, hemicellulose 1.13g, lignin 0.41g.
The purity of the cellulose isolated is 88.2%, and the purity of hemicellulose is 89.1%, and the purity of lignin is
87.6%.
Can be seen that to enter Jujun grasses raw material using the reagent of various combination, different ratio by embodiment 1, comparative example 3-4
After row pretreatment, the recovery rate and purity of cellulose, hemicellulose and lignin have marked difference, illustrate to enter for Jujun grasses
The used reagent of row pretreatment and its proportioning are not conventional selections.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by above-described embodiment
Limitation, one of ordinary skill in the art should be understood that on the basis of technical scheme those skilled in the art need not
The various modifications or deformation made by paying creative work are still within protection scope of the present invention.
Claims (8)
1. a kind of method that cellulose, hemicellulose and lignin are extracted from Jujun grasses, it is characterised in that step is as follows:
(1) pretreatment of raw material:To adding benzene -ol mixed liquor extracting 5-7h to be dewaxed in Jujun grasses, to the Jujun grasses after dewaxing
In in mass ratio be 1:(20-30) adds water, and 80-90 DEG C of extraction 2-4h, filtration is dried, and obtains final product pretreated Jujun grasses;
(2) cellulose is extracted:To sequentially adding NaOH-H in pretreated Jujun grasses2O2Mixed solution and tetraacetyl ethylene diamine,
To 55-95 DEG C, isothermal holding 1-4h is filtered, filter residue and drying, as cellulose for heating using microwave;The NaOH-H2O2Mixed solution
In, the concentration of NaOH is 1-4%, H2O2Concentration be 0.1-0.5%;
(3) hemicellulose is extracted:The pH to 5.0-5.5 of filtrate after cellulose is extracted in regulation, adds ethanol, is settled out half fiber
Element, centrifugation obtains hemicellulose;
(4) lignin extraction:Recycling step (3) centrifugation after supernatant in ethanol, regulation reclaim ethanol after raffinate pH to
1.5-2.5, centrifugation obtains lignin;
The purity of the cellulose of extraction is 85.7-89.3%, and the purity of hemicellulose is 87.1-92.2%, the purity of lignin
It is 86.4-93.3%.
2. the method for claim 1, it is characterised in that in step (1), the benzene -ol mixed liquor is toluene and ethanol
It is by volume (1.5-3):The solution of 1 mixing.
3. method as claimed in claim 2, it is characterised in that in step (1), the benzene -ol mixed liquor is toluene and ethanol
It is by volume 2:The solution of 1 mixing.
4. the method for claim 1, it is characterised in that in step (2), NaOH-H2O2Mixed solution with it is pretreated
The ratio of Jujun grasses addition is (15-25) ml:1g.
5. the method for claim 1, it is characterised in that in step (2), the addition of tetraacetyl ethylene diamine is 1-3%.
6. preparation method as claimed in claim 1, it is characterised in that in step (3), before ethanol is added, is first carried out to filtrate
Concentration, is concentrated into the 1/2-1/3 of former filtrate volume;To ethanol is added in the filtrate after concentration, the addition of ethanol is concentration
3-4 times of filtrate volume afterwards.
7. preparation method as claimed in claim 1, it is characterised in that in step (3) and step (4), using 6mol/L's
HCl adjusts pH value.
8. preparation method as claimed in claim 1, it is characterised in that in step (3) and step (4), centrifugal speed is
7000-8000r/min, centrifugation time is 15-20min.
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CN107903402A (en) * | 2017-11-21 | 2018-04-13 | 常州市鼎日环保科技有限公司 | A kind of preparation method of water hyacinth base purifying lignin |
CN108221432B (en) * | 2017-12-28 | 2020-07-07 | 潍坊友容实业有限公司 | Process method for extracting cellulose from suaeda salsa |
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CN114249842B (en) * | 2020-09-25 | 2023-07-21 | 广西中医药大学 | Method for extracting sugarcane leaf polysaccharide |
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