CN107540714B - A kind of highly effective extraction method of Eucalyptus xylose - Google Patents
A kind of highly effective extraction method of Eucalyptus xylose Download PDFInfo
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Abstract
The invention discloses a kind of highly effective extraction methods of Eucalyptus xylose, comprising: mixes ammonium hydroxide and dioctyl sodium sulfosuccinate with Eucalyptus wood powder, carries out decompression explosion, then using the mixed liquor of LiCl aqueous solution and ethyl alcohol as solvent, KOH and H is added2O2High shear separating treatment is carried out, solid phase residue is filtered to remove after separating treatment, filtrate pH value is adjusted, then carry out separating treatment, is then filtered, filtration product is finally freeze-dried i.e. acquisition high-purity xylose.The present invention can extract high-purity xylose effectively from the hard Eucalyptus of material, have the advantages that simple process and high-efficient, the solvent and chemicals used can be avoided the generation of toxic pollutant for green reagent；The structure stubbornly resisting property of Eucalyptus Fibers after separating xylose significantly reduces, and cellulose enzyme hydrolysis property is obviously improved, and glucose hydrolysis speed is fast, and yield is high, can be used as the preparation that good raw material carries out biorefinery downstream product.
Description
Technical field
The present invention relates to a kind of xylose highly effective extraction methods, in particular to a kind of to pass through at ammonia explosion and high shear chemistry
The method that reason extracts Eucalyptus xylose.
Background technique
Eucalyptus is about 20%~30% as a kind of fast growing hard wood, the mass fraction of hemicellulose, and hemicellulose is
A kind of important functional carbohydrate, can be used as plant cell wall adhesive and filler, is distributed in and is made of cellulose
Plant cell support frame in.Although hemicellulose and cellulose pass through other without chemistry key connection, between them
Mode is closely combined together, and is combined with lignin by chemical bond, is formed lignin-carbohydrate complex (LCC)；
Structure is complicated for hemicellulose, is a kind of low molecular weight carbohydrate, has many branches, hygroscopic swollen and whether there is or not formed-knots
The compound polysaccharide of structure.Hemicellulose includes various pentoses (arabinose, xylose), hexose (galactolipin, glucose, sweet dew
Sugar) and small part uronic acid.These monosaccharide components are formed by glucosides key connection, form the hemicellulose knot of configurations
Structure, can be different the hemicellulose type that the different parts of identical plant generate；For Eucalyptus, hemicellulose
The structure of element is increasingly complex, and main Types mainly have xylan class, polydextrose sweet dew carbohydrate, xylan glucose,
Middle xylose is hemicellulose main component.
For the separating technology technology of traditional plant fiber material component, the emphasis of research is cellulosic sections, and phase
When a part hemicellulose and lignin enter waste liquid part, by burn handled, thus cause plant fiber money
The waste in source.Hemicellulose is separated from plant resources and realizes that efficient utilize of hemicellulose is that people pay high attention to always
Focus.A variety of methods that hemicellulose is extracted from biomass have been developed in recent years, as alkaline process processing, steam blasting are located in advance
Manage the separation of ultrasonic wave auxiliary separation hemicellulose microwave electromagnetic auxiliary, alkaline hydrogen peroxide extracting etc..But with current research
From the point of view of achievement, all there is the problems such as low efficiency, impurity content are high, comprehensive utilization ratio is poor in above method；And hemicellulose is dividing
From different degrees of degradation can occur in the process.Therefore, it explores and develops a kind of method for efficiently separating wood sugars hemicellulose,
For extending biomass product field, improves added value of product and be of great significance.
Summary of the invention
Hemicellulose is improved for the above prior art in order to efficiently separate wood sugars hemi-cellulose components in Eucalyptus
Utility value, the object of the present invention is to provide a kind of using Eucalyptus as the method for raw material high efficiency extraction xylose, to improve hemicellulose
Value-added content of product extends biomass product field.
To achieve the above object, the present invention adopts the following technical scheme:
The first aspect of the invention provides a kind of highly effective extraction method of Eucalyptus xylose, comprising the following steps:
Ammonium hydroxide and dioctyl sodium sulfosuccinate are mixed with Eucalyptus wood powder, decompression explosion is carried out under setting condition, so
Afterwards using the mixed liquor of LiCl aqueous solution and ethyl alcohol as solvent, KOH and H is added2O2High shear separating treatment is carried out, after separating treatment
It is filtered to remove solid phase residue, filtrate pH value is adjusted, then carry out separating treatment, is then filtered, finally carries out filtration product
Freeze-drying obtains high-purity xylose.
The second aspect of the invention provides a kind of Eucalyptus xylose product that the above method is prepared.
The third aspect of the invention provides a kind of method of efficient coproduction Eucalyptus xylose and glucose, including following step
It is rapid:
Ammonium hydroxide and dioctyl sodium sulfosuccinate are mixed with Eucalyptus wood powder, decompression explosion is carried out under setting condition, so
Afterwards using the mixed liquor of LiCl aqueous solution and ethyl alcohol as solvent, KOH and H is added2O2High shear separating treatment is carried out, after separating treatment
It is filtered to remove solid phase residue, filtrate pH value is adjusted, then carry out centrifugal treating, is then filtered, finally carries out filtration product
Freeze-drying obtains high-purity xylose；
Wherein the solid phase residue produces glucose, condition for enzyme hydrolysis are as follows: and Eucalyptus solid phase sludge concentration 2.0~
2.5%,
PH value 4.8~5,50~55 DEG C of temperature, 16.0~18FPU/g of cellulase dosageSolid phase residue, β-glucosyl enzym dosage
20~24.0CBU/gSolid phase residue, dispersion revolving speed is 150~200rpm, handles 10~12h of time.
Compared with prior art, technical solution of the present invention has the following beneficial effects:
(1) present invention is pre-processed by explosion combines chemical high shear treatment, can effectively extract from the hard Eucalyptus of material
High-purity xylose has the advantages that simple process and high-efficient；
(2) solvent and chemicals used can effectively avoid toxic dirt in xylose extraction process for Green Chemistry reagent
The generation for contaminating object, alleviates the pollution to environment；
(3) the cellulose enzyme hydrolysis property of the Eucalyptus Fibers after separating xylose is obviously improved, and glucose hydrolysis speed is fast,
Glucose yield is high, can be used as the preparation that good raw material carries out biorefinery downstream product.
(4) present invention improves broadleaf Eucalyptus hemicellulose separative efficiency and purity, can solve hemicellulose at this stage
Existing low separation efficiency, the problems such as impurity content is high during the separation process.
(5) degradation present invention alleviates hemicellulose during the separation process improves the comprehensive utilization ratio of hemicellulose,
Expansible plant biomass product scope improves plant biomass value-added content of product.
Specific embodiment
It is noted that described further below be all exemplary, it is intended to provide further instruction to the present invention.Unless another
It indicates, all technical and scientific terms used herein has usual with general technical staff of the technical field of the invention
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to exemplary embodiments of the present invention.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation and/or their combination.
As background technique is introduced, the method for extracting hemicellulose from biomass in the prior art, such as " alkaline process
Processing, the separation of steam blasting pretreatment ultrasonic wave auxiliary separation hemicellulose microwave electromagnetic auxiliary, alkaline hydrogen peroxide extracting "
Etc. technologies there are low efficiency, impurity content is high, comprehensive utilization ratio is poor, hemicellulose can occur during the separation process it is different degrees of
The problems such as degradation, in order to solve the above-mentioned technical problem, for Eucalyptus raw material, the present invention proposes a kind of high efficiency extraction of Eucalyptus xylose
Method, comprising the following steps:
Ammonium hydroxide and dioctyl sodium sulfosuccinate are mixed with Eucalyptus wood powder, decompression explosion is carried out under setting condition, so
Afterwards using the mixed liquor of LiCl aqueous solution and ethyl alcohol as solvent, KOH and H is added2O2High shear separating treatment is carried out, after separating treatment
Be filtered to remove solid phase residue, glacial acetic acid be added and adjusts filtrate pH value, then carries out centrifugal treating, is then filtered, finally incited somebody to action
Filter product is freeze-dried i.e. acquisition high-purity xylose.
Those skilled in the art knows, the design feature that each biomass has its special, their hemicellulose,
The complicated link of the ingredients such as lignin and cellulose has the characteristics that oneself uniqueness.The composed structure of Eucalyptus has as background skill
The various features that art is introduced, the structure and type of hemicellulose are increasingly complex, the present invention first according to Eucalyptus composition this
A little design features have selected ammonium hydroxide explosion preconditioning technique, by the pretreatment, change the physicalchemical structure of Eucalyptus, mention
The high degradability of lignocellulosic, increases porosity, destroys the rigid composed structure of Eucalyptus hard and compact, and find
It joined dioctyl sodium sulfosuccinate during processing, strengthen this technical effect, strengthen the permeance property of ammonium hydroxide,
The diffusion for improving dissolution component, greatly enhances the sensitivity of Eucalyptus raw material, eachization in Eucalyptus composed structure
It learns key to be easier to be opened, provides good basis for subsequent preparation high-purity xylose；Then the present invention is according to using ammonium hydroxide
With the effect after the decompression explosion treatment of dioctyl sodium sulfosuccinate, high shear dispersion processing technique is used, in high shear
Under the action of power, the cohesive force of fibrocyte is weakened, even destroys, and improves the accessibility of hemicellulose, in the art
Using specific chemical reagent, using the mixed liquor of LiCl aqueous solution and ethyl alcohol as solvent, lithium ion can efficient swollen fiber, break
Hydrogen bond network in bad raw material keeps structure more loose, is conducive to the extracting of xylose, and KOH and H is added2O2, can not only be into one
Step improves the recovery rate of xylose, and can also significantly lower the structure stubbornly resisting property of the Eucalyptus Fibers after separating xylose, is conducive to wood
The comprehensive utilization of matter cellulose.
In currently preferred non-limiting embodiment, select less than 40 mesh Eucalyptus powder as raw material.It is found in test,
When the partial size of raw material is less than 40 mesh, the specific surface area of processing is increased, so that the purity and yield of Eucalyptus xylose are higher.
There are many factor for influencing ammonia explosion treatment, its effect generated of different pretreatment conditions also has difference.This
Invention has obtained preferable combination condition according to the specific composed structure feature of Eucalyptus, screening and optimizing, passes through these preferable group
Conjunction condition provides more good basis for preparation high-purity xylose and the structure stubbornly resisting property for reducing Eucalyptus Fibers.Therefore at this
It invents in preferred non-limiting embodiment, the condition of ammonia explosion treatment Eucalyptus wood powder are as follows: ammonia volume 1.5-3.0g/
gDry wood powder, dioctyl sodium sulfosuccinate dosage 0.01-0.03g/gDry wood powder, 105.0-135.0 DEG C of temperature, time 20.0-
45.0min.The present invention selects dioctyl sodium sulfosuccinate, can strengthen drug infiltration, soften raw material, can accelerate treatment process
In effect of mass transmitting, improve treatment effect, the structure stubbornly resisting property of lignocellulosic is effectively reduced.Relative to other surfaces activity
Agent, amber sodium dioctyl sulfo can not only strengthen infiltration, moreover it is possible to more effectively soften lignin, separation is made more to mostly occur wooden
The interface of element and hemicellulose creates favorable conditions for the extraction of subsequent xylose.
The present invention is imitated according to the technology after the specific structure of chemical composition feature of Eucalyptus and above-mentioned ammonia explosion treatment
Fruit, the technological parameter that screening and optimizing has obtained preferable chemical high shear treatment can be into one using these process conditions
Step improves the recovery rate and purity of xylose, and further decreases the structure stubbornly resisting property of the Eucalyptus Fibers after separating xylose.Therefore
In currently preferred non-limiting embodiment, high shear separating treatment condition are as follows: the solvent group becomes: LiCl content is
18.0-27.0wt%, water content 27.0-53.0wt%, ethanol content 20.0-55.0wt%；Solvent usage 5.0-8.0g/
gDry wood powder, KOH dosage is 0.35-0.85g/gDry wood powder, H2O2Dosage is 0.03-0.06g/gDry wood powder, 40-60 DEG C of temperature, high shear
Revolving speed 15000-20000rpm, decentralized processing time 90-150min.Experiment proves that LiCl can effective swollen fiber, destroy hydrogen
Key network structure creates conditions for xylose extraction, and ethyl alcohol can play the role of reducing lignin and cellulose dissolution, improves subsequent
Xylose DNA purity.
In currently preferred non-limiting embodiment, filtrate pH to 4.5-5.5 is adjusted using glacial acetic acid.
In currently preferred non-limiting embodiment, the separating treatment after adjusting pH, which uses, to be centrifugated, at centrifugation
Reason revolving speed is 4000-5000rpm, centrifugation time 20-30min.
In currently preferred non-limiting embodiment, filtration product in -20~-15 DEG C of 2~3h of pre-freeze, then -
50~-40 DEG C, 15~20MPa of pressure carry out freeze-drying 20~for 24 hours.It is further preferred that filtration product is in -20 DEG C of pre-freeze 3h,
Then it is freeze-dried for 24 hours in -50 DEG C, pressure 15MPa.
For the yield for improving glucose, in currently preferred non-limiting embodiment, Eucalyptus solid phase residue is used for enzyme
The optimal conditions of hydrolysis production glucose are as follows: Eucalyptus solid phase sludge concentration 2.0~2.5%, pH value 4.8~5, temperature 50~55
DEG C, 16.0~18FPU/g of cellulase dosageSolid phase residue, 20~24.0CBU/g of β-glucosyl enzym dosageSolid phase residue, dispersing revolving speed is
150~200rpm handles 10~12h of time.It is further preferred that Eucalyptus solid phase sludge concentration 2.0%, pH value 4.8, temperature 50
DEG C, cellulase dosage 16.0FPU/gSolid phase residue, β-glucosyl enzym dosage 24.0CBU/gSolid phase residue, dispersion revolving speed is 200rpm, place
Manage time 12h.
In currently preferred non-limiting embodiment, a kind of Eucalyptus wood being prepared using the above method is also provided
The purity of sugar product, the Eucalyptus xylose in the product is higher, and up to 95% or more.
In currently preferred non-limiting embodiment, a kind of side of efficient coproduction Eucalyptus xylose and glucose is also provided
Method, comprising the following steps:
Ammonium hydroxide and dioctyl sodium sulfosuccinate are mixed with Eucalyptus wood powder, decompression explosion is carried out under setting condition, so
Afterwards using the mixed liquor of LiCl aqueous solution and ethyl alcohol as solvent, KOH and H is added2O2High shear separating treatment is carried out, after separating treatment
It is filtered to remove solid phase residue, filtrate pH value is adjusted, then carry out centrifugal treating, is then filtered, finally carries out filtration product
Freeze-drying obtains high-purity xylose；
Wherein the solid phase residue produces glucose, condition for enzyme hydrolysis are as follows: and Eucalyptus solid phase sludge concentration 2.0~
2.5%, pH value 4.8~5,50~55 DEG C of temperature, 16.0~18FPU/g of cellulase dosageSolid phase residue, β-glucosyl enzym dosage 20
~24.0CBU/gSolid phase residue, dispersion revolving speed is 150~200rpm, handles 10~12h of time.
In order to enable those skilled in the art can clearly understand technical solution of the present invention, below with reference to tool
The embodiment and the comparative example technical solution that the present invention will be described in detail of body, in addition to having special instruction, other all percentages are equal
For mass percent.
Embodiment 1
Eucalyptus wood powder less than 40 mesh extracts xylose according to the following steps:
1. ammonium hydroxide and dioctyl sodium sulfosuccinate are mixed with Eucalyptus wood powder, ammonia explosion treatment, treatment conditions are carried out
Are as follows: ammonia volume 2.2g/g dry wood powder, dioctyl sodium sulfosuccinate dosage 0.01g/g dry wood powder, 110.0 DEG C of temperature,
Time 20.0min；
2. the processed Eucalyptus wood powder of above-mentioned steps 1 is carried out decompression explosion；
3. the processed Eucalyptus wood powder of above-mentioned steps 2 is carried out high shear extracting processing, with LiCl aqueous solution and ethyl alcohol
Mixed liquor is solvent, and required KOH and H is added2O2, treatment conditions are as follows: solvent forms LiCl content 20.0wt%, water content
30.0wt%, ethanol content 50.0wt%, solvent usage 8.0g/gDry wood powder, KOH dosage 0.35g/gDry wood powder, H2O2Dosage 0.03g/
gDry wood powder, 40 DEG C of temperature, high shear rates 17000rpm, decentralized processing time 110min；
4. being filtered the processed mixture of above-mentioned steps 3 to separate solid phase residue and liquid phase filtrate；
5. the isolated filtrate of above-mentioned steps 4 is adjusted to 5.5 with glacial acetic acid filtrate pH value, then centrifugal treating is carried out, is centrifuged
Treatment conditions are as follows: centrifugal rotational speed 4600rpm, centrifugation time 30min；
6. the filtrate that 5 centrifugal treating of above-mentioned steps is crossed is filtered, by filtration product at -20 DEG C pre-freeze 3h, then
It is freeze-dried under -50 DEG C and pressure 15MPa and obtains high-purity xylose for 24 hours；
7. the solid phase residue that above-mentioned steps 4 are separated by filtration carries out the enzymatic hydrolysis of cellulase, enzymatic hydrolysis condition are as follows: Eucalyptus solid phase
Sludge concentration 2.0%, pH value 4.8, temperature 50 C, cellulase dosage 16.0FPU/gSolid phase residue, β-glucosyl enzym dosage
24.0CBU/gSolid phase residue, dispersion revolving speed is 200rpm, handles time 12h；
8. above-mentioned steps 7 are obtained glucose hydrolysis liquid after cellulase and β-glucosyl enzym enzymatic hydrolysis.
As a result: by measurement, Eucalyptus xylose yield obtained by above-mentioned processing step is 72.9%, xylose purity 94.7%,
Glucose hydrolysis yield is 83.2%.14.0% is improved than conventional hydrothermal extraction method xylose yield.
Embodiment 2
Eucalyptus wood powder less than 40 mesh extracts xylose according to the following steps:
1. ammonium hydroxide and dioctyl sodium sulfosuccinate are mixed with Eucalyptus wood powder, ammonia explosion treatment, treatment conditions are carried out
Are as follows: ammonia volume 1.5g/gDry wood powder, dioctyl sodium sulfosuccinate dosage 0.02g/gDry wood powder, 125.0 DEG C of temperature, the time
25.0min；
2. the processed Eucalyptus wood powder of above-mentioned steps 1 is carried out decompression explosion；
3. the processed Eucalyptus wood powder of above-mentioned steps 2 is carried out high shear extracting processing, with LiCl aqueous solution and ethyl alcohol
Mixed liquor is solvent, and required KOH and H is added2O2, treatment conditions are as follows: solvent forms LiCl content 18.0wt%, water content
27.0wt%, ethanol content 55.0wt%, solvent usage 7.0g/gDry wood powder, KOH dosage 0.7g/gDry wood powder, H2O2Dosage 0.06g/
gDry wood powder, temperature 45 C, high shear rates 15000rpm, decentralized processing time 150min；
4. being filtered the processed mixture of above-mentioned steps 3 to separate solid phase residue and liquid phase filtrate；
5. the isolated filtrate of above-mentioned steps 4 is adjusted to 5.0 with glacial acetic acid filtrate pH value, then centrifugal treating is carried out, is centrifuged
Treatment conditions are as follows: centrifugal rotational speed 5000rpm, centrifugation time 24min；
6. the filtrate that 5 centrifugal treating of above-mentioned steps is crossed is filtered, by filtration product at -20 DEG C pre-freeze 3h, then
It is freeze-dried under -50 DEG C and pressure 15MPa and obtains high-purity xylose for 24 hours；
7. the solid phase residue that above-mentioned steps 4 are separated by filtration carries out the enzymatic hydrolysis of cellulase, enzymatic hydrolysis condition are as follows: Eucalyptus solid phase
Sludge concentration 2.0%, pH value 4.8, temperature 50 C, cellulase dosage 16.0FPU/gSolid phase residue, β-glucosyl enzym dosage
24.0CBU/gSolid phase residue, dispersion revolving speed is 200rpm, handles time 12h；
8. above-mentioned steps 7 are obtained glucose hydrolysis liquid after cellulase and β-glucosyl enzym enzymatic hydrolysis.
As a result: by measurement, Eucalyptus xylose yield obtained by above-mentioned processing step is 73.1%, xylose purity 93.9%,
Glucose hydrolysis yield is 83.0%.14.2% is improved than conventional hydrothermal extraction method xylose yield.
Embodiment 3
Eucalyptus wood powder less than 40 mesh extracts xylose according to the following steps:
1. ammonium hydroxide and dioctyl sodium sulfosuccinate are mixed with Eucalyptus wood powder, ammonia explosion treatment, treatment conditions are carried out
Are as follows: ammonia volume 3.0g/gDry wood powder, dioctyl sodium sulfosuccinate dosage 0.03g/gDry wood powder, 135.0 DEG C of temperature, the time
45.0min；
2. the processed Eucalyptus wood powder of above-mentioned steps 1 is carried out decompression explosion；
3. the processed Eucalyptus wood powder of above-mentioned steps 2 is carried out high shear extracting processing, with LiCl aqueous solution and ethyl alcohol
Mixed liquor is solvent, and required KOH and H is added2O2, treatment conditions are as follows: solvent forms LiCl content 27.0wt%, water content
53.0wt%, ethanol content 20.0wt%, solvent usage 6.2g/gDry wood powder, KOH dosage 0.55g/gDry wood powder, H2O2Dosage 0.05g/
gDry wood powder, temperature 60 C, high shear rates 18000rpm, decentralized processing time 130min；
4. being filtered the processed mixture of above-mentioned steps 3 to separate solid phase residue and liquid phase filtrate；
5. the isolated filtrate of above-mentioned steps 4 is adjusted to 4.9 with glacial acetic acid filtrate pH value, then centrifugal treating is carried out, is centrifuged
Treatment conditions are as follows: centrifugal rotational speed 4000rpm, centrifugation time 20min；
6. the filtrate that 5 centrifugal treating of above-mentioned steps is crossed is filtered, by filtration product at -20 DEG C pre-freeze 3h, then
It is freeze-dried under -50 DEG C and pressure 15MPa and obtains high-purity xylose for 24 hours；
7. the solid phase residue that above-mentioned steps 4 are separated by filtration carries out the enzymatic hydrolysis of cellulase, enzymatic hydrolysis condition are as follows: Eucalyptus solid phase
Sludge concentration 2.0%, pH value 4.8, temperature 50 C, cellulase dosage 16.0FPU/gSolid phase residue, β-glucosyl enzym dosage
24.0CBU/gSolid phase residue, dispersion revolving speed is 200rpm, handles time 12h；
8. above-mentioned steps 7 are obtained glucose hydrolysis liquid after cellulase and β-glucosyl enzym enzymatic hydrolysis.
As a result: by measurement, Eucalyptus xylose yield obtained by above-mentioned processing step is 71.8%, xylose purity 93.7%,
Glucose hydrolysis yield is 82.6%.12.9% is improved than conventional hydrothermal extraction method xylose yield.
Embodiment 4
Eucalyptus wood powder less than 40 mesh extracts xylose according to the following steps:
1. ammonium hydroxide and dioctyl sodium sulfosuccinate are mixed with Eucalyptus wood powder, ammonia explosion treatment, treatment conditions are carried out
Are as follows: ammonia volume 1.8g/gDry wood powder, dioctyl sodium sulfosuccinate dosage 0.02g/gDry wood powder, 105.0 DEG C of temperature, the time
35.0min；
2. the processed Eucalyptus wood powder of above-mentioned steps 1 is carried out decompression explosion；
3. the processed Eucalyptus wood powder of above-mentioned steps 2 is carried out high shear extracting processing, with LiCl aqueous solution and ethyl alcohol
Mixed liquor is solvent, and required KOH and H is added2O2, treatment conditions are as follows: solvent forms LiCl content 25.0wt%, water content
40.0wt%, ethanol content 35.0wt%, solvent usage 5.5g/gDry wood powder, KOH dosage 0.85g/gDry wood powder, H2O2Dosage 0.04g/
gDry wood powder, 55 DEG C of temperature, high shear rates 20000rpm, decentralized processing time 90min；
4. being filtered the processed mixture of above-mentioned steps 3 to separate solid phase residue and liquid phase filtrate；
5. the isolated filtrate of above-mentioned steps 4 is adjusted to 4.5 with glacial acetic acid filtrate pH value, then centrifugal treating is carried out, is centrifuged
Treatment conditions are as follows: centrifugal rotational speed 4500rpm, centrifugation time 28min；
6. the filtrate that 5 centrifugal treating of above-mentioned steps is crossed is filtered, by filtration product at -20 DEG C pre-freeze 3h, then
It is freeze-dried under -50 DEG C and pressure 15MPa and obtains high-purity xylose for 24 hours；
7. the solid phase residue that above-mentioned steps 4 are separated by filtration carries out the enzymatic hydrolysis of cellulase, enzymatic hydrolysis condition are as follows: Eucalyptus solid phase
Sludge concentration 2.0%, pH value 4.8, temperature 50 C, cellulase dosage 16.0FPU/gSolid phase residue, β-glucosyl enzym dosage
24.0CBU/gSolid phase residue, dispersion revolving speed is 200rpm, handles time 12h；
8. above-mentioned steps 7 are obtained glucose hydrolysis liquid after cellulase and β-glucosyl enzym enzymatic hydrolysis.
As a result: by measurement, Eucalyptus xylose yield obtained by above-mentioned processing step is 71.9%, xylose purity 95.4%,
Glucose hydrolysis yield is 85.4%.13.0% is improved than conventional hydrothermal extraction method xylose yield.
The present invention during the test, different surfaces activating agent is used in ammonia explosion treatment and is cut in chemical height
The investigation of technical effect, test result discovery, different chemical reagent groups are carried out when cutting decentralized processing using different solvents
Close the structure stubbornly resisting property to the Eucalyptus Fibers after the recovery rate and purity and separating xylose of the Eucalyptus xylose being finally prepared
With significant difference, be only illustrated by taking comparative example 1 and 2 as an example, but be not limited only to during experimental study it is following right
Ratio.
Comparative example 1
Eucalyptus wood powder less than 40 mesh extracts xylose according to the following steps:
1. ammonium hydroxide and fatty alcohol polyoxyethylene ether are mixed with Eucalyptus wood powder, ammonia explosion treatment, treatment conditions are carried out are as follows:
Ammonia volume 2.5g/gDry wood powder, fatty alcohol polyoxyethylene ether dosage 0.03g/gDry wood powder, 100.0 DEG C of temperature, time 30.0min；
2. the processed wood powder of above-mentioned steps 1 is carried out decompression explosion；
3. the processed wood powder of above-mentioned steps 2 is carried out high shear extracting processing, with the mixing of LiCl aqueous solution and ethyl alcohol
Liquid is solvent, and required KOH and H is added2O2, treatment conditions are as follows: solvent forms LiCl content 22.0wt%, water content
40.0wt%, ethanol content 38.0wt%, solvent usage 5.0g/gDry wood powder, KOH dosage 0.8g/gDry wood powder, H2O2Dosage 0.02g/
gDry wood powder, temperature 45 C, high shear rates 15000rpm, decentralized processing time 150min；
4. being filtered the processed mixture of above-mentioned steps 3 to separate solid phase residue and liquid phase filtrate；
5. the isolated filtrate of above-mentioned steps 4 is adjusted to 5.0 with glacial acetic acid filtrate pH value, then centrifugal treating is carried out, is centrifuged
Treatment conditions are as follows: centrifugal rotational speed 4800rpm, centrifugation time 28min；
6. the filtrate that 5 centrifugal treating of above-mentioned steps is crossed is filtered, filtration product is carried out in -20 DEG C of pre-freeze 3h, so
It is freeze-dried afterwards in -50 DEG C, pressure 15MPa and obtains high-purity xylose for 24 hours；
7. the solid phase residue that above-mentioned steps 4 are separated by filtration carries out the enzymatic hydrolysis of cellulase, enzymatic hydrolysis condition are as follows: Eucalyptus solid phase
Sludge concentration 2.0%, pH value 4.8, temperature 50 C, cellulase dosage 16.0FPU/gSolid phase residue, β-glucosyl enzym dosage
24.0CBU/gSolid phase residue, dispersion revolving speed is 200rpm, handles time 12h；
8. obtaining glucose hydrolysis liquid by above-mentioned steps 7 after cellulase hydrolysis.
As a result: by measurement, Eucalyptus xylose yield obtained by above-mentioned processing step is 54.7%, xylose purity 88.6%,
Glucose hydrolysis yield is 75.2%.
Comparative example 2
Eucalyptus wood powder less than 40 mesh extracts xylose according to the following steps:
1. ammonium hydroxide and dioctyl sodium sulfosuccinate are mixed with Eucalyptus wood powder, ammonia explosion treatment, treatment conditions are carried out
Are as follows: ammonia volume 2.5g/gDry wood powder, dioctyl sodium sulfosuccinate dosage 0.03g/gDry wood powder, 100.0 DEG C of temperature, the time
30.0min；
2. the processed wood powder of above-mentioned steps 1 is carried out decompression explosion；
3. the processed wood powder of above-mentioned steps 2 is carried out high shear extracting processing, takes water as a solvent, required KOH is added
And H2O2, treatment conditions are as follows: solvent usage 5.0g/gDry wood powder, KOH dosage 0.8g/gDry wood powder, H2O2Dosage 0.02g/gDry wood powder, temperature
45 DEG C, high shear rates 15000rpm of degree, decentralized processing time 150min；
4. being filtered the processed mixture of above-mentioned steps 3 to separate solid phase residue and liquid phase filtrate；
5. the isolated filtrate of above-mentioned steps 4 is adjusted to 5.0 with glacial acetic acid filtrate pH value, then centrifugal treating is carried out, is centrifuged
Treatment conditions are as follows: centrifugal rotational speed 4800rpm, centrifugation time 28min；
6. the filtrate that 5 centrifugal treating of above-mentioned steps is crossed is filtered, filtration product is carried out in -20 DEG C of pre-freeze 3h, so
It is freeze-dried afterwards in -50 DEG C, pressure 15MPa and obtains high-purity xylose for 24 hours；
7. the solid phase residue that above-mentioned steps 4 are separated by filtration carries out the enzymatic hydrolysis of cellulase, enzymatic hydrolysis condition are as follows: Eucalyptus solid phase
Sludge concentration 2.0%, pH value 4.8, temperature 50 C, cellulase dosage 16.0FPU/gSolid phase residue, β-glucosyl enzym dosage
24.0CBU/gSolid phase residue, dispersion revolving speed is 200rpm, handles time 12h；
8. obtaining glucose hydrolysis liquid by above-mentioned steps 7 after cellulase hydrolysis.
As a result: by measurement, Eucalyptus xylose yield obtained by above-mentioned processing step is 51.5%, xylose purity 89.1%,
Glucose hydrolysis yield is 72.9%.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of highly effective extraction method of Eucalyptus xylose, characterized in that the following steps are included:
Ammonium hydroxide and dioctyl sodium sulfosuccinate are mixed with Eucalyptus wood powder, decompression explosion is carried out under setting condition, then with
The mixed liquor of LiCl aqueous solution and ethyl alcohol is solvent, and KOH and H is added2O2High shear separating treatment is carried out, is filtered after separating treatment
Solid phase residue is removed, filtrate pH value is adjusted, then carry out centrifugal treating, is then filtered, finally freezes filtration product
It is dry to obtain high-purity xylose.
2. the method as described in claim 1, it is characterized in that: Eucalyptus wood powder is the wood powder less than 40 mesh.
3. the method as described in claim 1, it is characterized in that: the condition of ammonium hydroxide explosion treatment Eucalyptus wood powder are as follows: ammonia volume
1.5-3.0g/gDry wood powder, dioctyl sodium sulfosuccinate dosage 0.01-0.03g/gDry wood powder, 105.0-135.0 DEG C of temperature, the time
20.0-45.0min。
4. the method as described in claim 1, it is characterized in that: the solvent group becomes: LiCl content is 18.0-27.0wt%,
Water content is 27.0-53.0wt%, ethanol content 20.0-55.0wt%.
5. the method as described in claim 1, it is characterized in that: high shear separating treatment condition are as follows: solvent usage 5.0-8.0g/
gDry wood powder, KOH dosage is 0.35-0.85g/gDry wood powder, H2O2Dosage is 0.03-0.06g/gDry wood powder, 40-60 DEG C of temperature, high shear
Revolving speed 15000-20000rpm, decentralized processing time 90-150min.
6. the method as described in claim 1, it is characterized in that: adjusting filtrate pH to 4.5-5.5 using glacial acetic acid.
7. the method as described in claim 1, it is characterized in that: filtration product is in -20~-15 DEG C of 2~3h of pre-freeze, then -50
~-40 DEG C, 15~20MPa of pressure carry out freeze-drying 20~for 24 hours.
8. the method as described in claim 1, it is characterized in that: condition of the Eucalyptus solid phase residue for enzyme hydrolysis production glucose
Are as follows: Eucalyptus solid phase sludge concentration 2.0~2.5%, pH value 4.8~5,50~55 DEG C of temperature, cellulase dosage 16.0~
18FPU/gSolid phase residue, 20~24.0CBU/g of β-glucosyl enzym dosageSolid phase residue, dispersion revolving speed is 150~200rpm, handles the time 10
~12h.
9. a kind of method of efficient coproduction Eucalyptus xylose and glucose, characterized in that the following steps are included:
Ammonium hydroxide and dioctyl sodium sulfosuccinate are mixed with Eucalyptus wood powder, decompression explosion is carried out under setting condition, then with
The mixed liquor of LiCl aqueous solution and ethyl alcohol is solvent, and KOH and H is added2O2High shear separating treatment is carried out, is filtered after separating treatment
Solid phase residue is removed, filtrate pH value is adjusted, then carry out centrifugal treating, is then filtered, finally freezes filtration product
It is dry to obtain high-purity xylose；
Wherein the solid phase residue produces glucose, condition for enzyme hydrolysis are as follows: Eucalyptus solid phase sludge concentration 2.0~2.5%,
PH value 4.8~5,50~55 DEG C of temperature, 16.0~18FPU/g of cellulase dosageSolid phase residue, β-glucosyl enzym dosage 20~
24.0CBU/gSolid phase residue, dispersion revolving speed is 150~200rpm, handles 10~12h of time.
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