CN108456263A - A kind of method of quick separating extraction hemicellulose - Google Patents
A kind of method of quick separating extraction hemicellulose Download PDFInfo
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- CN108456263A CN108456263A CN201711484630.0A CN201711484630A CN108456263A CN 108456263 A CN108456263 A CN 108456263A CN 201711484630 A CN201711484630 A CN 201711484630A CN 108456263 A CN108456263 A CN 108456263A
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- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
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Abstract
The present invention provides a kind of methods that quick separating extracts hemicellulose, include the following steps：(1) preparation of degreasing raw material：Degreasing is stripped to plant fiber material and is obtained degreasing raw material with benzene and ethyl alcohol or the mixed solvent of toluene and ethyl alcohol；(2) the extraction separation of hemicellulose：The aqueous slkali of mass fraction 3~10% is added in degreasing raw material, stop being ultrasonically treated after being ultrasonically treated 20~60min in ultrasonic reactor at room temperature, continue to be stirred to react, obtain hemicellulose extract, separation, gained filtrate is adjusted with acid pH to 5.5~7.0, is then precipitated with ethanol solution, isolated hemicellulose precipitation；(3) purifying of hemicellulose：Hemicellulose is precipitated into dialysis soluble in water, is dried to obtain hemicellulose.The beneficial effects of the invention are as follows simple for process, easy to operate, time-consuming short, the good separating effects of separation.
Description
Technical field
The invention belongs to agricultural-forestry biomass comprehensive utilization of resources fields, and hemicellulose is extracted more particularly, to a kind of quick separating
The method of element.
Background technology
China's agricultural-forestry biomass is resourceful, increasingly prominent with environmental pollution and energy crisis, with agricultural-forestry biomass
The energy, material and the chemicals of conversion have become research hotspot.Agricultural-forestry biomass cell wall is mainly by cellulose, hemicellulose
It is formed with lignin.Agricultural-forestry biomass is converted and (need not be detached to biomass components) using mostly direct at present,
So that biomass conversion is chronically at the utilization state of one-component, such as traditional pulp and paper industry mainly utilizes cellulose,
Most of lignin and the concentrated after-combustion of hemicellulose, however the fuel value of hemicellulose is low, causes the significant wastage of resource
With the serious pollution of environment.Therefore, agricultural-forestry biomass each component is first detached into again high-valued conversion, to realize that biomass is complete
Component converts, and available resource maximally utilizes.
The inhomogenous complex plycan that hemicellulose is made of a variety of glycosyls, content account for about the three of agricultural-forestry biomass total amount
/ mono-, can be widely used in the industrial productions such as chemistry, papermaking, food, pharmacy, such as produce surfactant, paper additive,
Foodstuff glue, thickener, functional oligose etc..However, the complexity of hemicellulose structure is various to limit its application.Hemicellulose
Biogenesis it is different, structure is different, the knot of variety classes biomass such as leaf wood, needlebush and grass hemicellulose
Structure is different, and the content and component of hemicellulose are different.Hemicellulose by hydrogen bond and Van der Waals force closely with cellulose fento
Silk crosslinking forms carbohydrate complex by phenolic acid etc. and lignin, while with protein there is also connecting, in cell wall
Three-dimensional net structure is formed in matrix, this network structure seriously restricts hemicellulose from the complete separation in cell wall.
The separation method of hemicellulose has caustic extraction method, alkaline hydrogen peroxide extraction process, method of organic solvent extraction, hydro-thermal
Method, steam explosion, mechanochemistry extraction process etc..Wherein, aqueous slkali has swollen cellulose, makes between cellulose and hemicellulose
The effect for being broken and destroying hemicellulose and chemistry of lignin's key occurs for hydrogen bond, to make hemicellulose dissolve from cell wall
Come, therefore, the separation of caustic extraction method is the most commonly used.It is usually detached from agricultural-forestry biomass with caustic extraction method and is adopted hemicellulose more
With two-step method or multistep processes, i.e., the removing of lignin is first carried out to prepare holocellulose, is then taken out from holocellulose with lye
Hemicellulose is carried, this method extraction times are longer.With going deep into for research, it is aided with ultrasound during alkaline process detaches hemicellulose
Wave processing, extraction times shorten, however in traditional ultrasonic wave auxiliary lye method for extracting, Sonication assisted treatment is with entire
Separation process causes separating obtained hemicellulose molecule amount relatively low, limits the further conversion of hemicellulose to a certain extent.
Invention content
In view of this, the present invention is directed to propose a kind of quick separating extraction hemicellulose method, to solve hemicellulose
The technical problems such as low separation efficiency, complex process, time-consuming for separation, and the hemicellulose molecule amount after separation is little.
In order to achieve the above objectives, the technical proposal of the invention is realized in this way：
A kind of method of quick separating extraction hemicellulose, includes the following steps：
(1) preparation of degreasing raw material：Plant fiber material is carried out with the mixed solvent of ethyl alcohol or toluene and ethyl alcohol with benzene
Extracting degreasing obtains degreasing raw material；
(2) the extraction separation of hemicellulose：The aqueous slkali of mass fraction 3~10% is added in degreasing raw material, room temperature
Under in ultrasonic reactor be ultrasonically treated 20~60min after stop be ultrasonically treated, continue to be stirred to react, obtain hemicellulose
Extracting solution, separation, gained filtrate are adjusted with acid pH to 5.5~7.0, are then precipitated with ethanol solution, isolated half fiber
Dimension element precipitation；
(3) purifying of hemicellulose：Hemicellulose is precipitated into dialysis soluble in water, is dried to obtain hemicellulose.
Further, the plant fiber material in the step (1) is any one in leaf wood or grass
Or two kinds.
Further, plant fiber material is crushed to 20~100 mesh in the step (1), extraction times are 6~12h.
Further, benzene and ethyl alcohol or toluene and ethyl alcohol volume ratio 2 in the step (1)：1.
Further, aqueous slkali is NaOH solution or KOH solution, the ratio of degreasing raw material and aqueous slkali in the step (2)
Example is 1g：10~30ml.
Further, the frequency of ultrasonic reactor is 19~30kHz in the step (2), and the power of ultrasonic reactor is
180~1000W.
Further, the time being stirred to react in the step (2) is 2~4h；It is described to be separated into centrifugation or filtering
Separation.
Further, acid is hydrochloric acid or acetic acid in the step (2)；It is precipitated as filtrate adding to second with ethanol solution
It is added in filtrate in alcoholic solution or by ethanol solution.
Further, the bag filter or film that molecular cut off is 2000~5000Da when dialysis in the step (3) into
Row dialysis.
Further, dry in the step (3) to use freeze-drying or vacuum drying；The temperature of the freeze-drying
It it is -40~-60 DEG C, vacuum degree is 200~500mba, 12~48h of time；The vacuum drying temperature is 30~50 DEG C, very
Reciprocal of duty cycle is 0.5~1.5MPa, 12~48h of time.
Compared with the existing technology, the method for quick separating extraction hemicellulose of the present invention has the advantage that：
(1) for hemicellulose extraction separation method provided by the invention compared with general extraction methods, traditional ultrasonic wave is auxiliary
It helps in caustic extraction method, mostly using holocellulose as initial reactant, and concentration of lye used is higher, extraction temperature is higher, takes out
It carries and takes longer, and Sonication assisted treatment causes separating obtained hemicellulose molecule amount relatively low with entire separation process, one
Determine to limit the further conversion of hemicellulose in degree.Present invention process is simple, easy to operate, is only stirred at room temperature i.e.
Can, separation takes that short and total disengaging time is short, and consume energy low, good separating effect, gained hemicellulose purity is higher, molecular weight compared with
Greatly；The pretreatment that raw material is carried out using ultrasonic wave auxiliary law, the cavitation effect generated when being propagated in liquid medium using ultrasonic wave
It answers, cavitation blistering generates localized hyperthermia's high pressure and shock wave etc. when collapsing brokenly, within a short period of time so that mechanical effect, fuel factor
With chemical effect collective effect in agricultural-forestry biomass raw material.
(2) present invention uses leaf wood and grass for raw material, simple for process without the removing of lignin.
Specific implementation mode
The embodiment of the present invention proposes a kind of method of quick separating extraction hemicellulose, includes the following steps：
(1) preparation of degreasing raw material：Plant fiber material is carried out with the mixed solvent of ethyl alcohol or toluene and ethyl alcohol with benzene
Extracting degreasing obtains degreasing raw material；
(2) the extraction separation of hemicellulose：The aqueous slkali of mass fraction 3~10% is added in degreasing raw material, room temperature
Under in ultrasonic reactor be ultrasonically treated 20~60min after stop be ultrasonically treated, continue to be stirred to react, obtain hemicellulose
Extracting solution, separation, gained filtrate are adjusted with acid pH to 5.5~7.0, are then precipitated with ethanol solution, isolated half fiber
Dimension element precipitation；
(3) purifying of hemicellulose：Hemicellulose is precipitated into dialysis soluble in water, is dried to obtain hemicellulose.
The prior art is aided with ultrasonication during generally using alkaline process separation hemicellulose, and at ultrasonic wave auxiliary
Reason with entire separation process, the method mostly using holocellulose as initial reactant, concentration of lye used is higher, extraction temperature compared with
Height, extracting take longer, cause separating obtained hemicellulose molecule amount relatively low, limit to a certain extent hemicellulose into one
Step conversion.
The embodiment of the present invention proposes a kind of method of quick separating extraction hemicellulose, simple for process, easy to operate, only
It is stirred at room temperature, detaches and take short, good separating effect.The pretreatment that raw material is carried out using ultrasonic wave auxiliary law, in conjunction with
The degreasing of raw material and lye extraction, the cavitation effect generated when being propagated in liquid medium using ultrasonic wave, cavitation blistering are being collapsed
Localized hyperthermia's high pressure and shock wave etc. are generated when broken, within a short period of time so that mechanical effect, fuel factor and chemical effect are common
Act on agricultural-forestry biomass raw material.Without first removing lignin as prior art, applied without in entire extraction process
Add ultrasound, and can fully extract hemicellulose by being stirred to react at normal temperatures.
In addition, the hemicellulose that method is extracted through the embodiment of the present invention, molecular weight is larger, shortens the later separation time
And improve separating effect.
In an embodiment of the present invention, the plant fiber material in the step (1) is in leaf wood or grass
Any one or two kinds, wherein leaf wood can be poplar, Eucalyptus etc., and grass can be bagasse, corncob or bamboo
Material etc..
The embodiment of the present invention proposes a kind of method of quick separating extraction hemicellulose, is planted using leaf wood or grass family
Any one or two kinds in object simplify technique for raw material without the removing of lignin.Due to different types of biomass half
The structure of cellulose is different, and the content and component of hemicellulose are different, and height is separated and extracted from complicated cell wall structure
Purity, high molecular weight hemicellulose become the key of hemicellulose and biomass full constituent trans-utilization.
Specifically, the step (1) is that plant fiber material is crushed to 20~100 mesh, extraction times are 6~12h.
Specifically, benzene and ethyl alcohol or toluene and ethyl alcohol volume ratio 2 in the step (1)：1.
Specifically, aqueous slkali can be NaOH solution or KOH solution in the step (2).The wherein quality of aqueous slkali
Score is 3~10%.
Hemicellulose extraction separation method provided in an embodiment of the present invention uses aqueous slkali to degreasing raw material in room temperature first
Under the conditions of carry out ultrasonic pretreatment, then stop be ultrasonically treated, continue to be stirred to react certain time, to gained aqueous slkali carry out
Filtering is adjusted pH value, is precipitated with ethanol solution, and hemicellulose is dried to obtain after dialysis.The method of the present invention is simple for process, easy
Operation, alkali concentration used is low, separative efficiency is high, and gained hemicellulose molecule amount is big, is substantially shorter traditional hemicellulose separation
Time, improve efficiency, the production of double cellulose and structural research are significant.
Specifically, the ratio of degreasing raw material and aqueous slkali is 1g in the step (2)：10~30ml.
Specifically, the frequency of ultrasonic reactor is 19~30kHz in the step (2), the power of ultrasonic reactor is
180~1000W.The time of ultrasonic reaction is 20~60min.
The present invention carries out the pretreatment of raw material using ultrasonic wave auxiliary law, in conjunction with the ungrease treatment of raw material, in the short period
It is interior so that mechanical effect, fuel factor and chemical effect collective effect are in agricultural-forestry biomass raw material, the reaction was continued at ambient temperature
For a period of time, you can obtain hemicellulose.It is simple for process, easy to operate, separation take it is short, total disengaging time is also short, energy consumption it is low,
Without picture, Sonication assisted treatment causes disengaging time long with entire separation process in the prior art, and high energy consumption causes to detach
Gained hemicellulose molecule amount is relatively low, limits the further conversion of hemicellulose to a certain extent.
Specifically, the time being stirred to react in the step (2) is 2~4h.
Specifically, magnetic agitation or mechanical agitation may be used in stirring in the step (2).
In an embodiment of the present invention, acid is hydrochloric acid or acetic acid in the step (2).
In still another embodiment of the process, it is precipitated as filtrate adding to ethyl alcohol with ethanol solution in the step (2)
It is added in filtrate in solution or by ethanol solution.
In still another embodiment of the process, it is separated into centrifugation described in the step (2) or is separated by filtration.
In still another embodiment of the process, the volume fraction of ethanol solution described in the step (2) is 95% or anhydrous
Ethyl alcohol.
In an embodiment of the present invention, molecular cut off is the saturating of 2000~5000Da when dialysis in the step (3)
Analysis bag or film are dialysed.
A kind of method of quick separating extraction hemicellulose provided by the invention, easy to operate, separation take short, separation effect
Fruit is good, can get that purity is higher, the larger hemicellulose product of molecular weight.
In still another embodiment of the process, freeze-drying or vacuum drying may be used in drying in the step (3).
Specifically, dry using freeze-drying in the step (3), the temperature of freeze-drying is -40~-60 DEG C, very
Reciprocal of duty cycle is 200~500mba, 12~48h of time.
Specifically, dry using vacuum drying in the step (3), the vacuum drying temperature is 30~50 DEG C,
Vacuum degree is 0.5~1.5MPa, 12~48h of time.
Embodiment 1
A kind of method of quick separating extraction hemicellulose of the present embodiment, includes the following steps：
(1) extraction of degreasing raw material：
By 20~80 mesh poplar raw materials with toluene-ethano (2:1, v/v) flow back 8h in solution Soxhlet extractor, is obtained after dry
To the poplar raw material of degreasing.
(2) hemicellulose extraction separation：
The poplar raw material 40g for weighing degreasing is molten in the sodium hydroxide that 800ml mass fractions are 8% in reaction unit, is added
Liquid opens ultrasonic reactor, its power 360W, supersonic frequency 20kHz is arranged, and carries out hemicellulose and extracts 40min, closes ultrasound
Reactor；Reaction unit is removed into ultrasonic reactor, at ambient temperature with magnetic agitation the reaction was continued 3h, obtains hemicellulose
Extracting solution；
Hemicellulose extract is filtered, after filtrate 6M salt acid for adjusting pH to 5.8, carries out rotary evaporation to be concentrated into one
Determine volume, 95% ethanol solution that 3 times of volumes are added is precipitated, and after standing 3~4h at room temperature, is centrifuged at 4000r/min,
Obtain hemicellulose precipitation.
(3) hemicellulose purifies：
A small amount of deionized water is added in gained hemicellulose precipitation, is fitted into the bag filter that molecular cut off is 4000Da thoroughly
96h is analysed, hemicellulose after purification is obtained using freeze-drying after concentration, the temperature of freeze-drying is -40 DEG C, and vacuum degree is
200mba, time 36h.
Embodiment 2
A kind of method of quick separating extraction hemicellulose of the present embodiment, includes the following steps：
(1) extraction of degreasing raw material：
By 40~60 mesh Bagasse Materials with toluene-ethano (2:1, v/v) solution flows back 8h in Soxhlet extractor, after dry
Obtain the Bagasse Material of degreasing.
(2) hemicellulose extraction separation：
Degreasing Bagasse Material 30g is weighed in reaction unit, the potassium hydroxide solution that 600ml mass fractions are 5% is added,
Ultrasonic reactor is opened, its power 180W, supersonic frequency 21kHz are set, hemicellulose is carried out and extracts 20min, it is anti-to close ultrasound
Answer device；Reaction unit is removed into ultrasonic reactor, at ambient temperature with magnetic agitation the reaction was continued 3.5h, obtains hemicellulose
Extracting solution；
Hemicellulose extract is filtered, after filtrate adjusts pH to 5.5 with glacial acetic acid, carries out rotary evaporation to be concentrated into one
Determine volume, precipitated with 95% ethanol solution of 3 times of volumes, after standing 4~6h at room temperature, centrifuges, obtain at 3000r/min
It is precipitated to hemicellulose.
(3) hemicellulose purifies：
A small amount of water is added in gained hemicellulose precipitation, is fitted into the bag filter that molecular cut off is 3500Da the 72h that dialyses,
Hemicellulose after purification is obtained using freeze-drying after concentration, the temperature of freeze-drying is -40 DEG C, vacuum degree 200mba,
Time 36h.
Embodiment 3
A kind of method of quick separating extraction hemicellulose of the present embodiment, includes the following steps：
(1) extraction of degreasing raw material：
By 40~60 mesh bamboo materials with toluene-ethano (2:1, v/v) solution flows back 8h in Soxhlet extractor, after dry
Obtain the bamboo material of degreasing.
(2) hemicellulose extraction separation：
The bamboo material 20g for weighing degreasing is molten in the potassium hydroxide that 400ml mass fractions are 5% in reaction unit, is added
Liquid opens ultrasonic reactor, its power 180W, supersonic frequency 21kHz is arranged, and carries out hemicellulose and extracts 30min, closes ultrasound
Reactor；Reaction unit is removed into ultrasonic reactor, at ambient temperature with magnetic agitation the reaction was continued 3.5h, obtains hemicellulose
Plain extracting solution；
Hemicellulose extract is filtered, after filtrate adjusts pH to 5.5 with glacial acetic acid, carries out rotary evaporation to be concentrated into one
Determine volume, precipitated with 95% ethanol solution of 3 times of volumes, after standing 6h at room temperature, centrifuges, obtain at 3000r/min
Hemicellulose precipitates.
(3) hemicellulose purifies：
A small amount of water is added in gained hemicellulose precipitation, is fitted into the bag filter that molecular cut off is 3500Da the 72h that dialyses
Afterwards, freeze-drying temperature is used to obtain hemicellulose after purification for -40 DEG C, vacuum degree 200mba, time 36h after concentration.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (10)
1. a kind of method of quick separating extraction hemicellulose, which is characterized in that include the following steps：
(1) preparation of degreasing raw material：Plant fiber material is stripped with the mixed solvent of benzene and ethyl alcohol or toluene and ethyl alcohol
Degreasing obtains degreasing raw material；
(2) the extraction separation of hemicellulose：The aqueous slkali of mass fraction 3~10% is added in degreasing raw material, is existed at room temperature
Stop being ultrasonically treated after being ultrasonically treated 20~60min in ultrasonic reactor, continue to be stirred to react, obtains hemicellulose extraction
Liquid, separation, gained filtrate are adjusted with acid pH to 5.5~7.0, are then precipitated with ethanol solution, isolated hemicellulose
Precipitation；
(3) purifying of hemicellulose：Hemicellulose is precipitated into dialysis soluble in water, is dried to obtain hemicellulose.
2. the method for quick separating extraction hemicellulose according to claim 1, it is characterised in that：In the step (1)
Plant fiber material be any one or two kinds in leaf wood or grass.
3. the method for quick separating extraction hemicellulose according to claim 1, it is characterised in that：In the step (1)
Plant fiber material is crushed to 20~100 mesh, extraction times are 6~12h.
4. the method for quick separating extraction hemicellulose according to claim 1, it is characterised in that：In the step (1)
Benzene and ethyl alcohol or toluene and ethyl alcohol volume ratio 2：1.
5. the method for quick separating extraction hemicellulose according to claim 1, it is characterised in that：In the step (2)
Aqueous slkali is NaOH solution or KOH solution, and the ratio of degreasing raw material and aqueous slkali is 1g：10~30ml.
6. the method for quick separating extraction hemicellulose according to claim 1, it is characterised in that：In the step (2)
The frequency of ultrasonic reactor is 19~30kHz, and the power of ultrasonic reactor is 180~1000W.
7. the method for quick separating extraction hemicellulose according to claim 1, it is characterised in that：In the step (2)
The time being stirred to react is 2~4h；It is described to be separated into centrifugation or be separated by filtration.
8. the method for quick separating extraction hemicellulose according to claim 1, it is characterised in that：In the step (2)
Acid is hydrochloric acid or acetic acid；It is precipitated as adding to filtrate in ethanol solution with ethanol solution or ethanol solution is added into filtrate
In.
9. the method for quick separating extraction hemicellulose according to claim 1, it is characterised in that：In the step (3)
It is dialysed with the bag filter or film that molecular cut off is 2000~5000Da when dialysis.
10. the method for quick separating extraction hemicellulose according to claim 1, it is characterised in that：In the step (3)
It is dry to use freeze-drying or vacuum drying；The temperature of the freeze-drying be -40~-60 DEG C, vacuum degree be 200~
500mba, 12~48h of time；The vacuum drying temperature be 30~50 DEG C, vacuum degree be 0.5~1.5MPa, the time 12~
48h。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110669806A (en) * | 2019-09-29 | 2020-01-10 | 北京林业大学 | Synergistic pretreatment method for improving tobacco stalk hemicellulose yield and cellulose enzymolysis rate |
| 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 |
| CN112250775A (en) * | 2020-10-28 | 2021-01-22 | 西南民族大学 | Extraction equipment and extraction method for extracting hemicellulose from straws |
| CN115725006A (en) * | 2022-11-28 | 2023-03-03 | 昆明理工大学 | Method for extracting hemicellulose from coffee shells by virtue of ultrasonic-microwave synergy |
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| CN101792495A (en) * | 2010-02-11 | 2010-08-04 | 浙江理工大学 | Method for ultrasonically catalyzing and extracting hemicellulose, cellulose and lignin from plant straws |
| CN102585039A (en) * | 2012-02-28 | 2012-07-18 | 昆明理工大学 | Extraction separation method of hemicellulose |
| CN106632735A (en) * | 2016-10-28 | 2017-05-10 | 河南华禹环保科技有限公司 | Extracting method for medium and low temperature hemicellulose |
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| CN101792495A (en) * | 2010-02-11 | 2010-08-04 | 浙江理工大学 | Method for ultrasonically catalyzing and extracting hemicellulose, cellulose and lignin from plant straws |
| CN102585039A (en) * | 2012-02-28 | 2012-07-18 | 昆明理工大学 | Extraction separation method of hemicellulose |
| CN106632735A (en) * | 2016-10-28 | 2017-05-10 | 河南华禹环保科技有限公司 | Extracting method for medium and low temperature hemicellulose |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110669806A (en) * | 2019-09-29 | 2020-01-10 | 北京林业大学 | Synergistic pretreatment method for improving tobacco stalk hemicellulose yield and cellulose enzymolysis rate |
| 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 |
| CN112250775A (en) * | 2020-10-28 | 2021-01-22 | 西南民族大学 | Extraction equipment and extraction method for extracting hemicellulose from straws |
| CN115725006A (en) * | 2022-11-28 | 2023-03-03 | 昆明理工大学 | Method for extracting hemicellulose from coffee shells by virtue of ultrasonic-microwave synergy |
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Application publication date: 20180828 |