CN105732846A - Straw pretreatment method for extracting hemicellulose - Google Patents
Straw pretreatment method for extracting hemicellulose Download PDFInfo
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- CN105732846A CN105732846A CN201610172806.8A CN201610172806A CN105732846A CN 105732846 A CN105732846 A CN 105732846A CN 201610172806 A CN201610172806 A CN 201610172806A CN 105732846 A CN105732846 A CN 105732846A
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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
- C08B37/14—Hemicellulose; Derivatives thereof
Abstract
The invention discloses a straw pretreatment method for extracting hemicellulose. The straw pretreatment method comprises the steps of soaking and wetting straws by virtue of pretreatment liquid, sending the obtained mixture into a pulping machine, pulping until the particle sizes of obtained materials are smaller than or equal to 1.0mm, carrying out solid-liquid separation on the obtained materials, collecting solids, washing the solids with water, and extracting the hemicelluloses by virtue of the solids, wherein the pretreatment liquid is an alkali solution with the concentration of 1g/L-20g/L. According to the straw pretreatment method, straw fiber is wetted and softened by virtue of alkali liquid with a relatively low concentration, and the pulping machine is utilized for pulping the wetted straws, so that the contact area between the fiber in the straws and the pretreatment liquid is greatly improved, impurities such as acetyl, pigments and the like in the straw fiber are beneficially removed, the content of impurities in the subsequent hemicellulose extraction liquid is decreased without losing hemicelluloses in the straws, the extraction rate of the hemicellulose is increased, and furthermore, the consumption of treatment power of the materials is low.
Description
Technical field
The present invention relates to the extraction of active component in straw, be specifically related to a kind of straw pretreatment method for extracting hemicellulose.
Background technology
Straw is by-product produced by mankind's grain and Sugar Production process, belong to human society and concentrate the Renewable resource utilized with most convenient most, the main component of straw is made up of cellulose, hemicellulose and lignin, cellulose is that glucose (hexose) is with β-1, the polymer of 4 glycosidic bond compositions, hemicellulose is that content is only second to the renewable polysaccharide of cellulosic one, the polysaccharide class being mainly main constituent with xylan (pentose, the polymer of xylose).Macromole state xylan and the difference on cellulosic structure make it have physicochemical property and the biological activity of uniqueness, are respectively provided with important Development volue in fields such as food, medicine and chemical industry.
Cellulose in straw, hemicellulose and lignin are as the principal structural component of plant cell wall, using cellulose as " skeleton ", hemicellulose and there is the lignin macromole of tridimensional network be wound around mutually and be filled between microfibre, and connect formation natural complex with the form of chemical bond, extract hemicellulose, these attachment structures, the method currently mainly having acid hydrolysis, steam explosion, enzyme hydrolysis and alkaline extraction must be destroyed.
Acid hydrolysis and steam explosion are the important means destroying straw natural structure, but are difficult to obtain macromole state xylan owing to hemicellulose sugar chain is prone to hydrolysis, and cellulose is also affected by impact and is difficult to use in pulping and paper-making after these methods process.Enzyme hydrolysis method can reach to destroy the purpose of straw structure by hydrolytic lignin, publication number is that the patent of invention of CN103556517A discloses and a kind of adopts laccase directly to mix with bagasse, the specificity lignin degrading under certain condition of enzymatic reaction is utilized not affect hemicellulose and cellulose, thus improving the effect of follow-up oxygen alkali pulping.But this method yet suffers from the shielding action of cellulose and hemicellulose, enzymolysis efficiency is not high.
Can effectively dissolved lignin and hemicellulose by the method for alkaline extraction, but often there is more waxiness in the epidermis at straw, this is also the obstacle extracting solution contacting material, publication number is the preprocess method that the patent of invention of CN103205473A discloses a kind of bagasse, specifically bagasse is dried, cross after pulverizing and take 18～40 mesh sieve fraction, then with NaOH and H2O2Mixed aqueous solution process.This method can effectively dissolution hemicellulose and lignin, but bagasse is dried and pulverizes, power consumption is more, industrially application uneconomical, and cellulose can not as pulping and paper-making raw material.
Therefore, select suitable straw processing method, stalk fibre tissue is fully broken up separation, increase substantially fiber surface area, do not destroy again cellulosic structure, ensureing the high extraction of follow-up hemicellulose, cellulose still may be used for pulping and paper-making, and this will be greatly improved the overall benefit of straw resource utilization.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of straw pretreatment method for extracting hemicellulose.Straw after infiltration is carried out defibrination by introducing fiberizer by the method; it is greatly improved in straw fiber and the contact area of pretreatment fluid; it is more beneficial for the acetyl group sloughing in hemicellulose, straw reduces while hemicellulose the impurity content in follow-up hemicellulose extract not losing and improves the extraction ratio of hemicellulose.
Straw pretreatment method for extracting hemicellulose of the present invention is: takes straw pretreatment fluid and soaks, gained mixture sends into defibrination in fiberizer, make after defibrination the particle diameter of gained material less than or equal to 1.0mm, and gained material is carried out solid-liquid separation, collect solid, extract for hemicellulose after washing；Described pretreatment fluid is concentration is the alkaline solution of 1～20g/L.
In the method for the invention, described straw is the stem outside gramineae crop seed, reality, leaf or fringe part.Concrete, it is possible to one or more the combination being chosen from Caulis et Folium Oryzae, straw, corn stalk, sorghum stalk, corn cob, bagasse and leaf of Caulis Sacchari sinensis.When being chosen as above-mentioned arbitrarily two or more combination of straw, the proportioning between them can be any proportioning.Described straw preferably carries out pretreatment again after break process, described break process can be that to make straw be thread or coarse-grained process, process as undertaken rubbing silk by wire kneading machine, carry out the broken process obtaining the relatively granule in coarse grain footpath by disintegrating machine, or carried out the conventional treatment mode that can realize crushing in the prior aries such as squeezing process by squeezer.Concrete, when straw is the elongated straws such as Caulis et Folium Oryzae, corn stalk or leaf of Caulis Sacchari sinensis, available cutting machine is cut into the segment that length is 1～5cm；When the straw that straw is this kind of shape of corn cob, available squeezer flattens, or with the granule that crusher in crushing becomes granularity to be 2～10mm.
In the method for the invention, the consumption of pretreatment fluid is for can make straw fully be soaked, preferably, the ratio of described straw weight and pretreatment fluid consumption is 1g (over dry weight, lower same): 7～15mL, more preferably straw weight is 1g:8～10mL with the ratio of pretreatment fluid consumption.With excessive pretreatment fluid, straw can also be soaked.In order to improve fiberizer work efficiency, before material enters fiberizer, part pretreatment fluid can be discharged, make remaining pretreatment liquid measure can meet fiberizer service requirement.
In order to ensure that straw can fully soak by pretreated liquid, temperature when soaking can be realized by increase soak time or raising straw, time (preferably soaking 4～12h) such as straw immersion >=4h under normal temperature condition, or make time (preferably soaking 0.5～2h) of straw immersion >=0.5h under 50～70 DEG C of conditions, or straw is boiled >=10min (preferably boiling 10～30min).When moistening, preferably straw is placed in container, (make the air in straw tissue also be pumped) after evacuation to resorb pretreatment fluid to carry out the immersion under room temperature or heating condition, now pretreatment fluid can immerse rapidly organization internal after contacting with straw under vacuum, softening moistening swollen straw, increases the sliding of straw in material conveying process simultaneously.
In the method for the invention, described fiberizer is the middle concentration or high concentration disc type paper-making paste mill that paper industry is conventional, controls granularity or the length of solid matter in discharging by regulating fiberizer.In the application, for ensureing that material has good water filtering performance, increase again the contact area of material and alkali liquor simultaneously as far as possible, improve the extraction efficiency of subsequent technique, it will be preferred that after making defibrination, the particle diameter of gained material is 0.1～1.0mm, more preferably 0.1～0.5mm.
In the method for the invention, described pretreatment fluid can be specifically concentration is the metal ion K of 1～20g/L2+、Na+Or Ca2+Alkaline solution, more specifically, it is possible to be concentration be the NaOH aqueous solution of 1～20g/L, KOH aqueous solution, Na2CO3Aqueous solution or Ca (OH)2Aqueous solution etc..The concentration of described pretreatment fluid more preferably 2～10g/L, is further preferably 2～5g/L, more preferably 5g/L.By the immersion moistening of pretreatment fluid, make the impurity such as microbe metabolite, partial pigment that straw produces in depositing process dissolve in pretreatment fluid, reduce the purification cost of subsequent alkaline liquid extract；Straw after the immersion moistening of another aspect pretreatment fluid has good sliding capability, it is possible to decrease the power consumption in material conveying and defibrination process.
In the method for the invention, it is achieved the mode of solid-liquid separation is same as the prior art, the application preferably employs centrifugal or filter pressing mode.
In the method for the invention, the solid after washing generally adopts the alkalinity extraction of existing routine to extract hemicellulose.It has been found that the raw material of gained after above-mentioned pretreatment is used alkalinity extraction again, in gained extracting solution, impurity is few, and the extraction ratio of hemicellulose is high.
Compared with prior art; the present invention is first with the alkali liquor infiltration softening stalk fibre of low concentration; it is re-introduced into fiberizer and the straw after infiltration is carried out defibrination; it is greatly improved in straw fiber and the contact area of pretreatment fluid; the impurity such as acetyl group, the pigment being more beneficial for sloughing in stalk fibre; do not losing the impurity content reducing in follow-up hemicellulose extract in straw while hemicellulose, improving hemicellulose extraction ratio, and in method, material process power consumption is low.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, and to be more fully understood that present disclosure, but the present invention is not limited to following example.
In following embodiment, the weight of straw is the weight of over dry material.
Embodiment 1
Extraction pot adds bagasse 100kg, after extraction pot evacuation, sucks pretreatment fluid (concentration is 5g/L sodium hydrate aqueous solution) 1000L in the ratio that solid-to-liquid ratio is 1g:10mL, under normal temperature condition, soak 10h.Discharge the free alkali liquor 330L in bagasse afterwards, the solution discharged is dark-brown, in extraction pot, leftover materials are delivered in high concentration disc type paper-making paste mill, and material is worn into the filament that diameter is 0.1～0.5mm, are centrifuged by defibrination gained material, discharge the free alkali liquor in levigate fiber, collection obtains liquid 550L, and bagasse adds water 300L, and after stirring mixing, washing, recentrifuge is discharged containing neutralizing treatment water 295L, merge three liquid and obtain 1175L, wherein do not detect xylan；Collecting solid, be the sugarcane fiber after process, gained sugarcane fiber softness is fine and closely woven.
Comparative example 1
Extraction pot adds bagasse 100kg (being with a collection of raw material with the raw material of embodiment 1), after extraction pot evacuation, suck pretreatment fluid (concentration is 5g/L sodium hydrate aqueous solution) 1000L in the ratio that solid-to-liquid ratio is 1g:10mL, under normal temperature condition, soak 10h.The centrifugal free alkali liquor 850L discharged in bagasse, the solution of discharge is dark-brown, and bagasse adds water to be centrifuged after 300L stirs mixing, washing and discharges containing neutralizing treatment water 300L, merges twice alkali liquor and obtains 1150L, does not wherein detect xylan；Collect solid, be the sugarcane fiber after process.Gained sugarcane fiber thickness is uneven, and comparatively bulk, texture is harder.
Embodiment 2
Sugarcane fiber after weighing the sugarcane fiber 50kg after processing by method described in embodiment 1 and processing by method described in comparative example 1 is respectively with alkalinity extraction hemicellulose 50kg.
Extraction conditions is: solid-to-liquid ratio 1g:5mL, and the NaOH aqueous solution that alkali liquor is concentration 8% (w/v) extracted, extraction time 12h, temperature is room temperature.
Then the hemicellulose extract of gained is carried out NaOH concentration, color and luster contrast, and with being equivalent to 95% (v/v) ethanol precipitate with ethanol of 3 times of extracting liquid volumes, 75% washing with alcohol hemicellulose, finally dry hemicellulose powder color and luster, purity and extraction ratio being contrasted, result is as shown in table 1.
Table 1:
As shown in Table 1, when bagasse after adopting the method for the invention to process is again with conventional alkalinity extraction and refining hemicellulose, impurity in bagasse fibre is removed in a large number, extracting solution color is shallow compared with comparative example 1, after levigate process, bagasse specific surface area strengthens, and the purity of hemicellulose extraction ratio and gained hemicellulose all relatively comparative example 1 is higher.
Embodiment 3
Corn stalk is cut into the segment that length is 1～3cm, weighs 100kg and put in extraction pot, add pretreatment fluid (concentration is 5g/L sodium hydrate aqueous solution) 1000L in the ratio that solid-to-liquid ratio is 1g:10mL, after being warming up to 60 DEG C, soak 1h.Discharge the free alkali liquor 330L in material afterwards, solution is dark-brown, again leftover materials in extraction pot are delivered in high concentration disc type paper-making paste mill, material is worn into the filament that diameter is 0.1～0.5mm, defibrination gained material is centrifuged, discharge the free alkali liquor in levigate fiber, collection obtains liquid 560L, and bagasse adds water 300L, and after stirring mixing, washing, recentrifuge is discharged containing neutralizing treatment water 298L, merge three liquid and obtain 1188L, wherein do not detect xylan；Collecting solid, be the cornstalk fibers after process, gained cornstalk fibers softness is fine and closely woven.
Embodiment 4
Corn cob disintegrating machine is broken into the particle of 5～20mm, weighs 100kg and put in extraction pot, add pretreatment fluid (concentration is 5g/L potassium hydroxide aqueous solution) 1000L in the ratio that solid-to-liquid ratio is 1g:10mL, after being warming up to 60 DEG C, soak 1h.Discharge the free alkali liquor 320L in material afterwards, solution is dark-brown, again leftover materials in extraction pot are delivered in high concentration disc type paper-making paste mill, material is worn into the fine particle that diameter is 0.1～0.5mm, defibrination gained material is centrifuged, discharge the free alkali liquor in levigate fiber, collection obtains liquid 520L, and bagasse adds water 300L, and after stirring mixing, washing, recentrifuge is discharged containing neutralizing treatment water 290L, merge three liquid and obtain 1120L, wherein do not detect xylan；Collect solid, be the corn cob fiber after process.
Embodiment 5
Corn cob disintegrating machine is broken into the particle of 5～20mm, weighs 100kg and put in extraction pot, add pretreatment fluid (concentration is 1g/L sodium hydrate aqueous solution) 1500L in the ratio that solid-to-liquid ratio is 1g:15mL, after boiling, soak 20min.Discharge the free alkali liquor 500L in material afterwards, solution is dark-brown, leftover materials in extraction pot are delivered in middle concentration disc type paper-making paste mill again, material is worn into the fine particle that granularity is 0.5～1.0mm, defibrination gained material is centrifuged, discharge the free alkali liquor in levigate fiber, collection obtains liquid 830L, and bagasse adds water 300L, and after stirring mixing, washing, recentrifuge is discharged containing neutralizing treatment water 310L, merge three liquid and obtain 1640L, wherein do not detect xylan；Collect solid, be the corn cob fiber after process.
Embodiment 6
Corn stalk is cut into the segment that length is 1～2cm, weighs 100kg and put in extraction pot, after extraction pot evacuation, suck pretreatment fluid (concentration is 5g/L calcium hydroxide aqueous solution) 800L in the ratio that solid-to-liquid ratio is 1g:8mL, under normal temperature condition, soak 6h.Afterwards leftover materials in extraction pot are delivered in high concentration disc type paper-making paste mill, material is worn into the filament that diameter is 0.5～1.0mm, defibrination gained material is centrifuged, discharge the free alkali liquor in levigate fiber, collection obtains liquid 650L, and bagasse adds water 300L, and after stirring mixing, washing, recentrifuge is discharged containing neutralizing treatment water 290L, merge three liquid and obtain 940L, wherein do not detect xylan；Collecting solid, be the cornstalk fibers after process, gained cornstalk fibers softness is fine and closely woven.
Embodiment 7
Weigh each 50kg alkalinity extraction hemicellulose of sugarcane fiber after processing by method described in embodiment 3,4,5 and 6 respectively.
Extraction conditions is: solid-to-liquid ratio 1g:5mL, and the NaOH aqueous solution that alkali liquor is concentration 8% (w/v) extracted, extraction time 12h, temperature is room temperature.
Then the hemicellulose extract of gained is carried out NaOH concentration, color and luster contrast, and with being equivalent to 95% (v/v) ethanol precipitate with ethanol of 3 times of extracting liquid volumes, 75% washing with alcohol hemicellulose, finally dry hemicellulose powder color and luster, purity and extraction ratio being contrasted, result is as shown in table 2.
Table 2:
Claims (7)
1. the straw pretreatment method being used for extracting hemicellulose, it is characterized in that: take straw pretreatment fluid and soak moistening, gained mixture sends into defibrination in fiberizer, make after defibrination the particle diameter of gained material less than or equal to 1.0mm, and gained material is carried out solid-liquid separation, collect solid, extract for hemicellulose after washing；Described pretreatment fluid is concentration is the alkaline solution of 1～20g/L.
2. the straw pretreatment method for extracting hemicellulose according to claim 1, it is characterised in that: the ratio of described straw weight and pretreatment fluid consumption is 1g:7～15mL.
3. the straw pretreatment method for extracting hemicellulose according to claim 1, it is characterised in that: the ratio of described straw weight and pretreatment fluid consumption is 1g:8～10mL.
4. the straw pretreatment method for extracting hemicellulose according to claim 1, it is characterised in that: after making defibrination, the particle diameter of gained material is 0.1～1.0mm.
5. the straw pretreatment method for extracting hemicellulose according to any one of Claims 1 to 4, it is characterised in that: described pretreatment fluid is concentration is the metal ion K of 1～20g/L2+、Na+Or Ca2+Alkaline solution.
6. the straw pretreatment method for extracting hemicellulose according to any one of Claims 1 to 4, it is characterised in that: the concentration of described pretreatment fluid is 2～10g/L.
7. the straw pretreatment method for extracting hemicellulose according to any one of Claims 1 to 4, it is characterised in that: the concentration of described pretreatment fluid is 2～5g/L.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109867803A (en) * | 2019-01-28 | 2019-06-11 | 广西大学 | A kind of method that high concentration plate mill prepares hemicellulose film |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101987473A (en) * | 2010-04-15 | 2011-03-23 | 洛阳理工学院 | Method for making package materials from straws |
| CN102242521A (en) * | 2011-06-22 | 2011-11-16 | 陈集双 | Method for preparing pulp by gramineous straw and use of obtained pulp |
| CN104805151A (en) * | 2014-01-24 | 2015-07-29 | 华东理工大学 | Lignocellulosic feedstock pretreatment method without prepreg |
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2016
- 2016-03-24 CN CN201610172806.8A patent/CN105732846B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101987473A (en) * | 2010-04-15 | 2011-03-23 | 洛阳理工学院 | Method for making package materials from straws |
| CN102242521A (en) * | 2011-06-22 | 2011-11-16 | 陈集双 | Method for preparing pulp by gramineous straw and use of obtained pulp |
| CN104805151A (en) * | 2014-01-24 | 2015-07-29 | 华东理工大学 | Lignocellulosic feedstock pretreatment method without prepreg |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109867803A (en) * | 2019-01-28 | 2019-06-11 | 广西大学 | A kind of method that high concentration plate mill prepares hemicellulose film |
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