CN101864683A - Pretreatment method of wood fiber raw materials - Google Patents
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Abstract
The invention relates to a pretreatment method of wood fiber raw materials, which belongs to the technical field of biomass chemical engineering. The process comprises the following steps: carrying out the first-step treatment after the wood fiber raw materials are mixed with mixed liquid of an organic acid solution and catalysts to obtain a liquid-solid mixture; separating the obtained liquid-solid mixture to obtain pretreatment black liquid and cellulose solids; washing the obtained cellulose solids by the organic acid solution to obtain washing black liquid and cellulose solids; adopting diluted acid or alkali for carrying out the second-step treatment on the obtained cellulose solids; mixing the obtained pretreatment black liquid and the obtained black liquid to obtain mixed black liquid; circularly using the mixed black liquid in the first-step treatment process; and recovering organic acids, lignin products and syrup solutions from the black liquid in the cyclic use for at least three times. The invention has the advantages that the full-rate development of raw materials can be realized, in addition, the environment-friendly effect can be realized, and the invention conforms to the requirement of modern biorefinery development.
Description
Technical field
The invention belongs to the living beings chemical field, particularly relate to a kind of pretreatment method of wood fiber raw materials, improve lignocellulose raw material cellulase catalyzing hydrolysis efficient, can realize the coproduction of high-purity lignin, ethanol and hemicellulose product.
Background technology
In recent years, because energy shortage and environmental disruption is serious day by day, the development alcohol fuel is non-grain ethanol especially, as cellulosic ethanol as an alternative the energy received the concern of countries in the world.Lignocellulose raw material is the abundantest organic matter of occurring in nature.According to estimates, the dry that plant every year produces by photosynthesis is up to hundred million tons of 1500-2000, is unique material object resource that can ultra-large regeneration on the earth.In China, the annual agricultural crop straw that produces has more than 700,000,000 ton, is equivalent to 3.5 hundred million tons of standard coals, more than 1,000 ten thousand tons of forest harvesting industrial wood wastes, more than 400 ten thousand tons of bagasses only account for about 2% but be used for the cellulose resource of industrial process or burning every year, also have greatly not to be utilized.
Produce in the fermentable sugars process in the lignocellulose raw material bio-transformation, because cellulose is by the spatial network parcel of hemicellulose and lignin composition, reduced its accessibility to cellulase, therefore will obtain higher enzymolysis sugar yield, raw material often needs through preliminary treatment to improve its enzymolysis performance.Pretreated effect mainly is the structure that changes natural fabric, reduces cellulosic degree of crystallinity, sloughs lignin and/or hemicellulose, increases enzyme and cellulosic contact area.
At present people have developed multiple physics, the process for chemically pretreating that improves cellulase hydrolysis efficient, as quick-fried broken, the basic hydrolysis of radiation treatment, pulverizing, high-pressure water heating, organic solvent, diluted acid, low temperature concentrated acid, acid catalyzed steam hydrolysis, steam explosive-crushing, liquefied ammonia and use non-ionic surface active agent etc.But the present pretreating process of developing often only merely emphasizes to improve cellulase hydrolysis efficient, less effective utilization of considering lignin and hemicellulose.In addition, present most of pretreating process of developing, for example dilute acid pretreatment, steam blasting etc. improve cellulosic enzymolysis efficiency by approach such as hydrolyzed hemicellulose and change lignin structures, and most of lignin remain in the cellulose solids still.This has reduced cellulosic content on the one hand, has limited the concentration of glucose in the simultaneous saccharification and fermentation production ethanol process, has caused the ineffective adsorption of cellulase on the other hand, causes the loss of cellulase.In addition, the existence of lignin can increase the inhomogeneities of system and the stirring energy consumption in the sweat, restricted fermentation mass transfer carry out, and the lignin residue after the fermentation only makes the utilization of lignin be in the level of minimum added value by burning recovery heat.
In fact, lignin is a kind of of great value industrial chemicals, highly purified sulphur-free lignin can be used as (Zhang Y.-H.Percival.Reviving the carbohydrate economy via multi-product lignocellulosebioreWneries.J Ind Microbiol Biotechnol (2008) 35:367-375.) such as polymeric additive such as phenolic resin, polyurethane foam, epoxy resin and soil conditioner, pesticide slow-releasing agents, and lignin is used and can be made its added value in these areas and reclaim the added value of heat far above the burning back that acts as a fuel.At present, lignin is mainly as pulping and paper-making byproduct production, for example lignosulphonates, kraft lignin etc.But these lignins contain element sulphur simultaneously lower, the complicated component of lignin purity, molecular weight distribution is wide, viscosity is low, decentralization is high, poor processability, almost do not have a thermoplastic property, thereby limited greatly its commercial Application (Luo Xuegang. high-purity lignin extraction and thermoplastic modification. Beijing: Chemical Industry Press, 2008).Therefore, exploitation cleaning, can effectively improve the pretreating process that lignocellulose raw material enzymolysis performance obtains hemicellulose and high-purity, high added value lignin products simultaneously, be to realize the biorefinery of lignocellulose raw material and the key of higher value application.
Summary of the invention
The object of the present invention is to provide a kind of pretreatment method of wood fiber raw materials,, obtain high-purity lignin products and syrup solution simultaneously to improve the enzymolysis performance of lignocellulose.
Above-mentioned purpose is achieved through the following technical solutions
The invention provides a kind of pretreatment method of wood fiber raw materials and comprise and adopt the two-step method of organic acid and diluted acid or diluted alkaline that lignocellulose raw material is carried out preliminary treatment that concrete technology may further comprise the steps:
(1) with lignocellulose raw material and the organic acid soln that contains catalyst by 3: 1-20: carry out the first step after the liquid-solid ratio of 1 (L/kg) is mixed and handle, obtain liquid-solid mixture;
(2) liquid-solid mixture that obtains in the separating step (1) obtains preliminary treatment black liquor and cellulose solids;
(3) obtain cellulose solids in the employing organic acid soln washing step (2), obtain washing black liquid and cellulose solids;
(4) adopt diluted acid or alkali to carry out the cellulose solids that obtains in the second step treatment step (3);
(5) washing black liquid that obtains in the preliminary treatment black liquor that obtains in the step (2) and the step (3) is mixed after, obtain mixing the first step processing procedure that black liquor and circulation are used for step 1);
(6) black liquor that recycles at least 3 times in the step (5) being carried out organic acid, lignin products and syrup solution reclaims.
Employed organic acid is the aliphatic organic acid in the described step (1), is preferably selected from formic acid, acetate or propionic acid; Employed catalyst is an inorganic acid, is preferably selected from sulfuric acid, hydrochloric acid, nitric acid or phosphoric acid.
The condition that the first step is handled in the described step (1) is: the organic acid mass concentration is 30-100%, the mass concentration of catalyst is 0-2%, liquid-solid ratio (L/kg) is based on 3 of raw material weight: 1-20: 1, and temperature is 50 ℃-200 ℃, the processing time is 0.25-5.0h.
Identical in the organic acid soln of the cellulose solids that obtains in the washing step (2) in the described step (3) and the step (1), its mass concentration is 30-100%, the consumption of organic acid soln is based on 3 of initial feed weight: 1-20: 1.
Employed diluted acid is one or more mixing in dilute sulfuric acid, watery hydrochloric acid, phosphoric acid,diluted, the rare nitric acid in the described step (4); Perhaps employed alkali is one or more mixing in NaOH, calcium hydroxide, potassium hydroxide, calcium oxide, the ammoniacal liquor.
The condition that adopts diluted acid to carry out the processing of second step in the described step (4) is: the diluted acid mass concentration is 0-2%, and liquid-solid ratio (L/kg) is based on 0.5 of initial feed weight: 1-20: 1, and temperature is 80-200 ℃, the processing time is 0.1-5.0h; The condition that perhaps adopts alkali to carry out the processing of second step is: the alkali consumption is the 0-10% based on initial feed weight, and liquid-solid ratio (L/kg) is based on 0.5 of initial feed weight: 1-20: 1, and temperature is 80-200 ℃, the processing time is 0.1-5.0h.
The mixing black liquor that recycles in the described step 5) is used for adding before the first step is handled the catalyst based on black liquor weight 0%-1%, and described catalyst is an inorganic acid, is preferably selected from sulfuric acid, hydrochloric acid, nitric acid or phosphoric acid.
Preferably, black liquor carries out organic acid, lignin products and syrup solution and reclaims and realize by the following method in the described step 6): earlier black liquor is carried out flash distillation or evaporation, obtain organic acid and concentrated black liquor; The water that adds 2-10 times of volume in the concentrated black liquor obtains lignin products and syrup solution.
The present invention comprises that also the cellulose solids that will obtain in the step (4) is used for simultaneous saccharification and fermentation and produces ethanol; Gained lignin products in the step (6) is used for polymeric additive and/or modified lignin is synthetic; Gained syrup solution in the step (6) is used for being used for alcohol fermentation after furfural production and/or the detoxification.
Wherein said lignocellulose raw material is selected from woody living beings and this biolobic material of standing grain; Preferably, described woody living beings are selected from hardwood, cork and shrub; Described this biolobic material of standing grain is selected from bagasse, straw, wheat straw or cornstalk.
In sum, adopt method provided by the present invention not only lignocellulose raw material can be separated into products such as cellulose solids, lignin and hemicellulose, realize the comprehensive utilization of raw material, and used organic acid is easy to reclaim and recycle, can reduces discharge of wastewater even realize zero-emission.Used organic acid soln can remove lignin and effective hydrolyzed hemicellulose under atmospheric low-temperature, make cellulose fully expose.Compare with the organic alcohol of low boiling (methyl alcohol, ethanol etc.) preliminary treatment, significantly reduced the requirement of withstand voltage of inflammable and explosive danger and equipment, and compared, significantly reduced the solvent recovery energy consumption with the organic alcohol of higher boiling (ethylene glycol, glycerine etc.) preliminary treatment.And the formic acid and the acetate of the generation of lignocellulose raw material preprocessing process, can be used as effectively replenishing thereby the basic free of losses of used organic acid of solvent.In the preprocess method provided by the present invention; second step was adopted diluted acid or alkali treatment; but the acyl group that may introduce in the processing of the effective elimination first step carries out swollen to cellulose on the other hand on the one hand, reduces cellulose crystallity thereby further improves cellulosic enzymolysis performance.Used diluted acid or alkali consumption are compared obvious minimizing with traditional diluted acid or alkali treatment, thereby have significantly reduced the chemical reagent cost.The lignin products that obtains in the preprocessing process has higher purity, thereby has higher added value than traditional alkali paper-making gained lignin products.This shows, adopt preprocess method provided by the invention, can realize the full price exploitation of raw material, and have environment friendly, meet the requirement of modern biorefinery development.
Description of drawings
Fig. 1 is a lignocellulose raw material pretreating process flow chart provided by the present invention, and wherein the first step is that organic acid is handled, and second step was alkali treatment.
Fig. 2 is a lignocellulose raw material pretreating process flow chart provided by the present invention, and wherein the first step is that organic acid is handled, and second step handled for diluted acid.
The specific embodiment
Following embodiment is convenient to understand better the present invention, but does not limit the present invention.
Embodiment 1:
Used lignocellulose raw material is a bagasse, and the original producton location is the Nanning city.Bagasse is removed the less myelocyte of granularity through sieving after air-dry, select particle diameter greater than the part in aperture, 60 mesh sieve hole as raw material.Reference " pulping and paper-making analysis and detection " (Shi Shulan. pulping and paper-making analysis and detection. Beijing: China Light Industry Press, 2003.) in the related assays method bagasse component is analyzed, analysis result is: in this bagasse, content of ashes is 1.38%, the hot-water extraction thing is 5.16%, the 1%NaOH extract is 34.20%, benzene-pure extract is 3.17%, content of cellulose is 44.98%, holocellulose content is 76.76%, acid-insoluble lignin content is 18.45%, and acid soluble lignin content is 1.80%.
At mass fraction is that to add mass fraction in 68% the formic acid solution be that 0.2% sulfuric acid is as catalyst, with bagasse by liquid-solid ratio be mix at 10: 1 after, stir process is 1.5 hours under atmospheric boiling point (about 105 ℃), cooling also centrifugally removes that to adopt mass fraction behind the black liquor be that 68% formic acid solution is 10: 1 ratio washing gained cellulose solids in the liquid-solid ratio with initial bagasse, the centrifugal washing black liquid of removing, to neutral, place 105 ℃ of oven dry down with clear water washing solid.Gained cellulose solids yield is 47.4%, and beta-dextran content is 77.6%, and xylan content is 8.9%, and content of lignin is 17.5%, and formoxyl content is 2.95%.Hydrolysis is 120 hours under the cellulase of this cellulose solids employing 20FPU/gDS (over dry matrix) and the β one glucoside enzymatic of 40CBU/gDS, can obtain the reducing sugar yield (corresponding glycan conversion ratio is 70.6%) of 68g reducing sugar/100gDS, wherein cellobiose accounts for 1.47% of total reducing sugars, glucose accounts for 89.3%, and wood sugar accounts for 9.23%.
Embodiment 2:
Used lignocellulose raw material is with implementation column 1.
At mass fraction is that to add mass fraction in 78% the formic acid solution be that 0.1% sulfuric acid is as catalyst, with bagasse by liquid-solid ratio be mix at 8: 1 after, stir process is 1.5 hours under atmospheric boiling point (about 105 ℃), cooling also centrifugally removes that to adopt mass fraction behind the black liquor be that 78% formic acid solution is 8: 1 ratio washing gained cellulose solids in the liquid-solid ratio with initial bagasse, centrifugal remove washing black liquid after, to neutral, place 105 ℃ of oven dry down with clear water washing solid.Gained cellulose solids yield is 49.2%, and beta-dextran content is 83.8%, and xylan content is 7.53%, and content of lignin is 15.65%, and formoxyl content is 4.08%.Hydrolysis is 120 hours under the cellulase of this cellulose solids employing 20FPU/gDS (over dry matrix) and the beta-glucosidase enzymatic of 40CBU/gDS, can obtain the reducing sugar yield (corresponding glycan conversion ratio is 86.9%) of 84.5g reducing sugar/100gDS, wherein cellobiose accounts for 1.87% of total reducing sugars, glucose accounts for 92.1%, and wood sugar accounts for 6.03%.
Embodiment 3:
Used lignocellulose raw material is with implementation column 1.
At mass fraction is that to add mass fraction in 70% the acetic acid solution be that 0.3% sulfuric acid is as catalyst, with bagasse by liquid-solid ratio be mix at 10: 1 after, stir process is 3.0 hours under atmospheric boiling point, cooling also centrifugally removes that to adopt mass fraction behind the black liquor be that 70% acetic acid solution is 10: 1 ratio washing gained cellulose solids in the liquid-solid ratio with initial bagasse, centrifugal remove washing black liquid after, to neutral, place 105 ℃ of oven dry down with clear water washing solid.Gained cellulose solids yield is 52.4%, and beta-dextran content is 65.78%, and xylan content is 15.10%, and content of lignin is 12.61%, and acetyl content is 2.67%.Hydrolysis is 120 hours under the cellulase of this cellulose solids employing 20FPU/gDS (over dry matrix) and the beta-glucosidase enzymatic of 40CBU/gDS, can obtain the reducing sugar yield (corresponding glycan conversion ratio is 83.1%) of 75.0g reducing sugar/100gDS, wherein cellobiose accounts for 10.8% of total reducing sugars, glucose accounts for 73.0%, and wood sugar accounts for 16.2%.
Embodiment 4:
Used lignocellulose raw material is with implementation column 1.
At mass fraction is that to add mass fraction in 90% the acetic acid solution be that 0.1% sulfuric acid is as catalyst, with bagasse by liquid-solid ratio be mix at 10: 1 after, stir process is 3.0 hours under atmospheric boiling point, cooling also centrifugally removes that to adopt mass fraction behind the black liquor be that 90% acetic acid solution is 10: 1 ratio washing gained cellulose solids in the liquid-solid ratio with initial bagasse, centrifugal remove washing black liquid after, to neutral, place 105 ℃ of oven dry down with clear water washing solid.Gained cellulose solids yield is 54.9%, and beta-dextran content is 65.01%, and xylan content is 16.97%, and content of lignin is 12.95%, and acetyl content is 4.49%.Hydrolysis is 120 hours under the cellulase of this cellulose solids employing 20FPU/gDS (over dry matrix) and the beta-glucosidase enzymatic of 40CBU/gDS, can obtain the reducing sugar yield (corresponding glycan conversion ratio is 63.5%) of 58g reducing sugar/100gDS, wherein cellobiose accounts for 10.6% of total reducing sugars, glucose accounts for 69.3%, and wood sugar accounts for 20.1%.
Embodiment 5:
Used lignocellulose raw material is with implementation column 1, and concrete technological process as shown in Figure 1.
Mass fraction be 78% formic acid solution with bagasse by liquid-solid ratio be mix at 10: 1 after, stir process is 1.5 hours under atmospheric boiling point, cooling also centrifugally removes that to adopt mass fraction behind the black liquor be that 78% formic acid solution is 10: 1 ratio washing gained cellulose solids in the liquid-solid ratio with initial bagasse, centrifugal remove washing black liquid after, with clear water washing solid to neutral, extruding or centrifugal above-mentioned cellulose solids dewater to moisture be 72%.Take by weighing based on the NaOH of initial bagasse weight 4% and 3 times to the water of initial bagasse weight, add to after mixing in the above-mentioned cellulose solids and handled 1 hour down in 120 ℃.Washing gained cellulose solids and oven dry under 105 ℃.Gained cellulose solids yield is 41.8%, and beta-dextran content is 91.1%, and xylan content is 5.08%, and content of lignin is 9.25%, and formoxyl content is 0.32%.Hydrolysis can obtain 86.6% glycan conversion ratio in 24 hours under the cellulase of this cellulose solids employing 20FPU/gDS (over dry matrix) and the beta-glucosidase enzymatic of 20CBU/gDS, and enzymolysis can obtain 96.5% glycan conversion ratio in 48 hours.
Embodiment 6:
Used lignocellulose raw material is with implementation column 1, and concrete technological process as shown in Figure 1.
Mass fraction be 88% formic acid solution with bagasse by liquid-solid ratio be mix at 10: 1 after, stir process is 1.5 hours under atmospheric boiling point, cooling also centrifugally removes that to adopt mass fraction behind the black liquor be that 88% formic acid solution is 10: 1 ratio washing gained cellulose solids in the liquid-solid ratio with initial bagasse, centrifugal remove washing black liquid after, with clear water washing solid to neutral, extruding or centrifugal above-mentioned cellulose solids dewater to moisture be 75%.Take by weighing based on the calcium hydroxide of initial bagasse weight 4% and 2 times to the water of initial bagasse weight, add to after mixing in the above-mentioned cellulose solids and handled 1 hour down in 120 ℃.Washing gained cellulose solids and oven dry under 105 ℃.Gained cellulose solids yield is 38.3%, and beta-dextran content is 93.5%, and xylan content is 4.34%, and content of lignin is 6.17%, and formoxyl content is 0.45%.Hydrolysis can obtain 77.3% glycan conversion ratio in 24 hours under the cellulase of this cellulose solids employing 20FPU/gDS (over dry matrix) and the beta-glucosidase enzymatic of 20CBU/gDS, and enzymolysis can obtain 99.9% glycan conversion ratio in 48 hours.
Embodiment 7:
Used lignocellulose raw material is with implementation column 1, and concrete technological process as shown in Figure 1.
Mass fraction be 80% acetic acid solution add mass fraction be 0.3% sulfuric acid be behind the catalyst with bagasse by liquid-solid ratio be mix at 10: 1 after, stir process is 2 hours under atmospheric boiling point, cooling also centrifugally removes that to adopt mass fraction behind the black liquor be that 80% acetic acid solution is 10: 1 ratio washing gained cellulose solids in the liquid-solid ratio with initial bagasse, centrifugal remove washing black liquid after, with clear water washing solid to neutral, extruding or centrifugal above-mentioned cellulose solids dewater to moisture be 70%.Take by weighing based on the calcium hydroxide of initial bagasse weight 4% and 3 times to the water of initial bagasse weight, add to after mixing in the above-mentioned cellulose solids and handled 1 hour down in 120 ℃.Washing gained cellulose solids and oven dry under 105 ℃.Gained cellulose solids yield is 45.6%, and beta-dextran content is 84.8%, and xylan content is 11.5%, and content of lignin is 7.04%.Hydrolysis can obtain 71.1% glycan conversion ratio in 24 hours under the cellulase of this cellulose solids employing 20FPU/gDS (over dry matrix) and the beta-glucosidase enzymatic of 40CBU/gDS, and enzymolysis can obtain 81.9% glycan conversion ratio in 48 hours.
Embodiment 8:
Used lignocellulose raw material is with implementation column 1, and concrete technological process as shown in Figure 2.
Mass fraction be 80% acetic acid solution add mass fraction be 0.3% sulfuric acid be behind the catalyst with bagasse by liquid-solid ratio be mix at 10: 1 after, stir process is 1.5 hours under atmospheric boiling point, cooling also centrifugally removes that to adopt mass fraction behind the black liquor be that 80% acetic acid solution is 10: 1 ratio washing gained cellulose solids in the liquid-solid ratio with initial bagasse, centrifugal remove washing black liquid after, adopt 0.1% dilution heat of sulfuric acid to handle 1 hour down at 160 ℃.Washing gained cellulose solids and oven dry under 105 ℃.Gained cellulose solids yield is 44.3%, and beta-dextran content is 87.8%, and xylan content is 8.5%, and content of lignin is 8.04%.Hydrolysis can obtain 70.1% glycan conversion ratio in 24 hours under the cellulase of this cellulose solids employing 20FPU/gDS (over dry matrix) and the beta-glucosidase enzymatic of 40CBU/gDS, and enzymolysis can obtain 95.4% glycan conversion ratio in 48 hours.
Embodiment 9:
Used lignocellulose raw material is with implementation column 1.
Mass fraction be 60% acetic acid solution add mass fraction be 0.3% sulfuric acid be behind the catalyst with bagasse by liquid-solid ratio be mix at 10: 1 after, stir process is 3 hours under atmospheric boiling point, obtains black liquor behind the cold filtration.Black liquor is added 5 times to the water of concentrated black liquor volume in 50 ℃ of following reduction vaporizations to 1/10 back of stoste volume, be settled out acetic acid lignin, get lignin products and the syrup solution that contains fermentable sugars such as glucose and wood sugar after the filtration.By analysis, the C of lignin, H, O, N constituent content are respectively 59.09%, 5.64%, 34.66% and 0.61%, and the content of acid-insoluble lignin is greater than 90%, and carbohydrate content is less than 2%.
Claims (10)
1. a pretreatment method of wood fiber raw materials comprises and adopts the two-step method of organic acid and diluted acid or alkali that lignocellulose raw material is carried out preliminary treatment, and concrete technology may further comprise the steps:
(1) with lignocellulose raw material and the organic acid soln that contains catalyst by 3: 1-20: carry out the first step after the liquid-solid ratio of 1 (L/kg) is mixed and handle, obtain liquid-solid mixture;
(2) liquid-solid mixture that obtains in the separating step (1) obtains preliminary treatment black liquor and cellulose solids;
(3) obtain cellulose solids in the employing organic acid soln washing step (2), obtain washing black liquid and cellulose solids;
(4) adopt diluted acid or alkali to carry out the cellulose solids that obtains in the second step treatment step (3);
(5) washing black liquid that obtains in the preliminary treatment black liquor that obtains in the step (2) and the step (3) is mixed after, obtain mixing the first step processing procedure that black liquor and circulation are used for step (1);
(6) black liquor that recycles at least 3 times in the step (5) being carried out organic acid, lignin products and syrup solution reclaims.
2. method according to claim 1 is characterized in that, employed organic acid is the aliphatic organic acid in the described step (1), is selected from formic acid, acetate or propionic acid; Employed catalyst is an inorganic acid, is selected from sulfuric acid, hydrochloric acid, nitric acid or phosphoric acid;
3. method according to claim 1 and 2, it is characterized in that, the condition that the first step is handled in the described step (1) is: the organic acid mass concentration is 30-100%, the mass concentration of catalyst is 0-2%, liquid-solid ratio (L/kg) is based on 3 of raw material weight: 1-20: 1, temperature is 50 ℃-200 ℃, and the processing time is 0.25-5.0h.
4. method according to claim 1 and 2, it is characterized in that, identical in the organic acid soln of the cellulose solids that obtains in the washing step (2) in the described step (3) and the step (1), its mass concentration is 30-100%, and the consumption of organic acid soln is based on 3 of initial feed weight: 1-20: 1.
5. method according to claim 1 is characterized in that, employed diluted acid is one or more mixing in dilute sulfuric acid, watery hydrochloric acid, phosphoric acid,diluted, the rare nitric acid in the described step (4); Perhaps employed alkali is one or more mixing in NaOH, calcium hydroxide, potassium hydroxide, calcium oxide, the ammoniacal liquor.
6. method according to claim 1, it is characterized in that, the condition that adopts diluted acid to carry out the processing of second step in the described step (4) is: the diluted acid mass concentration is 0-2%, liquid-solid ratio (L/kg) is based on 0.5 of initial feed weight: 1-20: 1, temperature is 80-200 ℃, and the processing time is 0.1-5.0h; The condition that perhaps adopts alkali to carry out the processing of second step is: the alkali consumption is the 0-10% based on initial feed weight, and liquid-solid ratio (L/kg) is based on 0.5 of initial feed weight: 1-20: 1, and temperature is 80-200 ℃, the processing time is 0.1-5.0h.
7. method according to claim 1, it is characterized in that, the mixing black liquor that recycles in the described step (5) is used for adding before the first step is handled the catalyst based on black liquor weight 0%-1%, and described catalyst is an inorganic acid, is selected from sulfuric acid, hydrochloric acid, nitric acid or phosphoric acid.
8. method according to claim 1 is characterized in that, the middle black liquor of described step (6) carries out organic acid, lignin products and syrup solution recovery to be realized by the following method: earlier black liquor is carried out flash distillation or evaporation, obtain organic acid and concentrated black liquor; The water that adds 2-10 times of volume in the concentrated black liquor obtains lignin products and syrup solution.
9. according to the method for claim 1, it is characterized in that this method comprises that also the cellulose solids that will obtain in the step 4) is used for simultaneous saccharification and fermentation and produces ethanol; Gained lignin products in the step (6) is used for polymeric additive and/or modified lignin is synthetic; Gained syrup solution in the step (6) is used for being used for alcohol fermentation after furfural production and/or the detoxification.
10. according to the method for claim 1, it is characterized in that described lignocellulose raw material is selected from woody living beings and this biolobic material of standing grain; Described woody living beings are selected from hardwood, cork or shrub; Described this biolobic material of standing grain is selected from bagasse, straw, wheat straw or cornstalk.
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| MX2024002324A (en) * | 2021-08-27 | 2024-03-07 | Univ Maryland | Waste-free processing for lignin modification of fibrous plant materials, and lignin-modified fibrous plant materials. |
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| 《Bioresource Technology》 20051231 Xuejun Pan et al. Fractionation of wheat straw by atmospheric acetic acid process 1256-1263 1-10 第96卷, 第11期 2 * |
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