CN105350369B - The preparation technology of the lignocellulosic slurrying pre-hydrolyzed solution with high-efficiency fermenting ability - Google Patents
The preparation technology of the lignocellulosic slurrying pre-hydrolyzed solution with high-efficiency fermenting ability Download PDFInfo
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
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- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
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- C12P7/00—Preparation of oxygen-containing organic compounds
- C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
- C12P7/04—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
- C12P7/18—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic polyhydric
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- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P2203/00—Fermentation products obtained from optionally pretreated or hydrolyzed cellulosic or lignocellulosic material as the carbon source
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Abstract
For the problem that prior art exists in terms of ligno-cellulose hydrolysate detoxification, the invention provides a kind of preparation method of the slurrying pre-hydrolyzed solution with high-efficiency fermenting ability based on advanced oxidation processes and electrodialysis process, comprise the following steps：1. slurrying pre-hydrolyzed solution is prepared；2. concentrate and except precipitation；3. advanced oxidation treatment；4. electrodialysis process.Pre-hydrolyzed solution of the present invention produced by pulp and paper industry chemi-mechanical pulp and dissolving pulp production process is process object, first using advanced oxidation reagent degraded organic inhibitor molecule, the electrolyte inhibitor in electroosmose process removal pre-hydrolyzed solution is then used by, the two forms significantly cooperative effect.According to pre-hydrolyzed solution prepared by the above method, fermenting and producing SCP or preparation high added value compound can be used for as fermenting carbon source.Poison-removing method of the invention can not only remove the micromolecular inhibitors such as phenols but also can remove ionizable inhibitor in the case where fermentable sugars is not lost.
Description
Technical field
The invention belongs to bioenergy and pulping and paper-making field, and in particular to a kind of lignocellulosic slurrying pre-hydrolyzed solution
Preparation technology, more particularly to a kind of use advanced oxidation processes and electroosmose process prepare the lignocellulosic with high-efficiency fermenting ability
The process of slurrying pre-hydrolyzed solution.
Background technology
Due to excellent pulping and paper-making, there is lack of raw materials, traditional resource price continuous rise, labor cost rise and the whole world
Change the brought immense pressure of competition, tradition enterprises in pulp and paper industry is faced with unprecedented difficulty at present.Merely by wooden fibre
Dimension element changes into paper pulp and the old business model of sheet paper products has been difficult to be applicable existing market.By pulp and paper industry and life
Material refining is combined, and before slurrying, prehydrolysis is carried out to string resource, can not only reduce the energy in digestion process
Consumption, reduce bleaching process in bleaching liquor consumption, while improve pulp quality, can also reduce pulping and papermaking processes waste water BOD and
The hemicellulose and lignin that COD, reduction greenhouse gas emissions, and pretreatment are obtained can be also used for producing high added value
Biomass fuel and biomass chemicals etc..Researcher has been developed for prehydrolysis-chemi-mechanical pulp and prehydrolysis sulphite
The manufacturing process of dissolving pulp, using the method for sour prehydrolysis, hot water prehydrolysis or steam prehydrolysis to the leading pre- water of pulping materials
Solution is with extracting hemicelluloses.In slurrying pre-hydrolyzed solution and its acid hydrolysis products, except hemicellulose, xylose, the glucose degraded
Outward, the inhibitor for hindering biological utilisation is also inevitably produced, hydroxymethylfurfural, half fibre that for example cellulose degradation is produced
Acetic acid, furfural, levulinie acid and formic acid that dimension element degraded is produced, the small molecule phenols material (4- that lignin degradation is produced
Hydroxybenzoic acid, vanillic aldehyde and catechol) etc..Fermentation inhibitor in slurrying pre-hydrolyzed solution has that species is more, concentration model
Enclose wide (several micrograms are to tens grams), the features such as chemical property is complicated.
Regarding to the issue above, researcher develops various poison-removing methods for lignocellulosic acid hydrolysis liquid, mainly
Based on physical action, chemical action or biological agent.
(1) physical method is including evaporation, organic solvent extraction, activated carbon, ion exchange resin, UF membrane etc..1. rotate
Evaporation can reduce low-boiling-point organic compound in hydrolyzate, such as concentration of acetic acid, furfural and aldehydes vanillic aldehyde, but meeting again under high temperature
New inhibitor is produced, so as to cause fermentation efficiency to reduce.2. the volatile organic solvent extraction such as application ether, ethyl acetate
The most of mortifier of hydrolysis liquid energy removing, but there is organic difficult solvent recovery and organic solvent residual.3. it is active
Charcoal has stronger characterization of adsorption, but the suppressed physical property matter of absorption of the activated carbon to mortifier, pre-hydrolyzed solution pH, pretreatment temperature
The influence of degree, time and concentration of activated carbon, and remove the limitation of mortifier.4. ion exchange resin absorption presses down to faintly acid
The removal effect of thing processed is notable, but limited to the removal effect that furfural class suppresses, and this method is while inhibiting substances are removed
Substantial amounts of fermentable sugars can be also removed, causes the yield of tunning to be greatly lowered.5. during UF membrane can remove hydrolyzate
The mortifier such as furfural, hydroxymethylfurfural, acetic acid, but can not effectively remove small point close with glucose and xylose molecular weight
Sub- phenolic compound.
(2) chemical Treatment is mainly by adding the suppression that aqueous slkali (calcium hydroxide or NaOH) makes in pre-hydrolyzed solution
Thing processed forms precipitation or the ionization property of mortifier is changed by adjusting pH value, and the purpose of toxicity is reduced so as to reach.It is logical
The method for reducing the toxicity of fermentation inhibitor frequently with the pH value for changing hydrolyzate, most common of which is excess amount of Ca (OH)2
Neutralisation.The treated hydrolyzate of the method, fermentability is remarkably reinforced, and simple to operate, with low cost, mortifier removing effect
Fruit is substantially.However, due to the precipitation of calcium ion, easily separated to follow-up fermentation and product and had a negative impact.
(3) bioanalysis refers to be allowed to tie with some specific enzymes (laccase, peroxidase) or microbiological treatment mortifier
Structure changes so as to reduce its toxicity.Because enzymatic has specificity and selectivity, so ferment treatment can only also remove spy
Certain fixed mortifier.Although microbial pretreatment can have certain detoxification to the mortifier in pre-hydrolyzed solution,
Various carbohydrates and this method requirement process time in detoxification microbial consumption pre-hydrolyzed solution is long.
In sum, existing single poison-removing method has extremely obvious limitation, causes it efficiently to remove suppression
Preparation.
There is oxidation reaction in advanced oxidation processes, by substitution, break with hydroxy radical as oxidant with organic matter in solution
Key, electro transfer, with reference to etc. reaction, the difficult degradation in solution, larger molecular organicses is oxidized into small-molecule substance, or even directly
Connect oxidative degradation into CO2And H2O.Advanced oxidation processes can be by the small molecule aromatic compounds in solution such as aromatic aldehyde, aromatic ester
Or aromatic acid is degraded to long chain and alkane, last mineralising is CO2And H2O.Because high-level oxidation technology extensively should
Biodegradable for improving waste water, current technology is mainly used in drinking water treatment, special industrial water process, has
The treatment of the harmful high concentrated organic wastewater of poison and the Sewage advanced treatment for the purpose of reuse etc..Application for a patent for invention
" a kind of ferrous salt activation persulfate or single peroxosulphuric hydrogen salt advanced oxidation advanced treating are made disclosed in 201410052519.4
The method of paper waste water ".Using persulfate or single peroxosulphuric hydrogen salt and ferrous reactant salt generation strong oxidizing property sulfate radical freedom
Organic matter in base oxidative degradation paper waste.The method has efficiency high, easy to operate, the characteristics of applicable pH range is wider.But
It is that the method is applied to the detoxification of slurrying pre-hydrolyzed solution, then can produces high concentration sulfate, is highly detrimental to follow-up slurrying pre-
The biofermentation of hydrolyzate.Because, and unlike the purpose of water treatment field application advanced oxidation, water treatment field is
All organic matters of non-selective degraded are different, and the detoxification of slurrying pre-hydrolyzed solution requirement is while non-degradable fermentable sugars
The removal small molecule aromatics inhibitor of selectivity.Additionally, (Silva, et the al.Biotechnology for such as Silva
Biofuel,2013,6:23) method that straw dilute acid hydrolysis liquid is processed using advanced oxidation processes is reported, although the method can
To remove aromatic compounds, but can not effectively remove having of being produced in original and advanced oxidation processes in acid hydrolysis liquid
Machine acids (formic acid, acetic acid) fermentation inhibitor, therefore it is unsuitable for the detoxification requirement of the slurrying pre-hydrolyzed solution of organic acid content high.And
And, its process object is simple straw acid hydrolysis liquid, with the difference that slurrying pre-hydrolyzed solution of the invention has essence.
At present, electrodialysis is mainly used in waste water desalting processing and product separation field, therefore, its application field and this hair
Field difference belonging to bright is very big.Additionally, simple electrodialysis can only remove formic acid and acetic acid in slurrying pre-hydrolyzed solution etc.
Organic acid inhibitor, can hardly remove fragrant type small molecular inhibitor, and this results in simple electrodialysis can not be real
The high-efficiency detoxicating of existing slurrying pre-hydrolyzed solution.
The content of the invention
For the problem that prior art exists in terms of ligno-cellulose hydrolysate detoxification, it is based on the invention provides one kind
The preparation method of the slurrying pre-hydrolyzed solution with high-efficiency fermenting ability of advanced oxidation processes and electrodialysis process.Present invention exploitation
Poison-removing method can be in the case where fermentable sugars not be lost, and can not only remove the micromolecular inhibitors such as phenols but also can remove can
The inhibitor of ionization.
The principle of preparation technology：(1) using the hydroxy radical produced by advanced oxidation reagent by slurrying pre-hydrolyzed solution
Aromatics species fermentation inhibitor (aromatic aldehyde, aromatic ester or aromatic acid etc.) is degraded to the small molecular organic acids such as formic acid, nothing
The acid amides and alkane of fermentation inhibitory effect, or even it is degraded to CO2And H2O；(2) then electrodialysis technique removes pre-hydrolyzed solution
In ionizable fermentation inhibitor, such as formic acid, acetic acid and sulfate etc., its cardinal principle be DC electric field effect
Under, the anion-permeable cavity block in slurrying hydrolyzate migrates into dense room to anode direction, is stopped by anode membrane and stays in dense room
In, and stopped by cavity block and be trapped within also into dense room after the cation permeable anode membrane in hydrolyzate is migrated to cathode direction
In dense room.Therefore, the acid in light room is removed.And sugar is non-electrolyte, will not under the electric field migrate, can protect in principle
Stay in light room.Electrodialysis can effectively remove the impurity of the acid and other ionic conditions in slurrying hydrolyzate, can drop significantly
The loss late of low product simultaneously reclaims the acid in hydrolyzate.
Technical scheme：The preparation technology of the lignocellulosic slurrying pre-hydrolyzed solution with high-efficiency fermenting ability,
Comprise the following steps：1. slurrying pre-hydrolyzed solution is prepared；2. concentrate and except precipitation；3. advanced oxidation treatment；4. electrodialysis process.
It is pulping raw material of paper making that 1. the step prepares the material that slurrying pre-hydrolyzed solution uses.1. the step prepares slurrying
The method that pre-hydrolyzed solution is used is hot water prehydrolysis process or steam prehydrolysis process；The hot water prehydrolysis process is to be placed in raw material
Soaked 10-60 minutes in 70-100 DEG C of hot water, then to water is added in raw material, be warming up to uniform temperature, without Additional pressurizations, protected
Cooled down after warm a period of time；The steam prehydrolysis process is that raw material is placed in container, is passed through the steam of uniform temperature, without extra
Pressurization, insulation is cooled down after a period of time.
2. the step concentrates and concretely comprising the following steps except precipitation：The slurrying pre-hydrolyzed solution that 1. step is prepared is using decompression
The mode of distillation is concentrated, and pH value is then adjusted for the first time, is 1.0-2.5 to pH value, to precipitate lignin, then carries out solid-liquid
Separate to remove lignin deposit and collect pre-hydrolyzed solution；Then second regulation pH value, is 7-10 to pH value, stands, filters
Except precipitation, concentrated and except the pre-hydrolyzed solution after precipitation.
What the 3. advanced oxidation was processed concretely comprises the following steps：Certain density advanced oxidation reagent is added and is 2. concentrated and is removed
In pre-hydrolyzed solution after precipitation, a period of time is processed under certain pH value and temperature conditionss, produced in micro-filtration removal processing procedure
Raw colloidal precipitation thing, collects liquid phase pre-hydrolyzed solution.
4. the electrodialysis process is concretely comprised the following steps：The pH value of the 3. pre-hydrolyzed solution that advanced oxidation treatment is obtained is adjusted,
It is then injected into the light room of electric dialyzator, under the DC electric field effect of constant voltage or constant current, in slurrying pre-hydrolyzed solution
Anion-permeable anion-exchange membrane migrate into dense room to anode direction, stayed in after being stopped by cation-exchange membrane dense
In room.Similarly, also into dense room after the cation permeable cation-exchange membrane in pre-hydrolyzed solution is migrated to cathode direction, by the moon
Amberplex stop is trapped within dense room.The pre-hydrolyzed solution in light room is collected after treatment, is obtained final product with low fermentation inhibitors
Slurrying pre-hydrolyzed solution.
Pre-hydrolyzed solution of the present invention produced by pulp and paper industry chemi-mechanical pulp and dissolving pulp production process is treatment
Object, first application advanced oxidation reagent degraded organic inhibitor molecule, are then used by electroosmose process removal pre-hydrolyzed solution
Electrolyte inhibitor, including acetic acid, formic acid and sulfate, the two has mutually been jointly formed significantly cooperative effect.
Wherein, the step 1. in pulping raw material of paper making can be any lignocellulose-containing material, including poplar,
It is Eucalyptus, birch, larch, Korean pine, masson pine, pinus yunnanensis, pinus sylvestris var. mongolica, reed, bamboo, wheat, paddy rice, Chinese alpine rush, sorghum, sweet
Sugarcane, wheat, flax, jute, mestha, Tan Shu, mulberry or cotton stalk, and its any combination.The material bag of the lignocellulose-containing
Include stem, root, bar, blade, skin or the shell of above-mentioned material, and its any combination.Material and water in the hot water prehydrolysis process
Mass ratio is 1:3-1:10, the heating-up time is 20-60 minutes, and treatment temperature is 120-180 DEG C, and soaking time is 30-240 points
Clock, temperature is 30-80 DEG C after cooling；Vapor (steam) temperature is 120-180 DEG C in the steam prehydrolysis process, and soaking time is 30-240
Minute, temperature is 30-80 DEG C after cooling.
Wherein, 2. the step concentrates and except the temperature of vacuum distillation in precipitation is 40-60 DEG C, pre-hydrolyzed solution after concentration
Concentration is original 5-10 times；The first time regulation pH value uses hydrochloric acid, sulfuric acid, nitric acid or phosphoric acid；Described second
Regulation pH value uses NaOH, potassium hydroxide or ammoniacal liquor.
Wherein, the advanced oxidation reagent in the 3. advanced oxidation treatment is hydrogen peroxide, ozone, hydrogen peroxide/ozone mixing
Thing or hydrogen peroxide/ferrous sulfate mixture.The concentration of the hydrogen peroxide is 1-10g/L, and the concentration of the ozone is 0.5-2g/L,
The concentration of the ferrous sulfate is 0.1-2g/L.Each component in hydrogen peroxide/ozone mixture and hydrogen peroxide/ferrous sulfate mixture
Concentration range it is identical with exclusive use.The pH value of the advanced oxidation is 2-10, and temperature is 20-60 DEG C, and process time is
0.5-24 hours.Preferably, the concentration of the hydrogen peroxide is 2-8g/L, and the concentration of the ozone is 1-2g/L, the sulfuric acid
Ferrous concentration is 0.2-1g/L；The pH value of the advanced oxidation is 5-9, and temperature is 25-50 DEG C, and process time is 2-7 hours.
More preferably, the concentration of the hydrogen peroxide is 3-5g/L, and the concentration of the ozone is 1-1.5g/L, the ferrous sulfate it is dense
It is 0.2-0.5g/L to spend；The pH value of the advanced oxidation is 7-9, and temperature is 25-35 DEG C, and process time is 5-6 hours.
Wherein, 4. the middle pre-hydrolyzed solution pH value for injecting light room is 2-9 to the step；The voltage that the electrodialysis process is used
It is 0.5-300V, the electric current for using is 0.1-50A, the anion-exchange membrane and cation-exchange membrane for using are 1-500 pairs；It is described
The area of anion-exchange membrane and cation-exchange membrane is respectively 50 × 50-1000 × 2000mm2.Preferably, step 4. in
The pre-hydrolyzed solution pH value for injecting light room is 3.5-7.It is further preferred that the pre-hydrolyzed solution pH value of the step 4. light room of middle injection is 4.5-
5。
The purposes of the lignocellulosic slurrying pre-hydrolyzed solution with high-efficiency fermenting ability prepared according to the above method, as
Fermenting carbon source is used for fermenting and producing SCP or prepares high added value compound；The high added value compound is wood
Sugar, xylitol, wood oligose, arabinose or arabite.
With electrodialysis methods be combined gentle advanced oxidation processes by novelty of the present invention, using improved gentle
The ionizable fermentation inhibitors such as advanced oxidation processes degraded aromatics fermentation inhibitor, electrodialysis method removal organic acid, it is real
Show all fermentation inhibitors in efficient removal slurrying pre-hydrolyzed solution in the case of hardly loss fermentable sugars, meet system
Starch the requirement of pre-hydrolyzed solution detoxification.
Beneficial effects of the present invention：Compared with traditional poison-removing method, the present invention has the advantage that：
(1) present invention process mild condition, it is possible to achieve realize that slurrying is pre- in the case of hardly loss fermentable sugars
The detoxification treatment of hydrolyzate；
(2) efficient removal of Small Phenolic Molecule and ionizable inhibitor can be realized；
(3) detoxification process mild condition, it is not necessary to high temperature and high pressure, save energy and cost；
(4) process equipment is simple, it is easy to controls, reduce production cost；
(5) acid can be recycled in pre-hydrolyzed solution, reduce environmental pollution, it is easy to industrial applications.
Figure of description
Fig. 1 is the comparative test result with independent advanced oxidation/independent electrodialysis process pre-hydrolyzed solution of the invention.
Specific embodiment
With reference to embodiment, the present invention is described further.
Embodiment 1：
During 1kg peeling poplar wood chip and 6kg water added into digester jointly, 20-60min is warming up to 160 degree, keeps this temperature
Degree 2 hours, separates wood chip after pre-hydrolyzed solution and pretreatment after being cooled to 40 DEG C.Pre-hydrolyzed solution is subtracted under the conditions of being 40 DEG C in temperature
After 5 times of distillation and concentration of pressure, pre-hydrolyzed solution pH to 2.5 is adjusted by 1M sulfuric acid of concentration, stand 30 minutes, after filtering and collecting filtering
Pre-hydrolyzed solution.Pre-hydrolyzed solution pH to 8.0 is adjusted with NaOH, 30 minutes are stood, pre-hydrolyzed solution after filtering is filtered and collect.Connect
To hydrogen peroxide is added in pre-hydrolyzed solution to 5g/L, micro-filtration removal is precipitated after being processed 3 hours at 8.0,30 DEG C of pH.Regulation pH to
4.5, it is 400ml by volume, during initial conductivity is for the pre-hydrolyzed solution injection electric dialyzator of 46ms/cm, electrodialysis condition is perseverance
Determine current strength 0.25A, initial voltage 4V, anion-exchange membrane and cation exchange membrane area and be 95 × 215mm2, circulation
Flow velocity is 0.5L/min.After operation electrodialysis 6 hours, pre-hydrolyzed solution 100ml in light room is taken, add 3.5g/L peptones, 3g/L
Yeast extract, 2g/L potassium dihydrogen phosphates, 1g/L magnesium sulfate, 1g/L ammonium sulfate, adjust pH value to 6.8 after mixing, filtration sterilization,
It is inoculated with into Pichia pastoris CBS6054, cultivates 72 hours.Pre-hydrolyzed solution total phenol content reduction by 70% after final result display processing,
Furfural and hydroxymethyl furfural content reduction by 60%, acetic acid and formic acid content reduction by 90%, and reduced sugar loss late in pre-hydrolyzed solution
Only 4.2%, Pichia pastoris in pre-hydrolyzed solution growth rate with pure sugar culture-medium without significant difference.
Embodiment 2：
During 1kg peeling Eucalyptus wood chip and 3kg water added into digester jointly, 20-60min is warming up to 170 degree, keeps this temperature
Degree 4 hours, separates wood chip after pre-hydrolyzed solution and pretreatment after being cooled to 50 DEG C.By pre-hydrolyzed solution under conditions of being 60 DEG C in temperature
After vacuum distillation concentrates 10 times, the hydrochloric acid regulation pre-hydrolyzed solution pH to 2.0 with concentration as 1M stands 30 minutes, filters and collects
Pre-hydrolyzed solution after filtering.Pre-hydrolyzed solution pH to 8.0 is adjusted with potassium hydroxide, 30 minutes are stood, pre- water after filtering is filtered and collect
Solution liquid.Then to adding hydrogen peroxide and ferrous sulfate respectively to 3g/L and 0.2g/L, pH 3.0 in pre-hydrolyzed solution, processed under normal temperature
Micro-filtration removal precipitation after 2 hours.Regulation pH to 5, is 400ml by volume, and initial conductivity is injected for the pre-hydrolyzed solution of 46ms/cm
In electric dialyzator, electrodialysis condition is constant current strength 0.10A, initial voltage 10V, anion-exchange membrane and cation exchange
Membrane area is 95 × 215mm2, rate of circulating flow be 0.5L/min.After operation electrodialysis 6 hours, pre-hydrolyzed solution in light room is taken
100ml, adds 3.5g/L peptones, 3g/L yeast extracts, 2g/L potassium dihydrogen phosphates, 1g/L magnesium sulfate, 1g/L ammonium sulfate, mixes
To 6.8, filtration sterilization is inoculated with into Pichia pastoris CBS6054, after 72 hours final result display processings of culture regulation pH value after even
Pre-hydrolyzed solution total phenol content reduction by 50%, furfural and hydroxymethyl furfural content reduction by 60%, acetic acid and formic acid content reduction by 80%,
And reduced sugar loss late only has 5% in pre-hydrolyzed solution, Pichia pastoris in pre-hydrolyzed solution growth rate up to pure sugar culture-medium
87%.
Embodiment 3：
During 1kg peeling masson pine wood chip and 10kg water added into digester jointly, 20-60min is warming up to 180 degree, keeps
This temperature 1 hour, separates wood chip after pre-hydrolyzed solution and pretreatment after being cooled to 60 DEG C.By prehydrolysis under the conditions of being 50 DEG C in temperature
After liquid vacuum distillation concentrates 8 times, pre-hydrolyzed solution pH to 2.5 is adjusted by 1M nitric acid of concentration, stand 30 minutes, filtered and collected
Pre-hydrolyzed solution after filter.Pre-hydrolyzed solution pH to 9.0 is adjusted with ammoniacal liquor, 30 minutes are stood, pre-hydrolyzed solution after filtering is filtered and collect.Connect
To adding hydrogen peroxide in pre-hydrolyzed solution and being passed through ozone respectively to 8g/L and 0.5g/L, it is micro- after being processed 7 hours under 35 degrees Celsius
Filter off except precipitation.Regulation pH to 9, is 500ml by volume, and initial conductivity is the pre-hydrolyzed solution injection electric dialyzator of 50ms/cm
In, electrodialysis condition is that constant current strength 2.5A, initial voltage 50V, anion-exchange membrane and cation exchange membrane area are equal
It is 95 × 215mm2, rate of circulating flow be 0.5L/min.After operation electrodialysis 6 hours, pre-hydrolyzed solution 100ml in light room is taken, added
3.5g/L peptones, 3g/L yeast extracts, 2g/L potassium dihydrogen phosphates, 1g/L magnesium sulfate, 1g/L ammonium sulfate, adjust pH after mixing
To 6.8, filtration sterilization is inoculated with into Pichia pastoris CBS6054 value, cultivates 72 hours.Pre-hydrolyzed solution after final result display processing
Total phenol content reduction by 81%, furfural and hydroxymethyl furfural content reduction by 66%, acetic acid and formic acid content reduction by 82%, and prehydrolysis
Reduced sugar loss late only has 4.4% in liquid, Pichia pastoris in pre-hydrolyzed solution growth rate up to pure sugar culture-medium 90%.
Embodiment 4：
During 1kg peeling bamboo bamboo chip and 8kg water added into digester jointly, 20-60min is warming up to 120 degree, keeps this temperature
Degree 0.5 hour, separates wood chip after pre-hydrolyzed solution and pretreatment after being cooled to 30 DEG C.By pre-hydrolyzed solution under the conditions of being 55 DEG C in temperature
After vacuum distillation concentrates 6 times, pre-hydrolyzed solution pH to 1.5 is adjusted by 1M phosphoric acid of concentration, stand 30 minutes, filter and collect filtering
Pre-hydrolyzed solution afterwards.Pre-hydrolyzed solution pH to 8.0 is adjusted with ammoniacal liquor, 30 minutes are stood, pre-hydrolyzed solution after filtering is filtered and collect.Then
To ozone is added in pre-hydrolyzed solution to 1.5g/L, micro-filtration removal is precipitated after being processed 5 hours at 8.0,25 DEG C of pH.PH is to 5 for regulation,
It is 400ml by volume, during initial conductivity is for the pre-hydrolyzed solution injection electric dialyzator of 46ms/cm, electrodialysis condition is constant electricity
Intensity of flow 10A, initial voltage 20V, anion-exchange membrane and cation exchange membrane area are 95 × 215mm2, rate of circulating flow be
0.5L/min.After operation electrodialysis 6 hours, pre-hydrolyzed solution 100ml in light room is taken, add 3.5g/L peptones, 3g/L yeast to take out
Extract, 2g/L potassium dihydrogen phosphates, 1g/L magnesium sulfate, 1g/L ammonium sulfate, adjust pH value to 6.8 after mixing, filtration sterilization, be inoculated with into
Pichia pastoris CBS6054, cultivates 72 hours.After final result display processing pre-hydrolyzed solution total phenol content reduction by 70%, furfural and
Hydroxymethyl furfural content reduction by 60%, acetic acid and formic acid content reduction by 90%, and reduced sugar loss late only has in pre-hydrolyzed solution
4.2%, Pichia pastoris in pre-hydrolyzed solution growth rate with pure sugar culture-medium without significant difference.
Embodiment 5：
During 1kg peeling falx straw piece and 6kg water added into digester jointly, 20-60min is warming up to 140 degree, keeps this temperature
Degree 2 hours, separates wood chip after pre-hydrolyzed solution and pretreatment after being cooled to 80 DEG C.Pre-hydrolyzed solution is subtracted under the conditions of being 45 DEG C in temperature
After 5 times of distillation and concentration of pressure, pre-hydrolyzed solution pH to 2.5 is adjusted by 1M sulfuric acid of concentration, stand 30 minutes, after filtering and collecting filtering
Pre-hydrolyzed solution.Pre-hydrolyzed solution pH to 8.0 is adjusted with NaOH, 30 minutes are stood, pre-hydrolyzed solution after filtering is filtered and collect.Connect
To hydrogen peroxide is added in pre-hydrolyzed solution to 2g/L, micro-filtration removal is precipitated after being processed 5 hours at 7.0,50 DEG C of pH.Regulation pH to
4.5, it is 400ml by volume, during initial conductivity is for the pre-hydrolyzed solution injection electric dialyzator of 46ms/cm, electrodialysis condition is perseverance
Determine voltage 0.5V, initial current 0.25A, anion-exchange membrane and cation exchange membrane area and be 95 × 215mm2, recycle stream
Speed is 1L/min.After operation electrodialysis 4 hours, pre-hydrolyzed solution 100ml in light room is taken, add 3.5g/L peptones, 3g/L yeast
Extract, 2g/L potassium dihydrogen phosphates, 1g/L magnesium sulfate, 1g/L ammonium sulfate, adjust pH value to 6.8, filtration sterilization, inoculation after mixing
Enter Pichia pastoris CBS6054, cultivate 72 hours.Pre-hydrolyzed solution total phenol content reduction by 70%, furfural after final result display processing
With hydroxymethyl furfural content reduction by 60%, acetic acid and formic acid content reduce by 90%, and reduced sugar loss late only has in pre-hydrolyzed solution
4.2%, Pichia pastoris in pre-hydrolyzed solution growth rate with pure sugar culture-medium without significant difference.
Embodiment 6：
By in 1kg peeling sorghum bar segment addition digesters, steam is passed through, the boiling temperature of steam is 160 DEG C, keeps this temperature
Degree 3 hours, separates wood chip after pre-hydrolyzed solution and pretreatment after being cooled to 40 DEG C.Pre-hydrolyzed solution is subtracted under the conditions of being 60 DEG C in temperature
After 7 times of distillation and concentration of pressure, pre-hydrolyzed solution pH to 1.0 is adjusted by 1M hydrochloric acid of concentration, stand 30 minutes, after filtering and collecting filtering
Pre-hydrolyzed solution.Pre-hydrolyzed solution pH to 10.0 is adjusted with potassium hydroxide, 30 minutes are stood, pre-hydrolyzed solution after filtering is filtered and collect.
Then to adding hydrogen peroxide and ferrous sulfate respectively to processing 0.5 at 1g/L and 10.0,60 DEG C of 0.5g/L, pH in pre-hydrolyzed solution
Micro-filtration removal precipitation after hour.Regulation pH to 2.0, is 400ml by volume, and initial conductivity is noted for the pre-hydrolyzed solution of 46ms/cm
Enter in electric dialyzator, electrodialysis condition is constant voltage 300V, initial current 50A, anion-exchange membrane and cation-exchange membrane
Area is 95 × 215mm2, rate of circulating flow be 1L/min.After operation electrodialysis 4 hours, pre-hydrolyzed solution 100ml in light room is taken,
3.5g/L peptones, 3g/L yeast extracts, 2g/L potassium dihydrogen phosphates, 1g/L magnesium sulfate, 1g/L ammonium sulfate are added, is adjusted after mixing
To 6.8, filtration sterilization is inoculated with into Pichia pastoris CBS6054 section pH value, cultivates 72 hours.Pre- water after final result display processing
Solution liquid total phenol content reduction by 72%, furfural and hydroxymethyl furfural content reduction by 65%, acetic acid and formic acid content reduction by 90%, and it is pre-
Reduced sugar loss late only has 4.2% in hydrolyzate, Pichia pastoris in pre-hydrolyzed solution growth rate with pure sugar culture-medium without notable
Difference.
Embodiment 7：
By in 1kg peeling cotton stem addition digesters, steam is passed through, the boiling temperature of steam is 150 DEG C, keeps this temperature
2 hours, wood chip after pre-hydrolyzed solution and pretreatment is separated after being cooled to 60 DEG C.Pre-hydrolyzed solution is depressurized under the conditions of being 40 DEG C in temperature
After 9 times of distillation and concentration, pre-hydrolyzed solution pH to 2.0 is adjusted by 1M nitric acid of concentration, stand 30 minutes, filter and collect pre- after filtering
Hydrolyzate.Pre-hydrolyzed solution pH to 7.0 is adjusted with NaOH, 30 minutes are stood, pre-hydrolyzed solution after filtering is filtered and collect.Then
To ozone is added in pre-hydrolyzed solution to 1g/L, micro-filtration removal is precipitated after being processed 24 hours at 2.0,20 DEG C of pH.Regulation pH to 7, will
Volume is 400ml, and during initial conductivity is for the pre-hydrolyzed solution injection electric dialyzator of 46ms/cm, electrodialysis condition is constant voltage
100V, initial current 25A, anion-exchange membrane and cation exchange membrane area are 95 × 215mm2, rate of circulating flow be 1L/
min.After operation electrodialysis 4 hours, take pre-hydrolyzed solution 100ml in light room, add 3.5g/L peptones, 3g/L yeast extracts,
2g/L potassium dihydrogen phosphates, 1g/L magnesium sulfate, 1g/L ammonium sulfate, adjust pH value to 6.8 after mixing, filtration sterilization is inoculated with into complete red
Yeast CBS6054, cultivates 72 hours.Pre-hydrolyzed solution total phenol content reduction by 70%, furfural and hydroxyl first after final result display processing
Base furfural content reduction by 60%, acetic acid and formic acid content reduction by 90%, and reduced sugar loss late only has 5% in pre-hydrolyzed solution, finishes
Red yeast in pre-hydrolyzed solution growth rate with pure sugar culture-medium without significant difference.
Embodiment 8 (comparative examples, only advanced oxidation)
During 1kg peeling poplar wood chip and 6kg water added into digester jointly, 20-60min is warming up to 160 degree, keeps this temperature
Degree 2 hours, separates wood chip after pre-hydrolyzed solution and pretreatment after being cooled to 40 DEG C.Pre-hydrolyzed solution is subtracted under the conditions of being 40 DEG C in temperature
After 5 times of distillation and concentration of pressure, pre-hydrolyzed solution pH to 2.5 is adjusted by 1M sulfuric acid of concentration, stand 30 minutes, after filtering and collecting filtering
Pre-hydrolyzed solution.Pre-hydrolyzed solution pH to 8.0 is adjusted with NaOH, 30 minutes are stood, pre-hydrolyzed solution after filtering is filtered and collect.Connect
To hydrogen peroxide is added in pre-hydrolyzed solution to 3g/L, pH 8.0, micro-filtration removal is precipitated after being processed 3 hours under normal temperature.Add 3.5g/
L peptones, 3g/L yeast extracts, 2g/L potassium dihydrogen phosphates, 1g/L magnesium sulfate, 1g/L ammonium sulfate, after mixing adjust pH value to
6.8, filtration sterilization is inoculated with into Pichia pastoris CBS6054, is cultivated 72 hours.Final result shows pre- after simple dioxygen water process
Hydrolyzate total phenol content reduction by 60%, furfural and hydroxymethyl furfural content reduction by 20%, acetic acid and formic acid content rising 10%, but
It is that Pichia pastoris growth rate in pre-hydrolyzed solution after dioxygen water process is only the 40% of pure sugar culture-medium, and is also significantly lower than
Growth rate (as shown in Figure 1) of the Pichia pastoris in hydrogen peroxide and electrodialysis Combined Processing (embodiment 1) afterwards pre-hydrolyzed solution.
Embodiment 9 (comparative examples, only electrodialysis)
During 1kg peeling poplar wood chip and 6kg water added into digester jointly, 20-60min is warming up to 160 degree, keeps this temperature
Degree 2 hours, separates wood chip after pre-hydrolyzed solution and pretreatment after being cooled to 40 DEG C.Pre-hydrolyzed solution is subtracted under the conditions of being 40 DEG C in temperature
After 5 times of distillation and concentration of pressure, pre-hydrolyzed solution pH to 2.5 is adjusted by 1M sulfuric acid of concentration, stand 30 minutes, after filtering and collecting filtering
Pre-hydrolyzed solution.Pre-hydrolyzed solution pH to 8.0 is adjusted with NaOH, 30 minutes are stood, pre-hydrolyzed solution after filtering is filtered and collect, adjusted
Section pre-hydrolyzed solution pH to 4.5, is 400ml by volume, during initial conductivity is for the pre-hydrolyzed solution injection electric dialyzator of 40ms/cm,
Electrodialysis condition is 95 for constant voltage 4V, initial current 0.25A, anion-exchange membrane and cation exchange membrane area ×
215mm2, rate of circulating flow be 1L/min.After operation electrodialysis 4 hours, pre-hydrolyzed solution 100ml in light room is taken, add 3.5g/L eggs
White peptone, 3g/L yeast extracts, 2g/L potassium dihydrogen phosphates, 1g/L magnesium sulfate, 1g/L ammonium sulfate, adjust pH value to 6.8 after mixing,
Filtration sterilization, is inoculated with into Pichia pastoris CBS6054, cultivates 72 hours.Although final result shows after treatment second in pre-hydrolyzed solution
Acid and formic acid content reduction by 90%, but furfural and hydroxymethyl furfural content only reduce by 20%, and total phenol content also only reduces by 25%,
Significantly Pichia pastoris growth rate in simple electrodialysis pre-hydrolyzed solution can hardly grow (Fig. 1).
Claims (8)
1. there is the preparation technology of the lignocellulosic slurrying pre-hydrolyzed solution of high-efficiency fermenting ability, it is characterised in that：Including following
Step：
1. slurrying pre-hydrolyzed solution is prepared；2. concentrate and except precipitation；3. advanced oxidation treatment；4. electrodialysis process；
It is pulping raw material of paper making that 1. the step prepares the material that slurrying pre-hydrolyzed solution uses；
What the 3. advanced oxidation was processed concretely comprises the following steps：Certain density advanced oxidation reagent is added into 2. concentration and except precipitation
In pre-hydrolyzed solution afterwards, a period of time is processed under certain pH value and temperature conditionss, liquid phase pre-hydrolyzed solution is collected in filtering；
4. the electrodialysis process is concretely comprised the following steps：The pH value of the 3. pre-hydrolyzed solution that advanced oxidation treatment is obtained is adjusted, then
Electrodialysis process is carried out in the light room for injecting electric dialyzator, the pre-hydrolyzed solution in light room is collected after treatment, obtained final product with efficiently hair
The lignocellulosic slurrying pre-hydrolyzed solution of ferment ability；
Wherein, the advanced oxidation reagent in 3. advanced oxidation treatment be hydrogen peroxide, ozone, hydrogen peroxide/ozone mixture or
Hydrogen peroxide/ferrous sulfate mixture；The concentration of the hydrogen peroxide is 1-10g/L, and the concentration of the ozone is 0.5-2g/L, described
The concentration of ferrous sulfate is 0.1-2g/L；Each component is dense in hydrogen peroxide/ozone mixture and hydrogen peroxide/ferrous sulfate mixture
Degree scope is identical with exclusive use；The pH value of the advanced oxidation is 2-10, and temperature is 20-60 DEG C, and process time is 0.5-24
Hour.
2. the preparation technology of the lignocellulosic slurrying pre-hydrolyzed solution with high-efficiency fermenting ability according to claim 1,
It is characterized in that：4. the middle pre-hydrolyzed solution pH value for injecting light room is 2-9 to the step；The voltage that the electrodialysis process is used for
0.5-300V, the electric current for using is 0.1-50A, and the anion-exchange membrane and cation-exchange membrane for using are 1-500 pairs；Described the moon
The area of amberplex and cation-exchange membrane is respectively 50 × 50-1000 × 2000mm2。
3. the preparation technology of the lignocellulosic slurrying pre-hydrolyzed solution with high-efficiency fermenting ability according to claim 2,
It is characterized in that：The concentration of the hydrogen peroxide is 2-8g/L, and the concentration of the ozone is 1-2g/L, the concentration of the ferrous sulfate
It is 0.2-1g/L；The pH value of the advanced oxidation is 5-9, and temperature is 25-50 DEG C, and process time is 2-7 hours.
4. the preparation technology of the lignocellulosic slurrying pre-hydrolyzed solution with high-efficiency fermenting ability according to claim 2,
It is characterized in that：The concentration of the hydrogen peroxide is 3-5g/L, and the concentration of the ozone is 1-1.5g/L, the ferrous sulfate it is dense
It is 0.2-0.5g/L to spend；The pH value of the advanced oxidation is 7-9, and temperature is 25-35 DEG C, and process time is 5-6 hours.
5. the preparation technology of the lignocellulosic slurrying pre-hydrolyzed solution with high-efficiency fermenting ability according to claim 1,
It is characterized in that：It is hot water prehydrolysis process or steam prehydrolysis process that 1. the step prepares the method that slurrying pre-hydrolyzed solution uses；
The hot water prehydrolysis process is after material is mixed with water, to be warming up to uniform temperature, and insulation is cooled down after a period of time；The steam
Prehydrolysis process is that raw material is placed in container, is passed through the steam of uniform temperature, and insulation is cooled down after a period of time.
6. the preparation technology of the lignocellulosic slurrying pre-hydrolyzed solution with high-efficiency fermenting ability according to claim 5,
It is characterized in that：Material and the mass ratio of water are 1 in the hot water prehydrolysis process:3-1:10, the heating-up time is 20-60 minutes,
Treatment temperature is 120-180 DEG C, and soaking time is 30-240 minutes, and temperature is 30-80 DEG C after cooling；The steam prehydrolysis process
Middle vapor (steam) temperature is 120-180 DEG C, and soaking time is 30-240 minutes, and temperature is 30-80 DEG C after cooling.
7. the preparation technology of the lignocellulosic slurrying pre-hydrolyzed solution with high-efficiency fermenting ability according to claim 1,
It is characterized in that：3. the step concentrates and concretely comprising the following steps except precipitation：The slurrying pre-hydrolyzed solution that 1. step is prepared is used
The mode of vacuum distillation is concentrated, and pH value is then adjusted for the first time, is 1.0-2.5, standing, separation of solid and liquid to pH value；Then
Second regulation pH value, is 7-10 to pH value, is concentrated and except the pre-hydrolyzed solution after precipitation after standing, filtering.
8. the preparation technology of the lignocellulosic slurrying pre-hydrolyzed solution with high-efficiency fermenting ability according to claim 7,
It is characterized in that：3. the step concentrates and except the temperature of vacuum distillation in precipitation is 40-60 DEG C, pre-hydrolyzed solution is dense after concentration
Spend is original 5-10 times；The first time regulation pH value uses hydrochloric acid, sulfuric acid, nitric acid or phosphoric acid；Adjust for described second
Section pH value uses NaOH, potassium hydroxide or ammoniacal liquor.
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| CN102719490A (en) * | 2012-07-05 | 2012-10-10 | 南京林业大学 | Detoxification method of wood fiber hydrolyzed sugar liquid |
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