CN105350369A - Preparation process of lignocellulose pulping pre-hydrolysis liquid having efficient fermentation capability - Google Patents
Preparation process of lignocellulose pulping pre-hydrolysis liquid having efficient fermentation capability Download PDFInfo
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- D—TEXTILES; PAPER
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- C12P2203/00—Fermentation products obtained from optionally pretreated or hydrolyzed cellulosic or lignocellulosic material as the carbon source
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Abstract
The invention provides a preparation process of lignocellulose pulping pre-hydrolysis liquid having efficient fermentation capability based on an advanced oxidation process and electrodialysis treatment against the problems of lignocellulose hydrolysis liquid detoxification in the prior art. The preparation process comprises the following steps: 1, preparing pulping pre-hydrolysis liquid; 2, conducting concentration, and removing sediment; 3, conducting advanced oxidation treatment; 4, conducting electrodialysis treatment. According to the preparation process, the pre-hydrolysis liquid generated in the production processes of chemimechanical pulp and dissolving pulp in the pulping and papermaking industry serves as the treatment object, firstly, organic inhibitor molecules are degraded through advanced oxidized reagent, subsequently, electrolyte inhibitor in the hydrolysis liquid is removed through an electrodialysis method, and the advanced oxidized reagent and the electrodialysis method achieve a remarkable synergistic effect. The pre-hydrolysis liquid prepared through the preparation method can serve as a fermentation carbon source and be used for fermenting and producing unicellular protein or preparing high value-added compounds. By means of a detoxificaiton method of the preparation process, under the circumstance that fermentable sugar cannot be lost, small-molecule inhibitor such as phenols can be removed, and ionogenic inhibitor can be removed.
Description
Technical field
The invention belongs to bioenergy and pulping and paper-making field, be specifically related to a kind of preparation technology of lignocellulose slurrying pre-hydrolyzed solution, particularly relate to a kind of process adopting advanced oxidation processes and electroosmose process preparation to have the lignocellulose slurrying pre-hydrolyzed solution of high-efficiency fermenting ability.
Background technology
Due to the excellent pulping and paper-making immense pressure that there is lack of raw materials, traditional resource price continuous rise, labor cost rise and globalized competetion brings, current traditional enterprises in pulp and paper industry is faced with unprecedented difficulty.Simple old business model lignocellulose being changed into paper pulp and sheet paper products has been difficult to applicable existing market.Pulp and paper industry is combined with biorefinery, before slurrying, prehydrolysis is carried out to string resource, the energy consumption in digestion process can not only be reduced, reduce the consumption of bleaching liquor in bleaching process, improve pulp quality simultaneously, also can reduce BOD and COD of pulping and papermaking processes waste water, reduce greenhouse gas emissions, and the hemicellulose that obtains of preliminary treatment and lignin can also for the production of the biomass fuel of high added value and living beings chemicals etc.Researcher has developed the manufacturing technique of prehydrolysis-chemi-mechanical pulp and prehydrolysis sulphite dissolving pulp, apply sour prehydrolysis, hot water prehydrolysis or steam prehydrolysis method to the leading prehydrolysis of pulping materials with extracting hemicelluloses.In slurrying pre-hydrolyzed solution and acid hydrolysis products thereof; except the hemicellulose of degraded, wood sugar, except glucose; also inevitably produce the inhibitor hindering biological utilisation; the acetic acid that the hydroxymethylfurfural that such as cellulose degradation produces, hemicellulose degradation produce, furfural, levulinie acid and formic acid, lignin degradation produce Small molecular aldehydes matter (4-HBA, vanillic aldehyde and catechol) etc.Fermentation inhibitor in slurrying pre-hydrolyzed solution has that kind is many, concentration range wide (a few microgram is to tens grams), the features such as chemical property is complicated.
For the problems referred to above, researcher develops the multiple poison-removing method for lignocellulose acid hydrolysis liquid, main physically based deformation effect, chemical action or biological agent.
(1) physical method comprises evaporation, organic solvent extraction, active carbon, ion exchange resin, UF membrane etc.1. rotary evaporation can reduce low-boiling-point organic compound in hydrolyzate, as the concentration of acetic acid, furfural and aldehydes vanillic aldehyde etc., but can produce again new inhibitor under high temperature, thus cause fermentation efficiency to reduce.2. apply the volatile organic solvent extraction such as ether, ethyl acetate hydrolyzate and can remove most of mortifier, but there is the shortcoming of organic difficult solvent recovery and organic solvent residual.3. active carbon has stronger characterization of adsorption, but the suppressed properties of the absorption of active carbon on mortifier, pre-hydrolyzed solution pH, pretreatment temperature, time and concentration of activated carbon impact, and remove the limitation of mortifier.4. ion exchange resin absorption is remarkable to the removal effect of faintly acid mortifier, but limited to the removal effect of furfural class suppression, and this method also can remove a large amount of fermentable sugars while removing inhibiting substances, causes the output of tunning significantly to reduce.5. UF membrane can remove the mortifier such as furfural, hydroxymethylfurfural, acetic acid in hydrolyzate, but effectively can not remove the micromolecule phenolic close with glucose and xylose molecular weight.
(2) chemical Treatment mainly makes the mortifier in pre-hydrolyzed solution form precipitation or by adjust pH, the ionization property of mortifier be changed by adding aqueous slkali (calcium hydroxide or NaOH), thus reaches and fall hypotoxic object.Usual employing changes the pH value of hydrolyzate and reduces the method for the toxicity of fermentation inhibitor, and wherein that the most frequently used is excess amount of Ca (OH)
2neutralisation.This method treated water solution liquid, fermentability obviously strengthens, and simple to operate, with low cost, mortifier removal effect is obvious.But, due to the precipitation of calcium ion, very easily follow-up fermentation and product separation are had a negative impact.
(3) bioanalysis refers to that making it structure with some specific enzymes (laccase, peroxidase) or microbiological treatment mortifier changes thus reduce its toxicity.Because enzymatic has specificity and selectivity, so ferment treatment also can only remove certain mortifier specific.Although microbial pretreatment can have certain detoxification to the mortifier in pre-hydrolyzed solution, the various carbohydrate in detoxification microbial consumption pre-hydrolyzed solution and this method requires that the processing time is long.
In sum, existing single poison-removing method has extremely significantly limitation, causes it efficiently can not remove inhibitor.
Advanced oxidation processes take hydroxy radical as oxidant, with organic matter generation oxidation reaction in solution, by reactions such as replacement, scission of link, electro transfer, combinations, make the difficult degradation in solution, larger molecular organics is oxidized into small-molecule substance, even direct oxidation is degraded into CO
2and H
2o.Small molecular aromatic compounds in solution such as aromatic aldehyde, aromatic ester or aromatic acid can be degraded to long chain and alkane by advanced oxidation processes, and last mineralising is CO
2and H
2o.Because high-level oxidation technology is widely used in the biodegradable improving waste water, this technology is mainly used in drinking water treatment, special industrial water treatment, the process of poisonous and harmful high concentrated organic wastewater and the Sewage advanced treatment etc. for the purpose of reuse at present.Application for a patent for invention 201410052519.4 disclosed " a kind of method of ferrous salt activation persulfate or single peroxosulphuric hydrogen salt advanced oxidation Papermaking Wastewater Advanced Treatment ".Persulfate or single peroxosulphuric hydrogen salt and ferrous salt is adopted to react the organic matter generated in strong oxidizing property potentiometric titrations oxidative degradation paper waste.It is high that the method has efficiency, easy to operate, the feature that applicable pH range is wider.But, the method is applied to the detoxification of slurrying pre-hydrolyzed solution, then can produces high concentration sulfate, be unfavorable for very much the biofermentation of follow-up slurrying pre-hydrolyzed solution.This is because, with the object of water treatment field application advanced oxidation unlike, water treatment field is that all organic matters of nonselective degraded are different, and the detoxification of slurrying pre-hydrolyzed solution requires it is optionally remove Small molecular aromatics inhibitor not degrading fermentable sugars while.In addition, (the Silva such as Silva, etal.BiotechnologyforBiofuel, 2013,6:23) report the method for application advanced oxidation processes process straw dilute acid hydrolysis liquid, but although the method can remove aromatic compounds, effectively can not remove organic acid (formic acid, the acetic acid) fermentation inhibitor produced in original in acid hydrolysis liquid and advanced oxidation processes, therefore be unsuitable for the detoxification requirement of the slurrying pre-hydrolyzed solution of high organic acid content.Further, its handling object is simple straw acid hydrolysis liquid, has the different of essence from slurrying pre-hydrolyzed solution of the present invention.
At present, electrodialysis is mainly used in waste water desalting processing and product separation field, therefore, its Application Areas and the field difference belonging to the present invention very large.In addition, simple electrodialysis can only remove the organic acid inhibitor such as formic acid and acetic acid in slurrying pre-hydrolyzed solution, and almost can not remove aromatics micromolecular inhibitor, this just causes simple electrodialysis can not realize the high-efficiency detoxicating of slurrying pre-hydrolyzed solution.
Summary of the invention
For prior art Problems existing in ligno-cellulose hydrolysate detoxification, the invention provides a kind of preparation method with the slurrying pre-hydrolyzed solution of high-efficiency fermenting ability based on advanced oxidation processes and electrodialysis process.The poison-removing method of the present invention's exploitation when not losing fermentable sugars, not only can be removed the micromolecular inhibitors such as phenols but also can remove ionogenic inhibitor.
The principle of preparation technology: the aromatic class fermentation inhibitor (aromatic aldehyde, aromatic ester or aromatic acid etc.) in slurrying pre-hydrolyzed solution is degraded to the small molecular organic acids such as formic acid, without the inhibiting acid amides of fermentation and alkane, is even degraded to CO by the hydroxy radical that (1) utilizes advanced oxidation reagent place to produce
2and H
2o; (2) then electrodialysis technique removes the ionogenic fermentation inhibitor in pre-hydrolyzed solution, such as formic acid, acetic acid and sulfate etc., its cardinal principle is under DC electric field effect, anion-permeable cavity block anode direction in slurrying hydrolyzate is moved and enters dense room, being subject to anode membrane stop stays in dense room, and the cation permeable anode membrane in hydrolyzate also enters dense room after cathode direction migration, be subject to cavity block stop and be trapped within dense room.Therefore, the acid in light room is removed.And sugar is non-electrolyte, can not move under the electric field, can be retained in light room in principle.Electrodialysis effectively can remove the impurity of acid in slurrying hydrolyzate and other ionic condition, greatly can reduce the loss late of product and the acid of reclaiming in hydrolyzate.
Technical scheme of the present invention: the preparation technology with the lignocellulose slurrying pre-hydrolyzed solution of high-efficiency fermenting ability, comprises the following steps: 1. prepare slurrying pre-hydrolyzed solution; 2. concentrate and remove precipitation; 3. advanced oxidation process; 4. electrodialysis process.
The material that 1. described step prepares the employing of slurrying pre-hydrolyzed solution is pulping raw material of paper making.The method that 1. described step prepares the employing of slurrying pre-hydrolyzed solution is hot water prehydrolysis process or steam prehydrolysis process; Described hot water prehydrolysis process is that hot water raw material being placed in 70-100 DEG C soaks 10-60 minute, then in raw material, adds water, is warming up to uniform temperature, without Additional pressurizations, cools after insulation a period of time; Described steam prehydrolysis process, for be placed in container by raw material, passes into the steam of uniform temperature, without Additional pressurizations, cools after insulation a period of time.
The concrete steps that 2. described step concentrated and removed precipitation are: slurrying pre-hydrolyzed solution step 1. prepared adopts the mode of decompression distillation to concentrate, then first time adjust ph, be 1.0-2.5 to pH value, to precipitate lignin, then carry out Separation of Solid and Liquid to remove lignin deposit and to collect pre-hydrolyzed solution; Then second time adjust ph, is 7-10 to pH value, leaves standstill, crosses filtering precipitation, obtains concentrated and except the pre-hydrolyzed solution after precipitation.
The concrete steps of described 3. advanced oxidation process are: added by certain density advanced oxidation reagent in the pre-hydrolyzed solution after 2. concentrating and remove precipitation, a period of time is processed under certain pH value and temperature conditions, the colloidal precipitation thing produced in micro-filtration Transformatin process, collects liquid phase pre-hydrolyzed solution.
The concrete steps of described 4. electrodialysis process are: the pH value of the pre-hydrolyzed solution regulating 3. advanced oxidation process to obtain, then the light room of electric dialyzator is injected, under the DC electric field effect of constant voltage or constant current, anion-permeable anion-exchange membrane anode direction in slurrying pre-hydrolyzed solution is moved and enters dense room, is subject to staying in dense room after cation-exchange membrane stops.In like manner, the cation permeable cation-exchange membrane in pre-hydrolyzed solution also enters dense room after cathode direction migration, is subject to anion-exchange membrane stop and is trapped within dense room.Collect the pre-hydrolyzed solution in light room after process, the slurrying pre-hydrolyzed solution of low fermentation inhibitors must be had.
The pre-hydrolyzed solution that the present invention produces with pulp and paper industry chemi-mechanical pulp and dissolving pulp production process is for handling object, first advanced oxidation reagent degraded organic inhibitor molecule is applied, then the electrolyte inhibitor in electroosmose process removal pre-hydrolyzed solution is used, comprise acetic acid, formic acid and sulfate, the two is mutually combined and defines cooperative effect significantly.
Wherein, described step 1. in pulping raw material of paper making can be the material of any lignocellulose-containing; comprise poplar, Eucalyptus, birch, larch, Korean pine, masson pine, pinus yunnanensis, pinus sylvestris var. mongolica, reed, bamboo, wheat, paddy rice, Chinese alpine rush, Chinese sorghum, sugarcane, wheat, flax, jute, mestha, Tan Shu, mulberry or cotton stalk, and its any combination.The material of described lignocellulose-containing comprises the stem of above-mentioned material, root, bar, blade, skin or shell, and its any combination.In described hot water prehydrolysis process, the mass ratio of material and water is 1:3-1:10, and the heating-up time is 20-60 minute, and treatment temperature is 120-180 DEG C, and temperature retention time is 30-240 minute, and after cooling, temperature is 30-80 DEG C; In described steam prehydrolysis process, vapor (steam) temperature is 120-180 DEG C, and temperature retention time is 30-240 minute, and after cooling, temperature is 30-80 DEG C.
Wherein, the temperature that 2. described step concentrated and removed decompression distillation in precipitation is 40 – 60 DEG C, and after concentrated, the concentration of pre-hydrolyzed solution is original 5-10 times; What described first time, adjust ph adopted is hydrochloric acid, sulfuric acid, nitric acid or phosphoric acid; What described second time adjust ph adopted is NaOH, potassium hydroxide or ammoniacal liquor.
Wherein, the advanced oxidation reagent in the process of described 3. advanced oxidation is hydrogen peroxide, ozone, hydrogen peroxide/ozone mixture or hydrogen peroxide/ferrous sulfate mixture.The concentration of described hydrogen peroxide is 1-10g/L, and the concentration of described ozone is 0.5-2g/L, and the concentration of described ferrous sulfate is 0.1-2g/L.In hydrogen peroxide/ozone mixture and hydrogen peroxide/ferrous sulfate mixture each component concentration range be used alone identical.The pH value of described advanced oxidation is 2-10, and temperature is 20-60 DEG C, and the processing time is 0.5-24 hour.Preferably, the concentration of described hydrogen peroxide is 2-8g/L, and the concentration of described ozone is 1-2g/L, and the concentration of described ferrous sulfate is 0.2-1g/L; The pH value of described advanced oxidation is 5-9, and temperature is 25-50 DEG C, and the processing time is 2-7 hour.Be more preferably, the concentration of described hydrogen peroxide is 3-5g/L, and the concentration of described ozone is 1-1.5g/L, and the concentration of described ferrous sulfate is 0.2-0.5g/L; The pH value of described advanced oxidation is 7-9, and temperature is 25-35 DEG C, and the processing time is 5-6 hour.
Wherein, described step 4. in inject the pre-hydrolyzed solution pH value of light room be 2-9; The voltage that described electrodialysis process adopts is 0.5-300V, and the electric current of employing is 0.1-50A, and the anion-exchange membrane of employing and cation-exchange membrane are 1-500 couple; The area of described anion-exchange membrane and cation-exchange membrane is respectively 50 × 50-1000 × 2000mm
2.Preferably, step 4. in inject the pre-hydrolyzed solution pH value of light room be 3.5-7.It is further preferred that step 4. in inject the pre-hydrolyzed solution pH value of light room be 4.5-5.
According to the purposes with the lignocellulose slurrying pre-hydrolyzed solution of high-efficiency fermenting ability prepared by said method, be used for fermenting and producing SCP or preparation high added value compound as fermenting carbon source; Described high added value compound is wood sugar, xylitol, wood oligose, arabinose or arabite.
The novelty of the present invention advanced oxidation processes of gentleness is combined with electrodialysis methods, apply improved gentle advanced oxidation processes degraded aromatics fermentation inhibitor, electrodialysis method removes the ionizable fermentation inhibitors such as organic acid, achieve and efficiently remove all fermentation inhibitors in slurrying pre-hydrolyzed solution when losing fermentable sugars hardly, meet the requirement of slurrying pre-hydrolyzed solution detoxification.
Beneficial effect of the present invention: compared with traditional poison-removing method, the present invention has following advantage:
(1) present invention process mild condition, can be implemented in the detoxification treatment realizing slurrying pre-hydrolyzed solution when losing fermentable sugars hardly;
(2) efficient removal of Small Phenolic Molecule and ionizable inhibitor can be realized;
(3) detoxification process mild condition, does not need high temperature and high pressure, saves the energy and cost;
(4) process equipment is simple, is easy to control, decrease production cost;
(5) in pre-hydrolyzed solution, acid can be recycled, and reduces environmental pollution, is easy to industrial applications.
Figure of description
Fig. 1 is the comparative test result of the present invention and independent advanced oxidation/independent electrodialysis process pre-hydrolyzed solution.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1:
1kg is removed the peel poplar wood chip and 6kg water adds in digester jointly, 20-60min is warming up to 160 degree, keeps this temperature 2 hours, is separated wood chip after pre-hydrolyzed solution and preliminary treatment after being cooled to 40 DEG C.By after concentrated 5 times of pre-hydrolyzed solution decompression distillation under temperature is 40 DEG C of conditions, is that 1M sulfuric acid regulates pre-hydrolyzed solution pH to 2.5 with concentration, leaves standstill 30 minutes, filter and collect and filter rear pre-hydrolyzed solution.Regulate pre-hydrolyzed solution pH to 8.0 with NaOH, leave standstill 30 minutes, filter and collect and filter rear pre-hydrolyzed solution.Then in pre-hydrolyzed solution, add hydrogen peroxide to 5g/L, pH8.0, after processing 3 hours at 30 DEG C, micro-filtration removes precipitation.Regulating pH to 4.5, is 400ml by volume, and initial conductivity is that the pre-hydrolyzed solution of 46ms/cm injects electric dialyzator, and electrodialysis condition is constant current strength 0.25A, initial voltage 4V, anion-exchange membrane and cation exchange membrane area are 95 × 215mm
2, rate of circulating flow is 0.5L/min.Run electrodialysis after 6 hours, get pre-hydrolyzed solution 100ml in light room, add 3.5g/L peptone, 3g/L yeast extract, 2g/L potassium dihydrogen phosphate, 1g/L magnesium sulfate, 1g/L ammonium sulfate, adjust ph to 6.8 after mixing, filtration sterilization, inoculates into Pichia pastoris CBS6054, cultivates 72 hours.After final result Graphics Processing, pre-hydrolyzed solution total phenol content reduces by 70%, furfural and hydroxymethyl furfural content reduce by 60%, acetic acid and formic acid content reduce by 90%, and reducing sugar loss late only has 4.2% in pre-hydrolyzed solution, Pichia pastoris in pre-hydrolyzed solution growth rate and pure sugar culture-medium without significant difference.
Embodiment 2:
1kg is removed the peel Eucalyptus wood chip and 3kg water adds in digester jointly, 20-60min is warming up to 170 degree, keeps this temperature 4 hours, is separated wood chip after pre-hydrolyzed solution and preliminary treatment after being cooled to 50 DEG C.Being by after concentrated 10 times of pre-hydrolyzed solution decompression distillation under the condition of 60 DEG C in temperature, is that the hydrochloric acid of 1M regulates pre-hydrolyzed solution pH to 2.0 with concentration, standing 30 minutes, filters and collects and filter rear pre-hydrolyzed solution.Regulate pre-hydrolyzed solution pH to 8.0 with potassium hydroxide, leave standstill 30 minutes, filter and collect and filter rear pre-hydrolyzed solution.Then in pre-hydrolyzed solution, add hydrogen peroxide and ferrous sulfate respectively to 3g/L and 0.2g/L, pH3.0, after processing 2 hours under normal temperature, micro-filtration removes precipitation.Regulating pH to 5, is 400ml by volume, and initial conductivity is that the pre-hydrolyzed solution of 46ms/cm injects electric dialyzator, and electrodialysis condition is constant current strength 0.10A, initial voltage 10V, anion-exchange membrane and cation exchange membrane area are 95 × 215mm
2, rate of circulating flow is 0.5L/min.Run electrodialysis after 6 hours, get pre-hydrolyzed solution 100ml in light room, add 3.5g/L peptone, 3g/L yeast extract, 2g/L potassium dihydrogen phosphate, 1g/L magnesium sulfate, 1g/L ammonium sulfate, adjust ph to 6.8 after mixing, filtration sterilization, inoculate into Pichia pastoris CBS6054, after cultivating 72 hours final result Graphics Processings, pre-hydrolyzed solution total phenol content reduces by 50%, furfural and hydroxymethyl furfural content reduce by 60%, acetic acid and formic acid content reduce by 80%, and reducing sugar loss late only has 5% in pre-hydrolyzed solution, Pichia pastoris growth rate in pre-hydrolyzed solution can reach pure sugar culture-medium 87%.
Embodiment 3:
1kg is removed the peel masson pine wood chip and 10kg water adds in digester jointly, 20-60min is warming up to 180 degree, keeps this temperature 1 hour, is separated wood chip after pre-hydrolyzed solution and preliminary treatment after being cooled to 60 DEG C.By after concentrated 8 times of pre-hydrolyzed solution decompression distillation under temperature is 50 DEG C of conditions, is that 1M nitric acid regulates pre-hydrolyzed solution pH to 2.5 with concentration, leaves standstill 30 minutes, filter and collect and filter rear pre-hydrolyzed solution.Regulate pre-hydrolyzed solution pH to 9.0 with ammoniacal liquor, leave standstill 30 minutes, filter and collect and filter rear pre-hydrolyzed solution.Then in pre-hydrolyzed solution, add hydrogen peroxide and pass into ozone respectively to 8g/L and 0.5g/L, after processing 7 hours under 35 degrees Celsius, micro-filtration removes precipitation.Regulating pH to 9, is 500ml by volume, and initial conductivity is that the pre-hydrolyzed solution of 50ms/cm injects electric dialyzator, and electrodialysis condition is constant current strength 2.5A, initial voltage 50V, anion-exchange membrane and cation exchange membrane area are 95 × 215mm
2, rate of circulating flow is 0.5L/min.Run electrodialysis after 6 hours, get pre-hydrolyzed solution 100ml in light room, add 3.5g/L peptone, 3g/L yeast extract, 2g/L potassium dihydrogen phosphate, 1g/L magnesium sulfate, 1g/L ammonium sulfate, adjust ph to 6.8 after mixing, filtration sterilization, inoculates into Pichia pastoris CBS6054, cultivates 72 hours.After final result Graphics Processing, pre-hydrolyzed solution total phenol content reduces by 81%, furfural and hydroxymethyl furfural content reduce by 66%, acetic acid and formic acid content reduce by 82%, and in pre-hydrolyzed solution, reducing sugar loss late only has 4.4%, and Pichia pastoris growth rate in pre-hydrolyzed solution can reach 90% of pure sugar culture-medium.
Embodiment 4:
1kg is removed the peel bamboo bamboo chip and 8kg water adds in digester jointly, 20-60min is warming up to 120 degree, keeps this temperature 0.5 hour, is separated wood chip after pre-hydrolyzed solution and preliminary treatment after being cooled to 30 DEG C.By after concentrated 6 times of pre-hydrolyzed solution decompression distillation under temperature is 55 DEG C of conditions, is that 1M phosphoric acid regulates pre-hydrolyzed solution pH to 1.5 with concentration, leaves standstill 30 minutes, filter and collect and filter rear pre-hydrolyzed solution.Regulate pre-hydrolyzed solution pH to 8.0 with ammoniacal liquor, leave standstill 30 minutes, filter and collect and filter rear pre-hydrolyzed solution.Then in pre-hydrolyzed solution, add ozone to 1.5g/L, pH8.0, after processing 5 hours at 25 DEG C, micro-filtration removes precipitation.Regulating pH to 5, is 400ml by volume, and initial conductivity is that the pre-hydrolyzed solution of 46ms/cm injects electric dialyzator, and electrodialysis condition is constant current strength 10A, initial voltage 20V, anion-exchange membrane and cation exchange membrane area are 95 × 215mm
2, rate of circulating flow is 0.5L/min.Run electrodialysis after 6 hours, get pre-hydrolyzed solution 100ml in light room, add 3.5g/L peptone, 3g/L yeast extract, 2g/L potassium dihydrogen phosphate, 1g/L magnesium sulfate, 1g/L ammonium sulfate, adjust ph to 6.8 after mixing, filtration sterilization, inoculates into Pichia pastoris CBS6054, cultivates 72 hours.After final result Graphics Processing, pre-hydrolyzed solution total phenol content reduces by 70%, furfural and hydroxymethyl furfural content reduce by 60%, acetic acid and formic acid content reduce by 90%, and reducing sugar loss late only has 4.2% in pre-hydrolyzed solution, Pichia pastoris in pre-hydrolyzed solution growth rate and pure sugar culture-medium without significant difference.
Embodiment 5:
1kg is removed the peel falx straw sheet and 6kg water adds in digester jointly, 20-60min is warming up to 140 degree, keeps this temperature 2 hours, is separated wood chip after pre-hydrolyzed solution and preliminary treatment after being cooled to 80 DEG C.By after concentrated 5 times of pre-hydrolyzed solution decompression distillation under temperature is 45 DEG C of conditions, is that 1M sulfuric acid regulates pre-hydrolyzed solution pH to 2.5 with concentration, leaves standstill 30 minutes, filter and collect and filter rear pre-hydrolyzed solution.Regulate pre-hydrolyzed solution pH to 8.0 with NaOH, leave standstill 30 minutes, filter and collect and filter rear pre-hydrolyzed solution.Then in pre-hydrolyzed solution, add hydrogen peroxide to 2g/L, pH7.0, after processing 5 hours at 50 DEG C, micro-filtration removes precipitation.Regulating pH to 4.5, is 400ml by volume, and initial conductivity is that the pre-hydrolyzed solution of 46ms/cm injects electric dialyzator, and electrodialysis condition is constant voltage 0.5V, initial current 0.25A, anion-exchange membrane and cation exchange membrane area are 95 × 215mm
2, rate of circulating flow is 1L/min.Run electrodialysis after 4 hours, get pre-hydrolyzed solution 100ml in light room, add 3.5g/L peptone, 3g/L yeast extract, 2g/L potassium dihydrogen phosphate, 1g/L magnesium sulfate, 1g/L ammonium sulfate, adjust ph to 6.8 after mixing, filtration sterilization, inoculates into Pichia pastoris CBS6054, cultivates 72 hours.After final result Graphics Processing, pre-hydrolyzed solution total phenol content reduces by 70%, furfural and hydroxymethyl furfural content reduce by 60%, acetic acid and formic acid content reduce by 90%, and reducing sugar loss late only has 4.2% in pre-hydrolyzed solution, Pichia pastoris in pre-hydrolyzed solution growth rate and pure sugar culture-medium without significant difference.
Embodiment 6:
1kg being removed the peel kaoliang stalk section adds in digester, passes into steam, and the boiling temperature of steam is 160 DEG C, keeps this temperature 3 hours, is separated wood chip after pre-hydrolyzed solution and preliminary treatment after being cooled to 40 DEG C.By after concentrated 7 times of pre-hydrolyzed solution decompression distillation under temperature is 60 DEG C of conditions, is that 1M hydrochloric acid regulates pre-hydrolyzed solution pH to 1.0 with concentration, leaves standstill 30 minutes, filter and collect and filter rear pre-hydrolyzed solution.Regulate pre-hydrolyzed solution pH to 10.0 with potassium hydroxide, leave standstill 30 minutes, filter and collect and filter rear pre-hydrolyzed solution.Then in pre-hydrolyzed solution, add hydrogen peroxide and ferrous sulfate respectively to 1g/L and 0.5g/L, pH10.0, after processing 0.5 hour at 60 DEG C, micro-filtration removes precipitation.Regulating pH to 2.0, is 400ml by volume, and initial conductivity is that the pre-hydrolyzed solution of 46ms/cm injects electric dialyzator, and electrodialysis condition is constant voltage 300V, initial current 50A, anion-exchange membrane and cation exchange membrane area are 95 × 215mm
2, rate of circulating flow is 1L/min.Run electrodialysis after 4 hours, get pre-hydrolyzed solution 100ml in light room, add 3.5g/L peptone, 3g/L yeast extract, 2g/L potassium dihydrogen phosphate, 1g/L magnesium sulfate, 1g/L ammonium sulfate, adjust ph to 6.8 after mixing, filtration sterilization, inoculates into Pichia pastoris CBS6054, cultivates 72 hours.After final result Graphics Processing, pre-hydrolyzed solution total phenol content reduces by 72%, furfural and hydroxymethyl furfural content reduce by 65%, acetic acid and formic acid content reduce by 90%, and reducing sugar loss late only has 4.2% in pre-hydrolyzed solution, Pichia pastoris in pre-hydrolyzed solution growth rate and pure sugar culture-medium without significant difference.
Embodiment 7:
Add in digester by 1kg disbarked cotton line rod, pass into steam, the boiling temperature of steam is 150 DEG C, keeps this temperature 2 hours, is separated wood chip after pre-hydrolyzed solution and preliminary treatment after being cooled to 60 DEG C.By after concentrated 9 times of pre-hydrolyzed solution decompression distillation under temperature is 40 DEG C of conditions, is that 1M nitric acid regulates pre-hydrolyzed solution pH to 2.0 with concentration, leaves standstill 30 minutes, filter and collect and filter rear pre-hydrolyzed solution.Regulate pre-hydrolyzed solution pH to 7.0 with NaOH, leave standstill 30 minutes, filter and collect and filter rear pre-hydrolyzed solution.Then in pre-hydrolyzed solution, add ozone to 1g/L, pH2.0, after processing 24 hours at 20 DEG C, micro-filtration removes precipitation.Regulating pH to 7, is 400ml by volume, and initial conductivity is that the pre-hydrolyzed solution of 46ms/cm injects electric dialyzator, and electrodialysis condition is constant voltage 100V, initial current 25A, anion-exchange membrane and cation exchange membrane area are 95 × 215mm
2, rate of circulating flow is 1L/min.Run electrodialysis after 4 hours, get pre-hydrolyzed solution 100ml in light room, add 3.5g/L peptone, 3g/L yeast extract, 2g/L potassium dihydrogen phosphate, 1g/L magnesium sulfate, 1g/L ammonium sulfate, adjust ph to 6.8 after mixing, filtration sterilization, inoculates into Pichia pastoris CBS6054, cultivates 72 hours.After final result Graphics Processing, pre-hydrolyzed solution total phenol content reduces by 70%, furfural and hydroxymethyl furfural content reduce by 60%, acetic acid and formic acid content reduce by 90%, and in pre-hydrolyzed solution, reducing sugar loss late only has 5%, Pichia pastoris in pre-hydrolyzed solution growth rate and pure sugar culture-medium without significant difference.
Embodiment 8 (comparative examples, only advanced oxidation)
1kg is removed the peel poplar wood chip and 6kg water adds in digester jointly, 20-60min is warming up to 160 degree, keeps this temperature 2 hours, is separated wood chip after pre-hydrolyzed solution and preliminary treatment after being cooled to 40 DEG C.By after concentrated 5 times of pre-hydrolyzed solution decompression distillation under temperature is 40 DEG C of conditions, is that 1M sulfuric acid regulates pre-hydrolyzed solution pH to 2.5 with concentration, leaves standstill 30 minutes, filter and collect and filter rear pre-hydrolyzed solution.Regulate pre-hydrolyzed solution pH to 8.0 with NaOH, leave standstill 30 minutes, filter and collect and filter rear pre-hydrolyzed solution.Then in pre-hydrolyzed solution, add hydrogen peroxide to 3g/L, pH8.0, after processing 3 hours under normal temperature, micro-filtration removes precipitation.Add 3.5g/L peptone, 3g/L yeast extract, 2g/L potassium dihydrogen phosphate, 1g/L magnesium sulfate, 1g/L ammonium sulfate, adjust ph to 6.8 after mixing, filtration sterilization, inoculates into Pichia pastoris CBS6054, cultivates 72 hours.After final result shows simple hydrogen peroxide process, pre-hydrolyzed solution total phenol content reduces by 60%, furfural and hydroxymethyl furfural content reduce by 20%, acetic acid and formic acid content rise 10%, but Pichia pastoris after hydrogen peroxide process in pre-hydrolyzed solution growth rate be only 40% of pure sugar culture-medium, and also remarkable in the growth rate (as shown in Figure 1) of Pichia pastoris in hydrogen peroxide and electrodialysis Combined Processing (embodiment 1) afterwards pre-hydrolyzed solution.
Embodiment 9 (comparative examples, only electrodialysis)
1kg is removed the peel poplar wood chip and 6kg water adds in digester jointly, 20-60min is warming up to 160 degree, keeps this temperature 2 hours, is separated wood chip after pre-hydrolyzed solution and preliminary treatment after being cooled to 40 DEG C.By after concentrated 5 times of pre-hydrolyzed solution decompression distillation under temperature is 40 DEG C of conditions, is that 1M sulfuric acid regulates pre-hydrolyzed solution pH to 2.5 with concentration, leaves standstill 30 minutes, filter and collect and filter rear pre-hydrolyzed solution.Pre-hydrolyzed solution pH to 8.0 is regulated with NaOH, leave standstill 30 minutes, filter and collect and filter rear pre-hydrolyzed solution, regulate pre-hydrolyzed solution pH to 4.5, be 400ml by volume, initial conductivity is that the pre-hydrolyzed solution of 40ms/cm injects electric dialyzator, and electrodialysis condition is constant voltage 4V, initial current 0.25A, anion-exchange membrane and cation exchange membrane area are 95 × 215mm
2, rate of circulating flow is 1L/min.Run electrodialysis after 4 hours, get pre-hydrolyzed solution 100ml in light room, add 3.5g/L peptone, 3g/L yeast extract, 2g/L potassium dihydrogen phosphate, 1g/L magnesium sulfate, 1g/L ammonium sulfate, adjust ph to 6.8 after mixing, filtration sterilization, inoculates into Pichia pastoris CBS6054, cultivates 72 hours.Although in pre-hydrolyzed solution, acetic acid and formic acid content reduce by 90% after final result display process, but furfural and hydroxymethyl furfural content only reduce by 20%, total phenol content also only reduces by 25%, and significantly Pichia pastoris growth rate in simple electrodialysis pre-hydrolyzed solution almost can not grow (Fig. 1).
Claims (10)
1. there is the preparation technology of the lignocellulose slurrying pre-hydrolyzed solution of high-efficiency fermenting ability, it is characterized in that: comprise the following steps:
1. slurrying pre-hydrolyzed solution is prepared; 2. concentrate and remove precipitation; 3. advanced oxidation process; 4. electrodialysis process;
The material that 1. described step prepares the employing of slurrying pre-hydrolyzed solution is pulping raw material of paper making;
The concrete steps of described 3. advanced oxidation process are: added by certain density advanced oxidation reagent and 2. concentrate and except in the pre-hydrolyzed solution after precipitation, under certain pH value and temperature conditions, process a period of time, filter, collect liquid phase pre-hydrolyzed solution;
The concrete steps of described 4. electrodialysis process are: the pH value of the pre-hydrolyzed solution regulating 3. advanced oxidation process to obtain, then electrodialysis process is carried out in the light room injecting electric dialyzator, collect the pre-hydrolyzed solution in light room after process, the slurrying pre-hydrolyzed solution of low fermentation inhibitors must be had.
2. the preparation technology with the lignocellulose slurrying pre-hydrolyzed solution of high-efficiency fermenting ability according to claim 1, is characterized in that: the advanced oxidation reagent in the process of described 3. advanced oxidation is hydrogen peroxide, ozone, hydrogen peroxide/ozone mixture or hydrogen peroxide/ferrous sulfate mixture; The concentration of described hydrogen peroxide is 1-10g/L, and the concentration of described ozone is 0.5-2g/L, and the concentration of described ferrous sulfate is 0.1-2g/L; The pH value of described advanced oxidation is 2-10, and temperature is 20-60 DEG C, and the processing time is 0.5-24 hour.
3. the preparation technology with the lignocellulose slurrying pre-hydrolyzed solution of high-efficiency fermenting ability according to claim 1 and 2, is characterized in that: the described step 4. middle pre-hydrolyzed solution pH value injecting light room is 2-9; The voltage that described electrodialysis process adopts is 0.5-300V, and the electric current of employing is 0.1-50A, and the anion-exchange membrane of employing and cation-exchange membrane are 1-500 couple; The area of described anion-exchange membrane and cation-exchange membrane is respectively 50 × 50-1000 × 2000mm
2.
4. the preparation technology with the lignocellulose slurrying pre-hydrolyzed solution of high-efficiency fermenting ability according to claim 3, it is characterized in that: the concentration of described hydrogen peroxide is 2-8g/L, the concentration of described ozone is 1-2g/L, and the concentration of described ferrous sulfate is 0.2-1g/L; The pH value of described advanced oxidation is 5-9, and temperature is 25-50 DEG C, and the processing time is 2-7 hour.
5. the preparation technology with the lignocellulose slurrying pre-hydrolyzed solution of high-efficiency fermenting ability according to claim 3, it is characterized in that: the concentration of described hydrogen peroxide is 3-5g/L, the concentration of described ozone is 1-1.5g/L, and the concentration of described ferrous sulfate is 0.2-0.5g/L; The pH value of described advanced oxidation is 7-9, and temperature is 25-35 DEG C, and the processing time is 5-6 hour.
6. the preparation technology with the lignocellulose slurrying pre-hydrolyzed solution of high-efficiency fermenting ability according to claim 1 and 2, is characterized in that: the method that 1. described step prepares the employing of slurrying pre-hydrolyzed solution is hot water prehydrolysis process or steam prehydrolysis process; Described hot water prehydrolysis process is, after being mixed with water by material, be warming up to uniform temperature, cools after insulation a period of time; Described steam prehydrolysis process, for be placed in container by raw material, passes into the steam of uniform temperature, cools after insulation a period of time.
7. the preparation technology with the lignocellulose slurrying pre-hydrolyzed solution of high-efficiency fermenting ability according to claim 6, it is characterized in that: in described hot water prehydrolysis process, the mass ratio of material and water is 1:3-1:10, heating-up time is 20-60 minute, treatment temperature is 120-180 DEG C, temperature retention time is 30-240 minute, and after cooling, temperature is 30-80 DEG C; In described steam prehydrolysis process, vapor (steam) temperature is 120-180 DEG C, and temperature retention time is 30-240 minute, and after cooling, temperature is 30-80 DEG C.
8. the preparation technology with the lignocellulose slurrying pre-hydrolyzed solution of high-efficiency fermenting ability according to claim 1 and 2, it is characterized in that: the concrete steps that 3. described step concentrated and removed precipitation are: slurrying pre-hydrolyzed solution step 1. prepared adopts the mode of decompression distillation to concentrate, then first time adjust ph, be 1.0-2.5 to pH value, leave standstill, Separation of Solid and Liquid; Then second time adjust ph, is 7-10 to pH value, leave standstill, filter after obtain concentrated and except the pre-hydrolyzed solution after precipitation.
9. the preparation technology with the lignocellulose slurrying pre-hydrolyzed solution of high-efficiency fermenting ability according to claim 8, it is characterized in that: the temperature that 3. described step concentrated and removed decompression distillation in precipitation is 40 – 60 DEG C, after concentrated, the concentration of pre-hydrolyzed solution is original 5-10 times; What described first time, adjust ph adopted is hydrochloric acid, sulfuric acid, nitric acid or phosphoric acid; What described second time adjust ph adopted is NaOH, potassium hydroxide or ammoniacal liquor.
10. according to the purposes with the lignocellulose slurrying pre-hydrolyzed solution of high-efficiency fermenting ability prepared by claim 1 or 2, it is characterized in that: be used for fermenting and producing SCP or preparation high added value compound as fermenting carbon source; Described high added value compound is wood sugar, xylitol, wood oligose, arabinose or arabite.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107475466A (en) * | 2017-08-31 | 2017-12-15 | 四川雅华生物有限公司 | The technique that a kind of ozone acid hydrolyzed hemicellulose prepares xylose |
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