CN104611392A - Method for removing inhibitors from dilute acid steam-explosion lignocellulose material - Google Patents
Method for removing inhibitors from dilute acid steam-explosion lignocellulose material Download PDFInfo
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Abstract
The invention provides a method for removing inhibitors from a dilute acid steam-explosion lignocellulose material. The method comprises the following steps: (1) putting a mixed liquor of the dilute acid steam-explosion lignocellulose material and water into an airlift reactor, adding H2O2, starting the reactor to carry out ultrasonic treatment; (2) filtering and dewatering the mixed liquor from the step (1), adding lime milk to adjust Ph value to 7-10, and starting the airlift reactor to process; (3) filtering and dewatering the mixed liquor from the step (2) and repeating treating processes of the step (1); and (4) adjusting pH of the mixed liquor from the step (3) to 5-7, filtering and dewatering to obtain a detoxified material, and carrying out enzymolysis. By ultrasonic treatment and in synergism with H2O2, the dilute acid steam-explosion lignocellulose material undergoes detoxification treatment in the airlift reactor. The detoxification efficiency is high, and negative effects of inhibitors on enzymolysis and fermentation are reduced. Meanwhile, the method has high selectivity, and loss rate of reducing sugar during the treatment process is low.
Description
Technical field
The invention belongs to biological chemical field, be specifically related to one and utilize ultrasonic synergistic H
2o
2remove the method that diluted acid steams inhibition in quick-fried lignocellulosic material, be mainly used in the various plants stalks such as maize straw, straw, sweet sorghum bar and steam quick-fried pretreated detoxification through diluted acid.
Background technology
Due to the degraded of carbohydrate and xylogen in preprocessing process, the inhibitor of some microorganism growth can be discharged, there is weak acid class inhibition (formic acid, acetic acid, levulinic acid etc.), the materials such as furfural class inhibition (furfural, 5 hydroxymethyl furfural) and phenols inhibition (Vanillin, Resorcinol, 4-HBA).These inhibitions especially phenols have obvious restraining effect to enzymolysis subsequently and fermentable, reduce products collection efficiency, therefore should carry out necessary detoxification treatment before fermentation.The poison-removing method of current use is more, has the methods such as physics detoxification, chemical detoxication, biological detoxication, in order to reach better detoxification efficiency, often by used in combination for several poison-removing method.
Physics poison-removing method comprises rotary evaporation, solvent extraction and absorption etc.Rotary evaporation can reduce low-boiling-point organic compound, as acetic acid, furfural, but adds the concentration of non-volatile inhibition simultaneously, causes fermentation efficiency to reduce.There is the shortcoming of difficult solvent recovery in solvent extration, and cost is higher.Charcoal absorption can remove some fermentable sugars while removing inhibition, and fermentation product production is reduced.
Chemical detoxication mainly by chemical reaction as by chemical precipitation or the ionization property by changing pH value and some inhibitions.Wherein the most frequently used is use excessive solid Ca (OH)
2pre-treatment acid hydrolysis solution, the shortcoming of the method is the precipitation due to calcium ion, easily unfavorable to steps such as follow-up distillations, and excess base can make carbohydrate content be destroyed.
Biological detoxification method refers to some specific enzymes or microbial process in fermentation inhibitor, reduces its toxicity by changing the structure of inhibition.But enzyme costly, and microorganism needs to cultivate, and can consume carbohydrate in hydrolyzed solution.
(the Comparison of different detoxification methods for steam-exploded poplar wood as a substrate for the bioproduction of ethanol in SHF and SSF such as Cantarella M, Process Biochemistry, 2004,39 (11): 1533-1542) three kinds are steamed quick-fried white poplar wood matter poison-removing method to diluted acid is compared, comprise water to rinse, water-ethyl acetate two-stage extraction, excess amount of Ca (OH)
2process, wherein excess amount of Ca (OH)
2the effect of process is best, and after detoxification, carry out enzymolysis, cellulose conversion rate 88.4%, the alcohol concn of simultaneous saccharification and fermentation is 24.6g/L.(the Simultaneous detoxification and enzyme production of hemicellulose hydrolysates obtained after steam-pretreatment such as Palmqvist, EnzymeMicrob Techno, 1997,20 (4): 286-293) the willow wood raw material Trichodermareesei after steam explosion is carried out synchronous detoxification and cellulase production, most inhibition is consumed in the process of Trichodermareesei fermentation cellulase-producing, and in subsequent ethanol fermentation, alcohol yied significantly improves.
CN201210339024.0 discloses a kind of method of intensified by ultrasonic wave alkaline peroxide impregnation lignocellulose, while alkaline purification lignocellulose, carry out hyperacoustic strengthening effect, adds hydrogen peroxide and carry out strong oxidation after certain interval of time; After pre-treatment terminates, raw material is carried out solid-liquid separation, solid ingredient wherein carries out cellulase degradation and composition analysis after drying, and liquid ingredient is for reclaiming hemicellulose and lignin component.CN201010209198.6 discloses a kind of method removed straw enzymolysis and suppress the soluble lignin of butylic fermentation, and the method comprises with activated carbon treatment straw enzymolysis or uses alkaline hydrogen peroxide Treating straw, to remove the fermentation inhibitor that stalk produces.Employing activated carbon treatment straw enzymolysis can remove the soluble lignin in enzymolysis solution, and the enzymolysis solution obtained can be used for fermentation butyl alcohol after adding nitrogenous source; Employing alkaline hydrogen peroxide Treating straw can remove the xylogen in stalk, the generation of soluble lignin after minimizing enzymolysis.But aforesaid method, just for removing lignin component wherein, does not relate to the removal situation of other inhibition.Further, these methods all need to carry out solid-liquid separation to preprocessing lignocellulose raw material hydrolyzate or zymolyte, then carry out detoxification treatment to hydrolyzed solution or enzymolysis solution.
Summary of the invention
The invention provides and a kind ofly remove the method that diluted acid steams inhibition in quick-fried lignocellulosic material.This method adopts ultrasonic synergistic H
2o
2in airlift reactor, steam quick-fried lignocellulosic material to diluted acid carry out detoxification treatment, detoxification efficiency is higher, reduces the negative impact of inhibition to enzymolysis and fermentation; The present invention simultaneously has higher selectivity, and the rate of loss for the treatment of processes reducing sugar is low.
The present invention removes the method that diluted acid steams inhibition in quick-fried lignocellulosic material, comprises following content:
(1) mixed liquor diluted acid being steamed quick-fried lignocellulosic material and water is placed in airlift reactor, adds H
2o
2, start reactor and carry out ultrasonication;
(2) the mixed liquor filter dehydration of step (1), adding milk of lime adjust ph is 7-10, starts airlift reactor process;
(3) by the mixed liquor filter dehydration of step (2), the treating processes of repeating step (1);
(4) mixed liquor of step (3) is regulated pH to 5-7, the material after filter dehydration obtains detoxification carries out enzymolysis.
In the present invention, maintaining the liquid-solid mass ratio of mixed liquor in airlift reactor in the treating processes of each step is 10:1-2:1, is preferably 6:1-3:1.
In the present invention, step (1) is by H in the mixed feed liquid of certain liquid-solid mass ratio
2o
2add-on be 0.1-2g/L.Be provided with ultrasonic probe in airlift reactor, hyperacoustic acting frequency is 20-100kHz, and the time is 5-30min, and temperature is 25-50 DEG C.Air flow in airlift reactor is with can the abundant back-mixing of realization response system.After starting airlift reactor, material is at the H of intensified by ultrasonic wave
2o
2detoxification is carried out under condition, can the cavatition of combining ultrasonic ripple and the strong oxidation of hydrogen peroxide, remove the inhibition of difficult degradation.
In the present invention, the upper and lower ends of the airlift reactor inner core of step (1) is provided with wire cloth, diluted acid is steamed quick-fried lignocellulosic material and is placed in inner core, in urceolus, add gac, and wire cloth can stop activated carbon granule to enter inner core.The aperture of wire cloth is determined according to the size of activated carbon granule, as long as activated carbon granule can be stoped to enter inner core.Be 0.3-5g/L by the add-on of gac in the mixed feed liquid of certain liquid-solid mass ratio.Adopt gac strengthening H
2o
2steam explosive material to diluted acid and carry out detoxification treatment, gac can excite H
2o
2the cavatition producing more hydroxyl radical free radical (OH) synergistic supersonic wave promotes the oxidative degradation of the difficult degradation inhibitions such as phenols, furfural class and organic acid further; And gac self has absorption property, the inhibition of some difficult degradations can be adsorbed, contribute to the efficient removal of inhibition.
In the present invention, after step (2) adjust pH, start airlift reactor process 5-30min.
In the present invention, step (3) is by H in the mixed feed liquid of certain liquid-solid mass ratio
2o
2add-on be 0.1-1.5g/L.Hyperacoustic acting frequency is 20-100kHz, and the time is 5-30min, and temperature is 25-50 DEG C.
In the present invention, the filtrate that step (1), (2), (3) obtain is placed in same container and neutralizes.
Compared with existing poison-removing method, the present invention has following effect:
1, first at the acid H of intensified by ultrasonic wave
2o
2steam explosive material to diluted acid under condition to act on, then at intensified by ultrasonic wave alkalescence H
2o
2under condition, secondary action is carried out to material, namely under acidic conditions and alkaline condition, use intensified by ultrasonic wave H respectively
2o
2detoxification is carried out to material, efficient degradation can fall the inhibitions such as phenols, furfural class, organic acid.Under acidic conditions, be conducive to H
2o
2produce OH; Ultrasonic degradation occurs in cavitation bubble or the liquid-gas interface place of cavitation bubble, and under acidic conditions, the phenols inhibition etc. of molecular state easily enters gas phase zone.Therefore, most of aldehydes matter when pH is lower, by OH oxidative degradation.Under alkaline condition, be conducive to H
2o
2produce O, some aobvious acid inhibitions are more suitable for degrading in the basic conditions.Therefore, the inventive method can the cavatition of combining ultrasonic ripple and the strong oxidation of hydrogen peroxide, and difficult degradation inhibition exhaustive oxidation is degraded, and particularly aldehydes matter etc. are efficiently removed.
2, ultrasound oxidation technology degraded occurs in cavitation bubble or the liquid-gas interface place of cavitation bubble, adopts airlift reactor that gas phase can be made to dissolve feed liquor phase more, contributes to improving ultrasonication effect; And being uniformly mixed of material can be made more even, strengthen ultrasonic synergistic H
2o
2oxidative degradation phenols, the accessibility of the inhibitions such as furfural class.
3, adopt milk of lime to steam explosive material to diluted acid to process, do not need excessive milk of lime can neutralize the part organic acid steaming remaining mineral acid and generation in explosive material on the one hand, to the detoxification that material carries out to a certain degree; Be alkalescence simultaneously by the pH regulator of material, contribute to intensified by ultrasonic wave H under alkaline condition
2o
2detoxification, and excess base can be overcome carbohydrate content is destroyed.
4, operate at normal temperatures and pressures, action time is short, and mild condition is easy to control, energy efficient and cost of investment.
Embodiment
Below in conjunction with specific embodiment, method of the present invention is described in more detail.
The present invention removes diluted acid, and to steam the method for inhibition in quick-fried lignocellulosic material as follows: first diluted acid is steamed quick-fried lignocellulosic material and mix with water and be placed in airlift reactor, and add H
2o
2, start airlift reactor, carry out ul-trasonic irradiation simultaneously.Be provided with ultrasonic probe in airlift reactor, hyperacoustic acting frequency is 20-100kHz, and the time is 5-30min, and temperature is 25-50 DEG C.Air flow in airlift reactor is with can the abundant back-mixing of realization response system.Material filtering dehydration after process, adding lime milk solution adjust ph is 7-10, starts airlift reactor process 5-30min.After process, material filtering dehydration, adds water and appropriate H
2o
2, start airlift reactor, carry out ul-trasonic irradiation simultaneously.Hyperacoustic acting frequency is 20-100kHz, and the time is 5-30min, and temperature is 25-50 DEG C.Then material is regulated pH to 5-7, the diluted acid of filter dehydration acquisition detoxification steams quick-fried lignocellulosic material and carries out enzymolysis.
The upper and lower ends of airlift reactor inner core is provided with wire cloth, diluted acid is steamed quick-fried lignocellulosic material and is placed in inner core, in urceolus, add gac, and wire cloth can stop activated carbon granule to enter inner core.The aperture of wire cloth is determined according to the size of activated carbon granule, as long as activated carbon granule can be stoped to enter inner core.
Embodiment 1
(1) 300g water and 50g diluted acid are steamed quick-fried maize straw to mix, be placed in airlift reactor, add 0.2g H
2o
2, pass into the abundant back-mixing of gas, start ultrasonic unit, at frequency 40kHz, under temperature 30 DEG C of conditions, process 20min.
(2) filter dehydration after step (1) process, is placed in airlift reactor, adds 300g lime milk solution, make pH be 10, pass into the abundant back-mixing of gas, process 20min.
(3) filter dehydration after step (2) process, the material obtained adds 300g water, is placed in airlift reactor, adds 0.2gH
2o
2, pass into the abundant back-mixing of gas, start ultrasonic unit, at frequency 60kHz, process 30min.
(4) adjust material pH to 5.5 with sulfuric acid after step (2) process, filter dehydration obtains the material of detoxification.
Carry out enzymolysis in a conventional manner, add the raw cellulase in pool, Shandong, 50 DEG C of hydrolysis 120h, centrifugal enzymolysis solution.Detect the glucose in enzymolysis solution, wood sugar, 5 hydroxymethyl furfural, furfural, levulinic acid, formic acid, acetic acid, total phenol content, after detoxification, (glucose+wood sugar) is 94% of stoste, 5 hydroxymethyl furfural clearance is 73%, furfural clearance is 75%, and levulinic acid clearance is 89%, and formic acid clearance is 92%, acetic acid clearance is 90%, and total phenol clearance is 74%.
Embodiment 2
(1) 300g water and 50g diluted acid are steamed quick-fried maize straw to mix, be placed in the inner core of airlift reactor, the inner core upper and lower ends of airlift reactor is provided with wire cloth, adds 1g columnar activated carbon at the urceolus of airlift reactor, adds 0.2g H
2o
2, pass into the abundant back-mixing of gas, start ultrasonic unit, at frequency 40kHz, under temperature 30 DEG C of conditions, process 20min.
(2) filter dehydration after step (1) process, is placed in airlift reactor, adds 300g lime milk solution, make pH be 10, pass into the abundant back-mixing of gas, process 20min.
(3) filter dehydration after step (2) process, the material obtained adds 300g water, is placed in airlift reactor, adds 0.2gH
2o
2, start ultrasonic unit, at frequency 60kHz, process 30min.
(4) adjust material pH to 5.5 with sulfuric acid after step (2) process, filter dehydration obtains the material of detoxification.
Carry out enzymolysis in a conventional manner, add the raw cellulase in pool, Shandong, 50 DEG C of hydrolysis 120h, centrifugal enzymolysis solution.Detect the glucose in enzymolysis solution, wood sugar, 5 hydroxymethyl furfural, furfural, levulinic acid, formic acid, acetic acid, total phenol content, after detoxification, (glucose+wood sugar) is 95% of stoste, 5 hydroxymethyl furfural clearance is 76%, furfural clearance is 78%, and levulinic acid clearance is 91%, and formic acid clearance is 95%, acetic acid clearance is 92%, and total phenol clearance is 80%.
Embodiment 3
(1) 300g water and 100g diluted acid are steamed quick-fried maize straw to mix, be placed in the inner core of airlift reactor, the inner core upper and lower ends of airlift reactor is provided with wire cloth, adds 1g columnar activated carbon at the urceolus of airlift reactor, adds 0.4g H
2o
2, start ultrasonic unit, at frequency 60kHz, pass into the abundant back-mixing of gas, under temperature 30 DEG C of conditions, process 30min.
(2) filter dehydration after step (1) process, is placed in airlift reactor, adds 300g lime milk solution, make pH be 8, pass into the abundant back-mixing of gas, process 30min.
(3) filter dehydration after step (2) process, the material obtained adds 300g water, is placed in airlift reactor inner core, adds 0.4gH
2o
2, start ultrasonic unit, at frequency 80kHz, process 30min.
(4) adjust material pH to 5.5 with sulfuric acid after step (2) process, filter dehydration obtains the material of detoxification.
Carry out enzymolysis in a conventional manner, add the raw cellulase in pool, Shandong, 50 DEG C of hydrolysis 120h, centrifugal enzymolysis solution.Detect the glucose in enzymolysis solution, wood sugar, 5 hydroxymethyl furfural, furfural, levulinic acid, formic acid, acetic acid, total phenol content, after detoxification, glucose+wood sugar is 96% of stoste, 5 hydroxymethyl furfural clearance is 78%, furfural clearance is 82%, and levulinic acid clearance is 93%, and formic acid clearance is 96%, acetic acid clearance is 94%, and total phenol clearance is 82%.
Comparative example 1
300g water and 50g diluted acid are steamed quick-fried maize straw mix, be placed in common response device, add 0.2g H
2o
2, start ultrasonic unit, at frequency 40kHz, stir and realize back-mixing, under temperature 30 DEG C of conditions, process 40min.
Carry out enzymolysis in a conventional manner, add the raw cellulase in pool, Shandong, 50 DEG C of hydrolysis 120h, centrifugal enzymolysis solution.Detect the glucose in enzymolysis solution, wood sugar, 5 hydroxymethyl furfural, furfural, levulinic acid, formic acid, acetic acid, total phenol content, after detoxification, (glucose+wood sugar) is 90% of stoste, 5 hydroxymethyl furfural clearance is 55%, furfural clearance is 63%, and levulinic acid clearance is 80%, and formic acid clearance is 90%, acetic acid clearance is 85%, and total phenol clearance is 67%.
Comparative example 2
300g water and 50g diluted acid are steamed quick-fried maize straw mix, are placed in airlift reactor, add Ca (OH)
2the pH of solution regulation system is 10, starts ultrasonic unit, at frequency 40kHz, passes into the abundant back-mixing of gas, under temperature 30 DEG C of conditions, process 40min.
Carry out enzymolysis in a conventional manner, add the raw cellulase in pool, Shandong, 50 DEG C of hydrolysis 120h, centrifugal enzymolysis solution.Detect the glucose in enzymolysis solution, wood sugar, 5 hydroxymethyl furfural, furfural, levulinic acid, formic acid, acetic acid, total phenol content, glucose+wood sugar after detoxification) be 88% of stoste, 5 hydroxymethyl furfural clearance is 28%, furfural clearance is 32%, and levulinic acid clearance is 82%, and formic acid clearance is 90%, acetic acid clearance is 86%, and total phenol clearance is 50%.
Claims (10)
1. remove the method that diluted acid steams inhibition in quick-fried lignocellulosic material, it is characterized in that comprising the following steps:
(1) mixed liquor diluted acid being steamed quick-fried lignocellulosic material and water is placed in airlift reactor, adds H
2o
2, start reactor and carry out ultrasonication;
(2) the mixed liquor filter dehydration of step (1), adding milk of lime adjust ph is 7-10, starts airlift reactor process;
(3) by the mixed liquor filter dehydration of step (2), the treating processes of repeating step (1);
(4) mixed liquor of step (3) is regulated pH to 5-7, the material after filter dehydration obtains detoxification carries out enzymolysis.
2. method according to claim 1, is characterized in that: maintaining the liquid-solid mass ratio of mixed liquor in airlift reactor in the treating processes of each step is 10:1-2:1.
3. method according to claim 2, is characterized in that: the liquid-solid mass ratio 6:1-3:1 of mixed liquor.
4. method according to claim 1, is characterized in that: step (1) is by H in the mixed feed liquid of certain liquid-solid mass ratio
2o
2add-on be 0.1-2g/L.
5. method according to claim 1, is characterized in that: be provided with ultrasonic probe in airlift reactor, and hyperacoustic acting frequency is 20-100kHz, and the time is 5-30min, and temperature is 25-50 DEG C.
6. method according to claim 1, it is characterized in that: the upper and lower ends of the airlift reactor inner core of step (1) is provided with wire cloth, diluted acid is steamed quick-fried lignocellulosic material and be placed in inner core, in urceolus, add gac, wire cloth can stop activated carbon granule to enter inner core.
7. method according to claim 6, is characterized in that: the aperture of wire cloth is determined according to the size of activated carbon granule, as long as activated carbon granule can be stoped to enter inner core.
8. method according to claim 6, is characterized in that: be 0.3-5g/L by the add-on of gac in the mixed feed liquid of certain liquid-solid mass ratio.
9. method according to claim 1, is characterized in that: after step (2) adjust pH, starts airlift reactor process 5-30min.
10. method according to claim 1, is characterized in that: step (3) is by H in the mixed feed liquid of certain liquid-solid mass ratio
2o
2add-on be 0.1-1.5g/L.
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| CN114425314A (en) * | 2020-10-29 | 2022-05-03 | 中国石油化工股份有限公司 | Catalyst for removing steam explosion lignocellulose material inhibitor and preparation method and application thereof |
| CN114426277A (en) * | 2020-10-29 | 2022-05-03 | 中国石油化工股份有限公司 | Catalyst for degrading steam explosion lignocellulose material inhibitor and preparation method and application thereof |
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| CN104611392B (en) | 2018-04-10 |
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