CN105039424B - A method of producing ethyl alcohol using the biomass containing cellulose - Google Patents
A method of producing ethyl alcohol using the biomass containing cellulose Download PDFInfo
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- CN105039424B CN105039424B CN201510392637.4A CN201510392637A CN105039424B CN 105039424 B CN105039424 B CN 105039424B CN 201510392637 A CN201510392637 A CN 201510392637A CN 105039424 B CN105039424 B CN 105039424B
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The present invention relates to a kind of methods producing ethyl alcohol using the biomass containing cellulose, the biomass containing cellulose of crushing is mixed with ionic liquid, acid is added to be hydrolyzed, filtering, salting liquid is added in the mixing liquid of gained hydrolysis sugar and ionic liquid, two-phase is formed, split-phase is carried out, obtains phase liquid and lower phase liquid；Upper phase liquid is ionic liquid, is recycled again after processing；Saccharomycete is added in lower phase liquid and nutritive salt ferments, produces ethyl alcohol.Present invention solution ionic liquid is low to the solvability of the biomass containing cellulose, and treating capacity is small, and hydrolysis sugar detaches difficulty with ionic liquid, and the difficult problem of ionic liquid recycling is advantageously used for cellulosic ethanol industrialization, has preferable application prospect.
Description
Technical field
The present invention relates to a kind of method producing ethyl alcohol, it is specifically a kind of using the biomass containing cellulose from
The method of saccharification production ethyl alcohol in sub- liquid.
Background technology
With increasingly exhausted, the greenhouse effects getting worse caused by a large amount of discharges of carbon dioxide gas of fossil energy.
Develop the biorenewable energy（Such as alcohol fuel）, significant to social and economic development.First generation alcohol fuel is with main
Using amylum crops as raw material, it may appear that the contradiction of " striving grain with people ".Cellulose is to pass through 1,4- β-sugar by many D-Glucose bases
The high-molecular compound that glycosidic bond is formed by connecting is the main component of plant cell wall.With the second Replacing fuel second of cellulosic material
Alcohol is the emphasis of current development.Biomass source containing cellulose is extensive, such as vegetation, agriculture and forestry organic waste material, municipal solid waste
Object etc., but the composition of the biomass containing cellulose is complicated, further includes the components such as hemicellulose, lignin other than cellulose,
Crystalline texture with height, enzymolysis efficiency is low, and acidolysis condition is harsh.Green solvent-ionic liquid have dissolving cellulose with
And the ability of biomass, it is significantly improved through the regenerated biomass enzymatic saccharification efficiency of ion liquid dissolving, is the second Replacing fuel second
The production of alcohol provides new thinking.
Ionic liquid (Ionic Liquids) refers generally at a temperature of room temperature condition or near room temperature by organic or inorganic
Anion and organically cation constitutes a kind of salt compounds being in a liquid state.Ionic liquid enjoys the U.S. of " green solvent "
Reputation is because comparing and conventional solvent, and ionic liquid has following several outstanding advantages：(1) vapour pressure is extremely low, colorless and odorless,
Non-volatile, nonflammable, not oxidizable, the temperature range that liquid is presented is very wide；(2) " designability " by force, controllable ionic liquid
Acid-base property, hydrophilic hydrophobicity and polarity；(3) there is preferable solubility property to inorganic matter, organic matter and metallo-organic compound；
(4) ionic conductivity is good and electrochemical stability；(5) separate, recycle and recycle Reusability.
2002, Swatloski etc. had found -3 methylimidazole of chloro 1- butyl（[BMIM]Cl）Ionic liquid can be molten
Cellulose is solved, dissolved cellulose is easy to by adding water or ethanol precipitation to regenerate, to detach wooden fibre for ionic liquid
The plain raw material of dimension provides possibility.Its dissolution mechanism is generally believed that the anions and canons of ionic liquid and the hydroxyl of cellulose are made
With, destroy between cellulosic molecule, the hydrogen bond of intramolecular and make it dissolve.
Cellulose is not chemically reacted through ion liquid dissolving regeneration, and the regenerated cellulose degree of polymerization, crystallinity decline,
Enzymatic saccharification speed improves.So as to design biomass（Such as straw）The technique road of ethyl alcohol is produced through ionic liquid pretreatment
Line, stalk dissolve in ionic liquid, after filtering insoluble matter, obtain the mixed solution of ionic liquid and cellulose；Precipitation is added
Agent water, cellulose regenerated precipitation, ionic liquid can be by rotating water removal recycling；Obtained cellulose can be by enzyme（Or acid）Water
Solution adds yeast at glucose, and anaerobic fermentation produces ethyl alcohol.Although untreated raw material is compared in process hydrolysis with fermentation efficiency
It significantly improves.But problem also urgently to be resolved hurrily:First, ionic liquid is low to the solvability of raw material, treating capacity is small（Ionic liquid
Body is less than 25% to the solubility of microcrystalline cellulose, is less than 5% for biomass）；Second is that ionic liquid can cause enzyme to inactivate, yeast
Poisoning, regenerated cellulose will be washed fully, and obtained ionic liquid aqueous solution, ionic liquid content is low, and recycling is difficult, cost
It is high.
Invention content
Purpose of the present invention is to deficiencies to solve above-mentioned technical problem, provide a kind of biomass life utilized containing cellulose
The method of producing and ethanol, solve ionic liquid it is low to the solvability of the biomass containing cellulose, treating capacity is small, and hydrolysis sugar with
Ionic liquid separation is difficult, and ionic liquid treating capacity is low, recycles difficult problem.
Used technical solution is the present invention to solve above-mentioned technical problem：It is a kind of to utilize the biomass containing cellulose
The method for producing ethyl alcohol, the raw material of crushing is mixed with ionic liquid, and acid is added and is hydrolyzed, filters, in gained hydrolysis sugar（It is main
To be glucose）Be added salting liquid in the mixing liquid of ionic liquid, form two-phase, carry out split-phase, obtain phase liquid and
Lower phase liquid；Upper phase liquid is ionic liquid, is recycled again after processing；Saccharomycete and nutritive salt are added in lower phase liquid
It ferments, produces ethyl alcohol.
The method using the biomass production ethyl alcohol containing cellulose may be used following methods and be operated, should
Method includes the following steps：Cellulose powder is broken to 20-60 mesh, the 1- butyl -3- methylimidazole chlorine of 6-12 times of its quality is added
Salt dissolving ionic liquid, 1- ethyl-3-methylimidazole chlorination ionic liquids or 1- allyl -3- methylimidazole villaumite ionic liquids
In, the mass concentration of 0.05-0.4 times of material quality is then added as 70% sulfuric acid or the hydrochloric acid of 6mol/L, is subsequently placed in
1-2h is hydrolyzed at 80-120 DEG C；It is filtered to remove residue after hydrolysis, obtains the mixed solution of hydrolysis sugar and ionic liquid；Institute
In the mixed solution for obtaining hydrolysis sugar and ionic liquid, the mass concentration that 1-4 times of volume of mixed solution is added is the K of 40%-60%3PO4
Solution or the NaOH solution that mass concentration is 40%-60%, stand split-phase separation after concussion, are mutually that ionic liquid passes through on gained
It crosses revolving to recycle, saccharomycete is added under gained in phase solution, addition is that 0.5-2mg is added in phase solution under every 1mL；So
After add nutritive salt, after mixing adjust ph values be 4-5, anaerobic fermentation 24-48h is to get molten to ethyl alcohol at 30-37 DEG C
Liquid.
The constituent of the nutritive salt is yeast extract, peptone, ammonium sulfate, magnesium sulfate and calcium chloride,Wherein each composition
It is that yeast extract 0.3mg, peptone 0.5mg, ammonium sulfate 2mg, sulfuric acid are added in every milliliter of lower phase solution in lower phase solution additive amount
Magnesium 0.4mg, calcium chloride 0.2mg.
The saccharomycete is saccharomyces cerevisiae.
The biomass containing cellulose is the lignocellulosic material containing cellulose, especially agricultural wastes
Stalk, including maize straw, wheat stalk etc..
The temperature of the hydrolysis is preferably 90-100 DEG C.
The addition of the salting liquid is preferably 2-3 times of the mixed liquor volume of gained hydrolysis sugar and ionic liquid.
Advantageous effect is：
1. the present invention can be opened in the biomass molecule containing cellulose by ionic liquid and intermolecular hydrogen bond, biology
Matter height is poly-, polycrystalline structure part is stretched, and is easy to be acted on by acid, and acidolysis condition is mild, is measured with acid few.With being dissolved in ionic liquid
Biomass be hydrolyzed into monosaccharide, dissolution equilibrium is broken, new biomass be dissolved, treating capacity of the ionic liquid to biomass
Increase.In the prior art, cellulose is under the system of ionic liquid, can mild, efficient hydrocellulose at hydrolysis sugar, but water
It is a problem that how solution sugar detaches with ionic liquid；The present invention is saccharified production using cellulose-containing biomass in ionic liquid
The method of ethyl alcohol, cellulose-containing biomass is added in ionic liquid, and adds acid, is hydrolyzed.After hydrolysis, residue is filtered,
Obtain the mixed liquor of hydrolysis sugar and ionic liquid.Salting liquid is added and forms aqueous two-phase, it mutually can be by rotating back rich in ionic liquid
Ionic liquid is received, hydrolysis sugar is extracted to another water phase, yeast fermentative production of ethanol can be added；Therefore, hydrolysis sugar and ionic liquid
The mixed liquor of body carries out split-phase separation by the way that salting liquid is added.High rich in ionic liquid phase concentration, recycling is easy, and low energy consumption；In addition
One phase can be used for alcohol fermentation, and technical process is simple.
2, raw material sources of the present invention are extensive, of low cost；The cellulose-containing substance of agricultural and other industry can be carried out
Waste utilization；The present invention detaches hydrolysis sugar with ionic liquid, and is recycled, and solves and solves ionic liquid treating capacity
It is low, difficult problem is recycled, is conducive to that cellulosic material is industrially utilized to produce ethyl alcohol, there is preferable application prospect.This hair
It is bright that the biomass containing cellulose is handled using green solvent-ionic liquid, with difficult volatilization, nontoxicity and without dirt
The advantages such as dye, effectively degrade the biomass containing cellulose, reduce the expense of post-processing, reduce and wanted to equipment
It asks, securely and reliably.Ionic liquid can again be recycled by aqueous two-phase simultaneously, directly reduce processing cost, economically feasible
Property is high.
Description of the drawings
Fig. 1 is Technology Roadmap of the present invention using the method for the biomass production ethyl alcohol containing cellulose；
Fig. 2 is two phasors that [Bmim] Cl ionic liquids are formed with 50wt% sodium hydroxides in the embodiment of the present invention 2.
Specific implementation mode
A method of ethyl alcohol being produced using the biomass containing cellulose, the raw material of crushing is mixed with ionic liquid,
Acid is added to be hydrolyzed, filters, in gained hydrolysis sugar（Predominantly glucose）It is molten with salt is added in the mixing liquid of ionic liquid
Liquid forms two-phase, carries out split-phase, obtains phase liquid and lower phase liquid；Upper phase liquid is ionic liquid, is recycled again after processing
It utilizes；Saccharomycete is added in lower phase liquid and nutritive salt ferments, produces ethyl alcohol.
The method using the biomass production ethyl alcohol containing cellulose may be used following methods and be operated, should
Method includes the following steps：Biomass powder containing cellulose is broken to 20-60 mesh, the 1- butyl-of 6-12 times of its quality is added
3- methylimidazole chlorinations ionic liquid, 1- ethyl-3-methylimidazole chlorination ionic liquids or 1- allyl -3- methylimidazoles
In chloride salt ions liquid, the sulfuric acid that the mass concentration of 0.05-0.4 times of the biomass quality containing cellulose is 70% is then added
Or the hydrochloric acid of 6mol/L, it is subsequently placed at 80-120 DEG C and hydrolyzes 1-2h；Residue is filtered to remove after hydrolysis, obtain hydrolysis sugar and
The mixed solution of ionic liquid；In gained hydrolysis sugar（Predominantly glucose）In the mixed solution of ionic liquid, mixing is added
The mass concentration of 1-4 times of volume of solution is the K of 40-60%3PO4Solution or the NaOH solution that mass concentration is 40%-60%, by shake
Split-phase separation is stood after swinging, and is mutually that ionic liquid is recycled by revolving on gained, saccharomycete is added in phase solution under gained,
Addition is that 0.5-2mg is added in phase solution under every 1mL；Then nutritive salt is added, it is 4-5 to adjust ph values after mixing,
Anaerobic fermentation 24-48h is to get to ethanol solution at 30-37 DEG C.
The saccharomycete is saccharomyces cerevisiae.
The biomass containing cellulose is the lignocellulosic material containing cellulose, especially agricultural wastes
Stalk, including maize straw, wheat stalk etc..
The temperature of the hydrolysis is preferably 90-100 DEG C.
The addition of the salting liquid is preferably 2-3 times of the mixed liquor volume of gained hydrolysis sugar and ionic liquid.
The constituent of the nutritive salt is yeast extract, peptone, ammonium sulfate, magnesium sulfate and calcium chloride,Wherein each composition
It is that yeast extract 0.3mg, peptone 0.5mg, ammonium sulfate 2mg, sulfuric acid are added in every milliliter of lower phase solution in lower phase solution additive amount
Magnesium 0.4mg, calcium chloride 0.2mg.
The saccharomycete is
Embodiment 1
Maize straw through crushing crosses 50 mesh sieve, with [BMIM] Cl（1- butyl -3- methylimidazole chlorates）Ionic liquid
It is 1 by maize straw and the mass ratio of ionic liquid:8 mixing；Then it is 0.2 according to the mass ratio of sulfuric acid and maize straw:1, add
Enter the sulfuric acid that mass concentration is 70%；Then 1h is hydrolyzed at 100 DEG C.Later, residue is filtered, hydrolysis sugar and ionic liquid are obtained
Mixed solution.A concentration of 50% K of 2 times of volumes is added into mixed solution3PO4Solution stands split-phase separation after concussion.On
It is mutually that ionic liquid is recycled by revolving.0.2g S. cervisiaes and nutritive salt is added in lower phase solution, and it is 4 to adjust ph values,
The anaerobic fermentation 36h at 30 DEG C can get the ethanol solution that mass concentration is 10g/L.
Embodiment 2
Microcrystalline cellulose and [AMIM] Cl（1- allyl -3- methylimidazole villaumites）Ionic liquid ionic liquid in mass ratio 1:
10 mixing, are added the hydrochloric acid of 6mol/L, and the mass ratio of hydrochloric acid and microcrystalline cellulose is 0.1:1, hydrolyze 2h at 90 DEG C.Solid content
It completely disappears, obtains the mixed solution of hydrolysis sugar and ionic liquid.The NaOH of 1 times of volumetric concentration 45% is added into mixed solution
Solution stands split-phase separation after concussion.Upper phase is that ionic liquid is recycled by revolving.0.5g saccharomycete is added in lower phase solution
And nutritive salt, adjustment pH value are 4.5, the anaerobic fermentation 36h at 37 DEG C, and it is molten to can get the ethyl alcohol that mass concentration is 50 g/L
Liquid.
Embodiment 3
Wheat stalk through crushing crosses 40 mesh sieve, with [EMIM] Cl（1- ethyl-3-methylimidazole chlorates）Ionic liquid
It is 1 by wheat stalk and the mass ratio of ionic liquid:6 mixing；Then it is 0.2 according to the mass ratio of sulfuric acid and maize straw:1, add
Enter the sulfuric acid that mass concentration is 70%；Then 2h is hydrolyzed at 120 DEG C.Later, residue is filtered, hydrolysis sugar and ionic liquid are obtained
Mixed solution.A concentration of 50% K of 2 times of volumes is added into mixed solution3PO4Solution stands split-phase separation after concussion.On
It is mutually that ionic liquid is recycled by revolving.S. cervisiae and nutritive salt is added in lower phase solution, and it is 5 to adjust ph values, 37
Anaerobic fermentation for 24 hours, can get the ethanol solution that mass concentration is 20g/L at DEG C.
Embodiment 4
Maize straw through crushing crosses 30 mesh sieve, with [BMIM] Cl（1- butyl -3- methylimidazole chlorates）Ionic liquid
It is 1 by maize straw and the mass ratio of ionic liquid:12 mixing；Then it is 0.2 according to the mass ratio of sulfuric acid and maize straw:1, add
Enter the sulfuric acid that mass concentration is 70%；Then 2h is hydrolyzed at 90 DEG C.Later, filtering residue, acquisition hydrolysis sugar and ionic liquid
Mixed solution.A concentration of 60% K of 2 times of volumes is added into mixed solution3PO4Solution stands split-phase separation after concussion.Upper phase
It is recycled by revolving for ionic liquid.0.5g S. cervisiaes and nutritive salt is added in lower phase solution, and it is 4.5 to adjust ph values,
Anaerobic fermentation for 24 hours, can get the ethanol solution that mass concentration is 20g/L at 37 DEG C.
Embodiment 5
Maize straw through crushing crosses 60 mesh sieve, with [AMIM] Cl（1- allyl -3- methylimidazole villaumites）Ionic liquid from
Sub- liquid in mass ratio 1:10 mixing, are added the hydrochloric acid of 6mol/L, and the mass ratio of hydrochloric acid and microcrystalline cellulose is 0.1:1,80
2h is hydrolyzed at DEG C.Solid content completely disappears, and obtains the mixed solution of hydrolysis sugar and ionic liquid.4 times are added into mixed solution
The NaOH solution of volumetric concentration 50% stands split-phase separation after concussion.Upper phase is that ionic liquid is recycled by revolving.Lower phase
0.15g saccharomycete and nutritive salt is added in solution, and adjustment pH value is 4.5, the anaerobic fermentation 36h at 37 DEG C, and it is dense to can get quality
Degree is the ethanol solution of 50 g/L.
Claims (7)
1. the raw material of crushing is mixed with ionic liquid, is added by a kind of method using the biomass production ethyl alcohol containing cellulose
Enter acid to be hydrolyzed, it is characterised in that：Mixed material after hydrolysis is filtered, in the mixed of gained hydrolysis sugar and ionic liquid
Close the K for being added that the mass concentration of 1-4 times of mixed liquor volume is 40-60% in liquid3PO4Solution or mass concentration are 40%-60%
NaOH solution, formed two-phase, carry out split-phase, obtain phase liquid and lower phase liquid；Upper phase liquid is ionic liquid, after processing
It recycles again；Saccharomycete is added in lower phase liquid and nutritive salt ferments, produces ethyl alcohol；
The ionic liquid be 1- butyl -3- methylimidazole chlorinations ionic liquid, 1- ethyl-3-methylimidazoles chlorate from
Any one in sub- liquid and 1- allyl -3- methylimidazole villaumite ionic liquids.
2. the method using the biomass production ethyl alcohol containing cellulose as described in claim 1, which is characterized in that including with
Lower step：Biomass powder containing cellulose is broken to 20-60 mesh, is added to the 1- butyl -3- methyl miaows of 6-12 times of its quality
Azoles chlorination ionic liquid, 1- ethyl-3-methylimidazole chlorination ionic liquids or 1- allyl -3- methylimidazole villaumite ions
In liquid, the sulfuric acid or 6mol/ that the mass concentration of 0.05-0.4 times of the biomass quality containing cellulose is 70% are then added
The hydrochloric acid of L is subsequently placed at 80-120 DEG C and hydrolyzes 1-2h；It is filtered to remove residue after hydrolysis, obtains hydrolysis sugar and ionic liquid
The mixed solution of body；In the mixed solution of gained hydrolysis sugar and ionic liquid, the quality that 1-4 times of mixed liquor volume is added is dense
Degree is the K of 40-60%3PO4Solution or the NaOH solution that mass concentration is 40%-60%, stand split-phase separation, gained after concussion
Upper phase is that ionic liquid is recycled by revolving；Saccharomycete is added in phase solution under gained, the addition of saccharomycete is every
0.5-2mg is added in phase solution under 1mL；Then nutritive salt is added, it is 4-5 to adjust Ph values after mixing, at 30 DEG C -37 DEG C
Anaerobic fermentation 24-48h is to get to ethanol solution；
The constituent of the nutritive salt is yeast extract, peptone, ammonium sulfate, magnesium sulfate and calcium chloride,Wherein each composition is under
Phase solution additive amount is that yeast extract 0.3mg, peptone 0.5mg, ammonium sulfate 2mg, magnesium sulfate are added in every milliliter of lower phase solution
0.4mg, calcium chloride 0.2mg.
3. the method as claimed in claim 2 using the biomass production ethyl alcohol containing cellulose, it is characterised in that：Described
Saccharomycete is saccharomyces cerevisiae.
4. the method as claimed in claim 2 using the biomass production ethyl alcohol containing cellulose, it is characterised in that：It is described to contain
It is the straw containing cellulose to have the biomass of cellulose.
5. the method as claimed in claim 4 using the biomass production ethyl alcohol containing cellulose, it is characterised in that：Described
Straw is maize straw or wheat stalk.
6. the method for biomass production ethyl alcohol of the utilization as described in one of claim 1-5 containing cellulose, feature
It is：The temperature of the hydrolysis is 90-100 DEG C.
7. the method for biomass production ethyl alcohol of the utilization as described in one of claim 2-5 containing cellulose, feature
It is：The mass concentration is the K of 40-60%3PO4The addition of solution is the mixed solution body of gained hydrolysis sugar and ionic liquid
Long-pending 2-3 times.
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| CN110791596B (en) * | 2019-11-11 | 2020-10-30 | 西南科技大学 | Method for realizing regeneration and utilization of waste biomass by adopting alkaline electrolyzed water |
| CN115475656A (en) * | 2022-09-05 | 2022-12-16 | 河南科技大学 | Preparation method of magnetic solid acid and application of magnetic solid acid in biomass hydrolysis |
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| CA2677862C (en) * | 2007-02-07 | 2015-09-01 | Queensland University Of Technology | Fractionation of a lignocellulosic material |
| CN101333777B (en) * | 2007-06-27 | 2010-07-28 | 中国科学院大连化学物理研究所 | Method for high-efficiency hydrolyzing lignocellulose raw material in ionic liquid |
| CN101514375A (en) * | 2008-02-20 | 2009-08-26 | 青岛生物能源与过程研究所 | Method for preparing reducing sugar by catalyzing hydrocellulose |
| CN102071266A (en) * | 2010-12-03 | 2011-05-25 | 江南大学 | Application of ionic liquid to preparation of reducing sugar by cellulose hydrolysis |
| CN102925595A (en) * | 2011-08-11 | 2013-02-13 | 天津工业生物技术研究所 | New method for producing fermentable sugar through hydrolyzing biomasses by utilizing ionic liquid |
| CN103740867A (en) * | 2014-01-02 | 2014-04-23 | 上海大学 | Method for preparing glucose by hydrolyzing straw celluloses |
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