CN105886576A - Lignocellulose raw material pretreatment method and application - Google Patents
Lignocellulose raw material pretreatment method and application Download PDFInfo
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- CN105886576A CN105886576A CN201610464068.4A CN201610464068A CN105886576A CN 105886576 A CN105886576 A CN 105886576A CN 201610464068 A CN201610464068 A CN 201610464068A CN 105886576 A CN105886576 A CN 105886576A
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- lignocellulosic material
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- ethylenediamine
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/02—Monosaccharides
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- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P7/00—Preparation of oxygen-containing organic compounds
- C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
- C12P7/04—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
- C12P7/06—Ethanol, i.e. non-beverage
- C12P7/08—Ethanol, i.e. non-beverage produced as by-product or from waste or cellulosic material substrate
- C12P7/10—Ethanol, i.e. non-beverage produced as by-product or from waste or cellulosic material substrate substrate containing cellulosic material
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- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P2201/00—Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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Abstract
The invention relates to the technical field of renewable energy resources, and particularly discloses a lignocellulose raw material pretreatment method and application. The method includes that a mixed solution of ethanediamine and cyanamide is selected as an alkaline reagent for lignocellulose raw material pretreatment, and a mass ratio of ethanediamine and cyanamide and conditions like ultrasonic time and reaction temperature are adjusted, so that rate of converting cellulose into glucose is improved remarkably in the subsequent process of enzymolysis saccharifying, and conversion rate is higher than 92%. In addition, impurity content of a pre-treated lignocellulose raw material after being washed with water is obviously lower than that of existing pretreatment processes.
Description
Technical field
The present invention relates to technical field of renewable energy sources, a kind of lignocellulosic material is pre-
The method processed and application.
Background technology
Along with petering out of petroleum resources and going from bad to worse of environment, vigorously promote the use regenerative resource skill
Art becomes the important component part of China's energy development strategy, to reduce the Dependent Demand to fossil energy and temperature
The discharge of room gas.
Bio-fuel constantly comes into one's own in field of renewable energy in recent years.Bio-fuel refers to by biomass
Composition or solid, liquid or the gaseous fuel of extraction, can substitute the gasoline and diesel oil produced by oil, be
The important directions that regenerative resource develops.So-called biomass refer to utilize big gas and water, soil etc. logical
The various organisms crossing photosynthesis and produce, i.e. all lived organic substances that can grow, its bag
Include plant, animal and microorganism, be different from the traditional fuels such as oil, coal, nuclear energy, this emerging fuel
It it is recyclable fuel.
Cellulosic ethanol is an important part for bio-fuel, and it is unusable with timber, grass or crops
Part is lignocellulosic material, by pretreatment, enzymatic saccharification, fermentable, distills, is dehydrated five
The individual stage prepares.Lignocellulosic material is carried out pretreatment and can effectively destroy the knot of plant cellulose
Crystal structure, reduces the degree of polymerization of lignin, improves the porous of ligno-cellulosic materials, increases enzymolysis with this
The contact area of enzyme-to-substrate and then improve cellulose and be converted into the conversion ratio of glucose in saccharifying link.
In prior art, the pretreatment of lignocellulosic material can be divided into: (1) physical method, mainly machinery
Comminuting method, steam explosion, supercritical water treatment and wet oxygen method；(2) chemical method, mainly include alkali process,
The process of dilute acid pretreatment, concentrated acid, oxidizer treatment and organic solvent process；(3) biological method.Pre-at these
In processing method, alkali process is the method that present people are commonly used, i.e. uses alkaline matter to wood fibre
Element raw material processes, and conventional alkaline matter has ammonia, liquefied ammonia, sodium hydroxide, quick lime etc..But,
Needing when carrying out pretreatment to use high pressure equipment to carry out with ammonia or liquefied ammonia, condition is harsh；And use hydroxide
Although sodium or quick lime can be carried out at ambient pressure, but need a large amount of water to wash after pretreatment, remove
Alkaline reagent.These are all unfavorable for the industrialized production of lignocellulose pretreatment.It is more of paramount importance,
These alkali treatment methods existing after the complete lignocellulosic material of pretreatment, fiber in the enzymatic saccharification stage
The conversion ratio that element is converted into glucose is relatively low.Meanwhile, wash the lignocellulosic material through pretreatment, its
Impurity content is the highest, and this can strengthen the inhibitory action to enzymolysis undoubtedly.
CN 104404108 A discloses method and the application of a kind of lignocellulosic material pretreatment, uses second
Diamidogen is as the alkaline reagent of lignocellulosic material pretreatment, and reacting by heating in hermetic container, reaches
Effectively lignin degrading, improves the efficiency of cellulase hydrolysis transforming glucose.According to this preprocess method to wood
Matter cellulosic material processes, and then carries out follow-up enzymatic saccharification, and cellulose is converted into turning of glucose
Rate is 72-91%, but this conversion ratio is the most relatively low, needs to be improved further with satisfied actual application
Demand.
Summary of the invention
For the above-mentioned problems in the prior art, it is an object of the invention to provide a kind of lignocellulose
The method of pretreatment of raw material and application, improve through the pretreated lignocellulosic material of the method at enzymolysis sugar
Change cellulose in link and be converted into the conversion ratio of glucose.
Further object is that method and the application that a kind of lignocellulosic material pretreatment is provided,
Make to significantly reduce impurity content therein after the pretreated lignocellulosic material of the method is washed.
For achieving the above object, the present invention provides following technical scheme:
A kind of method of lignocellulosic material pretreatment, processes wooden with the mixed solution of ethylenediamine and cyanamide
Cellulosic material.
The present invention uses the mixed solution of ethylenediamine and cyanamide to process lignocellulosic material, by both alkali
The mating reaction of property material, can regulate hydrolysis rate, improve the surface activity of lignocellulose, so that
During obtaining follow-up enzymatic saccharification, cellulose is converted into the conversion ratio of glucose and improves, and conversion ratio is all 92%
Above.
Following as currently preferred technical scheme, but not as the limit to the technical scheme that the present invention provides
System, by following preferred technical scheme, can preferably reach and realize the technical purpose of the present invention and have
Benefit effect.
Preferably, in the mixed solution of described ethylenediamine and cyanamide, the mass ratio of ethylenediamine and cyanamide is
(5～20): (1～3), such as, can be 5:3,8:1,10:1,15:1,15:2,20:3 or 20:
1 etc., it is preferably (10～20): 1, more preferably 15:1.
By ethylenediamine and the mass ratio of cyanamide in the mixed solution of regulation ethylenediamine and cyanamide, ammonia can be regulated
Base content, mixed solution viscosity, dissolubility and this mixed solution surface active to lignocellulosic material
Degree, and then affect follow-up enzymatic saccharification process, affect cellulose and be converted into the conversion ratio of glucose,
In the range of preferably, the conversion ratio that cellulose is converted into glucose is higher.
As preferably, the method for the invention is by ethylenediamine and the mixed solution of cyanamide and lignocellulosic material
Mixing, ultrasonic, then in airtight high-pressure-resistant vessel reacting by heating, wash, filter, it is thus achieved that after pretreatment
Solid.
Preferably, the described ultrasonic time is 30～60min, can be such as 30min, 33min, 35min,
40min, 42min, 45min, 48min, 50min, 55min or 60min etc., preferably 50min.Super
Sound process can improve the mixed solution degree of surface activation to lignocellulosic material of ethylenediamine and cyanamide,
Preferably under the conditions of ultrasonic 50min, activation effect is best.
Wherein, as preferably, the addition of the mixed solution of described ethylenediamine and cyanamide is (30～40mL)/1g
Lignocellulosic material, such as, can be that 30mL/1g lignocellulosic material, 32mL/1g lignocellulose are former
Material, 34mL/1g lignocellulosic material, 35mL/1g lignocellulosic material, 38mL/1g wood fibre
Element raw material or 40mL/1g lignocellulosic material etc..
As preferably, described in be heated to be and be heated to 130～150 DEG C, can be such as 130 DEG C, 135 DEG C, 140 DEG C,
142 DEG C or 150 DEG C etc..
As preferably, the time of described reaction is 3～10min, such as, can be 3min, 4min, 5min, 7min
Or 10min etc..
In the method for the invention, lignocellulosic material is preferably corn straw or rice straw.
According to preprocess method of the present invention, lignocellulosic material is processed, then carry out follow-up
Enzymatic saccharification, pretreated raw material impurity after washing is (in addition to cellulose, hemicellulose and lignin
Material) content is less than 3%, cellulose is converted into the conversion ratio of glucose more than 92%；And with tradition alkali
Property reagent carries out pretreated lignocellulosic material, and in follow-up enzymatic saccharification, cellulose is converted into Portugal
The conversion ratio of grape sugar is only 58-71%, and pretreated raw material impurity content after washing is 11-24%.
Based on above-mentioned technique effect, the present invention also provides for the method for the invention in cellulosic ethanol production
Application.
More specifically, a kind of method that the invention provides lignocellulosic material enzymolysis, with of the present invention
Method preprocessing lignocellulose raw material, the most pretreated lignocellulosic material and cellulase, half
Cellulase, water mixed enzymolysis.
Wherein, as preferably, described pretreated lignocellulosic material, cellulase, hemicellulose
Ratio between enzyme, water is 1g:0.08mL:0.04mL:14mL.
As preferably, described cellulase is Accellarase1500.
As preferably, described hemicellulase is Multifect Xylanase.
As preferably, described enzymolysis in pH value is 4.8 systems in 50 DEG C, enzymolysis under 200rpm rotating speed
Reaction 72h.
Compared with the prior art, there is advantages that
The present invention uses the mixed solution of ethylenediamine and cyanamide to process lignocellulosic material, and regulates the two
Mass ratio, and ultrasonic time, the condition such as reaction temperature, during significantly improving follow-up enzymatic saccharification,
Cellulose is converted into the conversion ratio of glucose and improves, and conversion ratio is more than 92%, meanwhile, pretreated
Lignocellulosic material washing rear impurity content is significantly lower than existing pretreating process.
Detailed description of the invention
The invention discloses method and application, those skilled in the art of a kind of lignocellulosic material pretreatment
Present disclosure can be used for reference, be suitably modified technological parameter and realize.Special needs to be pointed out is, all similar
Replacing and change apparent to those skilled in the art, they are considered as being included in the present invention.
The method of the invention and application are described by preferred embodiment, and related personnel substantially can be not
In disengaging present invention, spirit and scope, method described herein and application it is modified or suitably changes
With combination, realize and apply the technology of the present invention.
Technical scheme is further illustrated below by detailed description of the invention.
Embodiment 1: lignocellulosic material preprocess method of the present invention and enzyme solution
(1) preprocess method
Corn straw after being sheared by 5g is put in vial, adds 150mL ethylenediamine and the mixing of cyanamide
Solution (mass ratio of ethylenediamine and cyanamide is 5:3), stirs, ultrasonic 30min.
The above-mentioned vial filling solidliquid mixture is put in the baking oven of 130 DEG C and react 10 minutes.
Material in vial is taken out, is placed in pallet, in an oven 160 DEG C of drying.
(2) enzyme solution
Take 1g and add 100mL conical flask through the lignocellulosic material of pretreatment, and be added thereto to
0.08mL cellulase Accellarase1500,0.04mL hemicellulase Multifect Xylanase and
18mL water, then be added thereto to concentrated sulphuric acid and make system pH=4.8；
By system that pH value obtained above is 4.8 at 50 DEG C, enzyme digestion reaction 72h in 200rpm shaking table.
According to the concentration of glucose in the enzymolysis solution that detection obtains, it is calculated cellulose in the present embodiment and converts
Conversion ratio for glucose is 92%.
Embodiment 2: lignocellulosic material preprocess method of the present invention and enzyme solution
(1) preprocess method
Rice straw after being sheared by 2g puts into the stainless steel reactor of with closure, adds 80mL second two
The mixed solution (mass ratio of ethylenediamine and cyanamide is 20:1) of amine and cyanamide, stirs, ultrasonic 60min.
The above-mentioned reactor filling solidliquid mixture is put in the sand-bath pot of 150 DEG C and react 3 minutes.
Material in reactor is taken out, is placed in pallet, in an oven 150 DEG C of drying.
(2) enzyme solution
Take 1g and add 100mL conical flask through the lignocellulosic material of pretreatment, and be added thereto to
0.08mL cellulase Accellarase1500,0.04mL hemicellulase Multifect Xylanase and
18mL water, then be added thereto to concentrated sulphuric acid and make system pH=4.8；
By system that pH value obtained above is 4.8 at 50 DEG C, enzyme digestion reaction 72h in 200rpm shaking table.
According to the concentration of glucose in the enzymolysis solution that detection obtains, it is calculated cellulose in the present embodiment and converts
Conversion ratio for glucose is 92.5%.
Embodiment 3: lignocellulosic material preprocess method of the present invention and enzyme solution
(1) preprocess method
Corn straw after being sheared by 12g is put in 1L vial, adds 480mL ethylenediamine and cyanamide
Mixed solution (mass ratio of ethylenediamine and cyanamide is 15:1), stirs, ultrasonic 50min.
The above-mentioned vial filling solidliquid mixture is put in the baking oven of 135 DEG C and react 10 minutes.
Material in vial is taken out, is placed in pallet, in an oven 100 DEG C of drying.
(2) enzyme solution
Take 1g and add 100mL conical flask through the lignocellulosic material of pretreatment, and be added thereto to
0.08mL cellulase Accellarase1500,0.04mL hemicellulase Multifect Xylanase and
18mL water, then be added thereto to concentrated sulphuric acid and make system pH=4.8；
By system that pH value obtained above is 4.8 at 50 DEG C, enzyme digestion reaction 72h in 200rpm shaking table.
According to the concentration of glucose in the enzymolysis solution that detection obtains, it is calculated cellulose in the present embodiment and converts
Conversion ratio for glucose is 95%.
Comparative example 1
Comparative example 1 of the present invention is CN 104404108A disclosed embodiment 1, and cellulose is converted into Portugal
The conversion ratio of grape sugar is 81%.
Comparative example 2
In addition to the mixed solution of ethylenediamine and cyanamide is replaced with pure cyanamide, additive method and condition and enforcement
Example 3 is identical.
After testing and analyze obtain, it is 46% that cellulose is converted into the conversion ratio of glucose.
Comparative example 3
In addition to the most ultrasonic, other preparation methoies and condition are same as in Example 3.
After testing and analyze obtain, it is 88% that cellulose is converted into the conversion ratio of glucose.
Applicant states, the present invention illustrates the method detailed of the present invention by above-described embodiment, but the present invention
It is not limited to above-mentioned method detailed, does not i.e. mean that the present invention has to rely on above-mentioned method detailed and could implement.
Person of ordinary skill in the field is it will be clearly understood that any improvement in the present invention, each former to product of the present invention
The equivalence of material is replaced and the interpolation of auxiliary element, concrete way choice etc., all falls within the protection model of the present invention
Within the scope of enclosing and disclosing.
Claims (10)
1. the method for a lignocellulosic material pretreatment, it is characterised in that mixed with ethylenediamine and cyanamide
Close solution and process lignocellulosic material.
Method the most according to claim 1, it is characterised in that the mixing of described ethylenediamine and cyanamide is molten
In liquid, the mass ratio of ethylenediamine and cyanamide is (5～20): (1～3), is preferably (10～20): 1, further
It is preferably 15:1.
Method the most according to claim 1 or claim 2, it is characterised in that by molten for the mixing of ethylenediamine and cyanamide
Liquid and lignocellulosic material mixing, ultrasonic, then in airtight high-pressure-resistant vessel reacting by heating, washing,
Filter, it is thus achieved that pretreated solid.
4. according to method described in any one of claim 1-3, it is characterised in that the described ultrasonic time is
30～60min, preferably 50min.
5. according to method described in any one of claim 1-4, it is characterised in that described ethylenediamine and cyanamide
The addition of mixed solution is the wooden fibre of (30～40mL)/1g lignocellulosic material, preferably 40mL/1g
Dimension element raw material.
6. according to method described in any one of claim 1-5, it is characterised in that described in be heated to be and be heated to
130～150 DEG C.
7. according to method described in any one of claim 1-6, it is characterised in that the time of described reaction is
3～10min.
8. according to method described in any one of claim 1-7, it is characterised in that described lignocellulosic material
For corn straw or rice straw.
9. method application in cellulosic ethanol production described in claim 1-8 any one.
10. the method for a lignocellulosic material enzymolysis, it is characterised in that any with claim 1-8
One described method preprocessing lignocellulose raw material, the most pretreated lignocellulosic material and fiber
Element enzyme, hemicellulase, water mixed enzymolysis.
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Cited By (1)
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Application publication date: 20160824 |