CN106929544A - A kind of preprocess method of lignocellulosic material - Google Patents
A kind of preprocess method of lignocellulosic material Download PDFInfo
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- CN106929544A CN106929544A CN201511026162.3A CN201511026162A CN106929544A CN 106929544 A CN106929544 A CN 106929544A CN 201511026162 A CN201511026162 A CN 201511026162A CN 106929544 A CN106929544 A CN 106929544A
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- Prior art keywords
- lignocellulosic material
- carbon dioxide
- preprocess method
- cellulose
- constant temperature
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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
- 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
-
- 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
- C12P2201/00—Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
-
- 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
- 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
-
- 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
- Y02P20/141—Feedstock
Abstract
The invention discloses a kind of preprocess method of lignocellulosic material, the method is comprised the following steps:(1) lignocellulosic material is crushed, particle diameter is 40~60 mesh, compression forming after crushing;(2) lignocellulosic material obtained by step (1) is placed in closed reactor, to carbon dioxide is passed through in reactor under constant temperature, normal pressure is then down to after 4~6h of pressurize, dip time is 16~20min.The present invention is using the superpower solution pervasion ability of supercriticality carbon dioxide, in carbon dioxide is penetrated into and is crushed the compressing short grained network crystal structure of cellulose under the conditions of constant temperature and pressure, then escape carbon dioxide by pressure release, the strong interactions such as the crystal structure and covalent bond and hydrogen bond between cellulose, hemicellulose and lignin of cellulose are destroyed, so that cellulose, hemicellulose and lignin separation.
Description
Technical field
The invention belongs to technical field of biochemical industry, and in particular to a kind of lignocellulosic materials for fuel ethanol
Preprocess method, more particularly to one kind is without catalyst and cosolvent, the production of efficient lignocellulosic
The preprocess method of alcohol fuel.
Background technology
With coming quietly for " fossil energy epoch afterwards ", various countries are in field of renewable energy research and probe
Dynamics reach unprecedented levels.Wherein alcohol fuel so that its raw material sources is abundant, production technology relative into
The regenerative resource that ripe simple the features such as first develops as numerous countries.But at present alcohol fuel it is many with
Used as raw material, its direct result causes in world wide especially the starchiness cereal crops of high added value
The grain security and energy security problem severe exacerbation of developing country.And lignocellulose-like biomass is
Unique predictable energy provides the sustainable resource of material and fuel for the mankind in the world.The annual agriculture of China
About 1,500,000,000 tons altogether of woods discarded object, produces 1 ton of ethanol and calculates, with 3.75 hundred million tons of ethanol of production by 4 tons
Resource potential.
However, lignocellulosic structure is complicated, its main component is lignin, hemicellulose, fiber
Element, wherein hemicellulose are crosslinked and form network structure in the form of covalent bond with lignin, this works
Cellulose is interted wherein in the form of hydrogen bond again, ultimately form a kind of structure of exceptional stability, make its right
The factor such as microbial degradation and physical chemistry has stronger resistance, and this structure makes later use cellulase
The efficiency for being translated into fermentable sugars is extremely inefficient, therefore lignocellulosic pretreatment is whole wooden fibre
Dimension element prepares the most important thing in the numerous sport technique segments of ethanol.
Traditional pretreatment is broadly divided into comminuting method, acid-alkali treatment method and ammonia steam explosion method and bioanalysis, respectively
There are advantage and disadvantage.Comminuting method can effectively reduce the degree of polymerization of cellulose, but high energy consumption, account for cellulose sugar
More than the 50% of change process total energy consumption, to the increase rate very little of follow-up enzymolysis process.Chinese patent
It is pre- that CN200810020226.2,200810020227.7 and CN 200810020228.1 discloses a kind of acid
The method for processing lignocellulosic, effectively improves removing for cellulose, hemicellulose conversion ratio and lignin
Go.But pretreating effect is poor at normal temperatures for diluted acid used, generally requires and for temperature to bring up to 100 DEG C
The above just has obvious effect, and acid used is also required to reclaim or neutralizes, and increased complex process journey
Degree.Compared with low-kappa number method, oxygenation pretreatment method treatment temperature is relatively low, the smaller (Chinese patent of energy consumption
CN200810023926.7 is alkali process method), but in view of environmental issue, subsequent treatment is stilled need
In and/or recycle.Chinese patent CN200710130844.8 discloses a kind of ammoniacal liquor immersion+vacuum
The method that explosion is pre-processed to lignocellulosic material, treated raw material is than undressed original
Material gas production improves 70%, and pretreating effect is improve well.But hemicellulose after being processed through steam explosion
Loss greatly reduces raw material availability and sugared yield up to more than 50%.And bioanalysis reaction condition
Gently, safety and environmental protection, energy consumption are low, but the cycle is long, efficiency is low, it is difficult to industrial production, and addition is total to
Solvent can all produce influence to enzyme in follow-up enzymolysis, fermentation process and bacterium activity.
The content of the invention
It is a primary object of the present invention to propose a kind of preprocess method of lignocellulosic material, to solve
Catalyst, cosolvent etc. are added in prior art preprocess method to enzyme in follow-up enzymolysis, fermentation process and
Bacterium activity produces the defect of influence.
To achieve the above object, the present invention proposes a kind of preprocess method of lignocellulosic material, the party
Method is comprised the following steps:
(1) lignocellulosic material is crushed, particle diameter is 40~60 mesh after crushing, is compressed into
Type;And
(2) lignocellulosic material obtained by step (1) is placed in closed reactor, constant temperature
Lower to be then down to normal pressure after 4~6h of pressurize to carbon dioxide is passed through in reactor, dip time is
16~20min.
The preprocess method of lignocellulosic material of the present invention, wherein, the lignocellulosic is former
Material is preferably agricultural crop straw, wood chip or corncob.
The preprocess method of lignocellulosic material of the present invention, wherein, in the step (1)
Particle diameter is preferably 50~60 mesh after lignocellulosic material is crushed.
The preprocess method of lignocellulosic material of the present invention, wherein, in the step (1)
Density after lignocellulosic material compression forming is preferably 300kg/m3~350kg/m3。
The preprocess method of lignocellulosic material of the present invention, wherein, described in step (2)
Constant temperature any temperature in being preferably 28~32 DEG C.
The preprocess method of lignocellulosic material of the present invention, these, it is preferred to, the step
Suddenly it is 6~8Mpa that carbon dioxide to pressure is passed through in (2).
The preprocess method of lignocellulosic material of the present invention, wherein, in the step (2)
Dwell time is preferably 5~6h.
The preprocess method of lignocellulosic material of the present invention, wherein, in the step (2)
Dip time is preferably 16~18min.
Beneficial effects of the present invention:
(1) crystalline texture of lignocellulosic be can completely break, cellulose, hemicellulose and wood realized
Efficiently separating for quality, reaches pretreatment purpose.
(2) it is not required to add catalyst, without catalyst subsequent treatment removal process, process is simple.
(3) cosolvent such as addition alcohols, aldehydes are not required to, cosolvent is reduced to follow-up enzymolysis, fermentation
During enzyme and bacterium activity influence.
(4) it is environmentally safe without soda acid waste discharge.
Specific embodiment
Embodiments of the invention are elaborated below:The present embodiment is with technical solution of the present invention as preceding
Put and implemented, give detailed implementation method and process, but protection scope of the present invention is not limited to
Following embodiments, the experimental technique of unreceipted actual conditions in the following example, generally according to conventional strip
Part.
A kind of problem that the present invention exists for Several Traditional Preconditioning Methods, there is provided the pre- place of lignocellulosic
Reason method, has the advantages that the residence time is short, production efficiency is high, Product inhibiton is small, high conversion rate, energy
The problems such as enough overcoming conventional art high pollution and strong biotechnology product inhibition.
Specifically, to realize technical purpose of the invention, the technical scheme is that:
First, segment is cut into after lignocellulosic material is dried, is then crushed with pulverizer, powder
Broken rear particle diameter is 40~60 mesh, afterwards compression forming.
Then, the lignocellulosic material of above-mentioned gained is placed in closed reactor, under constant temperature to
Carbon dioxide to a certain constant pressure is passed through in reactor, then normal pressure is rapidly decreased to after 4~6h of pressurize, is depressured
Time is 16~20min.
The raw material of above-mentioned lignocellulosic is agricultural crop straw, wood chip, corncob etc..
Above-mentioned reactor thermostat temperature is any temperature in 28~32 DEG C.
Above-mentioned pressure carbon dioxide is 6~8Mpa.
The above-mentioned dwell time is preferably 5~6h.
The time that normal pressure is depressurized to after above-mentioned pressurize is preferably 16~18min.
The present invention penetrates into carbon dioxide using the strong solution pervasion ability of supercriticality carbon dioxide
To in the netted crystalline texture of lignocellulosic stabilization, quickly escaped by carbon dioxide after pressure release, destroyed
Covalent bond and hydrogen bond between the crystal structure and cellulose, hemicellulose and lignin of cellulose etc. are strong
Interact, so that cellulose, hemicellulose and lignin separation.By control process temperature, pressure
Power, dwell time and pressure release speed can realize the regulation and control to pretreating effect, reach optimal treatment effect
Really.And carbon dioxide can be utilized with repetitive cycling.
Embodiment 1
With maize straw as raw material, the little particle for 40~60 mesh is crushed with pulverizer, then use particle
Forming machine is pressed into diameter about 4mm, is about the little particle of 6mm so that the density of stalk by
80kg/m3Bring up to 300kg/m3.Then, compressed stalk particle is loaded into pretreatment tank,
30 DEG C are moved in the heating mantle of constant temperature, carbon dioxide is passed through, fastened after the air in tank is displaced
Deflation valve.Continue injecting carbon dioxide to pressure be 6MPa, stop injecting carbon dioxide, close into
Air valve, constant temperature pressurize 4h, then to normal pressure, venting duration is controlled in 16min quick pressure releasing.
By 12:1 part by weight to adding water in pretreatment product, 30 DEG C of stirring 30min of constant temperature.
Solution is taken by being analyzed to filtrate after filtering, is surveyed using Shimadzu HPLC-MS instrument
The concentration of the compositions such as fixed xylose therein, acetic acid, furfural, specific data are shown in Table 1.
The filtrate component analysis result of 1 embodiment of table 1
Xylose | Acetic acid | Furfural | |
Concentration, wt.% | 1.8 | 0.12 | 0.15 |
Embodiment 2
Stalk particle compressed in embodiment 1 is loaded into pretreatment tank, 32 DEG C of constant temperature are moved to
Heating mantle in, be passed through carbon dioxide, deflation valve is fastened after the air in tank is displaced.Continue to note
It is 7MPa to enter carbon dioxide to pressure, stops injecting carbon dioxide, closes air intake valve, constant temperature pressurize
6h, then to normal pressure, venting duration is controlled in 20min quick pressure releasing.
By 12:1 part by weight to adding water in pretreatment product, 30 DEG C of stirring 30min of constant temperature.
Solution is taken by being analyzed to filtrate after filtering, is surveyed using Shimadzu HPLC-MS instrument
The concentration of the compositions such as fixed xylose therein, acetic acid, furfural, specific data are shown in Table 2.
The filtrate component analysis result of 2 embodiment of table 2
Xylose | Acetic acid | Furfural | |
Concentration, wt.% | 2.2 | 0.15 | 0.1 |
Embodiment 3
Stalk particle compressed in embodiment 1 is loaded into pretreatment tank, 28 DEG C of constant temperature are moved to
Heating mantle in, be passed through carbon dioxide, deflation valve is fastened after the air in tank is displaced.Continue to note
It is 8MPa to enter carbon dioxide to pressure, stops injecting carbon dioxide, closes air intake valve, constant temperature pressurize
5h, then to normal pressure, venting duration is controlled in 20min quick pressure releasing.
By 12:1 part by weight to adding water in pretreatment product, 30 DEG C of stirring 30min of constant temperature.
Solution is taken by being analyzed to filtrate after filtering, is surveyed using Shimadzu HPLC-MS instrument
The concentration of the compositions such as fixed xylose therein, acetic acid, furfural, specific data are shown in Table 3.
The filtrate component analysis result of 3 embodiment of table 3
Xylose | Acetic acid | Furfural | |
Concentration, wt.% | 2.0 | 0.12 | 0.1 |
Embodiment 4
Stalk particle compressed in embodiment 1 is loaded into pretreatment tank, 30 DEG C of constant temperature are moved to
Heating mantle in, be passed through carbon dioxide, deflation valve is fastened after the air in tank is displaced.Continue to note
It is 8MPa to enter carbon dioxide to pressure, stops injecting carbon dioxide, closes air intake valve, constant temperature pressurize
4h, then to normal pressure, venting duration is controlled in 16min quick pressure releasing.
By 12:1 part by weight to adding water in pretreatment product, 30 DEG C of stirring 30min of constant temperature.
Solution is taken by being analyzed to filtrate after filtering, is surveyed using Shimadzu HPLC-MS instrument
The concentration of the compositions such as fixed xylose therein, acetic acid, furfural, specific data are shown in Table 4.
The filtrate component analysis result of 4 embodiment of table 4
Xylose | Acetic acid | Furfural | |
Concentration, wt.% | 1.9 | 0.12 | 0.16 |
Effect of the invention:
(1) crystalline texture of lignocellulosic be can completely break, cellulose, hemicellulose and wood realized
Efficiently separating for quality, reaches pretreatment purpose.
(2) it is not required to add catalyst, without catalyst subsequent treatment removal process, process is simple.
(3) cosolvent such as addition alcohols, aldehydes are not required to, cosolvent is reduced to follow-up enzymolysis, fermentation
During enzyme and bacterium activity influence.
(4) it is environmentally safe without soda acid waste discharge.
Certainly, the present invention can also have other various embodiments, without departing substantially from spiritual and its essence of the invention
In the case of, those of ordinary skill in the art can make various corresponding changes and deformation according to the present invention,
But these corresponding changes and deformation should all belong to the protection domain of the claims in the present invention.
Claims (8)
1. a kind of preprocess method of lignocellulosic material, it is characterised in that the method includes following
Step:
(1) lignocellulosic material is crushed, particle diameter is 40~60 mesh after crushing, is compressed into
Type;And
(2) lignocellulosic material obtained by step (1) is placed in closed reactor, constant temperature
Lower to be then down to normal pressure after 4~6h of pressurize to carbon dioxide is passed through in reactor, dip time is
16~20min.
2. the preprocess method of lignocellulosic material according to claim 1, its feature exists
In the lignocellulosic material is agricultural crop straw, wood chip or corncob.
3. the preprocess method of lignocellulosic material according to claim 1, its feature exists
In particle diameter is 50~60 mesh after lignocellulosic material is crushed in the step (1).
4. the preprocess method of lignocellulosic material according to claim 1, its feature exists
In the density in the step (1) after lignocellulosic material compression forming is 300kg/m3~
350kg/m3。
5. the preprocess method of lignocellulosic material according to claim 1, its feature exists
In constant temperature described in step (2) is any temperature in 28~32 DEG C.
6. the preprocess method of lignocellulosic material according to claim 1, its feature exists
In it is 6~8Mpa that carbon dioxide to pressure is passed through in the step (2).
7. the preprocess method of lignocellulosic material according to claim 1, its feature exists
In the dwell time is 5~6h in the step (2).
8. the preprocess method of lignocellulosic material according to claim 1, its feature exists
In dip time is 16~18min in the step (2).
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108586770A (en) * | 2018-03-20 | 2018-09-28 | 青岛大学 | A method of clean separation lignin and hemicellulose from plant biomass |
CN111778293A (en) * | 2020-06-28 | 2020-10-16 | 龚春晓 | Method for preparing cellulose hydrolysate by using lignocellulose as raw material |
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CN101824436A (en) * | 2009-03-06 | 2010-09-08 | 华东理工大学 | Improved method for preprocessing lignocellulose raw material |
CN103849664A (en) * | 2012-12-03 | 2014-06-11 | 华东理工大学 | Post-treatment method for strengthening pretreatment effect of lignocellulose raw material through pulping |
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2015
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CN101824436A (en) * | 2009-03-06 | 2010-09-08 | 华东理工大学 | Improved method for preprocessing lignocellulose raw material |
CN103849664A (en) * | 2012-12-03 | 2014-06-11 | 华东理工大学 | Post-treatment method for strengthening pretreatment effect of lignocellulose raw material through pulping |
Non-Patent Citations (2)
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108586770A (en) * | 2018-03-20 | 2018-09-28 | 青岛大学 | A method of clean separation lignin and hemicellulose from plant biomass |
CN108586770B (en) * | 2018-03-20 | 2020-11-17 | 青岛大学 | Method for cleaning and separating lignin and hemicellulose from plant biomass |
CN111778293A (en) * | 2020-06-28 | 2020-10-16 | 龚春晓 | Method for preparing cellulose hydrolysate by using lignocellulose as raw material |
CN111778293B (en) * | 2020-06-28 | 2024-04-12 | 龚春晓 | Method for preparing cellulose hydrolysate by taking lignocellulose as raw material |
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Application publication date: 20170707 |