CN104561130A - Microwave-assisted pretreatment method for maize straws - Google Patents
Microwave-assisted pretreatment method for maize straws Download PDFInfo
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- CN104561130A CN104561130A CN201510020718.1A CN201510020718A CN104561130A CN 104561130 A CN104561130 A CN 104561130A CN 201510020718 A CN201510020718 A CN 201510020718A CN 104561130 A CN104561130 A CN 104561130A
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- China
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- microwave
- maize straw
- treatment
- ethylenediamine solution
- maize straws
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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
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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
- 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
Abstract
The invention discloses a microwave-assisted pretreatment method for maize straws. The microwave-assisted pretreatment method comprises the steps of mixing the maize straws and an ethylenediamine solution; and sequentially carrying out microwave treatment and thermal treatment under a closed condition to obtain pretreated maize straws. According to the method, the maize straws are pretreated by using the ethylenediamine solution under the assistance of microwaves, so that lignin can be effectively degraded, the crystallinity of cellulose can be reduced, and the enzymolysis efficiency of the cellulose and hemicellulose in the maize straws can be increased. The microwave-assisted pretreatment method is simple in operation, free of high-pressure equipment, low in equipment requirement and energy consumption and suitable for industrial production.
Description
Technical field
The invention belongs to cellulosic ethanol technical field, be specifically related to a kind of method of microwave-assisted pre-treatment maize straw.
Background technology
Liquid fuel conveniently transports and is convenient to utilize, and has become important industry and daily energy derive.Wherein, oil is that at present the whole world uses maximum liquid fuels, but, the non-renewable and CO of petroleum resources
2the deterioration of environment can be caused with the discharge of other dusty gass.Develop the most important thing that reproducible clean energy becomes the energy development strategy of China.Ethanol is paid close attention to widely as the alternative cleaning liq energy and is paid attention to, the method of traditional mode of production ethanol take grain as raw material, adopt the method for yeast direct fermentation to produce ethanol, but this kind of method needs to consume a large amount of grain, face the problem of " strive ground with people, strive grain with people ".People turn one's attention to agricultural wastes gradually, as maize straw, broomcorn straw, wheat stalks etc., because agricultural wastes are also carbohydrate, and annual output is huge, maize straw, broomcorn straw, wheat stalk etc. just have 700,000,000 tons annual, these wastes can not get effective utilization and just can be burnt by peasant, not only waste energy but also contaminate environment.The glucose and xylose utilizing agricultural wastes and lignocellulose to obtain through enzymolysis after pre-treatment can utilize by yeast generation cellulosic ethanol; adopt and namely protect environment in this way; effectively make use of resource; having got back clean energy, is very promising Energy utilization patterns.
But at present, the bottleneck that restriction lignocellulose utilizes is due to high pre-treatment cost, and first the utilization of lignocellulose will destroy the rock steady structure of plant cell wall, remove xylogen, reduce degree of crystallinity, increase the contact area of substrate and enzyme, thus improve cellulosic enzymolysis efficiency.
Existing preprocessing means comprises: physical method, chemical process, physical chemistry-method and biological method.Physical method, mainly comprises mechanical crushing method, steam explosion, supercritical water treatment and wet oxygen method; Chemical process, mainly comprises alkaline purification, dilute acid pretreatment, concentrated acid process, oxidizer treatment and organic solvent process; Biological method adopts fungi to process lignocellulose.
In these pretreatment processs, alkaline process can open the ehter bond between xylogen and hemicellulose, removes xylogen, retains Mierocrystalline cellulose and hemicellulose largely.Alkaline matter conventional in prior art has ammoniacal liquor, liquefied ammonia, sodium hydroxide, unslaked lime etc.But, although adopt sodium hydroxide or unslaked lime to carry out at ambient pressure, after pre-treatment, need large water gaging to wash, removing alkaline reagents, and the discharge of alkaline reagents pollutes the environment; And need when carrying out pre-treatment with ammoniacal liquor or liquefied ammonia to adopt high-tension apparatus to carry out, condition is harsh.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is a kind of method providing microwave-assisted pre-treatment maize straw, and pretreatment process of the present invention, without the need to adopting high-tension apparatus, requires low to conversion unit.
The invention provides a kind of method of microwave-assisted pre-treatment maize straw, comprise the following steps:
Maize straw is mixed with ethylenediamine solution, in confined conditions, successively through microwave treatment and thermal treatment, obtains pretreated maize straw.
Preferably, the quality volume fraction of described ethylenediamine solution is 1% ~ 40%.
Preferably, the dry-matter of described maize straw and the mass volume ratio of ethylenediamine solution are 1g:(2 ~ 40) mL.
Preferably, the power of described microwave treatment is 500 ~ 800W, and the time of microwave treatment is 3 ~ 10min, and the temperature of microwave treatment is 120 ~ 200 DEG C.
Preferably, described heat treated temperature is 120 ~ 200 DEG C, and the heat treated time is 10 ~ 60min.
Preferably, before described microwave treatment, also thermal pretreatment is comprised.
Preferably, the temperature of described thermal pretreatment is 50 ~ 110 DEG C.
Preferably, after described thermal treatment, also comprise maize straw successively through filtering, washing and drying.
Compared with prior art, maize straw mixes with ethylenediamine solution by the present invention, in confined conditions, successively through microwave treatment and thermal treatment, obtains pretreated maize straw.The method applied microwave assists ethylenediamine solution to carry out pre-treatment to maize straw, can effective lignin degrading, reduces cellulose crystallity, improves the enzymolysis efficiency of Mierocrystalline cellulose and hemicellulose in maize straw.The present invention is simple to operate, and without the need to adopting high-tension apparatus, low for equipment requirements, energy consumption is low, is applicable to suitability for industrialized production.
Result shows, the yield of the glucose of maize straw after pre-treatment enzymolysis is 50 ~ 90%.
Embodiment
The invention provides a kind of method of microwave-assisted pre-treatment maize straw, comprise the following steps:
Maize straw is mixed with ethylenediamine solution, in confined conditions, successively through microwave treatment and thermal treatment, obtains pretreated maize straw.
The present invention is preferably to pass through broken maize straw for raw material.Wherein, the degree of crushing of the present invention to described maize straw does not have particular restriction.Above-mentioned maize straw and ethylenediamine solution are placed in reactor mix, obtain mixture.Described reactor is airtight reactor, to prevent the vaporization losses of quadrol in follow-up microwave treatment and heat treatment process.
Wherein, the quality volume fraction of described ethylenediamine solution is 1% ~ 40%, in some embodiments of the invention, the quality volume fraction of the solution of described quadrol is 1%, in other embodiments of the present invention, the quality volume fraction of the solution of described quadrol is 20%, and in other embodiments of the present invention, the quality volume fraction of the solution of described quadrol is 40%.
The dry-matter of described maize straw and the mass volume ratio of ethylenediamine solution are 1g:(2 ~ 40) mL, be preferably 1g:(5 ~ 10) mL.
After described maize straw mixes with ethylenediamine solution, described reactor is sealed, carry out microwave treatment.In the present invention, microwave generator is preferably adopted to carry out microwave and heating to described reactor.Wherein, the power of described microwave treatment is 500 ~ 800W, is preferably 600 ~ 750W; The time of microwave treatment is 3 ~ 10min, is preferably 5 ~ 8min; The temperature of microwave treatment is 120 ~ 200 DEG C, is preferably 150 ~ 180 DEG C.In the present invention, the temperature of described microwave treatment is the pretreated temperature of reaction of maize straw.
After maize straw is mixed with ethylenediamine solution, carry out microwave treatment before, preferably described mixture is carried out thermal pretreatment, the temperature of described thermal pretreatment should be less than the temperature of microwave treatment maize straw, and on the basis of described thermal pretreatment temperature, the temperature of described microwave treatment maize straw can be reached within the time of microwave treatment.In the present invention, the temperature of described thermal pretreatment is 50 ~ 110 DEG C, is preferably 70 ~ 100 DEG C.
After microwave treatment terminates, heat-treat mixture, concrete, thermal treatment of the present invention is for maintaining described maize straw pretreated temperature of reaction for some time, and described heat treated temperature is 120 ~ 200 DEG C, is preferably 150 ~ 180 DEG C; The described heat treated time is 10 ~ 60min, is preferably 30 ~ 50min.
To cool through heat treated mixture, take out mixture, mixture will be filtered, obtain maize straw and reaction feed liquid.Above-mentioned maize straw is carried out wash, dry, obtain pretreated maize straw.
Maize straw mixes with ethylenediamine solution by the present invention, in confined conditions, successively through microwave treatment and thermal treatment, obtains pretreated maize straw.Quadrol has stronger alkalescence, can open the ehter bond between xylogen and hemicellulose, lignin degrading, and retain Mierocrystalline cellulose and hemicellulose largely, microwave can reduce cellulosic degree of crystallinity, and the enzymolysis efficiency of pretreated maize straw is improved.The method applied microwave assists ethylenediamine solution to carry out pre-treatment to maize straw, can effective lignin degrading, reduces cellulose crystallity, improves the enzymolysis efficiency of Mierocrystalline cellulose and hemicellulose in maize straw.The present invention is simple to operate, and without the need to adopting high-tension apparatus, low for equipment requirements, energy consumption is low, is applicable to suitability for industrialized production.
Result shows, the yield of the glucose of maize straw after pre-treatment enzymolysis is 50 ~ 90%.
In order to understand the present invention further, be described below in conjunction with the method for embodiment to microwave-assisted pre-treatment maize straw provided by the invention, protection scope of the present invention is not limited by the following examples.
Embodiment 1
The dry matter content taken through fragmentation is the reactor that the maize straw of 5g puts into 250mL with closure, and adding 200mL mass body volume concentrations is the ethylenediamine solution of 1%, stirs, and screwing hermetic lid is preheating to 50 DEG C.Microwave generator is utilized to carry out microwave and heating to reactor, microwave power is 500W, process 3min, temperature of reaction is 120 DEG C, maintains above-mentioned temperature of reaction, reaction 10min, cooling reactor, take out solidliquid mixture filtered through gauze, solid 400mL washes, filter, drying obtains pretreated maize straw.
Pretreated maize straw is through saccharification analysis, and glucose yield is 50%.
Embodiment 2
The dry matter content taken through fragmentation is the reactor that the maize straw of 5g puts into 250mL with closure, and adding 25mL mass body volume concentrations is the ethylenediamine solution of 40%, stirs, and screwing hermetic lid, without the need to preheating.Microwave generator is utilized to carry out microwave and heating to reactor, microwave power is 800W, process 10min, temperature of reaction is 200 DEG C, maintains above-mentioned temperature of reaction, reaction 60min, cooling reactor, take out solidliquid mixture filtered through gauze, solid 400mL washes, filter, drying obtains pretreated maize straw.
Pretreated maize straw is through saccharification analysis, and glucose yield is 90%.
Embodiment 3
The dry matter content taken through fragmentation is the reactor that the maize straw of 5g puts into 250mL with closure, and adding 50mL mass body volume concentrations is the ethylenediamine solution of 20%, stirs, and screwing hermetic lid, without the need to preheating.Microwave generator is utilized to carry out microwave and heating to reactor, microwave power is 750W, process 8min, temperature of reaction is 180 DEG C, maintains above-mentioned temperature of reaction, reaction 30min, cooling reactor, take out solidliquid mixture filtered through gauze, solid 400mL washes, filter, drying obtains pretreated maize straw.
Pretreated maize straw is through saccharification analysis, and glucose yield is 85%.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (8)
1. a method for microwave-assisted pre-treatment maize straw, is characterized in that, comprises the following steps:
Maize straw is mixed with ethylenediamine solution, in confined conditions, successively through microwave treatment and thermal treatment, obtains pretreated maize straw.
2. method according to claim 1, is characterized in that, the quality volume fraction of described ethylenediamine solution is 1% ~ 40%.
3. method according to claim 1, is characterized in that, the dry-matter of described maize straw and the mass volume ratio of ethylenediamine solution are 1g:(2 ~ 40) mL.
4. method according to claim 1, is characterized in that, the power of described microwave treatment is 500 ~ 800W, and the time of microwave treatment is 3 ~ 10min, and the temperature of microwave treatment is 120 ~ 200 DEG C.
5. method according to claim 1, is characterized in that, described heat treated temperature is 120 ~ 200 DEG C, and the heat treated time is 10 ~ 60min.
6. method according to claim 1, is characterized in that, before described microwave treatment, also comprises thermal pretreatment.
7. method according to claim 6, is characterized in that, the temperature of described thermal pretreatment is 50 ~ 110 DEG C.
8. method according to claim 1, is characterized in that, after described thermal treatment, also comprises maize straw successively through filtering, washing and drying.
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| CN201510020718.1A CN104561130A (en) | 2015-01-16 | 2015-01-16 | Microwave-assisted pretreatment method for maize straws |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107178965A (en) * | 2017-05-31 | 2017-09-19 | 镇江虎瑞生物科技有限公司 | A kind of stalk material method for microwave drying |
| CN113416760A (en) * | 2021-07-09 | 2021-09-21 | 河南农业大学 | Method for promoting hydrolysis of lignocellulose by heat treatment |
| CN113773665A (en) * | 2021-09-17 | 2021-12-10 | 吉林农业大学 | Preparation method of mycelium buffer material |
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| CN103597041A (en) * | 2011-05-27 | 2014-02-19 | 克拉里安特国际有限公司 | New sustainable range of dyestuffs for textile and paper dyeing |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107178965A (en) * | 2017-05-31 | 2017-09-19 | 镇江虎瑞生物科技有限公司 | A kind of stalk material method for microwave drying |
| CN113416760A (en) * | 2021-07-09 | 2021-09-21 | 河南农业大学 | Method for promoting hydrolysis of lignocellulose by heat treatment |
| CN113416760B (en) * | 2021-07-09 | 2024-03-01 | 河南农业大学 | Method for promoting lignocellulose hydrolysis by heat treatment |
| CN113773665A (en) * | 2021-09-17 | 2021-12-10 | 吉林农业大学 | Preparation method of mycelium buffer material |
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