CN107488682A - A kind of efficient green improves the combination pretreating process of lignocellulosic enzymolysis saccharification efficiency - Google Patents
A kind of efficient green improves the combination pretreating process of lignocellulosic enzymolysis saccharification efficiency Download PDFInfo
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- CN107488682A CN107488682A CN201710817133.1A CN201710817133A CN107488682A CN 107488682 A CN107488682 A CN 107488682A CN 201710817133 A CN201710817133 A CN 201710817133A CN 107488682 A CN107488682 A CN 107488682A
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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
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- C12P2201/00—Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
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Abstract
The present invention relates to a kind of technique for improving lignocellulosic saccharification efficiency using NADES and NU combined pretreatments.Mix the processing that the first step is carried out to lignocellulosic material by a certain percentage with Choline Chloride/lactic acid first, remove partial lignin, hemicellulose, and destroy the fine and close structure of lignocellulosic to a certain extent；NU is recycled to carry out second step pretreatment to lignocellulosic at different temperatures.The present invention can reduce lignin, hemi-cellulose components proportion, and lignocellulosic surface is become loose porous, the accessible surface of increased fiber element enzyme, improve the saccharification efficiency of lignocellulosic.This combination pretreating process has the advantages that equipment requirement is not high, simple to operate, treatment conditions are gentle, cost is cheap, green, and the saccharification efficiency of lignocellulosic can be substantially improved.
Description
Technical field
The present invention relates to lignocellulosic to produce bio-ethanol preconditioning technique field, is specifically a kind of NADES（My god
Right depth congruent melting solvent）Choline Chloride/lactic acid combines the technique that pretreatment improves lignocellulosic enzymolysis saccharification efficiency with NU.
Background technology
Under the tight demand of the alive bound pair energy and the background of traditional fossil energy increasingly depleted, reproducible bioenergy
Increasingly it is valued by people.Lignocellulosic is the renewable resource that reserves are maximum on the earth, is produced as raw material
Alcohol fuel is considered as one of current effective way for solving energy crisis.Lignocellulosic is mainly by cellulose, hemicellulose
Element and lignin form complicated and stable structure by hydrogen bond, covalent bond etc., and it, which is converted into alcohol fuel, mainly includes pre- place
Three reason, enzymatic saccharification, fermentation processes.Lignocellulosic structure has height stubbornly resisting property, makes its enzymatic saccharification efficiency low, it is necessary to
By appropriate pretreatment to improve enzymolysis efficiency.Therefore, pretreatment is the committed step in wood-based composites conversion process.
In recent years, global scholar has been carried out widely studied to lignocellulose pretreatment method, is broadly divided into：Physics is located in advance
The methods of reason, Chemical Pretreatment, physical chemistry pretreatment and Biological Pretreatment.Physical has mechanical crushing, high-energy radiation, high temperature
The methods of decomposition, microwave treatment.Physical-chemical process has steam blasting, hydro-thermal method etc..Chemical method has the side such as acid, alkali, organic solvent
Method.Biological treatment typically uses fungi（Such as whiterot fungi）Or some actinomyces are handled.Although steam explosion enzymolysis effect
Rate is higher, but it is high to equipment requirement, and input is big, constrains large-scale production.Low-kappa number is failed to understand delignification effect
It is aobvious, add the intractability of subsequent treatment, acid solution is also that to restrict its industrialized to the corrosivity that pretreatment unit has
One of major reason；Oxygenation pretreatment cost is relatively low, safe operation, but waste water and residue need to be recycled.Bioanalysis
Then mainly using the pretreatment of the fungies such as whiterot fungi, treatment conditions are gentle, but pretreatment time is long, less efficient, are unsuitable for work
Industry application.Therefore, the high-efficiency pretreatment technology of developing low-cost is for promoting lignocellulosic to produce the development of alcohol fuel
It is significant.
Depth congruent melting solvent（Deep eutectic solvent）Vehicle economy S, it is by 2 kinds or of more than two kinds organic molten
The respective lower mixture of fusing point of ratio of agent composition, this, which allows for mixture, melt in lower temperature, for mixed solvent
Formation reduces energy consumption.The DES being made up of natural organic matter is known as NADES（natural deep eutectic
solvent）, NADES is a kind of mainly glucide by being widely present in metabolite, various amino acid and nature
Deng the depth congruent melting solvent of composition.Similar to ionic liquid, NADES is also a kind of green solvent, but it is more natural, be easy to get and pass through
Ji material benefit, cause the great interest of researchers.There are some researches show NADES to biological species natural product not soluble in water at present
There are special dissolubility, such as lignin, cellulose, DNA etc., therefore had using NADES come preprocessing lignocellulose material
There is good application prospect.Choline Chloride is a kind of water soluble vitamin product, is a kind of common NADES components, can be with urine
The hydrogen bond donor such as element, lactic acid is mixed to form NADES according to a certain percentage.In recent years, researcher is used based on Choline Chloride
Want the NADES of composition to pre-process lignocellulosic, there is the characteristics of economic and environment-friendly, but pre-process efficiency and need to be carried
It is high.The pretreatment that more efficient NADES is developed applied to lignocellulosic is current hot research direction, but correlative study is entered
Postpone slow.Therefore, NADES is combined with other method, lignocellulosic is increased substantially on the basis of economic and environment-friendly
Hydrolysis and saccharification efficiency, be NADES treatment technologies another developing direction.
Using cellulose under cryogenic（Less than -20 DEG C）The characteristic of NU mixed solutions is dissolved in, has researcher will
NU mixed solutions are applied to the pretreatment of lignocellulosic.In NU preprocessing process, alkali can destroy in cellulosic molecule with
Intermolecular hydrogen bond, while urea hydrate can cause the depolymerization and dissolving of cellulose as the donor and acceptor of hydrogen bond.Cause
This, NU pre-processes the enzymatic saccharification efficiency that can significantly improve lignocellulosic.But this method needs instead in processing procedure
Multiple freeze thawing and high-speed stirred, harsh condition cause it to be difficult to the large-scale application in lignocellulosic pre-processes.
When NADES and NU is applied to lignocellulosic pretreatment, there is the advantages of respective, but obvious lack also all be present
Two methods are combined by point, the present invention, then while played respective advantage, be it also avoid the shortcomings that respective, can be obtained
A kind of equipment requirement is not high, simple to operate, treatment conditions are gentle, cost is cheap, green lignocellulosic pretreatment
Technique, have a good application prospect.
The content of the invention
In order to solve the problems, such as that existing Pretreatment Technologies of Lignocellulose is present, the invention provides a kind of Choline Chloride/
The technique of lactic. acid combination NU pretreatments, improve the enzymatic saccharification efficiency of lignocellulosic.
The technical scheme is that：
（1）Lignocellulosic is dry, crushes, and it is 180-425 μm to control particle diameter；
（2）Lactic acid presses 2 with Choline Chloride:1-8:1 mixed in molar ratio, it is put in 40-100 DEG C of shaking table, it is to be formed a kind of complete
Merge the liquid of water white transparency, then make it stable take out after 10 min it is standby；
（3）By 10%（W/W）Content adds lignocellulosic, adds above-mentioned（2）In congruent melting solvent, and in 40-100 DEG C of shaking table
After middle vibration mixes pretreatment 12-72 h, filter and using distilled water cleaning filter residue, until cleaning fluid pH will clean in neutrality
Filter residue afterwards is placed in 50-60 DEG C of drying, obtains the lignocellulosic sample after NADES processing；
（4）Lignocellulosic after NADES is handled is placed in appropriately sized container, is 1 by solid-to-liquid ratio:10-1:30（g/mL）
The NU solution that concentration is 2%/3%-4%/6% is added, is statically placed in after handling 2-6 h in -5 DEG C to 25 DEG C isoperibols, filtering is simultaneously
Filter residue is cleaned using distilled water, until the filter residue after cleaning is placed in 50-60 DEG C of drying, obtained final by cleaning fluid pH in neutrality
Lignocellulosic sample after processing；
（5）Lignocellulosic sample after two step combined pretreatments is pressed to 10-30 mg/mL concentration and Citrate buffer
Liquid（0.1 mol/L, pH 4.8）Mixing, adds 10-40 FPU/g substrate cellulases, in 40-60 DEG C, 100-200
After digesting 24-72 h under the conditions of rpm/min, enzymatic saccharification efficiency is determined.
The advantage of preprocess method provided by the invention is：
（1）The two-step method combined using Choline Chloride/lactic acid pretreatment with NU, is removed most of lignin component, reduced wooden
Cellulose crystallity, the accessible surface of increased fiber element enzyme so that raw material surface becomes coarse and loose porous, improves wooden fibre
Tie up the saccharification efficiency of element；
（2）Enzymatic saccharification efficiency can be greatly improved through the pretreated lignocellulosic of the combined method, can from 32.6% highest
Bring up to 91.33%；
（3）Second step temperature conditionss can be carried out at normal temperatures in preprocessing process, and the economic benefit of this method shows under the conditions of making originally
Write increase；
（4）The preprocess method is green, low for equipment requirements, simple to operate, treatment conditions are gentle, cost is cheap.
Brief description of the drawings:
Fig. 1：Change of component before and after lignocellulosic pretreatment
Fig. 2：The front and rear hydrolysis result of lignocellulosic pretreatment
Fig. 3：Lignocellulosic pre-processes front and rear surfaces structure change
Embodiment：
The present invention is further illustrated with rice straw research embodiment below in conjunction with the accompanying drawings, but it is not as a limitation of the invention.
Embodiment 1：
（）Rice straw is dry, crushes, and it is 180-425 μm to control particle diameter；
（）Lactic acid presses 4 with Choline Chloride:1 mixed in molar ratio, it is put in 70 DEG C of shaking tables, a kind of nothing of fusion completely to be formed
The transparent liquid of color, then make it stable take out after 10min it is standby；
（）By 10%（W/W）Content adds rice straw, adds above-mentioned（）In congruent melting solvent, and in 70 DEG C of shaking tables
Vibration mix pretreatment 48 h after, filter simultaneously using distilled water cleaning filter residue, until cleaning fluid pH in neutrality, by the filter after cleaning
Slag is placed in 55 DEG C of drying, obtains the rice straw sample after NADES processing；
（）Rice straw after NADES is handled is placed in appropriately sized container, is 1 by solid-to-liquid ratio:20（g/mL）Add dense
The NU solution for 4%/6% is spent, is statically placed in after handling 4h in 25 DEG C of isoperibols, filters and cleans filter residue using distilled water, directly
To cleaning fluid pH in neutrality, the filter residue after cleaning is placed in 55 DEG C of drying, obtains the rice straw sample after final process；
（）Rice straw sample after two step combined pretreatments is pressed to 25 mg/mL concentration and citrate buffer
（0.1 mol/L, pH 4.8）Mixing, adds 12 FPU/g substrate cellulases, under the conditions of 50 DEG C, 100 rpm/min
After digesting 72 h, enzymatic saccharification efficiency is determined.
By the implementation of the present embodiment, lignin significantly reduces with hemicellulose level in the rice straw after processing（It is attached
Fig. 1）, content of cellulose lifting to 73.53%, digest concentration of reduced sugar and bring up to 21 g/L from 7.5 g/L（Accompanying drawing 2）, saccharification effect
Rate brings up to 91.33% from 32.6%, is original 2.8 times, the hydrolysis result of rice straw is significantly carried after combined pretreatment
It is high.With reference to scanning electron microscope image（Accompanying drawing 3）It is shown, raw water rice straw（a、b）In direct rod shape and bar footpath it is thicker, surfacing
It is smooth；And through the pretreated rice straw of the present embodiment（c、d）Rough surface, there is serious hole phenomenon, considerably increase
The accessible surface of enzyme, improve the enzymatic saccharification effect of rice straw.
Embodiment 2：
（）Rice straw is dry, crushes, and it is 180-425 μm to control particle diameter；
（）Lactic acid presses 4 with Choline Chloride:1 mixed in molar ratio, it is put in 70 DEG C of shaking tables, a kind of nothing of fusion completely to be formed
The transparent liquid of color, then make it stable take out after 10min it is standby；
（）By 10 %（W/W）Content adds rice straw, adds above-mentioned（）In congruent melting solvent, and in 70 DEG C of shaking tables
Vibration mix pretreatment 48 h after, filter simultaneously using distilled water cleaning filter residue, until cleaning fluid pH in neutrality, by the filter after cleaning
Slag is placed in 55 DEG C of drying, obtains the rice straw sample after NADES processing；
（）Rice straw after NADES is handled is placed in appropriately sized container, is 1 by solid-to-liquid ratio:20 （g/mL）Add dense
The NU solution for 4%/6% is spent, is statically placed in after handling 4h in 4 DEG C of isoperibols, is filtered and using distilled water cleaning filter residue, until clear
Filter residue after cleaning is placed in 55 DEG C of drying, obtains the rice straw sample after final process by washing lotion pH in neutrality；
（）Rice straw sample after two step combined pretreatments is pressed to 25 mg/mL concentration and citrate buffer
（0.1 mol/L, pH 4.8）Mixing, adds 12 FPU/g substrate cellulases, under the conditions of 50 DEG C, 100 rpm/min
After digesting 72 h, enzymatic saccharification efficiency is determined.
After the pretreated rice straw of the present embodiment digests 72 h, reduction candy output is set to be brought up to from 7.5 g/L
17.56 g/L（Accompanying drawing 2）, saccharification efficiency brings up to 76.38% from 32.6%, is original 2.34 times.
Embodiment 3：
（a）Rice straw is dry, crushes, and it is 180-425 μm to control particle diameter；
（）Lactic acid presses 4 with Choline Chloride:1 mixed in molar ratio, it is put in 70 DEG C of shaking tables, a kind of nothing of fusion completely to be formed
The transparent liquid of color, then taken out after making it stable 10 minutes standby；
（c）By 10%（W/W）Content adds rice straw, adds above-mentioned（）In congruent melting solvent, and shaken in 70 DEG C of shaking tables
It is dynamic mix 48 h of pretreatment after, filter simultaneously using distilled water cleaning filter residue, until cleaning fluid pH is in neutrality, by the filter residue after cleaning
55 DEG C of drying are placed in, obtain the rice straw sample after NADES processing；
（）Rice straw after NADES is handled is placed in appropriately sized container, is 1 by solid-to-liquid ratio:20（g/mL）Add dense
The NU solution for 2%/3% is spent, is statically placed in after handling 4h in 25 DEG C of isoperibols, is filtered and using distilled water cleaning filter residue, until
Filter residue after cleaning is placed in 55 DEG C of drying, obtains the rice straw sample after final process by cleaning fluid pH in neutrality；
（）Rice straw sample after two step combined pretreatments is pressed to 25 mg/mL concentration and citrate buffer
（0.1 mol/L, pH 4.8）Mixing, adds 12 FPU/g substrate cellulases, under the conditions of 50 DEG C, 100 rpm/min
After digesting 72 h, enzymatic saccharification efficiency is determined.
After the pretreated rice straw enzymolysis 72h of the present embodiment, reduction candy output brings up to 15.7 from 7.5 g/L
g/L（Accompanying drawing 2）, saccharification efficiency brings up to 68.3% from 32.6%, is original 2.09 times.
Claims (3)
1. one kind improves lignocellulosic saccharification result combination pretreating process, it is characterised in that lignocellulosic is pretreated
Journey is divided into two steps, after first being handled using NADES, further utilizes alkali/urea（NU）Handled.
2. the combination pretreating process according to claim 1 for improving lignocellulosic saccharification result, it is characterised in that
NADES processing procedures are：Under the conditions of 40-100 DEG C, lactic acid and Choline Chloride are pressed 2:1-8:1 mixed in molar ratio obtains
After NADES, by 10-20 %（W/W）Content adds lignocellulosic, and 2-6 h, the wooden fibre of gained are pre-processed under oscillating condition
The cleaning of dimension element is dried after being in neutrality to pH.
3. the combination pretreating process according to claim 1 for improving lignocellulosic saccharification result, it is characterised in that NU
Processing procedure is：After NADES is handled, it is 1 that gained lignocellulosic is pressed into solid-to-liquid ratio:10-1:30 （g/mL）It is dense to add quality
The NU solution for 2%/3%-4%/6% is spent, is statically placed in -5 DEG C to 25 DEG C isoperibols and is separated by filtration after 2-6 h, gained
Lignocellulosic is cleaned to pH in after neutral, is dried to constant weight, is completed the pretreatment of lignocellulosic.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108441530A (en) * | 2018-03-13 | 2018-08-24 | 北京化工大学 | A method of utilizing alkaline eutectic solvent preprocessing lignocellulose |
| CN108660837A (en) * | 2018-05-29 | 2018-10-16 | 南京林业大学 | The separation method of three component of cellulose, hemicellulose and lignin in one plant fiber raw material |
| CN112316860A (en) * | 2020-10-13 | 2021-02-05 | 华南农业大学 | Biomass-based hydrogel and preparation method and application thereof |
| US11136249B1 (en) | 2020-05-26 | 2021-10-05 | Qatar University | Destabilization and separation of high stable colloids |
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| CN105002232A (en) * | 2015-07-31 | 2015-10-28 | 湘潭大学 | Combined pretreatment process for improving lignocellulose saccharification effect |
| CN105177055A (en) * | 2015-07-31 | 2015-12-23 | 湘潭大学 | Biological-chemical combined treatment process for improving saccharifying effect of lignocellulose |
| CN106755189A (en) * | 2016-10-31 | 2017-05-31 | 广东工业大学 | It is a kind of to pre-process to improve the green method of rice straw cellulase solution efficiency using two kinds of depth congruent melting solvent substeps |
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| CN105002232A (en) * | 2015-07-31 | 2015-10-28 | 湘潭大学 | Combined pretreatment process for improving lignocellulose saccharification effect |
| CN105177055A (en) * | 2015-07-31 | 2015-12-23 | 湘潭大学 | Biological-chemical combined treatment process for improving saccharifying effect of lignocellulose |
| CN106755189A (en) * | 2016-10-31 | 2017-05-31 | 广东工业大学 | It is a kind of to pre-process to improve the green method of rice straw cellulase solution efficiency using two kinds of depth congruent melting solvent substeps |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108441530A (en) * | 2018-03-13 | 2018-08-24 | 北京化工大学 | A method of utilizing alkaline eutectic solvent preprocessing lignocellulose |
| CN108660837A (en) * | 2018-05-29 | 2018-10-16 | 南京林业大学 | The separation method of three component of cellulose, hemicellulose and lignin in one plant fiber raw material |
| US11136249B1 (en) | 2020-05-26 | 2021-10-05 | Qatar University | Destabilization and separation of high stable colloids |
| CN112316860A (en) * | 2020-10-13 | 2021-02-05 | 华南农业大学 | Biomass-based hydrogel and preparation method and application thereof |
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