CN105838608A - Method for segment pretreatment on straws through ammonia water and hydrogen peroxide - Google Patents
Method for segment pretreatment on straws through ammonia water and hydrogen peroxide Download PDFInfo
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- CN105838608A CN105838608A CN201510870893.XA CN201510870893A CN105838608A CN 105838608 A CN105838608 A CN 105838608A CN 201510870893 A CN201510870893 A CN 201510870893A CN 105838608 A CN105838608 A CN 105838608A
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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
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
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Abstract
The invention discloses a method for segment pretreatment on straws through ammonia water and hydrogen peroxide. The method utilizes straws as raw materials and comprises ammonia water and water addition, sealing, uniform blending, standing, hydrogen peroxide addition, sealing, uniform blending and standing. Through segment pretreatment with ammonia water and hydrogen peroxide, a microbial growth inhibitor produced by ammonia water pretreatment is effectively reduced, a reagent price is low, an addition amount is less, safety and environmental friendliness are obtained, pretreatment conditions are mild, a high temperature and high pressure are avoided, equipment requirements are low and energy consumption is low. After enzymatic hydrolysis of straw products pretreated through the method for 15h, a DNS test result shows that a reducing sugar yield is 0.523g/g straw. The method can be simply operated, has mild conditions, has high efficiency and is suitable for industrial large-scale treatment.
Description
Technical field
The invention belongs to applied technical field, be specifically related to a kind of method utilizing ammonia and hydrogen peroxide that straw is carried out segmentation pretreatment.
Background technology
China is a large agricultural country, and annual straw yield is more than 900,000,000 tons, but its effective rate of utilization is less than 50%, and most straw is all given up
Abandoning or burn, abandoned piles land occupation, and burning can cause serious air pollution, the most now to the dependence of fossil energy to environment and can
Sustainable development brings the biggest pressure, and improving stalk comprehensive utilization efficiency is the effective way solving the problem such as above-mentioned.
Straw main component is lignocellulose, and wood fibre is mainly made up of cellulose, hemicellulose and lignin, and these three composition is closely handed over
Being linked togather and cause stalk effectively can not be degraded by cellulase, it is necessary to the most just can be used effectively, this is also to limit straw utilization
Key factor, so straw utilization efficiency to be improved, first have to find suitable preprocess method.The method of straw pretreatment has multiple, mainly
It is the preparation phase coupling with bioenergy, includes among these at mechanical means (grind and pulverize), heat treatment (heat treatment or steam explosion), acid
The preprocess method etc. that reason, alkali process and Oxidation and ammonia and carbon dioxide combine.But these methods or condition are harsh high to equipment requirements,
Or reagent addition big post processing trouble, the problem that all there is high expensive, the most just hinder the process that straw industrialization utilizes.
200510011217 " utilizing the method that straw pretreatment and enzymolysis process make the complete enzymolysis of stalk cellulose " describe a kind of by straw steam explosion
Rear washing, then with ionic liquid mixed processing, then the preprocess method of cyclic washing, cellulose degradation rate nearly 100% after process；201310394002
" a kind of preprocess method realizing wheat straw waste efficient enzyme hydrolysis conversion " describes after wheat straw waste is soaked by one and carries out screw extrusion, adds
Sulphuric acid or naoh treatment, then carry out two sections of grindings and process the processing method of enzymolysis again after water bath with thermostatic control, the off-the-shelf equipment of available pulp industry；
A kind of method that 201110007487 " a kind of lignocellulose acid/alkali coupling pretreatment methods " describe lignocellulose acid/alkali coupling pretreatment, uses
Hemicellulose and part monosaccharide are reclaimed in acid treatment, then process recovery lignin with alkali, and liquid enzymatic saccharification utilizes, and the separation reaching three elements utilizes.
Above-mentioned straw pretreatment method is many, and there are the following problems: the condition having is harsh, high to equipment requirements；Some consuming soda acid amounts are big, at waste liquid
Reason difficulty；Some processes are complicated, complex operation；In commercial Application, all there is certain difficulty.
Summary of the invention
It is an object of the invention to provide a kind of method utilizing ammonia and hydrogen peroxide that straw is carried out pretreatment, the method is easy and simple to handle, mild condition,
Efficiency is high, it is adaptable to the process of industrial mass, pretreatment product can be easy to the industrial applications of straw simultaneously.
In order to achieve the above object, the present invention takes techniques below measure:
A kind of method utilizing ammonia and hydrogen peroxide that straw is carried out segmentation pretreatment, including: the stalk after Crushing of Ultrafine, it is initially charged ammonia
And water, seal, mixing, stand；Rear addition hydrogen peroxide, seals, mixing, and standing processes.
Approach described above, according to straw content in final system 60～80% (w/w), ammonia content 0.5～2.5% (w/w), content of hydrogen peroxide
1～3% (w/w) calculate need to add the water yield, ammonia vol and the dioxygen water yield.
In schemes described above, it is preferred that described straw is corn straw, it is crushed to >=200 mesh；
In schemes described above, it is preferred that in final system straw content be 70% (w/w), ammonia content be 2.5% (w/w), content of hydrogen peroxide
It is 2% (w/w)；
In schemes described above, it is preferred that standing duration twice and be 24h, ambient temperature during standing is 20～25 DEG C；
In schemes described above, it is preferred that second time is put into when standing in the water of 20～25 DEG C.
Utilize the pretreated corn straw of the method for the invention, can be directly used for strain fermentation, or the preparation for methane, or other are the most existing
Commercial Application with straw as raw material.
Compared with prior art, the invention have the advantages that
1. during pretreatment, material is solid fraction, and utilization rate of equipment and installations is high, processes product and is easy to industrialized utilization.
2. pretreatment agents useful for same is ammonia and hydrogen peroxide, and cheap, addition is low, safety and environmental protection.
3. ammonia and hydrogen peroxide treatment by stages, can effectively reduce the growth of microorganism mortifier that pretreatment with agueous Ammonia produces.
4. pretreatment condition is gentle, it is not necessary to High Temperature High Pressure, relatively low to equipment requirements, energy consumption is low.
5. pretreating process is easy and simple to handle, pretreatment low cost.
6. the method pretreated straw product enzymolysis 15h utilizing the present invention to provide, records reducing sugar (glucose and xylose) yield with DNS and reaches
0.523g/g straw.
Detailed description of the invention
Embodiment 1:
A kind of method utilizing ammonia and hydrogen peroxide that straw is carried out segmentation pretreatment, including:
Taking fine corn straw (>=200 mesh), add water and ammonia, mixing, 25 DEG C stand 24h；Add hydrogen peroxide again, mixing, will add
Enter the mixture after hydrogen peroxide and put into (meeting aerogenesis heat release after addition hydrogen peroxide) in 20 DEG C of water, water stands 24h.
Add water, ammonia, the amount of hydrogen peroxide according to straw content in final system be 70% (w/w), ammonia content be 2.5% (w/w), peroxide
Changing hydrogen content is that 2% (w/w) calculates.
The ammonia initial concentration added is 25%, and the initial concentration of the hydrogen peroxide of addition is 30%.
Concrete system is as follows:
Embodiment 2:
A kind of method utilizing ammonia and hydrogen peroxide that straw is carried out segmentation pretreatment, including:
The method of the present embodiment is substantially the same manner as Example 1, and difference is: in final system, ammonia content is 0.5% (w/w), content of hydrogen peroxide
It is 1% (w/w).Concrete system is as follows:
Embodiment 3:
A kind of method utilizing ammonia and hydrogen peroxide that straw is carried out segmentation pretreatment, including:
The method of the present embodiment is substantially the same manner as Example 1, and difference is: in final system, ammonia content is 2.5% (w/w), content of hydrogen peroxide
It is 3% (w/w).
Concrete system is as follows:
Embodiment 4:
A kind of method utilizing ammonia and hydrogen peroxide that straw is carried out segmentation pretreatment, including:
The method of the present embodiment is substantially the same manner as Example 1, and difference is: in final system, ammonia content is 1.5% (w/w), content of hydrogen peroxide
It is 3% (w/w).
Concrete system is as follows:
Embodiment 5:
A kind of method utilizing ammonia and hydrogen peroxide that straw is carried out segmentation pretreatment, including:
The method of the present embodiment is substantially the same manner as Example 1, and difference is: in final system, ammonia content is 1.5% (w/w), content of hydrogen peroxide
It is 2% (w/w).
Concrete system is as follows:
Embodiment 6:
Pretreated corn straw is the detection of sugar yield after enzymolysis:
After weighing 10g pretreatment, straw (moisture content 30%) is in 250mL triangular flask, adds bead, adds the compound system of cellulase
Agent 50FPU/g (pretreatment substrate), the 0.1mol/L acetic acid-sodium acetate buffer solution adding pH 5.0 is settled to 100mL.By triangular flask plastics
Film seal, puts 50 DEG C, 15h in 150r/min shaking bath.Draw 2mL enzymolysis solution, measure content of reducing sugar by DNS method.
DNS method: take enzymolysis solution 2mL, 8000r/min is centrifuged 10min and collects supernatant, and content of reducing sugar dilution supernatant, takes 1mL on the estimation
Supernatant adds in 25mL glass color comparison tube, adds 3mL DNS reagent, boiling water bath 5min, and flowing water is cooled to room temperature, adds distilled water to 25mL
Graduation mark, in 540nm colorimetric after shaking up.Sugared yield after calculating enzymolysis according to standard curve.
Specification Curve of Increasing method: at 105 DEG C of drying baker, AG glucose is dried 3h, takes 1g glucose and is dissolved in deionized water, constant volume
To 100mL.Take 1mL, 2mL, 3mL, 4mL, 5mL, 6mL, 7mL glucose the most respectively, then be settled to 100mL, i.e. can get dense
Degree is the Standard for Sugars liquid of 0.1g/L, 0.2g/L, 0.3g/L, 0.4g/L, 0.5g/L, 0.6g/L and 0.7g/L, draws 1mL titer and adds 3mL DNS
Reagent, in 540nm colorimetric after boiling water bath 5min, draws standard curve according to absorbance and sugar concentration.
Utilize the pretreated straw of embodiment 1～5, after said method enzymolysis, final sugar yield such as following table:
Table 1
Embodiment 7:
The application in strain fermentation of the pretreated corn straw:
Used by the present embodiment is the corn straw of gained after embodiment 1 method pretreatment.
Culture medium: straw 45g (moisture content 30%), water 50ml, molasses 4g, phosphoric acid 0.14ml, carbamide 0.84g after pretreatment, uses phosphoric acid
Regulation PH to about 7.0.
The unsterilised direct inoculation of culture medium that will prepare, seed liquor consumption is 10mL (a type candida mycoderma and each 5ml of Lactobacillus pentosus seed liquor),
Adding 1g aspergillus niger again, postvaccinal type candida mycoderma is 100,000,000/g, and Lactobacillus pentosus is 500,000,000/g.
After inoculation mix, be loaded in wide mouthed bottle, gauze seal, as in 30 DEG C of incubators cultivate, every 24h stirring once, 72h fermentation ends.
With untreated corn straw as matched group, other conditions are identical.Blood counting chamber method measures yeast quantity in fermented product, mixed bacterium method
Measure Lactobacillus pentosus content.The results are shown in Table 2.
Type candida mycoderma growth result between table 2-1 mixed fungus fermentation pretreated straw and untreated straw
Table 2-2 mixed fungus fermentation pretreated straw and untreated straw Lactobacillus pentosus growth result
Result shows: with matched group, i.e. not having the result of pretreatment to compare, yeast count at least improves 10 times, and lactic acid bacteria number improves 25 times,
Illustrate that the straw of Combined Treatment can be effectively improved fermentable effect.The utilization ratio of this method pretreated straw apparently higher than untreated straw,
Confirm that the inventive method is the most feasible, apply effective.
Embodiment 8:
Between type candida mycoderma and Lactobacillus pentosus the carbon source in pretreated straw and nitrogen source can effectively be utilized:
Used by the present embodiment is the corn straw of gained after embodiment 7 is fermented.
By pretreated straw, survey reducing sugar by DNS, survey nitrogen content by Kjeldahl's method.
Reducing sugar and nitrogen content result before and after table 3 pretreated straw mixed fungus fermentation
Result shows: as compared to matched group, i.e. result before fermentation, after fermentation, in material, reducing sugar reduces close to half, it was demonstrated that above-mentioned
Type candida mycoderma and Lactobacillus pentosus growth are to carbon source and effective utilization in nitrogen source.
Embodiment 9:
Pretreated corn straw methane phase is tested:
Used by the present embodiment is the corn straw of gained after embodiment 1 method pretreatment.
The pretreated straw of method described in 50g (over dry) embodiment 1, adds anaerobic sludge 150mL (dry matter content is 10%).
Anaerobic fermentation total solids content is 8%, supplements corresponding moisture, carries out 55 DEG C of wet fermentations of anaerobism, and before fermentation, paraffin seals, and bottling is as far as possible
Fill, air-out.
Being added as needed on carbamide, controlling total carbon-nitrogen ratio is 25:1, records aerogenesis volume, circulation of qi promoting body composition analysis of going forward side by side.Experiment contrast group is not
Processing straw, other conditions keep consistent.
Table 4 methane fermentation result
From experimental result it can be seen that through the present invention provide the pretreated corn straw of method can produce total gas 395mL, the wherein amount of CH4
For 316mL.And unpretreated corn straw, its CH4Yield only have 90mL, illustrate that fermenting property is poor, experimental group is more right than untreated
Improve more than 2 times according to group biogas output.
Claims (8)
1. utilize the method that ammonia and hydrogen peroxide carry out segmentation pretreatment to straw, including: the stalk after Crushing of Ultrafine, it is initially charged ammonia and water, seals, mixing, stand；Rear addition hydrogen peroxide, seals, mixing, and standing processes.
Method the most according to claim 1, the ammonia of interpolation, the amount of water and hydrogen peroxide is according to straw content 60 ~ 80%, ammonia content 0.5 ~ 2.5% in final system, and content of hydrogen peroxide 1 ~ 3% carries out calculating.
Method the most according to claim 1, described straw is corn straw, is crushed to >=200 mesh.
Method the most according to claim 1, the ammonia of interpolation, the amount of water and hydrogen peroxide be according to straw content in final system be 70%, ammonia content be 2.5%, content of hydrogen peroxide is 2% to carry out calculating.
Method the most according to claim 1, stands duration twice and is 24h, and ambient temperature during standing is 20 ~ 25 DEG C.
Method the most according to claim 1, second time is put into when standing in the water of 20 ~ 25 DEG C.
7. the pretreated corn straw of method described in claim 1 application in strain fermentation.
8. the pretreated corn straw of method described in claim 1 application in methane phase.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111316860A (en) * | 2020-03-06 | 2020-06-23 | 辛小辉 | Method for producing edible fungus sticks by using reed straws |
| CN113854044A (en) * | 2021-09-25 | 2021-12-31 | 广西壮族自治区环境保护科学研究院 | Process for producing wood-rotting fungus base material by using crop straws |
| CN114190475A (en) * | 2021-12-04 | 2022-03-18 | 中国农业科学院特产研究所 | Straw fermented feed and production method thereof |
| CN114668076A (en) * | 2022-02-07 | 2022-06-28 | 吉林农业大学 | Method for preparing silage by using compound microbial agent |
| CN115251240A (en) * | 2022-06-22 | 2022-11-01 | 江苏集萃工业生物技术研究所有限公司 | Preparation method of modified straw through mechanical-assisted in-situ ammoniation |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111316860A (en) * | 2020-03-06 | 2020-06-23 | 辛小辉 | Method for producing edible fungus sticks by using reed straws |
| CN113854044A (en) * | 2021-09-25 | 2021-12-31 | 广西壮族自治区环境保护科学研究院 | Process for producing wood-rotting fungus base material by using crop straws |
| CN114190475A (en) * | 2021-12-04 | 2022-03-18 | 中国农业科学院特产研究所 | Straw fermented feed and production method thereof |
| CN114190475B (en) * | 2021-12-04 | 2024-05-24 | 中国农业科学院特产研究所 | Straw fermented feed and production method thereof |
| CN114668076A (en) * | 2022-02-07 | 2022-06-28 | 吉林农业大学 | Method for preparing silage by using compound microbial agent |
| CN114668076B (en) * | 2022-02-07 | 2023-11-21 | 吉林农业大学 | Method for preparing yellow storage feed by using composite microbial agent |
| CN115251240A (en) * | 2022-06-22 | 2022-11-01 | 江苏集萃工业生物技术研究所有限公司 | Preparation method of modified straw through mechanical-assisted in-situ ammoniation |
| CN115251240B (en) * | 2022-06-22 | 2023-10-27 | 江苏集萃工业生物技术研究所有限公司 | Preparation method of mechanical-assisted in-situ ammoniation modified straw |
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Application publication date: 20160810 |