CN107988269A - A kind of Cold pretreatment of lignocellulose biomass and its method for preparing hydrogen - Google Patents
A kind of Cold pretreatment of lignocellulose biomass and its method for preparing hydrogen Download PDFInfo
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- CN107988269A CN107988269A CN201711217973.0A CN201711217973A CN107988269A CN 107988269 A CN107988269 A CN 107988269A CN 201711217973 A CN201711217973 A CN 201711217973A CN 107988269 A CN107988269 A CN 107988269A
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- lignocellulose biomass
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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
- C12P3/00—Preparation of elements or inorganic compounds except carbon dioxide
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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
- C12P2201/00—Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
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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
- C12P2203/00—Fermentation products obtained from optionally pretreated or hydrolyzed cellulosic or lignocellulosic material as the carbon source
Abstract
A kind of Cold pretreatment of lignocellulose biomass and its method for preparing hydrogen, belong to field of efficient resource utilization of organic solid waste.The present invention solves preferable not to the utmost in terms of pretreating effect during existing Hydrogen Production in Straw Fermentation, cost, operability, versatility and scale application, the especially application problem in cold district winter.Preprocess method：Hydroxide/aqueous solution of urea of alkali metal is cooled to 8 DEG C~20 DEG C in advance；Then the lignocellulose biomass of pulverization process after drying is added, at ambient temperature quick stir process 3min, washs to neutrality, be dried for standby after suction filtration.The lignocellulose biomass handled in above-mentioned Cold pretreatment method adds fluid nutrient medium as substrate, then inoculation production hydrogen microorganism, anaerobic fermentation reaction, collects the gas of output.
Description
Technical field
Cold pretreatment and its method for preparing hydrogen the present invention relates to a kind of lignocellulose biomass, belong to organic
Solid waste high-efficiency resource recycling field.
Background technology
Since the 21th century, the fossil fuel such as coal, oil, natural gas is non-renewable, and petroleum refining production
A variety of environmental problems such as greenhouse effects, acid rain, dust pollution caused by industry, cause people's common concern.Wind is greatly promoted
The research and development of the regenerative resource industries such as energy, solar energy, biomass energy, water energy, geothermal energy, ocean energy.Biomass energy one
Directly important energy source for the survival of mankind, it be only second to coal, oil and natural gas and occupy world energy sources total quantity consumed
The energy of, occupies critical role in whole energy resource system.Modern biotechnology mass-energy, which utilizes, to be referred to by heat chemistry, bioid
Etc. means, by a series of advanced switch technologies, produce the high-grade energies such as solid, liquid, gas to replace fossil fuel.According to
Relevant expert estimates that biomass energy, to the middle of this century, is used as the important component of following sustainable energy system
The biogas of new technology production, alcohol fuel, the new energy such as biodiesel will account for more than global total energy consumption.Stalk is a kind of rich
Rich agricultural wastes, because it has sufficient supply and cheap price, if being translated into hydrogen using microbial technique
And biogas, aerogenesis cost can be reduced and improve its trans-utilization rate, while discarded object is obtained recycling, from cleaning energy
Source is developed and the angle of waste utilization all has great Social benefit and economic benefit.China's agricultural straw resource enriches,
The biomass resources such as stalk are efficiently used, the hydrogen, biogas and organic by-products for being translated into high added value are the stalk energy
Change an important channel in utilizing.
Stalk is mainly made of cellulose, hemicellulose and lignin, and wherein cellulose and hemicellulose are fermentabilities
Carbohydrate, can be translated into after sugar under the action of microorganism or enzyme and generate fuel hydrogen, first for microorganism utilization again
Alkane.Due to lignocellulosic stubbornly resist characteristic and cellulose still suffers from the deficiencies of hydrolysis efficiency is low, cellulase is expensive,
Therefore, lignocellulosic pretreatment is to improve its hydrolysis and saccharification efficiency, reduce the necessary links of processing cost, and is restricted at present
Lignocellulosic efficiently utilizes one of bottleneck.
Lignocellulose pretreatment method is numerous, including the conventional new preconditioning technique for pre-processing and reporting in recent years,
These technologies respectively have advantage and disadvantage in terms of pretreating effect, cost, operability, versatility and scale application.Common
Lignocellulose pretreatment method has ball-milling method, dilute sulfuric acid process, pretreatment with agueous Ammonia, Lime Pretreatment, hot-water pretreatment, the steam quick-fried
Broken method and biologic pretreatment method etc..In recent years, some new preprocess methods are reported both at home and abroad, such as：Chemistry
Combination pretreatment (such as soda acid coupling pretreatment, cellulose solvent/organic solvent pretreatment), physical-chemical combination pretreatment
(such as pretreatment of microwave radiation technology ionic liquid, Microwave Irradiation Assisted Chemical, ethanol boiling-ball-milling method), physical/chemical-life assemblage
Pretreatment, Cold pretreatment, green solvent method, electrochemical pre-treatment etc..
Pretreating effect, cost, operability, versatility and scale application side during existing Hydrogen Production in Straw Fermentation
Face is preferable not to the utmost, and the efficiency of Physical processing is low, high energy consumption；Chemical Treatment high energy consumption (it is generally necessary to high temperature and pressure)；Biology
Method processing time is grown；New pretreatment mode, service condition harshness etc., the especially application problem in cold district winter.
The content of the invention
It is an object of the present invention to provide a kind of using the lignocellulose biomass of cheap operability and scale application
Cold pretreatment and its method for preparing hydrogen；To solve pretreating effect, cost during existing Hydrogen Production in Straw Fermentation, can grasp
The property made, versatility and scale application aspect are preferable not to the utmost, especially the application problem in cold district winter.
In order to solve the above technical problems, a kind of Cold pretreatment method of lignocellulose biomass is to press in the present invention
State step progress：
Step a, crushed after lignocellulose biomass is dried；
Step b, hydroxide/urea (Urea) aqueous solution of alkali metal is cooled to -8 DEG C~-20 DEG C in advance；Then warp is added
The lignocellulose biomass of step a processing, quick stir process 3min at ambient temperature, after suction filtration washing dried to neutrality
It is dry.
Further limit, lignocellulose biomass described in step a for rice straw, maize straw, wheat stalk and
One kind in broomcorn straw or wherein several mixtures by any mass ratio.
Further limit, 35~60 mesh sieves are crossed after being crushed in step a.
Further limit, by hydroxide/aqueous solution of urea of lignocellulose biomass and alkali metal in step b
Solid-to-liquid ratio is (3~40):100 proportionings add the lignocellulose biomass handled through step a.
Further limit, the hydroxide of alkali metal is lithium hydroxide, sodium hydroxide or potassium hydroxide in step b.
Further limit, in step b in hydroxide/aqueous solution of urea of alkali metal, the hydroxide of alkali metal
Mass percent concentration is 1%~7%, and the mass percent concentration of urea is 2%~12%.
Further limit, suction filtration processing is carried out using distilled water Vacuum filtration device in step b.
Further limit, mixing speed 300r/min~800r/min in step b.
A kind of lignocellulose biomass prepares the method for hydrogen and carries out in the steps below in the present invention：
The lignocellulose biomass handled in above-mentioned Cold pretreatment method adds fluid nutrient medium, so as substrate
Inoculation production hydrogen microorganism, anaerobic fermentation react afterwards, collect the gas of output.
Further limit, the seed liquor of production hydrogen microorganism is the liquid for growing to logarithmic phase that inoculum concentration is 5%~10%
Body suspension
Beneficial effects of the present invention：
Method using the present invention, increases hydrolysis efficiency.
The method of the present invention is simple, easy to operate.
The method of the present invention is especially suitable for very cold regional winter to agricultural crop straw progress recycling treatment.
Using the method for the present invention Cold pretreatment lignocellulose biomass (stalk etc.), lignocellulose biomass is improved
The enrichment of cellulose, recycles its conversion of biomass energy fermentation and hydrogen production, and technology reason is provided for efficiently fermented cellulosic aerogenesis
By foundation, the pretreatment for very cold area agricultural crop straw energy conversion provides new approaches.
Embodiment
Embodiment one：A kind of Cold pretreatment method of lignocellulose biomass is to press in present embodiment
State step progress：
Step a, crushed after rice straw is dried under the conditions of 60 DEG C, cross 40 mesh sieves；
Step b, by the precooling of 7%NaOH-12%Urea, 7%LiOH-12%Urea or 7%KOH-12%Urea aqueous solution-
8 DEG C, -10 DEG C, -12 DEG C, -15 DEG C, -18 DEG C and -20 DEG C；Then solid-to-liquid ratio 3 is pressed:100 ratio adds the wood handled through step a
Matter cellulose biomass, carries out quick stir process 3min with the speed of 300r/min at ambient temperature, true using distilled water
Empty Suction filtration device carries out suction filtration processing, is washed with water to neutrality, is dried under the conditions of 105 DEG C.
Lignocellulose biomass prepares the method for hydrogen and carries out in the steps below in present embodiment：
The lignocellulose biomass handled in above-mentioned Cold pretreatment method is substrate, amount of substrate 5g/L,
PH7.0, adds fluid nutrient medium, and then inoculation production hydrogen microorganism T.thermosaccharolyticum M18 bacterial strains, production hydrogen are micro-
The seed liquor of biology is the liquid suspension for growing to logarithmic phase that inoculum concentration is 10%, and anaerobic fermentation reacts under the conditions of 60 DEG C
120h, collects the gas of output.
The fluid nutrient medium is per L by the ammonium chloride of 1.0g, the sodium chloride of 1.0g, the dipotassium hydrogen phosphate of 1.0g, 1.0g
Potassium dihydrogen phosphate, the cysteine of 0.5g, the MgCl of 0.5g2·6H2O, the potassium chloride of 0.2g, the dusty yeast of 2g, the albumen of 2g
Peptone, the minor metallic element reservoir of 1ml, 0.1 ‰ (w/v) resazurins composition of the vitamin reservoir of 1ml and 1ml；
The minor metallic element reservoir is per L by the frerrous chloride of 1.5g, the zinc chloride of 70mg, the boric acid of 6mg, 0.1g
MnCl2·4H2O, the CuCl of 2mg2·2H2O, the CoCl of 0.19g2·6H2O, the NiCl of 24mg2·6H2O, the Na of 36mg2MO4·
H2O, the Na of the sodium tungstate of 15mg and 15mg2SeO4·5H2O is formed；
The vitamin reservoir is per L by the lipoic acid of 50.0mg, the biotin of 20.0mg, the nicotinic acid of 0.35g, 5.0mg
Thiamine hydrochloride, the p-aminobenzoic acid of 50.0mg, the folic acid of 20.0mg, the calcium pantothenate of 50.0mg, the vitamin B12 of 1.0mg
Formed with the puridoxine hydrochloride of 100.0mg.
As a result
The temperature of pretreatment is to utilize 7%NaOH-12%Urea, and 7%LiOH-12%Urea, 7%KOH-12%Urea are molten
For liquid from -8 DEG C to -20 DEG C, pretreated sample carries out the fermentation of production hydrogen in fact using T.thermosaccharolyticum M18
Test.As a result draw, it is 30% or so to go solid rate by the pretreatment sample under low temperature, while can effectively remove lignin,
Retain cellulose and hemicellulose, lignin removing rate is 60.98%~79.00%.LiOH/Urea and NaOH/Urea systems
Removal to lignin is higher than KOH/Urea systems, when the precooling temperature of alkalinuria system is -15 DEG C, the wood of three kinds of alkalinuria systems
Quality removal rate and cellulose accumulation rate are best, are respectively NaOH/Urea systems, and cellulose is 48.98 ± 2.56, hemicellulose
32.66 ± 0.67, lignin is 4.08 ± 0.08, LiOH/Urea systems, and cellulose is 48.00 ± 2.90, hemicellulose
30.39 ± 0.98, lignin is 5.22 ± 0.68, KOH/Urea systems, and cellulose is 47.00 ± 2.55, hemicellulose 32.35
± 0.98, lignin is 5.91 ± 1.92.
Sample biological hydrogen production after alkalinuria system Cold pretreatment, gas production is all apparently higher than undressed sample
Product, gas production 53.9-77.66, reaches particularly through sample gas production of the NaOH/urea solution after -15 DEG C of processing
77.66ml/g substrates, 54.7% is higher by compared to the sample gas production 50.2ml/gs substrates not gone out.
For NaOH/Urea alkalinuria systems, the sample of the pretreatment at -15 DEG C, carries out turning for further biological hydrogen production process
Neutralizing analysis, it turns out that react very slow within when 14 is small, next into the quick stage of reaction, stalk when 120h
Conversion ratio is 54%, and reaction mainly carries out in 20-60h, the more undressed stalk of conversion ratio of the stalk by pretreatment
High conversion rate 14%.Reaction obtains cumulative gas in 120h, by the pretreated stalks of NaOH/Urea
209.68ml/L, substrate factor of created gase are 9.35mmol/g substrates.Undressed stalk is then cumulative gas 100.2ml/L,
Substrate factor of created gase is 4.47mmol/g substrates.
Treated and untreated sample is in 4000-400cm-1Wave number section carries out FTIR infrared scans, finds
The lignocellulose biomass after alkalinuria system pre-processes at low temperature, effectively destroys lignin structure, reduces wood
The stubbornly resisting property of matter cellulose, in 1735cm-1C=O stretching vibrations in hemicellulose, equivalent to the acetyl group and sugar in hemicellulose
Forulic acid in aldehydic acid ester group either lignin connects the ester bond vibrations of carboxyl with p- coumaric acids.Equally in wave number 1647,
1514and 1425cm-1The stretching vibration of phenyl ring skeleton and C=C in lignin.These results chemically analyze by structural point,
By effectively destroying the structure of lignocellulosic under alkalinuria system Cold pretreatment, its stubbornly resisting property is reduced, increases it and compares table
Area, is allowed to easily utilize.
Claims (10)
1. a kind of Cold pretreatment method of lignocellulose biomass, it is characterised in that straw low temperature preprocess method is to press
State step progress：
Step a, crushed after lignocellulose biomass is dried；
Step b, hydroxide/aqueous solution of urea of alkali metal is cooled to -8 DEG C~-20 DEG C in advance；Then add through step a processing
Lignocellulose biomass, quick stir process 3min at ambient temperature, after suction filtration washing be dried for standby to neutrality.
A kind of 2. Cold pretreatment method of lignocellulose biomass according to claim 1, it is characterised in that step a
The lignocellulose biomass is one kind or wherein several in rice straw, maize straw, wheat stalk and broomcorn straw
By the mixture of any mass ratio.
A kind of 3. Cold pretreatment method of lignocellulose biomass according to claim 1, it is characterised in that step a
35~60 mesh sieves are crossed after middle crushing.
A kind of 4. Cold pretreatment method of lignocellulose biomass according to claim 1, it is characterised in that step b
Described in the hydroxide of alkali metal be lithium hydroxide, sodium hydroxide or potassium hydroxide；Hydroxide/urea of the alkali metal
In aqueous solution, the mass percent concentration of the hydroxide of alkali metal is 1%~7%, and the mass percent concentration of urea is 2%
~12%.
A kind of 5. Cold pretreatment method of lignocellulose biomass according to claim 1, it is characterised in that step b
It is middle to carry out suction filtration processing using distilled water Vacuum filtration device.
A kind of 6. Cold pretreatment method of lignocellulose biomass according to claim 1, it is characterised in that step b
In mixing speed 300r/min~800r/min.
A kind of 7. Cold pretreatment method of lignocellulose biomass according to claim 1, it is characterised in that step b
In by the solid-to-liquid ratio of hydroxide/aqueous solution of urea of lignocellulose biomass and alkali metal be (3~40):100 proportionings add
Enter the lignocellulose biomass handled through step a.
8. a kind of method that lignocellulose biomass prepares hydrogen, it is characterised in that the method for the hydrogen manufacturing is in the steps below
Carry out：The lignocellulosic handled in the Cold pretreatment method described in any one claim in claim 1-7 is given birth to
Material is substrate, adds fluid nutrient medium, then inoculation production hydrogen microorganism, anaerobic fermentation reaction, collects the gas of output.
9. the method that a kind of lignocellulose biomass according to claim 8 prepares hydrogen, it is characterised in that
The fluid nutrient medium per L by the ammonium chloride of 1.0g, the sodium chloride of 1.0g, the dipotassium hydrogen phosphate of 1.0g, 1.0g phosphoric acid
Potassium dihydrogen, the cysteine of 0.5g, the MgCl of 0.5g2·6H2O, the potassium chloride of 0.2g, the dusty yeast of 2g, the peptone of 2g, 1ml
Minor metallic element reservoir, 0.1 ‰ (w/v) resazurins composition of the vitamin reservoir of 1ml and 1ml；
The minor metallic element reservoir is per L by the frerrous chloride of 1.5g, the zinc chloride of 70mg, the boric acid of 6mg, 0.1g
MnCl2·4H2O, the CuCl of 2mg2·2H2O, the CoCl of 0.19g2·6H2O, the NiCl of 24mg2·6H2O, the Na of 36mg2MO4·
H2O, the Na of the sodium tungstate of 15mg and 15mg2SeO4·5H2O is formed；
The vitamin reservoir per L by the lipoic acid of 50.0mg, the biotin of 20.0mg, the nicotinic acid of 0.35g, 5.0mg hydrochloric acid
Thiamine, the p-aminobenzoic acid of 50.0mg, the folic acid of 20.0mg, the calcium pantothenate of 50.0mg, 1.0mg vitamin B12 and
100.0mg puridoxine hydrochloride composition.
10. the method that a kind of lignocellulose biomass according to claim 8 prepares hydrogen, it is characterised in that the production
Hydrogen microorganism is T.thermosaccharolyticum M18 bacterial strains, the seed liquor of production hydrogen microorganism for inoculum concentration be 5%~
10% liquid suspension for growing to logarithmic phase；Amount of substrate is 5g/L, pH value 7.0.
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Cited By (5)
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| CN109486864A (en) * | 2018-11-14 | 2019-03-19 | 江南大学 | A kind of solid-state alkali treatment method improving organic waste anaerobic fermentation efficiency |
| CN109988797A (en) * | 2019-04-19 | 2019-07-09 | 哈尔滨工业大学 | A kind of method of the pretreatment of low temperature high solid-liquid ratio alkalinuria solution and its enzymatic hydrolysis conversion of agricultural crop straw |
| CN110079570A (en) * | 2019-05-17 | 2019-08-02 | 哈尔滨工业大学 | A kind of method of the pretreatment of alkalinuria solution and its enzymatic hydrolysis conversion outside the cold district winter room of lignocellulose biomass |
| CN112626903A (en) * | 2020-12-18 | 2021-04-09 | 安徽工业大学 | Method for extracting lignin from urea-assisted low-temperature alkali liquor |
| CN112852683A (en) * | 2021-03-24 | 2021-05-28 | 华南理工大学 | Thermosaccharophilus anaerobacter and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112626903A (en) * | 2020-12-18 | 2021-04-09 | 安徽工业大学 | Method for extracting lignin from urea-assisted low-temperature alkali liquor |
| CN112852683A (en) * | 2021-03-24 | 2021-05-28 | 华南理工大学 | Thermosaccharophilus anaerobacter and application thereof |
| CN112852683B (en) * | 2021-03-24 | 2022-10-25 | 华南理工大学 | Thermosaccharophilus anaerobacter and application thereof |
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