CN107937446A - A kind of technique using maize straw as waste ethanol - Google Patents
A kind of technique using maize straw as waste ethanol Download PDFInfo
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- CN107937446A CN107937446A CN201711404719.1A CN201711404719A CN107937446A CN 107937446 A CN107937446 A CN 107937446A CN 201711404719 A CN201711404719 A CN 201711404719A CN 107937446 A CN107937446 A CN 107937446A
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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
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Abstract
The invention discloses a kind of technique using maize straw as waste ethanol, comprise the following steps：By corn straw smashing, raw material is pre-processed using formic acid hydrochloric acid mixed acid；Pretreated maize straw residue is through two step sulfuric acid process hydrolysis and saccharifications；Gained sulphuric acid hydrolysis liquid realizes saccharic acid separation and the detoxification of saccharified liquid using sour retardance process；Sugared concentration needed for fermentation is concentrated into using efficient concentration device through saccharic acid separating obtained sugared eluent；To concentrate liquid glucose as carbon source, yeast progress alcohol prepared by fermenting is put into fermentation tank.The technique can efficiently utilize maize straw, separated as coupling acid retardance with efficient concentration device process, purify and concentration stalk acid hydrolysis liquid after obtained by liquid glucose, sugared concentration is high, separated in synchronization fermentation inhibitor, fermentability is good, substantially increase alcohol yied, and solvent recovery, non-secondary pollution can be completed.
Description
Technical field
The present invention relates to renewable new energy source technical field, more particularly to a kind of work using stalk as waste ethanol
Skill.
Background technology
With the development of world economy and the growth of population, grain, energy and environment are the masters that mankind's persistent existence faces
Challenge.Extensive concern is increasingly subject to lignocellulosic material production renewable and clean energy resource, and using maize straw as raw material
It is particularly noticeable to produce bio-ethanol.China is large agricultural country, and maize straw gross annual output amount reaches several hundred million tons, studies maize straw
Bio-ethanol is prepared to have a extensive future.The basic process that maize straw prepares ethanol is by the cellulose in raw material and hemicellulose water
Solve as monose, monose fermentation is then become into alcohol fuel again.Patent No. 200610114240.X's《Maize straw produces wine
Smart technology》Disclose a kind of side for producing primary ethanol through crushing, material all in one piece plus yeast, pit entry fermentation, distillation by maize straw
Method, this method technique is simple, operation is easy, but ethanol output capacity is low, discarded object is more, has secondary pollution.
Maize straw is mainly coupled by cellulose, hemicellulose and lignin three parts to be formed, it is necessary to uses effective hand
Duan Jinhang pretreatments could produce ethanol or other high valuable chemicals by polysaccharide conversion therein is monose.Enzyme hydrolysis and
Sour water solution is usually the method for industrial more common two kinds of maize straw hydrolysis and saccharifications.In recent decades to enzyme law catalysis wood
Although the research of matter saccharification of cellulose also has made great progress, the efficiency and cost problem of enzyme are still to limit its industrialization
Where the bottleneck of application.Acid hydrolysis cellulose ethanol is similarly faced with lot of challenges, requirement height such as corrosion-resistant to equipment,
The accessory substance produced in acid recovery difficulty and hydrolytic process acts on follow-up fermentation inhibitory obvious etc..
The main bugbear of the alcohol fuel of maize straw production at present is that can not realize cellulose, hemicellulose and lignin three
The comprehensive utilization of big component, and the high efficiente callback of acidification hydrolization rear catalyst and effective removing of mortifier are, it is necessary to which one is real
The high production technology of green, ethanol output capacity.
The content of the invention
The purpose of the present invention, is to overcome the shortcomings of the prior art and method, there is provided a kind of energy-efficient, green corn
The technique of stalk ethanol production.
To achieve these goals, the technical solution adopted in the present invention, includes the following steps：
1) pretreatment of raw material：After corn straw smashing, it is pre-processed using the mixed acid of formic acid and concentrated hydrochloric acid
With the most hemicelluloses of removing and most of lignin；
2) hydrolysis and saccharification：Maize straw residue after pretreatment (overwhelming majority composition is cellulose) is put into saccharification
In container, it is hydrolyzed using sulphuric acid hydrolysis, the hydrolyzate containing sugar and acid is obtained after the separation of solid and liquid that is saccharified；
3) hydrolyzate saccharic acid separates：Saccharic acid separation is carried out to hydrolyzate using sour retardance process, de- tree is washed with deionized water
Fat, obtains by appropriate diluted sugared eluent and sour eluent；
4) catalyst sulfuric acid recycles：Catalyst sulfuric acid is realized through the concentrated device concentration of the separating obtained sour eluent of saccharic acid
Recycling.
5) sugared eluent concentration：Sugared eluent is concentrated into by sugared concentration needed for fermentation using inspissator, while realizes that sugar is molten
The detoxification of liquid；
6) ferment：Using detoxification, concentration after stalk acid hydrolysis liquid for the culture medium that carbon source is prepared it is sterilized after, put into necessarily
The yeast of amount carries out alcohol prepared by fermenting in fermentation tank.
Further, in step 1) gained formic acid hydrolysis liquid, formic acid can be recycled through vacuum distillation or the methods of UF membrane,
Surplus material after formic acid recycling can add water to obtain hemicellulose hydrolysate, which can be used for preparing furfural or other height are attached
Value added compound, the lignin residue for filtering gained can be used for preparing aldehydes matter or being used for subsequent technique mistake directly as fuel
The energy supply of journey.
Further, the sulphuric acid hydrolysis in step 2), be first use higher concentration sulfuric acid, add water be diluted to it is relatively low dense
Spend sulfuric acid and the bistep hydrolysis to heat up；High-concentration sulfuric acid hydrolysising condition is preferably：70-75% sulfuric acid, liquid-solid ratio 3.5:1-
4.5:1 (mL/g), 20-30 DEG C of temperature, when reaction time 1.5-2.5 is small；Low-concentration sulfuric acid hydrolysising condition is preferably：15-25%
Sulfuric acid, 100-105 DEG C of temperature, when reaction time 1-1.5 is small.
Further, the separation of solid and liquid obtained solid in step 2) is lignin residue, can be used for follow-up work as fuel
The energy supply of skill process, it can also be used to the synthesis conversion of aldehydes matter.
Further, the sour Retarding resin described in step 3) is strongly basic anionic resin, affinity interaction/suction to acid
Attached effect is significantly stronger than affinity interaction/suction-operated to sugar.Meanwhile it can effectively remove the toxicant in hydrolyzate.
Further, in the acid retardance eluent removal process described in step 3), sugared eluent stops collecting preferred
Condition is pH<2.3, the optimum condition that sour eluent stops collecting is pH<2.5-3.5.
Further, step 4) and 5) described in inspissator include but not limited to multiple-effect membrane distillation, pressure steam distillation, multiple-effect steam
One or more processing units in hair, nanofiltration.
Wherein multiple-effect membrane distillation equipment (referenced patent：ZL201010570625.3 and ZL201010570653.5), it is one
Kind is with the internal gap field orientation equipment from heat exchange function, and energy-efficient, heat utilization efficiency is high, and multiple-effect membrane distillation process is made
Water ratio is up to 6-15, and modularized equipment, equipment volume is small, and scale is changeable.Multiple-effect membrane distillation is to acids, phenols, furans
The removal efficiency of material is different, the effect with removing volatility mortifier while liquid glucose is concentrated.
Compared with prior art, the beneficial effects of the invention are as follows：
1st, cellulose, hemicellulose, lignin in maize straw can be achieved to make full use of, obtain ethanol, furfural and its
His high valuable chemicals.
2nd, sour retardance process realizes saccharic acid separation and hydrolyzate detoxification efficiency at the same time, simplifies technological process, improves sugar
The separated economy of acid and the feature of environmental protection.
3rd, using multiple-effect membrane distillation etc. is energy saving, efficient concentration device (or several inspissators combine) takes off sugared eluent and pickling
Liquid concentrates respectively, obtains higher concentration, sugared concentrate beneficial to later stage fermentation, concentration process is at the same time to poisonous in sugar juice
Material is removed；The acid solution of higher concentration, is back to use hydrolyzing process, and realization recycles.
4th, lignin residue obtained by maize straw preprocessing process can be directly used for burning and provide energy for later processing operation
Amount, it can also be used to the synthesis conversion of aldehydes matter.
Brief description of the drawings
Fig. 1 is the process flow chart of maize straw of the present invention hydrolysis production ethanol.
Embodiment
Below in conjunction with the accompanying drawings and specific implementation case is described further the present invention.In the attached drawing or one of the present invention
Elements and features described in kind of embodiment can be with the element that is shown in one or more other drawings or embodiments
It is combined with feature.It should be noted that for purposes of clarity, unrelated to the invention, this area is eliminated in attached drawing and explanation
Component known to those of ordinary skill or the expression and description of processing.
Example 1
Maize straw is crushed, wherein particle diameter is that the stalk material composition of 20-40 mesh is：Cellulose 45.03%, half
Cellulose 30.97%, lignin 17.00%, weighs the stalk 1000g of 20-40 mesh, adds 10L formic acid (88%) and 100mL is dense
Hydrochloric acid (37%), when processing 3 is small under being 150rpm in 60 DEG C, hunting speed, filtrate is recycled through vacuum distillation obtained by separation of solid and liquid
Formic acid and hydrochloric acid, the hemicellulose hydrolysate that main component is xylose can be obtained by, which being dissolved in water, can be used for the preparation of furfural, and recycle
Water-insoluble lignin residue；Weigh the dry maize straw residual solid of 500g pretreatment gained to be put into saccharification vessel, add
When 2L sulfuric acid (72%) is so that fully infiltration 2 is small at 25 DEG C, then add 7.983L water that sulfuric acid is diluted to 20wt%, be warming up to 100
When DEG C reaction 1 is small, the hydrolyzate of the 38.5g/L containing glucose of 10L or so is can obtain after separation of solid and liquid, and recycle insoluble wooden
Plain solid；1L hydrolyzates are taken with 1.0h-1Air speed enter the splitter equipped with sour Retarding resin, operation temperature is 50 DEG C, sample introduction
After the completion of with identical flow velocity add deionized water eluted, can finally obtain the sugared eluent of the 21.0g/L containing glucose and contain
The sour eluent of sulfuric acid 5.0%, wherein the glucose rate of recovery are up to 99.1%, and sulfuric acid can be substantially essentially completely recovered or profit
The fermentation inhibitor in hydrolyzate can also be effectively removed with, the process, and hydrolyzate mainly forms contrast and is shown in Table 1 before and after process；
Sour eluent is first concentrated into 43% or so through multiple-effect membrane distillation process, during maximum water generation ratio up to 14.51, the water generation ratio
It is worth the thermal efficiency that evaporator is imitated equivalent to tradition 18, is then evaporated through the effect of high temperature one by sulphuric acid concentration to 72%, realize catalysis
The Recycling of agent sulfuric acid；Sugared eluent is concentrated into 100g/L or so through multiple-effect membrane distillation process, the glucose in whole process
Rejection up to 100%, during maximum flux and water generation ratio can reach 4.84L/ (m respectively2H) and 15.27, the water generation ratio value
Equivalent to the thermal efficiency that tradition 19 imitates evaporator；Liquid glucose is concentrated as carbon source using gained, since the concentrate contains very small amount sulphur
Acid, can achieve the purpose that required nutritive salt, with saccharomyces cerevisiae after sterilizing by adding magnesium hydroxide and dipotassium hydrogen phosphate
CICC1308 is fermenting microbe, fermentation temperature be 30 DEG C, speed of agitator 175rpm, inoculum concentration 10%, initial pH be 5.0
Under conditions of fermentation can obtain the ethanol of 43.06g/L.
Example 2
Pretreatment, hydrolysis and saccharification, saccharic acid separation and acid catalyst recycling method and example 1 are basically identical, are hindered through acid
Sugared eluent obtained by stagnant resin treatment is 30 DEG C in feed temperature, under conditions of pressure is 1.0MPa, is handled through nanofiltration operation
Sugared eluent is concentrated into glucose content up to 100g/L or so, whole process carries out under Room-temperature low-pressure, and the sugared rate of recovery is reachable
92.3%；Then using the concentration liquid glucose as carbon source, saccharomyces cerevisiae CICC1308 is fermenting microbe, is 30 DEG C, stirs in fermentation temperature
Mix rotating speed is 175rpm, inoculum concentration 10%, initial pH carry out alcohol fermentation under conditions of being 5.0, can obtain 42.32g/L second
Alcohol.
The acid of table 1 retardance hydrolyzate composition change before and after the processing
Although the present invention and its advantage is described in detail it should be appreciated that without departing from by appended claim
Various changes, replacement and conversion can be carried out in the case of the spirit and scope of the present invention limited.Moreover, the model of the application
Enclose and be not limited only to the described process of specification, equipment, means, the specific embodiment of method and steps.In the art is common
Technical staff will readily appreciate that from the disclosure, can use perform and corresponding reality described herein according to the present invention
Apply the essentially identical function of example or obtain process essentially identical with it result, existing and that future is to be developed, equipment,
Means, method or step.Therefore, appended claim includes such process, equipment, hand in the range of being directed at them
Section, method or step.
Claims (8)
- A kind of 1. technique using maize straw as waste ethanol, it is characterised in that：Comprise the following steps：1) stalk pretreatment：Maize straw is pre-processed using formic acid and a small amount of concentrated hydrochloric acid, removes most hemicelluloses Element and most of lignin, obtain the maize straw residue that most compositions are celluloses, realize cellulose, hemicellulose With efficiently separating for lignin；2) hydrolysis and saccharification：Maize straw residue after pretreatment is hydrolyzed using sulfuric acid catalysis, is contained after separation of solid and liquid The hydrolyzate of sugar and acid；3) hydrolyzate saccharic acid separates：Saccharic acid separation is carried out to hydrolyzate using sour Retarding resin, deresination is washed with deionized water, obtains To by appropriate diluted sugared eluent and acid solution；4) acid catalyst recycles：Hydrolytic process is back to use after being concentrated using inspissator to low concentration acid solution, realizes catalyst sulphur The Recycling of acid；5) sugared eluent concentration：Sugared eluent is concentrated into by sugared concentration needed for fermentation using inspissator；6) ferment：Using detoxification, concentration after stalk acid hydrolysis liquid for the culture medium that carbon source is prepared it is sterilized after, put into it is a certain amount of Yeast carries out alcohol prepared by fermenting in fermentation tank.
- 2. technique according to claim 1, it is characterised in that：The formic acid hydrolysis liquid of gained in step 1), through vacuum distillation Or membrane separating method recycling formic acid, the surplus material after formic acid recycling add water to obtain hemicellulose hydrolysate, which is used for Furfural or other high added value compounds are prepared, the lignin residue for filtering gained is used to prepare aldehydes matter or directly as combustion Energy supply of the material for subsequent technique process.
- 3. technique according to claim 1, it is characterised in that：Sulphuric acid hydrolysis in step 2), is first to use high concentration Sulfuric acid, adds water the bistep hydrolysis for being diluted to low-concentration sulfuric acid and heating up.
- 4. technique according to claim 3, it is characterised in that：High-concentration sulfuric acid hydrolysising condition is：70-75% sulfuric acid, liquid Gu than being 3.5:1-4.5:1 (mL/g), 20-30 DEG C of temperature, when reaction time 1.5-2.5 is small；Low-concentration sulfuric acid hydrolysising condition is excellent Elect as：15-25% sulfuric acid, 100-105 DEG C of temperature, when reaction time 1-1.5 is small.
- 5. technique according to claim 1, it is characterised in that：Stalk acid hydrolysis liquid in step 2) is through obtained by separation of solid and liquid Solid is lignin residue, and the energy supply of subsequent technique process or the synthesis conversion of aldehydes matter are used for as fuel.
- 6. technique according to claim 1, it is characterised in that：Sour Retarding resin described in step 3) for strong basicity the moon from Subtree fat, affinity interaction/suction-operated to acid are significantly stronger than affinity interaction/suction-operated to sugar.
- 7. technique according to claim 1, it is characterised in that：Acid retardance eluent removal process described in step 3) In, the condition that sugared eluent stops collecting is pH<2.3, the optimum condition that sour eluent stops collecting is pH<2.5-3.5.
- 8. technique according to claim 1, it is characterised in that：Inspissator described in step 4) or step 5) steams for multiple-effect film Evaporate, press one or more processing units in steam distillation, multiple-effect evaporation, nanofiltration.
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Cited By (4)
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| CN108823071A (en) * | 2018-09-10 | 2018-11-16 | 北京鑫泽清源植物秸秆技术有限公司 | The dynamic hydrolysis monosaccharide of straw industrialization heat and alcohol ester process system |
| CN110452933A (en) * | 2018-05-08 | 2019-11-15 | 中国石油天然气股份有限公司 | Method for producing ethanol |
| CN114276885A (en) * | 2022-01-05 | 2022-04-05 | 湖南华诚生物资源股份有限公司 | Method for preparing ethanol from fresh momordica grosvenori |
| CN115820943A (en) * | 2022-12-05 | 2023-03-21 | 华南农业大学 | Method for preparing glucose by converting corn straws in molten salt hydrate acid system |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110452933A (en) * | 2018-05-08 | 2019-11-15 | 中国石油天然气股份有限公司 | Method for producing ethanol |
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| CN114276885A (en) * | 2022-01-05 | 2022-04-05 | 湖南华诚生物资源股份有限公司 | Method for preparing ethanol from fresh momordica grosvenori |
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| CN115820943A (en) * | 2022-12-05 | 2023-03-21 | 华南农业大学 | Method for preparing glucose by converting corn straws in molten salt hydrate acid system |
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