CN106362707B - A method of lignin is improved to butanol, acetone, Ethanol Adsorption performance in ABE fermentation liquid - Google Patents
A method of lignin is improved to butanol, acetone, Ethanol Adsorption performance in ABE fermentation liquid Download PDFInfo
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Abstract
The present invention be a kind of raising lignin to butanol in ABE fermentation liquid, acetone, Ethanol Adsorption performance method.Lignin is classified as water-soluble fraction and the insoluble fraction of water first with water by the invention, then recycle ketones solvent that the insoluble lignin fraction of water is classified as the molten fraction of ketone and the insoluble fraction of ketone again, it is finally obtained water is insoluble and the insoluble fraction of ketone is used for butanol, acetone, ethyl alcohol in adsorbing separation fermentation liquid.The dissolution stage division relates only to the dissolution classification of lignin, is not related to chemical modification, therefore have the advantages such as simple process and low cost.
Description
Technical field
The present invention relates to low-concentration organic adsorption technology fields, in particular to a kind of be classified by solvent to improve lignin
To butanol in ABE fermentation liquid, acetone, Ethanol Adsorption performance method.
Background technique
Biological butanol is a kind of new bio liquid fuel with high-energy density and high gasoline degree of mixing, because it can make
Good organic solvent and fuel performance is excellent, biofermentation production are highly valued.Pass through traditional acetone
(Acetone)-butanol (Butanol)-ethyl alcohol (Ethanol) i.e. ABE fermentation method produces biological butanol, and product deposits fermenting microbe
In toxicity inhibition, leads to problems such as final product concentrations low and later separation energy consumption is high.(biological fermentation process prepares the product of butanol
In be also also known as ABE solvent comprising a large amount of acetone and a small amount of ethyl alcohol equal solvent, product.) it therefore must use effective method
Product butanol, acetone and ethyl alcohol are removed in time from fermentation liquid, reduce Product inhibiton, so that improving fermentation production rate reduces production
Cost.It is a kind of main isolation technics using absorption method separation and fermentation product, which utilizes adsorbent selective absorption fourth
Alcohol, acetone and ethyl alcohol eliminate the purpose of Product inhibiton to realize, by suction-operated, effectively improve butanol, third after fermentation
The concentration of ketone and ethyl alcohol reduces energy consumption.Currently, both at home and abroad to the report of butanol adsorbent mainly include active carbon, molecular sieve,
Polyvinylpyrrolidone (PVP), diatomite, resin and bamboo charcoal etc..Wherein, the adsorption capacity with higher such as active carbon, bamboo charcoal,
But adsorptive selectivity is poor, especially has higher adsorption capacity to the glucose in fermentation liquid, will lead to the loss of fermentation liquid.
Because having ion exchangeable, tradable ion can exchange with certain ions in fermentation liquid, cause rear molecular sieve
There is biological inconsistent problem during supervention ferment.PVP and resin have the effect of preferably adsorbing, but higher cost, prepare
Journey is unfavorable for sustainable development using petrochemical industry synthetic route.It develops and has both high-adsorption-capacity, highly selective, at low cost
The adsorbent of the features such as honest and clean, environmental-friendly has important practical significance for the sustainable development of biological butanol industry.
Lignin is the natural biomass macromolecule that reserves are only second to cellulose.Ladisch discovery lignin can adsorb
Butanol, acetone and ethyl alcohol in solution, Griffith has reaffirmed that lignin has butanol by tracer method later
There is certain adsorption capacity, and points out that lignin is expected the adsorbing separation for biological alcohol fuel.Although lignin is for giving birth to
It is shown good application prospect when the adsorbing separation of object alcohol and potentiality, but its complicated structure and polydispersity lead to lignin
Performance is inhomogenous, especially non-modified lignin, and application performance is unsatisfactory, limits answering for it to a certain extent
With.Currently, mostly using chemical method, but chemical method high production cost greatly to the modification of lignin, process is relative complex, and may produce
Raw secondary pollution.
Summary of the invention
It is an object of the present invention to be directed in the adsorption separation technology of current biological butanol fermentation product existing for adsorbent not
Foot, provide a kind of raising lignin to butanol in ABE fermentation liquid, acetone, Ethanol Adsorption performance method.The invention first with
Lignin is classified as water-soluble fraction and the insoluble fraction of water by water, then recycle ketones solvent by the insoluble lignin fraction of water again
It is classified as the molten fraction of ketone and the insoluble fraction of ketone, it is finally obtained water is insoluble and the insoluble fraction of ketone is used in adsorbing separation fermentation liquid
Butanol, acetone, ethyl alcohol.The dissolution stage division relates only to the dissolution classification of lignin, is not related to chemical modification, therefore have
There are the advantages such as simple process and low cost.Water and ketones solvent for dissolving classification can be recycled by recycling,
Any consumption and loss are not generated, therefore have many advantages, such as green, environmental protection.
A method of improving lignin to butanol, acetone, Ethanol Adsorption performance in ABE fermentation liquid, the method includes
Following steps:
(1) water-soluble lignin lignin classification insoluble with water: lignin is mixed with distilled water, Sonication assisted treatment 2-
Lower layer's solid after sedimentation and filtering is collected in 5min, sedimentation separation after stirring, filtering, and vacuum drying obtains the insoluble lignin of water；Its
In, every 0.1-2L distilled water adds lignin 10-50g；
(2) the molten lignin of ketone lignin classification insoluble with ketone: the insoluble lignin of water that upper step obtains is filled with ketones solvent
Dividing mixing, Sonication assisted treatment 2-5min is sufficiently stirred, sedimentation separation, filters, lower layer's solid after collecting sedimentation and filtering,
Obtain the insoluble lignin of the insoluble ketone of water；Wherein every 0.1-2L ketone reagent adds the insoluble lignin 30-60g of water；
(3) the insoluble lignin of the insoluble ketone of the water obtained upper step is dried in vacuo 12-48h at 20-60 DEG C, bottles, sealing
It saves.
The lignin raw material is corn alkali lignin, pine alkali lignin, Wheat Straw Lignin from Alkali Pulping, poplar alkali lignin
Or bamboo pulp black liquor alkali lignin.
Ketone reagent is butanone, pentanone, acetone, cyclohexanone or hexanone in the step (2).
Lignin and distilled water incorporation time are 2-28h in the step (1).
The insoluble lignin of water and ketone reagent incorporation time are 2-24h in the step (2).
The sedimentation separation is natural subsidence or is centrifuged at a high speed that filter method is suction filtration or micro-filtration.
Compared with prior art, beneficial effects of the present invention:
The present invention proposes to carry out selective dissolution to lignin using water and organic solvent to obtain high-performance lignin
Adsorbent can significantly improve lignin to the adsorption capacity of butanol, acetone, ethyl alcohol in fermentation liquid, help to solve biological fourth
The Product inhibiton problem of alcohol fermentation technology.This method is a kind of physical and chemical process, is not related to chemical modification, therefore have preparation
It is at low cost, easy to operate, the advantages that process is environmentally protective.Lignin can be improved to low concentration butanol, acetone, ethanol solution
Absorption property improves yield to solve the problems, such as the Product inhibiton of biofermentation production butanol, reduces energy consumption.It is embodied in:
(1) adsorption capacity with higher, to butanol, acetone, ethyl alcohol saturated adsorption capacity respectively up to 198mg/g,
151.3mg/g, 98.5mg/g, lignin improves 19.3%, 30.2%, 53.2% respectively before relatively handling.
(2) rate of adsorption is fast.
(3) adsorption process has no toxic side effect, environmentally friendly, prepares that raw material sources are convenient extensively, and preparation cost is cheap.
(4) preparation process is simple, not high to equipment requirement, it is easy to accomplish industrialized production is effectively increased to hair
Ferment method produces the adsorbance of the zymotic fluid product of butanol, reduces product inhibition.
Detailed description of the invention
Fig. 1 is the infared spectrum of the insoluble lignin adsorbent material of embodiment 1-3 Central Plains lignin ketone insoluble with water；
Fig. 2 is suction of the insoluble lignin adsorbent material of 4 Central Plains lignin of embodiment ketone insoluble with water to butanol in aqueous solution
Attached thermoisopleth；
Fig. 3 is suction of the insoluble lignin adsorbent material of 5 Central Plains lignin of embodiment ketone insoluble with water to acetone in aqueous solution
Attached thermoisopleth；
Fig. 4 is suction of the insoluble lignin adsorbent material of 6 Central Plains lignin of embodiment ketone insoluble with water to ethyl alcohol in aqueous solution
Attached thermoisopleth；
Fig. 5 is the insoluble lignin adsorbent material of 7 Central Plains lignin of embodiment ketone insoluble with water to butanol in ABE fermentation liquid
Adsorption isotherm；
Fig. 6 is the insoluble lignin adsorbent material of 8 Central Plains lignin of embodiment ketone insoluble with water to acetone in ABE fermentation liquid
Adsorption isotherm；
Fig. 7 is the insoluble lignin adsorbent material of 9 Central Plains lignin of embodiment ketone insoluble with water to ethyl alcohol in ABE fermentation liquid
Adsorption isotherm；
Fig. 8 is the insoluble lignin adsorbent material of the insoluble ketone of water in embodiment 10 to the absorption power of butanol, acetone and ethyl alcohol
Learn curve.
Specific embodiment
Below by way of specific embodiment, the present invention will be described in more detail.Embodiment is only to a kind of theory of the invention
It is bright, but not to limit the present invention.Embodiment is practical application example, and those skilled in the art are easy to
It grasps and verifies.If making certain change on the basis of the present invention, then its essence is without departing from the scope of the present invention.
Embodiment 1:
It the described method comprises the following steps:
(1) water-soluble lignin lignin classification insoluble with water: corn alkali lignin 30g and distilled water 500ml is sufficiently mixed
20h is closed, 40KHz Sonication assisted treatment 2min is sufficiently stirred, sedimentation separation, 0.45 μm of membrane filtration, collects sedimentation and filtering
Lower layer's solid afterwards, vacuum drying 20h obtain the insoluble lignin 17g of water.
(2) the molten lignin of ketone lignin classification insoluble with ketone: water insoluble lignin 17g and acetone solvent 500ml is abundant
18h is mixed, 40KHz Sonication assisted treatment 3min is sufficiently stirred, sedimentation separation, 0.45 μm of membrane filtration, collects sedimentation and mistake
Lv Hou lower layer solid obtains the insoluble lignin of the insoluble ketone of water.
(3) the insoluble lignin of the insoluble ketone of product water obtains 6 grams after being dried in vacuo 15h at 50 DEG C, and bottling is sealed.
Embodiment 2:
It the described method comprises the following steps:
(1) water-soluble lignin lignin classification insoluble with water: poplar lignin 50g and distilled water 500ml are sufficiently mixed
16h, Sonication assisted treatment 3min, is sufficiently stirred, sedimentation separation, 0.45 μm of membrane filtration, collects lower layer after sedimentation and filtering
Solid vacuum drying obtains the insoluble lignin 35g of water for 24 hours.
(2) the molten lignin of ketone lignin classification insoluble with ketone: water insoluble lignin 35g and butanone solvent 500ml is abundant
20h is mixed, Sonication assisted treatment 2min is sufficiently stirred, sedimentation separation, 0.45 μm of membrane filtration, after collecting sedimentation and filtering
Lower layer's solid obtains the insoluble lignin of the insoluble ketone of water.
(3) the insoluble lignin of the insoluble ketone of product water obtains 15g after being dried in vacuo 18h at 45 DEG C, and bottling is sealed.
Embodiment 3:
It the described method comprises the following steps:
(1) water-soluble lignin lignin classification insoluble with water: Wheat Straw Lignin from Alkali Pulping 30g and distilled water 1000ml is sufficiently mixed
18h is closed, Sonication assisted treatment 3min is sufficiently stirred, sedimentation separation, 0.45 μm of membrane filtration, under collecting after sedimentation and filtering
Layer solid vacuum drying 48h obtains the insoluble lignin 18g of water.
(2) the molten lignin of ketone lignin classification insoluble with ketone: water insoluble lignin 18g and ketones solvent 1000ml is abundant
15h is mixed, Sonication assisted treatment 3min is sufficiently stirred, sedimentation separation, 0.45 μm of membrane filtration, after collecting sedimentation and filtering
Lower layer's solid obtains the insoluble lignin of the insoluble ketone of water.
(3) the insoluble lignin of the insoluble ketone of product water obtains 7g after being dried in vacuo 20h at 40 DEG C, and bottling is sealed.
The Fourier transform infrared spectroscopy pair of the insoluble ketone of water obtained by embodiment 1-3 insoluble lignin and lignin raw material
According to figure as shown in Figure 1, having been carried out using Fourier Transform Infrared Spectrometer to log quality and the insoluble lignin of the insoluble ketone of water red
Outer characterization obtains infrared spectrogram and characteristic peak ownership.If Fig. 1 finds out, the insoluble lignin of the insoluble ketone of water exists in infrared spectrum
Hydroxyl at 3399cm-1, phenyl ring C=O, 1510cm-1,1426cm-1 at the CH of methylmethylene at 2936cm-1,1600cm-1
With nuclear skeleton fragrant at 1126cm-1, the C-H deformation vibration of methylmethylene at 1462cm-1, aromatic proton C-C at 1222cm-1
C-O is added to add C=O, the absorption of lignum-vitae phenolic aromatic proton is remarkably reinforced compared with log quality at 836cm-1, and at 2843cm-1
CH2 stretching vibration, the absorption of carboxyl weakens at 1700cm-1.Illustrate compared with lignin stock blend, the insoluble wood of the insoluble ketone of water
The hydrophobic grouping of quality increases, and hydrophobic performance is stronger, therefore has better absorption property to butanol, acetone, ethyl alcohol in fermentation liquid.
Embodiment 4:
The insoluble lignin of the insoluble ketone of water adsorbs the application of butanol as adsorbent in aqueous solution, and step is, by embodiment 1
The insoluble lignin of the insoluble ketone of the water of middle preparation is added separately in the butanol aqueous solution of 1-50g/L, adsorbent and solution quality ratio
It for 1:100, is mixed using concussion mode, temperature is 25 DEG C, and the time is 24 hours, after completing absorption, carries out separation of solid and liquid water outlet
The insoluble lignin adsorbent of insoluble ketone, butanol concentration of aqueous solution after measurement absorption.
The insoluble lignin of the insoluble ketone of water is with lignin raw material to comparison diagram such as Fig. 2 of the adsorption isotherm of butanol.To fourth
Alcohol adsorption capacity is obviously improved, and up to 198mg/g, improves 19.3% before being relatively classified.
Embodiment 5:
The insoluble lignin of the insoluble ketone of water adsorbs the application of acetone in aqueous solution, and step is the water that will be prepared in embodiment 1
The insoluble lignin of insoluble ketone is added separately in the aqueous acetone solution of 1-50g/L, and adsorbent and solution quality ratio are 1:100, is adopted
It is mixed with concussion mode, temperature is 25 DEG C, and the time is 24 hours, and after completing absorption, it is insoluble to carry out the insoluble ketone of separation of solid and liquid water outlet
Lignin adsorbent, aqueous acetone solution concentration after measurement absorption.
The insoluble lignin of the insoluble ketone of water is with lignin raw material to comparison diagram such as Fig. 3 of the adsorption isotherm of acetone.To third
Ketone adsorption capacity is obviously improved, and up to 151.3mg/g, improves 30.2% before being relatively classified.
Embodiment 6:
The insoluble lignin of the insoluble ketone of water adsorbs the application of ethyl alcohol in aqueous solution, and step is the water that will be prepared in embodiment 1
The insoluble lignin of insoluble ketone is added separately in the ethanol water of 1-50g/L, and adsorbent and solution quality ratio are 1:100, is adopted
It is mixed with concussion mode, temperature is 25 DEG C, and the time is 24 hours, and after completing absorption, it is insoluble to carry out the insoluble ketone of separation of solid and liquid water outlet
Lignin adsorbent, ethanol water concentration after measurement absorption.
The insoluble lignin of the insoluble ketone of water is with lignin raw material to comparison diagram such as Fig. 4 of the adsorption isotherm of ethyl alcohol.To second
Alcohol adsorption capacity is obviously improved, and up to 98.5mg/g, improves 53.2% before being relatively classified.
Embodiment 7:
The insoluble lignin of the insoluble ketone of water adsorbs the application of butanol in ABE fermentation liquid, and step is will to prepare in embodiment 2
The insoluble lignin of the insoluble ketone of water be added separately to (its in the aqueous solution that butanol concentration is the butanol of 1-50g/L, acetone, ethyl alcohol
Middle butanol, acetone, ethyl alcohol mass ratio be 6:3:1), adsorbent and solution quality ratio are 1:100, mixed using concussion mode,
Temperature is 25 DEG C, and the time is 24 hours, after completing absorption, carries out being separated by solid-liquid separation the insoluble lignin adsorbent of the insoluble ketone of water outlet, survey
Surely butanol concentration in post-fermentation liquid is adsorbed.
The insoluble lignin of the insoluble ketone of water is such as schemed in ABE fermentation liquid with the comparison diagram of the adsorption isotherm of butanol in aqueous solution
5.Competitive Adsorption reduces the insoluble lignin of the insoluble ketone of water to the adsorbance of butanol in fermentation liquid, but competitive Adsorption phenomenon is not
Obviously, 192.1mg/g is reached to the adsorbance of butanol in fermentation liquid.
Embodiment 8:
The insoluble lignin of the insoluble ketone of water adsorbs the application of acetone in ABE fermentation liquid, and step is will to prepare in embodiment 2
The insoluble lignin of the insoluble ketone of water be added separately to (its in the aqueous solution that acetone concentration is the butanol of 1-50g/L, acetone, ethyl alcohol
Middle butanol, acetone, ethyl alcohol mass ratio be 6:3:1), adsorbent and solution quality ratio are 1:100, mixed using concussion mode,
Temperature is 25 DEG C, and the time is 24 hours, after completing absorption, carries out being separated by solid-liquid separation the insoluble lignin adsorbent of the insoluble ketone of water outlet, survey
Surely acetone concentration in post-fermentation liquid is adsorbed.
The insoluble lignin of the insoluble ketone of water is such as schemed in ABE fermentation liquid with the comparison diagram of the adsorption isotherm of acetone in aqueous solution
6.Competitive Adsorption reduces the insoluble lignin of the insoluble ketone of water to the adsorbance of acetone in fermentation liquid, but competitive Adsorption phenomenon is not
Obviously, 149mg/g is reached to the adsorbance of acetone in fermentation liquid.
Embodiment 9:
The insoluble lignin of the insoluble ketone of water adsorbs the application of ethyl alcohol in ABE fermentation liquid, and step is will to prepare in embodiment 2
The insoluble lignin of the insoluble ketone of water be added separately to (fourth in the aqueous solution that concentration of alcohol is the butanol of 1-50g/L, acetone, ethyl alcohol
Alcohol, acetone, ethyl alcohol mass ratio 6:3:1), adsorbent and solution quality ratio are 1:100, are mixed using concussion mode, temperature 25
DEG C, the time is 24 hours, after completing absorption, carries out being separated by solid-liquid separation the insoluble lignin adsorbent of the insoluble ketone of water outlet, after measurement absorption
Concentration of alcohol in fermentation liquid.
The insoluble lignin of the insoluble ketone of water is such as schemed in ABE fermentation liquid with the comparison diagram of the adsorption isotherm of ethyl alcohol in aqueous solution
7.Competitive Adsorption reduces the insoluble lignin of the insoluble ketone of water to the adsorbance of ethyl alcohol in fermentation liquid, but competitive Adsorption phenomenon is not
Obviously, 95.1mg/g is reached to the adsorbance of ethyl alcohol in fermentation liquid.
Embodiment 10:
Different time condition is lauched the adsorption experiment that the insoluble lignin of insoluble ketone adsorbs butanol in aqueous solution, and step is,
The insoluble lignin of the insoluble ketone of the water prepared in embodiment 3 is added separately to containing butanol (18g/L), acetone (9g/L), ethyl alcohol
In the aqueous solution of (3g/L), adsorbent and solution quality ratio are 1:100, are mixed using concussion mode, and temperature is 25 DEG C, the time
It is 24 hours, after completing absorption, carries out being separated by solid-liquid separation the insoluble lignin adsorbent of the insoluble ketone of water outlet, respectively fourth after measurement absorption
Alcohol, acetone, ethanol water concentration.
The curve of adsorption kinetics such as Fig. 8 of the insoluble lignin adsorbent material of the insoluble ketone of water to butanol, acetone and ethyl alcohol.It can
See, to balance close after butanol adsorption reaction about 40min, then slowly rises, basically reach adsorption saturation after 50min.It is right
Acetone adsorption reaction, close to balance, then slowly rises about after 37min, basically reaches adsorption saturation after 45min.To ethyl alcohol
Adsorption reaction, close to balance, then slowly rises about after 30min, basically reaches adsorption saturation after 35min.Can water breakthrough it is insoluble
The insoluble lignin adsorbent material of ketone is very fast to the rate of adsorption of butanol, acetone and ethyl alcohol.
Unaccomplished matter of the present invention is well-known technique.
Claims (4)
1. it is a kind of improve lignin to butanol in ABE fermentation liquid, acetone, Ethanol Adsorption performance method, it is characterized in that the side
Method the following steps are included:
(1) water-soluble lignin lignin classification insoluble with water: lignin is mixed with distilled water, Sonication assisted treatment 2-
Lower layer's solid after sedimentation and filtering is collected in 5min, sedimentation separation after stirring, filtering, and vacuum drying obtains the insoluble lignin of water；Its
In, every 0.1-2L distilled water adds lignin 10-50g；
(2) the molten lignin of ketone lignin classification insoluble with ketone: the insoluble lignin of the water that upper step is obtained and ketone reagent are sufficiently mixed
It closes, Sonication assisted treatment 2-5min is sufficiently stirred, sedimentation separation, filters, and collects lower layer's solid after sedimentation and filtering, obtains
The insoluble lignin of the insoluble ketone of water；Wherein every 0.1-2L ketone reagent adds the insoluble lignin 30-60g of water；
(3) the insoluble lignin of the insoluble ketone of the water obtained upper step is dried in vacuo 12-48h at 20-60 DEG C, and bottling, sealing is protected
It deposits；
The lignin raw material is corn alkali lignin, pine alkali lignin, Wheat Straw Lignin from Alkali Pulping, poplar alkali lignin or bamboo
Starch black liquor alkali lignin；
Ketone reagent is butanone, pentanone, acetone, cyclohexanone or hexanone in the step (2).
2. improve as described in claim 1 lignin to butanol in ABE fermentation liquid, acetone, Ethanol Adsorption performance method,
Feature is that lignin and distilled water incorporation time are 2-28h in the step (1).
3. improve as described in claim 1 lignin to butanol in ABE fermentation liquid, acetone, Ethanol Adsorption performance method,
Feature is that the insoluble lignin of water and ketone reagent incorporation time are 2-24h in the step (2).
4. improve as described in claim 1 lignin to butanol in ABE fermentation liquid, acetone, Ethanol Adsorption performance method,
Feature is that the sedimentation separation is natural subsidence or is centrifuged at a high speed, and filter method is suction filtration or micro-filtration.
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| EP2007945B1 (en) * | 2006-03-29 | 2011-01-26 | Virginia Tech Intellectual Properties, Inc. | Cellulose-solvent-based lignocellulose fractionation with modest reaction conditions and reagent cycling |
| CN102864672B (en) * | 2012-09-17 | 2015-06-24 | 北京林业大学 | Method for extracting lignin |
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