CN104419733A - Detoxification and fermentation method of large red algae biomass degradation liquid - Google Patents
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Abstract
The invention provides a detoxification and fermentation method of large red algae biomass degradation liquid. The detoxification and fermentation method comprises the following steps: degrading the large red algae biomass to obtain the degradation liquid, adding an appropriate amount of molecular-sieve or non-molecular-sieve adsorbent having adsorption property as a detoxifying agent into the degradation liquid to carry out double detoxification or multiple detoxification on the degradation liquid so as to remove substances of preventing the activities of microorganisms in the degradation liquid, finally removing the detoxifying agent and producing bio-fuels or chemical intermediates by fermentation of the corresponding fermentation microorganisms. By virtue of experimental verification, compared with the existing fermentation method of algae, the detoxification and fermentation method disclosed by the invention has the advantages that the treatment process of the degradation liquid is simple and consumes less time; the detoxifying agent is low in cost, wide in resources and can be recycled; the fermentation of the microorganisms has the advantages of high starting speed, short time, high yield and less byproducts and the fermented products are easily separated and purified.
Description
Technical field
The invention belongs to bioenergy technical field, particularly relate to a kind of detoxification fermentation novel method of large-scale red algae biomass degradation liquid.
Background technology
Along with the development of human industryization society, the Environment pollution that fossil fuel energy faces and non-renewable problem are on the rise.Biomass energy has the characteristic such as environmental friendliness, substantial amounts as renewable energy source, is expected to progressively to substitute the energy substance that fossil energy becomes emerging.At present, the production of most of biomass energy is that raw material, particularly food crop such as corn, sugarcane etc. are widely used because its carbohydrate content is high with terrestrial plant.But the plantation of terrestrial plant occupy human survival must soil and Freshwater resources, long-run development will inevitably impact human lives.
At present, existing research and utilization marine algae is raw material production biodiesel, wood-based composites, biogas, hydrogen energy source etc.Compared with terrestrial life matter, marine algae biomass reserves are large, and such as, in Asian countries, red algae and the brown alga output of unit surface reach as high as 70 ~ 80 tons/hectare/years, are 2 ~ 4 times of land plant output; And, marine algae fast growth, without the need to fresh water and unnecessary soil, production fluid fluid fuel ability is strong, photosynthetic efficiency is high, therefore be the preferred material of China's Biomass Energy Development, wherein red algae accounts for the half of marine alga ultimate production, has good Prospect of R & D.
Research shows, often generates with to the virose compound of biological tool, thus inhibit the fermentation of degradation solution in the degradation process of marine algae.This compound mainly comprises three class materials, and a class is lipid acid, such as acetic acid, formic acid, levulinic acid etc.; One class is furan derivative, such as furfural, 5 hydroxymethyl furfural (HMF) etc.; Another kind of is phenolic epoxy acrylate.In addition, in the frond of ocean, comprise a small amount of heavy metal ion, rotten black substance, inorganic salt etc., also will affect the vigor of bacterial classification.These suppress degradation solution to ferment in the degradable fermented process of marine algae or the material that affects spawn activity is called as inhibition.
The technology of traditional removal inhibition comprises crosses neutralization, ion exchange resin absorption, peroxidase process etc. by degradation solution vacuum distilling, calcium hydroxide.But the inhibition kind utilizing these methods to remove is single, and removal efficiency is lower.In addition, also have correlative study to be by optimizing preprocessing process to reduce the inhibition in fermented liquid, or improvement bacterial classification is to strengthen the tolerance to inhibition, but these methods will increase considerably additional cost, and still be in development.
Summary of the invention
For above-mentioned technical problem, the invention provides a kind of detoxification fermentation novel method of large-scale red algae biomass degradation liquid, can effectively reduce or remove inhibition, improve the productive rate that large-scale red algae biomass ferment produces biofuel or chemical intermediate.
The technical solution used in the present invention is: a kind of detoxification fermentation process of large-scale red algae biomass degradation liquid, and the method is:
(1) large-scale red algae biomass obtain degradation solution after degraded;
(2) pH value of degradation solution is adjusted to 4.0 ~ 10.0, in degradation solution add 0.5 ~ 5%(w/v) detoxifying agent, be 15 DEG C ~ 50 DEG C in temperature, degradation solution carried out under the condition of vibrations or continuously stirring to the detoxification treatment of more than twice or twice, to remove the material of the microbiostatic activity in degradation solution, then filter or precipitation removal detoxifying agent, obtain the degradation solution after detoxification treatment;
(3) repeating step (2) once or more than twice, then carries out fermentative processing to the degradation solution after detoxification treatment, obtain biofuel or chemical intermediate;
Described detoxifying agent has the molecular sieve of absorption property or non-molecular sieve adsorbent, include but not limited to gac, diatomite, wilkinite ,-molecular sieve, ZSM-5 molecular sieve, NaY molecular sieve,
any one or two or more combinations in molecular sieve, chitosan etc.; The detoxifying agent adopted in each time described detoxification is different.
Described large-scale red algae biomass are the macros containing taking galactosyl as main polysaccharide, comprise the kelp of Porphyra (Porphyra), chicken feather Lepidium (Pterocladia), centipede Trentepohlia (Grateloupia), fragrant plant mentioned in ancient texts section (Gracilariaceae), Gelidium (Gelidiales), Eucheuma (Eucheuma).
As preferably, in described step (1), the degradation method of large-scale red algae biomass is not limit, and comprises one or several the combination in mineral substance acid acid hydrolysis, hydro-thermal sulfurous gas hydrolysis method, acid gas explosion method, enzymolysis process.
As preferably, in described step (2), the quality of detoxifying agent is 0.5 ~ 5% grams per milliliter with the ratio of degradation solution volume.
As preferably, in described step (2), the detoxification treatment time is 10 minutes ~ 24 hours.
As preferably, in described step (3), fermentative processing carries out anaerobically fermenting after specifically comprising the bacterial classifications such as access yeast.Wherein, as preferably, described bacterial classification and the volume ratio of fermentation liquid are 1:10 ~ 1:1; Described anaerobically fermenting carries out at 25 ~ 35 DEG C; The described anaerobically fermenting time is preferably 12 hours ~ 168 hours; Described anaerobically fermenting includes but not limited to intermittent type anaerobically fermenting, continuous anaerobic fermentation or semicontinuous anaerobically fermenting.
In sum, the invention provides a kind of with galactosyl be the large-scale red algae biomass degradation liquid of main polysaccharide detoxification fermentation novel method, the method carries out dual detoxification or multiple detoxification to have the molecular sieve of absorption property or non-molecular sieve adsorbent for detoxifying agent, the particle aperture utilizing this detoxifying agent larger and specific surface area adsorb the various organism in fermented liquid, small molecules acid, the inhibitions such as metal ion, thus high-efficiency fermenting production comprises ethanol, butanols, isopropylcarbinol, propyl alcohol, 1, ammediol, 1, the biofuel of the alcohols organic substances such as 4-propylene glycol and alkanes organic substance or chemical intermediate.Verification experimental verification, compared with existing algae fermentation process, degradation solution treating processes of the present invention is simple, consuming time short; Detoxifying agent cost is low, source is wide, recoverable; Fermentable toggle speed is fast, the time is short, output is high, by product is few, easily separated purification.
Accompanying drawing explanation
Fig. 1 is embodiment 1 and gelidium acid hydrolysate producing and ethanol concentration changes with time curve in anaerobically fermenting products therefrom in comparative example 1;
Fig. 2 is that embodiment 1 produces 5 hydroxymethyl furfural concentration changes with time curve with gelidium acid hydrolysate in comparative example 1 in anaerobically fermenting products therefrom;
Fig. 3 is embodiment 2 and Grateloupia filicina (Wulf.) enzymolysis product producing and ethanol concentration changes with time curve in anaerobically fermenting products therefrom in comparative example 2;
Fig. 4 is that embodiment 2 produces 5 hydroxymethyl furfural concentration changes with time curve with Grateloupia filicina (Wulf.) enzymolysis product in comparative example 2 in anaerobically fermenting products therefrom;
Fig. 5 is that embodiment 3 produces butanol concentration change curve in time with the acid gas explosion product of laver in comparative example 3 in anaerobically fermenting products therefrom.
Embodiment
Below in conjunction with accompanying drawing and embodiment, illustrate the present invention further.Should be understood that these embodiments are only for illustration of the present invention, and be not used in and limit the scope of the invention.
Embodiment 1:
In the present embodiment, algae bio matter is gelidium (Gelidiales), and the liquid acids hydrolysate of this algae bio matter obtains ethanol after anaerobically fermenting.Detoxifying agent is gac and wilkinite.Detailed process is as follows.
(1) get drystone cauliflower 200 grams, add the sulphuric acid soln of 1 liter 2% after pulverizing, fully mix thoroughly.Under the environment of 125 degrees Celsius, acidolysis 2 hours, obtains gelidium degradation solution after press filtration.In degradation solution, add sodium hydroxide pH is adjusted to 6.0.
(2) measure degradation solution 50 milliliters, add 1 gram of gac, detoxification 30 minutes in shaking table, shaking speed is 150 rpms, and after detoxification, suction filtration removes gac.Then, take calcium-base bentonite 1 gram, add in the degradation solution of gac detoxification, carry out dual detoxification, detoxification condition is: shaking speed is 150 rpms, detoxification 30 minutes, and after detoxification, suction filtration removes wilkinite, and the degradation solution obtained is for ethanol fermentation.
After tested, before and after detoxification, in degradation solution, the content of sugared source and major inhibitor 5 hydroxymethyl furfural is as shown in table 1 below.
Table 1: sugared part and inhibitor contents in gelidium degradation solution During Detoxification
(3) in the degradation solution after dual detoxification be by volume 10% inoculum size access centrifugal after yeast thalline, in 30 DEG C, shaking speed is anaerobically fermenting producing and ethanol under the condition of 150 rpms.
Comparative example 1:
The present embodiment is the comparative example of above-described embodiment 1.
In the present embodiment, algae bio matter is identical with embodiment 1, is gelidium (Gelidiales), is also to obtain ethanol by the liquid acids hydrolysate of this algae bio matter of anaerobically fermenting.
The acid hydrolysis liquid treating processes that the present embodiment adopts, except not adding gac and wilkinite does dual detoxification, all the other steps are identical with preparation condition and embodiment 1.
Concrete steps are after step (1) in the present embodiment: measure degradation solution 50 milliliters, in degradation solution be by volume 10% inoculum size access centrifugal after yeast thalline, in 30 DEG C, shaking speed is anaerobically fermenting producing and ethanol under the condition of 150 rpms.
Above-described embodiment 1 and the alcohol concn curve contrasted in enforcement 1 in anaerobically fermenting after product are as shown in Figure 1.Wherein, " ■ " is the alcohol concn curve of embodiment 1, and " ▲ " is the alcohol concn curve of comparative example 1.Degradation solution is after gac and the dual detoxification of wilkinite as shown in Figure 1, after adding yeast, 12 hours ethanol contents just reach 16.7 grams often liter, semi-lactosi reduces to 3.0 grams often liter by initial 37.5 grams often liter, wherein have the semi-lactosi of 32.66 grams to be converted into ethanol, semi-lactosi effective rate of utilization reaches 94.7%.But within 48 hours, still ethanol do not detected without the degradation solution of detoxification in fermentation.
Above-described embodiment 1 and the 5 hydroxymethyl furfural concentration curve contrasted in enforcement 1 in anaerobically fermenting after product are as shown in Figure 2.Wherein, " ■ " is the 5 hydroxymethyl furfural concentration curve of embodiment 1, and " ▲ " is the 5 hydroxymethyl furfural concentration curve of comparative example 1.As shown in Figure 2, degradation solution is after dual detoxification, and the content of major inhibitor 5 hydroxymethyl furfural reduces 8.2 grams often liter, and the 5 hydroxymethyl furfural close to half is removed.During the fermentation, in the degradation solution of dual detoxification, the content of 5 hydroxymethyl furfural is in continuous decline, littlely all to consume constantly 24, and in the fermented liquid of non-detoxification in contrast, the content of 5 hydroxymethyl furfural does not change substantially along with fermentation time is passed.
In above-described embodiment 1, in fermentation after 24 hours, semi-lactosi only surplus 0.8 gram often liter, the transformation efficiency of semi-lactosi is 97.8%, ethanol content reaches 17.5 grams often liter, semi-lactosi except small portion be used for volunteer growth need other metabolism except, 93% for anaerobically fermenting producing and ethanol, the amount through unit of the present invention gelidium biomass producing and ethanol reach 87.5 kilograms per ton.And to contrast under equal conditions in enforcement 1 without the transformation efficiency of the degradation solution sugar of detoxification be zero substantially.
Embodiment 2:
In the present embodiment, algae bio matter is Grateloupia filicina (Wulf.) (Grateloupia), and the enzymolysis product of this algae bio matter obtains ethanol through anaerobically fermenting.Detoxifying agent is β-molecular sieve and diatomite.
(1) take 300 grams of Grateloupia filicina (Wulf.) powder, the phosphate aqueous solution adding 1 liter 4% is fully mixed thoroughly.In 100 DEG C of degradeds 1 hour, supply the biodiversity evaporated.By sodium hydroxide powder, the pH of acid degradation liquid is adjusted to 6.5, adds the α-amylase of 200U/ gram, degrade 72 hours for 60 DEG C.α-amylase degradation process terminates rear degradation solution and adjusts pH to 5.0 through hydrochloric acid, then the saccharifying enzyme adding 100U/ gram continues enzymolysis 72 hours under the environment of 60 DEG C, and then squeeze and filter obtains degradation solution.
(2) measure degradation solution 50 milliliters, with sodium hydroxide, pH is adjusted to 6.0, add 2 grams of β-molecular sieves, 30 degrees Celsius shake detoxification 10 minutes, and then suction filtration removes β-molecular sieve.Take 0.5 gram, diatomite, add in the degradation solution of β-molecular sieve detoxification, carry out dual detoxification, detoxification condition is: 30 degrees Celsius shake 1 hour, and after detoxification, suction filtration removes diatomite, and the degradation solution obtained is for ethanol fermentation.
After tested, before and after detoxification, in degradation solution, the content of sugared source and major inhibitor 5 hydroxymethyl furfural is as shown in table 2 below.
Table 2: sugared part and inhibitor contents in Grateloupia filicina (Wulf.) degradation solution During Detoxification
(3) in the degradation solution after dual detoxification by volume 5% inoculum size access centrifugal after yeast thalline, in 30 DEG C, shaking speed is anaerobically fermenting producing and ethanol under the condition of 150 rpms.
Comparative example 2:
The present embodiment is the comparative example of above-described embodiment 2.
In the present embodiment, algae bio matter is identical with embodiment 2, is Grateloupia filicina (Wulf.) (Grateloupia), is also to obtain ethanol by the enzymolysis product of this algae bio matter of anaerobically fermenting.
The enzymolysis solution treating processes that the present embodiment adopts, except not adding β-molecular sieve and diatomite does dual detoxification, all the other steps are identical with preparation condition and embodiment 2.
After step (1) in the present embodiment, concrete steps are: measure degradation solution 50 milliliters, with sodium hydroxide, pH is adjusted to 6.0.Yeast thalline after the inoculum size access of 5% is by volume centrifugal, in 30 DEG C, shaking speed is anaerobically fermenting producing and ethanol under the condition of 150 rpms.
Above-described embodiment 2 and the alcohol concn curve contrasted in enforcement 2 in anaerobically fermenting after product are as shown in Figure 3.Wherein, " ■ " is the alcohol concn curve of embodiment 2, and " ▲ " is the alcohol concn curve of comparative example 2.In the degradation solution of β-molecular sieve and the dual detoxification of diatomite, add yeast secondary fermentation reaction as shown in Figure 3 start fast, within 24 hours, ethanol content just reaches 18.7 grams often liter, semi-lactosi reduces to 0.5 gram often liter by initial 39.4 grams often liter, wherein have the semi-lactosi of 36.57 grams to be converted into ethanol, semi-lactosi effective rate of utilization reaches 94.0%.But still ethanol do not detected without the degradation solution of detoxification constantly fermentation 24 is little, at the 36 little ethanol just detecting 1.1 grams often liter constantly, start time is obviously later than the degradation solution through dual detoxification.
Above-described embodiment 2 and the 5 hydroxymethyl furfural concentration curve contrasted in enforcement 2 in anaerobically fermenting after product are as shown in Figure 4.Wherein, " ■ " is the 5 hydroxymethyl furfural concentration curve of embodiment 2, and " ▲ " is the 5 hydroxymethyl furfural concentration curve of comparative example 2.As shown in Figure 4, degradation solution is after dual detoxification, and the content of major inhibitor 5 hydroxymethyl furfural reduces 1.1 grams often liter.During the fermentation, in the degradation solution of dual detoxification, the content of 5 hydroxymethyl furfural is in continuous decline, at the content of fermentation termination 5 hydroxymethyl furfural lower than 1 gram often liter.In contrast, the content of degradation solution is also in minimizing, but the speed reduced is obviously than slow in dual detoxification degradation solution.
In fermentation after 48 hours, in the fermented liquid of the dual poison-removing method of the present invention the amount of unit Grateloupia filicina (Wulf.) biomass producing and ethanol reach 61.7 kilograms per ton.And under equal conditions without the degradation solution unit Grateloupia filicina (Wulf.) biomass producing and ethanol amount of detoxification be only 6.0 kilograms per ton.
Embodiment 3:
In the present embodiment, algae bio matter is laver (Porphyra), and the acid gas explosion hydrolysate of this algae bio matter obtains butanols through anaerobically fermenting.Detoxifying agent is gac, ZSM-5 molecular sieve and NaY molecular sieve.
(1) take 300 grams of laver powder, the aqueous nitric acid adding 0.5 liter 4% is fully mixed thoroughly, soaking at room temperature 2 hours.Add in steam explosion machine, 180 degrees Celsius, process 3 minutes under 1.2Mpa, in products therefrom, add 0.5 premium on currency after quick pressure releasing, fully stir, squeeze and filter obtains degradation solution, with calcium hydroxide powder, the pH of degradation solution is adjusted to 7.0.
(2) measure degradation solution 50 milliliters, add gac 0.25 gram, 50 degrees Celsius of continuously stirring detoxifications 10 minutes, after detoxification, suction filtration removes gac.Add ZSM-5 molecular sieve and each 0.25 gram of NaY molecular sieve again, 30 degrees Celsius of continuously stirring detoxifications 12 hours, after detoxification, suction filtration removes molecular sieve.
(3) access clostridium acetobutylicum by the degradation solution of inoculum size after dual detoxification of 15%, in 30 degrees Celsius, shaking speed is that under the condition of 200 rpms, anaerobically fermenting produces butanols.
Comparative example 3:
The present embodiment is the comparative example of above-described embodiment 3.
In the present embodiment, algae bio matter is identical with embodiment 3, is laver (Porphyra), is also to obtain butanols by the acid gas explosion hydrolysate of anaerobically fermenting.
The enzymolysis solution treating processes that the present embodiment adopts, do multiple detoxification except not adding gac, ZSM-5 molecular sieve and NaY molecular sieve, all the other steps are identical with preparation condition and embodiment 2.
After step (1) in the present embodiment, concrete steps are: measure degradation solution 50 milliliters, clostridium acetobutylicum is accessed in the degradation solution of inoculum size by 15% after dual detoxification, in 30 degrees Celsius, shaking speed is that under the condition of 200 rpms, anaerobically fermenting produces butanols.
Above-described embodiment 3 and the butanol concentration curve contrasted in enforcement 3 in anaerobically fermenting after product are as shown in Figure 5.Wherein, " ■ " is the alcohol concn curve of embodiment 3, and " ▲ " is the alcohol concn curve of comparative example 3.As shown in Figure 5, ferment after 48 hours, in the fermented liquid of multiple detoxification, the content of butanols is 20.5 grams often liter, and is only 1.3 grams often liter without butanol content in the fermented liquid of detoxification.
Above-described embodiment has been described in detail technical scheme of the present invention; be understood that and the foregoing is only specific embodiments of the invention; be not limited to the present invention; all make in spirit of the present invention any amendment, supplement or similar fashion substitute etc., all should be included within protection scope of the present invention.
Claims (10)
1. a detoxification fermentation process for large-scale red algae biomass degradation liquid, is characterized in that: comprise the steps:
(1) large-scale red algae biomass obtain degradation solution after degraded;
(2) pH value of degradation solution is adjusted to 4.0 ~ 10.0, in degradation solution add 0.5 ~ 5%(w/v) detoxifying agent, be 15 DEG C ~ 50 DEG C in temperature, detoxification treatment carried out to degradation solution under the condition of vibrations or continuously stirring, to remove the material of the microbiostatic activity in degradation solution, then filter or precipitation removal detoxifying agent, obtain the degradation solution after detoxification treatment;
(3) repeating step (2) once or more than twice, then carries out fermentative processing to the degradation solution after detoxification treatment, obtain biofuel or chemical intermediate;
Described detoxifying agent has the molecular sieve of absorption property or non-molecular sieve adsorbent, include but not limited to gac, diatomite, wilkinite, β-molecular sieve, ZSM-5 molecular sieve, NaY molecular sieve,
any one or two or more combinations in molecular sieve, chitosan; The detoxifying agent adopted in each time described detoxification is different.
2. the detoxification fermentation process of large-scale red algae biomass degradation liquid as claimed in claim 1, is characterized in that: described large-scale red algae is Porphyra (Porphyra), chicken feather Lepidium (Pterocladia), centipede Trentepohlia (Grateloupia), fragrant plant mentioned in ancient texts section (Gracilariaceae), Gelidium (Gelidiales), Eucheuma (Eucheuma).
3. the detoxification fermentation process of large-scale red algae biomass degradation liquid as claimed in claim 1, it is characterized in that: in described step (1), the degradation method of large-scale red algae biomass is one or several the combinations in mineral substance acid degradation, hydro-thermal sulfurous gas hydrolysis method, acid gas explosion method and enzymolysis process.
4. the detoxification fermentation process of large-scale red algae biomass degradation liquid as claimed in claim 1, is characterized in that: in described step (2), the quality of detoxifying agent is 0.5 ~ 5% grams per milliliter with the ratio of degradation solution volume.
5. the detoxification fermentation process of large-scale red algae biomass degradation liquid as claimed in claim 1, it is characterized in that: in described step (2), the detoxification time is 10 minutes to 24 hours.
6. the detoxification fermentation process of large-scale red algae biomass degradation liquid as claimed in claim 1, is characterized in that: in described step (3), in fermentative processing, the volume ratio of bacterial classification and fermentation liquid is 1:10 ~ 1:1.
7. the detoxification fermentation process of large-scale red algae biomass degradation liquid as claimed in claim 1, is characterized in that: in described step (3), fermentative processing is anaerobically fermenting.
8. the detoxification fermentation process of large-scale red algae biomass degradation liquid as claimed in claim 7, is characterized in that: described anaerobically fermenting is intermittent type anaerobically fermenting, continuous anaerobic fermentation or semicontinuous anaerobically fermenting.
9. the detoxification fermentation process of large-scale red algae biomass degradation liquid as claimed in claim 7, it is characterized in that: in described step (3), anaerobically fermenting carries out at 25 ~ 35 DEG C, the anaerobically fermenting time is 12 hours ~ 168 hours.
10. the detoxification fermentation process of the large-scale red algae biomass degradation liquid as described in claim arbitrary in claim 1 to 9, is characterized in that: described biofuel or chemical intermediate are alcohols organic substance and alkanes organic substance.
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| CN106381217A (en) * | 2016-11-30 | 2017-02-08 | 广西东奇能源技术有限公司 | Preparation method of biological fuel with high combustion value |
| CN108165587A (en) * | 2018-03-23 | 2018-06-15 | 福州大学 | A kind of method that biological butanol is prepared using algal polysaccharides agar |
| CN108821467A (en) * | 2018-05-29 | 2018-11-16 | 中科院广州能源所盱眙凹土研发中心 | The purified treatment and circulation utilization method of alcohol fermentation wastewater |
| CN117678727A (en) * | 2023-12-14 | 2024-03-12 | 山东海之宝海洋科技有限公司 | Use of lactobacillus fermentation in the preparation of a flavoring |
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