CN107136317A - It is a kind of to comprehensively utilize the method that vinasse prepare xylo-oligosaccharide and protein feed simultaneously - Google Patents
It is a kind of to comprehensively utilize the method that vinasse prepare xylo-oligosaccharide and protein feed simultaneously Download PDFInfo
- Publication number
- CN107136317A CN107136317A CN201710531535.5A CN201710531535A CN107136317A CN 107136317 A CN107136317 A CN 107136317A CN 201710531535 A CN201710531535 A CN 201710531535A CN 107136317 A CN107136317 A CN 107136317A
- Authority
- CN
- China
- Prior art keywords
- vinasse
- xylan
- oligosaccharide
- xylo
- solid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/80—Food processing, e.g. use of renewable energies or variable speed drives in handling, conveying or stacking
- Y02P60/87—Re-use of by-products of food processing for fodder production
Landscapes
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Saccharide Compounds (AREA)
- Fodder In General (AREA)
Abstract
The method that vinasse prepare xylo-oligosaccharide and protein feed simultaneously is comprehensively utilized the invention discloses a kind of, is related to abandoned biomass comprehensive utilization of resources field.This method obtains xylan crude extract and vinasse residue by the xylan (accounting for hemicellulose more than 90%) in ultrasonic assistant aqueous slkali low temperature rapid extraction vinasse solid, separation of solid and liquid；Adjust xylan crude extract pH and add zytase and acquisition xylo-oligosaccharide hydrolyzate is hydrolyzed, further carry out xylo-oligosaccharide and refine；The vinasse residue extracted after xylan is mixed into progress low temperature drying with distiller's grains liquor and obtains protein feed.Using the method for the present invention, the waste of xylan composition in traditional lees feedses can not only be avoided, and improves xylo-oligosaccharide yield, the content of xylobiose and xylotriose is selectively improved.Prepare high added value xylo-oligosaccharide while, obtain the vinasse albumen feed with good palatability and digestibility, it is achieved thereby that in vinasse a variety of constituents comprehensive utilization.
Description
Technical field
Prepared simultaneously the present invention relates to abandoned biomass comprehensive utilization of resources field, more particularly to a kind of comprehensive utilization vinasse
The method of xylo-oligosaccharide and protein feed.
Background technology
China is alcohol (white wine, edible ethanol and alcohol fuel) production and consumption big country, annual alcoholic fermentation industry
Produce 20,000,000 tons of abandoned vinasses.The starch component in cereal is only consumed in alcoholic fermentation production process, and in vinasse still
Many valuable compositions so have been remained, including：Protein component (corn gluten protein and mycoprotein account for 15-25% butts), in
Property washing fiber (cellulose, hemicellulose and lignin account for 30-45% butts), and micro-nutrient composition (glycerine, B races dimension
Raw element and several amino acids account for 8-15%) etc..Therefore the characteristics of constituent above-mentioned according to discarded fresh grain stillage, its main utilization
Mode has fraction to be used to extract the battalion such as glycerine and amino acid in addition for processing protein feed or directly as farmland compost
Support material and be used as edible fungus culture medium etc..But these Land use systems be present：(1) added value of product is low, plus
The lees feedses and fertilizer of work production are cheap；(2) solid matter is remained, and extracting still can not be thorough after effective nutritional ingredient
Eliminate waste residue；(3) principal component can not be comprehensively utilized, and only consider, using wherein single component, to cause other active ingredients
Waste.
The content of the invention
The method that vinasse prepare xylo-oligosaccharide and protein feed simultaneously is comprehensively utilized it is an object of the invention to provide a kind of,
So as to solve foregoing problems present in prior art.
To achieve these goals, the technical solution adopted by the present invention is as follows：
It is a kind of to comprehensively utilize the method that vinasse prepare xylo-oligosaccharide and protein feed simultaneously, comprise the following steps
Step one, fresh grain stillage raw material is subjected to separation of solid and liquid, obtains vinasse solid and distiller's grains liquor；
Step 2, the vinasse solid is dried, and is crushed to the solid powder that particle diameter is less than 40 mesh；
Step 3, according to 1:10-1:25 solid masses and liquid volume ratio, by the vinasse solid powder and matter after crushing
Measure after percent concentration is well mixed for 2%-10% aqueous slkali and add in reactor, 20 are reacted under the conditions of ultrasonic assistant
- 3 hours minutes extracted xylan, obtained reactant mixture；
Step 4, separation of solid and liquid is carried out by reactant mixture, obtains xylan crude extract and vinasse residue；
Step 5, the xylan crude extract is hydrolyzed 3-24 hours in the presence of zytase, obtains xylo-oligosaccharide
Solution；
Step 6, activated carbon decolorizing, ion exchange imurity-removal ion, vacuum distillation are carried out by gained xylo-oligosaccharide solution
Concentration, obtains refined xylo-oligosaccharide liquid.
Step 7, vinasse residue obtained by step 4 is mixed with step one gained distiller's grains liquor, obtains the mixing of vinasse solid-liquid
Thing, is carried out low temperature drying processing, and distiller's dried grain protein feed is made.
Preferably, in step one, in vinasse of the fresh grain stillage selected from spirit stillage, beer vinasse and amylofermentation ethanol
One or more of mixtures.
Preferably, in step 3, one or more of mixtures of the aqueous slkali in NaOH, KOH and ammoniacal liquor.
Preferably, in step 3, the ultrasonic assistant condition is：Frequency 25-40kHz, power 100-1200W, temperature
20-50℃。
Preferably, step is also included between step 4 and step 5, the vinasse residue is washed, by washing for obtaining
De- liquid is added in the xylan crude extract.
Preferably, it is described to hydrolyze xylan crude extract in the presence of zytase in step 5, specifically, regulation
The pH of the xylan crude extract is 4-6, adds zytase, hydrolyzes under certain conditions.
Preferably, in step 5, the zytase is selected from outside endoxylanase, or endoxylanase and xylan
The mixture of enzyme cutting, or endoxylanase and feruloyl esterase mixture, or endoxylanase and acetyl xylan ester
The mixture of enzyme.
Preferably, it is described to hydrolyze xylan crude extract in the presence of zytase in step 5, specifically, described
The consumption of zytase is 100-1000U/g xylan dries, and the temperature of hydrolysis is 30-60 DEG C, the speed of agitator of reactor
For 50-200rpm.
Preferably, in step 6, the low temperature drying processing is dry selected from freeze-drying, low temperature spray drying or cryogenic vacuum
One kind in dry.
The beneficial effects of the invention are as follows：Comprehensive utilization vinasse provided in an embodiment of the present invention prepare xylo-oligosaccharide and egg simultaneously
The method of white feed, by carrying out separation of solid and liquid to fresh grain stillage, obtains vinasse solid and distiller's grains liquor；Pass through ultrasonic assistant again
Xylan (accounting for hemicellulose more than 90%) in aqueous slkali low temperature rapid extraction vinasse solid, it is thick that separation of solid and liquid obtains xylan
Extract and vinasse residue；Adjust xylan crude extract pH and add zytase and acquisition xylo-oligosaccharide hydrolyzate is hydrolyzed, enter
One step carries out xylo-oligosaccharide and refined；The vinasse residue extracted after xylan is mixed into progress low temperature drying with distiller's grains liquor and obtains egg
White feed.Using the method for the present invention, the waste of xylan composition in traditional lees feedses can not only be avoided, xylan is carried
Take to be rapidly completed at low temperature, be prevented effectively from the loss of the nutritional ingredients such as protein；And improved using enzymolysis process low
Xylan yield, and selectively improve the content of wherein xylobiose and xylotriose.Prepared extracting and converting vinasse xylan
While high added value xylo-oligosaccharide, the vinasse albumen feed with good palatability and digestibility is obtained, so as to realize
The comprehensive utilization of a variety of constituents in vinasse.
Brief description of the drawings
Fig. 1 is vinasse while preparing the method flow schematic diagram of xylo-oligosaccharide and protein feed；
Fig. 2 is influence of the ultrasonic wave added method with traditional soda to extraction xylan；
Fig. 3 is ultrasonic wave added method and influence of the traditional soda to residual protein content in vinasse；
Fig. 4 is the result that xylo-oligosaccharide is prepared using the enzymolysis xylan of embodiment 4；
Fig. 5 is the result that xylo-oligosaccharide is prepared using the enzymolysis xylan of embodiment 5；
Fig. 6 is the result that xylo-oligosaccharide is prepared using acidolysis xylan；
In Fig. 4-6, X2, X3, X4, X5, X6 represent xylobiose, xylotriose, Xylotetrose, wooden pentasaccharides and wooden six sugar and account for low respectively
Xylan relative amount；XOS represents xylo-oligosaccharide yield.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, the present invention is carried out below further
Describe in detail.It should be appreciated that embodiment described herein is not used to limit this hair only to explain the present invention
It is bright.
As shown in figure 1, preparing xylo-oligosaccharide and albumen feeding simultaneously the embodiments of the invention provide one kind comprehensive utilization vinasse
The method of material, comprises the following steps：
Step one, fresh grain stillage raw material is subjected to separation of solid and liquid, obtains vinasse solid and distiller's grains liquor；
Step 2, the vinasse solid is dried, and is crushed to the solid powder that particle diameter is less than 40 mesh；
Step 3, according to 1:10-1:25 solid masses and liquid volume ratio, by the vinasse solid powder and matter after crushing
Measure after percent concentration is well mixed for 2%-10% aqueous slkali and add in reactor, 20 are reacted under the conditions of ultrasonic assistant
- 3 hours minutes extracted xylan, obtained reactant mixture；
Step 4, separation of solid and liquid is carried out by reactant mixture, obtains xylan crude extract and vinasse residue；
Step 5, the xylan crude extract is hydrolyzed 3-24 hours in the presence of zytase, obtains xylo-oligosaccharide
Solution；
Step 6, activated carbon decolorizing, ion exchange imurity-removal ion, vacuum distillation are carried out by gained xylo-oligosaccharide solution
Concentration, obtains refined xylo-oligosaccharide liquid.
Step 7, vinasse residue obtained by step 4 is mixed with step one gained distiller's grains liquor, obtains the mixing of vinasse solid-liquid
Thing, is carried out low temperature drying processing, and distiller's dried grain protein feed is made.
At present, the main Land use systems of abandoned vinasse are production protein feeds, mainly in the following way：Fresh grain stillage is entered
Row separation of solid and liquid and respectively concentrate drying obtain vinasse albumen feed, still, meeting in the vinasse albumen feed that this mode is produced
Containing substantial amounts of neutral detergent fiber, wherein xylan accounts for more than the 20% of butt.During use, although ruminant
The xylose of solubility can be translated into, but xylose can not be absorbed by animal, so as to cause vinasse albumen feed
The waste of middle xylan resource.In addition, nonruminant can not effective these cellulosan materials of digestibility and utilization, substantial amounts of solid-state is fine
Dimension makes in enteron aisle food movement difficult, not only hinders the interaction between digestive ferment and feed, and reduction digestion product to
The diffusion and absorption of mucosal surface, so as to influence the growth of animal.
Regarding to the issue above and prior art, the present invention proposes new scheme, is not simple only to consider reduction wine
Unemployed xylan in poor protein feed, because even by adding hydrolase or can by methods such as microbial fermentations
The content of xylan in feed is reduced, but the xylose that enzymolysis is produced can not still cause the wasting of resources by animal use；Moreover,
Digest the xylose produced and xylo-oligosaccharide is still present in vinasse albumen feed, it is impossible to efficiently separated and utilized, from
And the added value of vinasse albumen feed can not be improved.
Method proposed by the present invention is before using vinasse production protein feed, to efficiently separate and extract xylan composition,
Not only facilitating improves the palatability of protein feed, improves digestibility, and improves value-added content of product.
Specifically, in the present invention, before using vinasse production protein feed, the xylan composition contained in vinasse is extracted,
So as to improving the utilization rate of protein feed, and xylo-oligosaccharide is prepared using xylan, its added value is apparently higher than protein feed
Value, so as to improve the overall added value for the product that vinasse twice laid is obtained.
At present, the production of xylo-oligosaccharide is main using corncob as raw material, passes through diluted acid cooking process and enzymolysis alkali carries xylan
Method prepared.Although China produces a large amount of corncobs every year, most of to be used for xylose, xylitol and furfural
Industrial production, and only a small amount of corncob can be used for producing xylo-oligosaccharide.So, oligomeric wood is produced by raw material of corncob
Sugar, it is impossible to meet the production requirement of xylo-oligosaccharide.
Scheme proposed by the present invention, produces before protein feed by raw material of vinasse, first extracts xylan, recycle wood poly-
Sugar production xylo-oligosaccharide, because vinasse resource is enriched very much, and containing a large amount of xylans, thus it is possible to which it is oligomeric to meet production
The demand of xylose.
But, in the prior art, the method for producing xylo-oligosaccharide using diluted acid cooking process and enzymolysis alkali carries xylan, it is impossible to
Effectively it is applied to vinasse raw material.
Wherein, diluted acid cooking process can not effectively control the content of different polymerization degree component in xylo-oligosaccharide in hydrolytic process
Distribution, easily occurs excessive hydrolysis and produces substantial amounts of xylose monose, so as to cause final xylo-oligosaccharide yield to decline.
The method for digesting alkali carries xylan extracts xylan in raw material by high-temperature alkali solution, then will by zytase
It is converted into xylo-oligosaccharide, and improves wherein xylobiose and xylotriose content.But the method that high-temperature alkali solution extracts xylan
Vinasse raw material is not appropriate for, because aqueous slkali is easily destroyed the protein in vinasse at high temperature, so as to influence follow-up vinasse egg
The quality of white Feed Manufacturing.
For problem present in the above method, in the present invention, it is proposed that the method that low temperature extracts xylan, i.e., in ultrasound
Under ripple subsidiary conditions, the extraction operation of xylan is carried out, this method effectively can not only extract xylan from vinasse,
And the protein component that will not be destroyed in vinasse, so as to not interfere with the vinasse albumen quality of the fodder of subsequent production.And then
The method for being converted into xylo-oligosaccharide by zytase mixing enzymatic xylan improves enzymolysis yield, and selectively improves wherein
Xylobiose and xylotriose content.
Method provided in an embodiment of the present invention, by can not be come out by the xylan constituents extraction of animal use in fresh grain stillage
Afterwards, then by remaining vinasse by low temperature drying processing vinasse albumen feed is prepared, so that vinasse are comprehensively utilized, kept away
Exempt from the waste of remaining vinasse residue.
In the embodiment of the present invention, step can also be included between step 4 and step 5, water-filling is entered to the vinasse residue
Wash, obtain eluent, the eluent is added in the xylan crude extract.
By using the above method, the xylan composition in vinasse can be further reclaimed, its recovery rate is improved.While energy
The aqueous slkali remained on vinasse is enough avoided to influence the quality of production of following protein feed.
In the embodiment of the present invention, in step one, the fresh grain stillage can be selected from spirit stillage, beer vinasse and amylofermentation
One or more of mixtures in the vinasse of ethanol.
As will be understood by the skilled person in the art, for different manufacturers, can according to the actual conditions of itself,
The species of fresh grain stillage is selected, such as, if spirit stillage is easier to obtain, or cost is relatively low, then can select white wine wine
Grain, similarly, can select other kinds of vinasse.
In step 3, one or more of mixtures that the aqueous slkali can be in NaOH, KOH and ammoniacal liquor.
As will be understood by the skilled person in the art, can also be from other similar to NaOH, KOH and ammoniacal liquor property
Aqueous slkali.
In the embodiment of the present invention, in step 3, the ultrasonic assistant condition can be：Frequency 25-40kHz, power
100-1200W, 20-50 DEG C of temperature.
As shown in Figures 2 and 3, the method for xylan being extracted using the specific embodiment of the invention 1-3 ultrasonic assistants provided,
With use traditional soda extracting method (condition for：NaOH concentration 8%, speed of agitator 150rpm, 80 DEG C of temperature is extracted 5 hours)
Compare, ultrasound assisted extraction method can not only effectively reduce the temperature needed for extracting, and be prevented effectively from traditional soda thermophilic digestion and carry
Degraded of the xylan process to protein component in vinasse is taken to destroy.It is to extract to need 5 hours to be additionally, since conventional method, is surpassed
Sound wave typically only needs to just reach the xylan extraction rate in embodiment in -3 hours 30 minutes, so, it is auxiliary using ultrasonic wave
Method is helped more efficiently to extract xylan, obtained xylan content is higher.
It is described to hydrolyze the xylan crude extract in the presence of zytase in step 5 in the embodiment of the present invention,
Specifically, the pH for adjusting the xylan crude extract is 4-6, zytase is added, is hydrolyzed under certain conditions.
In the embodiment of the present invention, in step 5, the zytase is selected from endoxylanase, endoxylanase and wood
The mixture of the mixture of glycan excision enzyme, endoxylanase and feruloyl esterase, or endoxylanase and acetyl wood it is poly-
The mixture of sugar ester enzyme.
In the present embodiment, the enzyme of the most critical used is endoxylanase, and its effect is in the long-chain of xylan
Portion random hydrolysis β-Isosorbide-5-Nitrae xylose glycosidic bond, can hydrolyze the xylo-oligosaccharide for obtaining that the degree of polymerization is 2-6.
Excision enzyme be the long-chain of xylan non-reducing end hydrolyze one by one generation xylose monose, it produces oligomeric wood really
Unimportant in sugar, single use can not obtain xylo-oligosaccharide, it is necessary to be used in mixed way with restriction endonuclease, and its mixed proportion can be：
1:2-1:10。
Feruloyl esterase can the ester bond that is connected with lignin of hydrolyzed xylan, so as to effectively discharge xylan, reduce
The steric hindrance that lignin is produced to zytase, but be single use on xylo-oligosaccharide prepare do not influence, in xylan
Enzyme cutting, which is used in mixed way, is favorably improved xylo-oligosaccharide enzymolysis yield.
Acetyl xylan esterase property is similar with feruloyl esterase, is also that to be used in mixed way effect with restriction endonuclease good.
In the embodiment of the present invention, the consumption of the zytase is 100-1000U/g xylan dries, the temperature of hydrolysis
For 30-60 DEG C, the speed of agitator of reactor is 50-200rpm.
Xylo-oligosaccharide yield and wherein xylobiose and xylotriose of the gained xylan under above-mentioned enzymatic hydrolysis condition is extracted to contain
Amount is substantially better than the effect of dilute acid hydrolysis xylan, as Figure 4-Figure 6.
In the embodiment of the present invention, in step 6, the low temperature drying processing can be selected from freeze-drying, low temperature spray drying
Or one kind in low-temperature vacuum drying.
Embodiment 1
The fresh grain stillage that extracting corn starch fermentation alcohol is produced, by its separation of solid and liquid, obtains vinasse solid respectively and vinasse is clear
Liquid.By the drying of vinasse solid, crushing, 40 mesh sieves are crossed, are mixed with concentration for 6% NaOH solution, solid-to-liquid ratio is 1:20, in ultrasound
Extracted 3 hours under the conditions of frequency 25kHz, power 200W, 20 DEG C of temperature.By mixture separation of solid and liquid, xylan is respectively obtained thick
Extract and remaining vinasse residue, and remaining vinasse residue is washed, eluent is mixed with xylan extraction liquid.By xylan
Crude extract adjusts pH 4.0, adds commercial enzyme Pentopan Plus BG, enzyme dosage is 1000U/g xylan dries, in temperature
Hydrolyzed 3 hours under the conditions of 30 DEG C of degree, speed of agitator 150rpm, xylo-oligosaccharide digests yield up to 70.7%, xylobiose and wooden three
Sugar does not account for the 48.8% and 23.7% of xylo-oligosaccharide total amount.Further pass through activated carbon decolorizing, ion exchange column imurity-removal
Ion, vacuum distillation concentration, obtain refined xylo-oligosaccharide liquid.Finally, remaining vinasse residue and vinasse after xylan will be extracted dense
Contracting liquid is mixed, and is carried out frozen drying processing, is obtained distiller's dried grain protein feed, wherein crude protein content is up to 27.5%.
Embodiment 2
Take young beer grain to carry out separation of solid and liquid, vinasse solid and distiller's grains liquor are obtained respectively.By the drying of vinasse solid, powder
Broken, 40 mesh sieves excessively, are mixed, solid-to-liquid ratio is 1 with concentration for 8% KOH solution:10, in supersonic frequency 40kHz, power 600W, temperature
Extracted 30 minutes under the conditions of 40 DEG C of degree.By mixture separation of solid and liquid, xylan crude extract and remaining vinasse residue are respectively obtained, and
Remaining vinasse residue is washed, eluent is mixed with xylan extraction liquid.Xylan crude extract is adjusted into pH 6.0, added
Commercial enzyme Shearzyme500L, enzyme dosage 100U/g xylan dries, under the conditions of temperature 60 C, speed of agitator 200rpm
Hydrolysis 24 hours, xylo-oligosaccharide yield is up to 75.6%, and xylobiose and xylotriose account for 45.3% He of xylo-oligosaccharide total amount respectively
28.2%.Further concentrated by activated carbon decolorizing, ion exchange column imurity-removal ion, vacuum distillation, obtain refined oligomeric
Xylose.Finally, remaining vinasse residue after xylan will be extracted to mix with vinasse concentrate, frozen drying processing is carried out,
Distiller's dried grain protein feed is obtained, wherein crude protein content is up to 30.7%.
Embodiment 3
Fresh distillers ' grains drying is taken, crushes, cross 40 mesh sieves, is mixed with concentration for 10% ammonia spirit, solid-to-liquid ratio is 1:
25, in supersonic frequency 30kHz, power 900W is extracted 30 minutes under the conditions of temperature 50 C.By mixture separation of solid and liquid, obtain respectively
To xylan crude extract and remaining vinasse residue, and remaining vinasse residue is washed, eluent is mixed with xylan extraction liquid
Close.Xylan crude extract is adjusted into pH 5.5, commercial enzyme Bakezyme-HSP is added, enzyme dosage is 500U/g xylan dries
Matter, is hydrolyzed 12 hours under the conditions of temperature 50 C, speed of agitator 180rpm, and xylo-oligosaccharide digests yield up to 75.7%, wherein
Xylobiose accounts for 43.1%, and xylotriose accounts for 24.2%.Further by activated carbon decolorizing, ion exchange column imurity-removal ion, subtract
Distillation and concentration is pressed, refined xylo-oligosaccharide liquid is obtained.Finally, it will extract after xylan at remaining vinasse residue low-temperature vacuum drying
Reason, obtains distiller's dried grain protein feed, wherein crude protein content is up to 25.7%.
Embodiment 4
The fresh grain stillage that extracting corn starch fermentation alcohol is produced, by its separation of solid and liquid, obtains vinasse solid respectively and vinasse is clear
Liquid.Vinasse solid dries, crushes, crosses 40 mesh sieves, is mixed with concentration for 2% NaOH solution, solid-to-liquid ratio is 1:20, in supersonic frequency
Extracted 2 hours under the conditions of rate 25kHz, power 1200W, temperature 50 C.By mixture separation of solid and liquid, respectively obtain xylan and slightly carry
Liquid and remaining vinasse residue, and remaining vinasse residue is washed, eluent is mixed with xylan extraction liquid.Xylan is thick
Extract adjusts pH 5.5, adds zytase Pentopan Plus BG and feruloyl esterase, enzyme dosage be respectively 400U/g and
100U/g xylan dries, are hydrolyzed 6 hours under the conditions of 40 DEG C of temperature, speed of agitator 50rpm, and xylo-oligosaccharide enzymolysis yield can
Up to 78.3%, wherein xylobiose accounts for 37.8%, and xylotriose accounts for 24.5%.Further taken off by activated carbon decolorizing, ion exchange column
Removal of impurity ion, vacuum distillation concentration, obtain refined xylo-oligosaccharide liquid.Finally, remaining vinasse residue after xylan will be extracted low
Warm vacuum drying treatment, obtains distiller's dried grain protein feed, wherein crude protein content is up to 28.1%.
Embodiment 5
The fresh grain stillage that extracting corn starch fermentation alcohol is produced, by its separation of solid and liquid, obtains vinasse solid respectively and vinasse is clear
Liquid.Vinasse solid dries, crushes, crosses 40 mesh sieves, is mixed with concentration for 5% KOH solution, solid-to-liquid ratio is 1:15, in supersonic frequency
Extracted 40 minutes under the conditions of rate 25kHz, power 400W, 30 DEG C of temperature.By mixture separation of solid and liquid, respectively obtain xylan and slightly carry
Liquid and remaining vinasse residue, and remaining vinasse residue is washed, eluent is mixed with xylan extraction liquid.Xylan is thick
Extract adjusts pH 4.8, adds commercial enzyme Bakezyme-HSP and acetyl xylan esterase, enzyme dosage be respectively 300U/g and
100U/g xylan dries, are hydrolyzed 12 hours under the conditions of temperature 50 C, speed of agitator 150rpm, xylo-oligosaccharide enzymolysis yield
Up to 85.7%, wherein xylobiose accounts for 43.5%, and xylotriose accounts for 34.8%.Further pass through activated carbon decolorizing, ion exchange column
Imurity-removal ion, vacuum distillation concentration, obtain refined xylo-oligosaccharide liquid.Finally, remaining vinasse residue after xylan will be extracted
Low-temperature vacuum drying processing, obtains distiller's dried grain protein feed, wherein crude protein content is up to 31.3%.
Embodiment 6
Take young beer grain to carry out separation of solid and liquid, vinasse solid and distiller's grains liquor are obtained respectively.By the drying of vinasse solid, powder
Broken, 40 mesh sieves excessively, are mixed, solid-to-liquid ratio is 1 with concentration for 8% NaOH solution:10, in supersonic frequency 30kHz, power 900W,
Extracted 30 minutes under the conditions of 25 DEG C of temperature.By mixture separation of solid and liquid, xylan crude extract and remaining vinasse residue are respectively obtained,
And remaining vinasse residue is washed, eluent is mixed with xylan extraction liquid.Xylan crude extract is adjusted into pH 5.0, plus
Enter zytase Pentopan Plus BG and feruloyl esterase, enzyme dosage is respectively 200U/g and 50U/g xylan dries,
Hydrolyzed 24 hours under the conditions of 30 DEG C of temperature, speed of agitator 150rpm, xylo-oligosaccharide digests yield up to 78.7%, wherein wood two
Sugar accounts for 38.4%, and xylotriose accounts for 25.8%.Further steamed by activated carbon decolorizing, ion exchange column imurity-removal ion, decompression
Concentration is evaporated, refined xylo-oligosaccharide liquid is obtained.Finally, remaining vinasse residue low-temperature vacuum drying after xylan will be extracted to handle, obtained
To distiller's dried grain protein feed, wherein crude protein content is up to 27.9%.
Enzyme preparation involved in the present invention is not limited to above-mentioned endoxylanase Bakezyme-HSP, Pentopan used
The commercial enzymes such as Plus BG and Shearzyme500L, can also for above-mentioned endoxylanase and other xylan excision enzymes, Ah
One or more of mixed enzymes in Wei's acid commercial enzyme such as esterase and acetyl xylan esterase, or by microbial fermentation produce it is upper
State the crude enzyme liquid of multienzyme complex.
By using above-mentioned technical proposal disclosed by the invention, following beneficial effect has been obtained：
(1) method provided in an embodiment of the present invention, xylo-oligosaccharide and protein feed are prepared using abandoned vinasse resource simultaneously,
By the way that the hemi-cellulose components not utilized in vinasse by poultry are converted into xylo-oligosaccharide, key component in vinasse not only avoid
Waste, effectively improve the palatability and digestibility during vinasse albumen feed, and produced the oligomeric of high added value
Xylose, adds the added value of vinasse converted product, realizes the high-efficiency comprehensive utilization of vinasse waste, is expected to further extend wine
The industrial chain of essence fermentation enterprise；
(2) the applicable vinasse raw material type of the present invention extensively, includes distillers ' grains, the beer of a variety of technology of alcohol generation
One or more mixing in the vinasse that grain and Alcohol Production with Corn Starch Fermentation are produced；
(3) present invention increases ultrasonic wave added low temperature xylan extracted with alkali on the basis of traditional lees feedses production technology
Operation, shortens the xylan extraction time, reduces the temperature of xylan extracted with alkali, so as to avoid protein etc. in vinasse
The loss that hydrolysis is caused occurs during conventional high-temperature xylan extracted with alkali for nutriment；
(4) the xylan liquid obtained by being extracted using the method for the present invention, only need to adjust pH just can directly carry out follow-up enzyme
Solution prepares the process of xylo-oligosaccharide, and xylan content in raw material is improved without concentration, so, operational sequence is effectively simplified,
Reduce running cost；
(5) in the method that the present invention is provided, xylo-oligosaccharide is prepared by biological enzyme hydrolyzed xylan, steamed with traditional diluted acid
Boil or hydro-thermal reaction prepares xylo-oligosaccharide method and compared, xylo-oligosaccharide yield, and effectively controlled enzymatic hydrolysis product can be significantly improved
The degree of polymerization distribution of middle xylo-oligosaccharide, improves the content of wherein xylobiose and xylotriose isoreactivity functional component.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
Depending on protection scope of the present invention.
Claims (9)
1. a kind of comprehensively utilize the method that vinasse prepare xylo-oligosaccharide and protein feed simultaneously, it is characterised in that including following step
Suddenly
Step one, fresh grain stillage raw material is subjected to separation of solid and liquid, obtains vinasse solid and distiller's grains liquor；
Step 2, the vinasse solid is dried, and is crushed to the solid powder that particle diameter is less than 40 mesh；
Step 3, according to 1:10-1:25 solid masses and liquid volume ratio, by the vinasse solid powder after crushing and quality hundred
Divide specific concentration to be added after being well mixed for 2%-10% aqueous slkali in reactor, 20 points are reacted under the conditions of ultrasonic assistant
Clock extracts xylan in -3 hours, obtains reactant mixture；
Step 4, separation of solid and liquid is carried out by reactant mixture, obtains xylan crude extract and vinasse residue；
Step 5, the xylan crude extract is hydrolyzed 3-24 hours in the presence of zytase, obtains xylo-oligosaccharide solution；
Step 6, gained xylo-oligosaccharide solution progress activated carbon decolorizing, ion exchange imurity-removal ion, vacuum distillation is dense
Contracting, obtains refined xylo-oligosaccharide liquid.
Step 7, vinasse residue obtained by step 4 is mixed with step one gained distiller's grains liquor, vinasse solidliquid mixture is obtained, will
It carries out low temperature drying processing, and distiller's dried grain protein feed is made.
2. the method that comprehensive utilization vinasse according to claim 1 prepare xylo-oligosaccharide and protein feed simultaneously, its feature
It is, in step one, one kind or several in vinasse of the fresh grain stillage selected from spirit stillage, beer vinasse and amylofermentation ethanol
The mixture planted.
3. the method that comprehensive utilization vinasse according to claim 1 prepare xylo-oligosaccharide and protein feed simultaneously, its feature
It is, in step 3, one or more of mixtures of the aqueous slkali in NaOH, KOH and ammoniacal liquor.
4. the method that comprehensive utilization vinasse according to claim 1 prepare xylo-oligosaccharide and protein feed simultaneously, its feature
It is, in step 3, the ultrasonic assistant condition is：Frequency 25-40kHz, power 100-1200W, 20-50 DEG C of temperature.
5. the method that comprehensive utilization vinasse according to claim 1 prepare xylo-oligosaccharide and protein feed simultaneously, its feature
It is, step is also included between step 4 and step 5, the vinasse residue is washed, obtained eluent is added into institute
State in xylan crude extract.
6. the method that comprehensive utilization vinasse according to claim 1 prepare xylo-oligosaccharide and protein feed simultaneously, its feature
It is, it is described to hydrolyze xylan crude extract in the presence of zytase in step 5, specifically, adjusting the xylan
The pH of crude extract is 4-6, adds zytase, hydrolyzes under certain conditions.
7. the method that comprehensive utilization vinasse according to claim 1 prepare xylo-oligosaccharide and protein feed simultaneously, its feature
It is, in step 5, mixing of the zytase selected from endoxylanase, or endoxylanase and xylan excision enzyme
Thing, or endoxylanase and feruloyl esterase mixture, or endoxylanase and acetyl xylan esterase mixture.
8. the method that comprehensive utilization vinasse according to claim 1 prepare xylo-oligosaccharide and protein feed simultaneously, its feature
It is, it is described to hydrolyze xylan crude extract in the presence of zytase in step 5, specifically, the zytase
Consumption is 100-1000U/g xylan dries, and the temperature of hydrolysis is 30-60 DEG C, and the speed of agitator of reactor is 50-
200rpm。
9. the method that comprehensive utilization vinasse according to claim 1 prepare xylo-oligosaccharide and protein feed simultaneously, its feature
It is, in step 6, the low temperature drying handles one in freeze-drying, low temperature spray drying or low-temperature vacuum drying
Kind.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710531535.5A CN107136317B (en) | 2017-07-03 | 2017-07-03 | Method for preparing xylo-oligosaccharide and protein feed by comprehensively utilizing vinasse |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710531535.5A CN107136317B (en) | 2017-07-03 | 2017-07-03 | Method for preparing xylo-oligosaccharide and protein feed by comprehensively utilizing vinasse |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107136317A true CN107136317A (en) | 2017-09-08 |
| CN107136317B CN107136317B (en) | 2020-05-08 |
Family
ID=59784756
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710531535.5A Active CN107136317B (en) | 2017-07-03 | 2017-07-03 | Method for preparing xylo-oligosaccharide and protein feed by comprehensively utilizing vinasse |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107136317B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107475467A (en) * | 2017-09-14 | 2017-12-15 | 齐鲁工业大学 | A kind of highly effective extraction method of poplar xylose |
| CN109744367A (en) * | 2019-03-22 | 2019-05-14 | 东莞市澹一生物科技有限公司 | The method and feedstuff of resource utilization wheat vinasse production feedstuff |
| CN109744368A (en) * | 2019-03-22 | 2019-05-14 | 东莞市澹一生物科技有限公司 | Utilize the method and feedstuff of wheat vinasse production feedstuff |
| CN109793260A (en) * | 2019-01-30 | 2019-05-24 | 四川中烟工业有限责任公司 | A kind of spirit distiller grain oil and its preparation method and application |
| CN117903332A (en) * | 2024-01-11 | 2024-04-19 | 江西师范大学 | Distilled grain water-soluble arabinoxylan, preparation method thereof, pharmaceutical composition and application |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103936868A (en) * | 2014-05-05 | 2014-07-23 | 江南大学 | Method for extracting resistant starch from yellow wine lees through ultrahigh pressure and ultrasonic assisted treatment |
| CN103936869A (en) * | 2014-05-05 | 2014-07-23 | 江南大学 | Method for extracting slowly digestible starch from sweet yellow wine vinasse |
| CN105211627A (en) * | 2014-06-25 | 2016-01-06 | 都江堰惠农生物技术有限责任公司 | Soy sauce-and vinegar-residue produces microbial protein feed |
| CN106359894A (en) * | 2016-09-13 | 2017-02-01 | 贵州华清科维环境能源有限责任公司 | Method for preparing high-protein feed from distillers' grain |
-
2017
- 2017-07-03 CN CN201710531535.5A patent/CN107136317B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103936868A (en) * | 2014-05-05 | 2014-07-23 | 江南大学 | Method for extracting resistant starch from yellow wine lees through ultrahigh pressure and ultrasonic assisted treatment |
| CN103936869A (en) * | 2014-05-05 | 2014-07-23 | 江南大学 | Method for extracting slowly digestible starch from sweet yellow wine vinasse |
| CN105211627A (en) * | 2014-06-25 | 2016-01-06 | 都江堰惠农生物技术有限责任公司 | Soy sauce-and vinegar-residue produces microbial protein feed |
| CN106359894A (en) * | 2016-09-13 | 2017-02-01 | 贵州华清科维环境能源有限责任公司 | Method for preparing high-protein feed from distillers' grain |
Non-Patent Citations (3)
| Title |
|---|
| 张蜀艳: "丢糟中木聚糖的提取工艺优化", 《中国酿造》 * |
| 曹海等: "啤酒糟资源化利用技术的研究进展", 《啤酒科技》 * |
| 薛枫等: "双酶法降解细胞壁物质制备低聚木糖和阿魏酸研究进展", 《粮食与饲料工业》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107475467A (en) * | 2017-09-14 | 2017-12-15 | 齐鲁工业大学 | A kind of highly effective extraction method of poplar xylose |
| CN107475467B (en) * | 2017-09-14 | 2020-12-22 | 齐鲁工业大学 | Efficient extraction method of poplar xylose |
| CN109793260A (en) * | 2019-01-30 | 2019-05-24 | 四川中烟工业有限责任公司 | A kind of spirit distiller grain oil and its preparation method and application |
| CN109744367A (en) * | 2019-03-22 | 2019-05-14 | 东莞市澹一生物科技有限公司 | The method and feedstuff of resource utilization wheat vinasse production feedstuff |
| CN109744368A (en) * | 2019-03-22 | 2019-05-14 | 东莞市澹一生物科技有限公司 | Utilize the method and feedstuff of wheat vinasse production feedstuff |
| CN117903332A (en) * | 2024-01-11 | 2024-04-19 | 江西师范大学 | Distilled grain water-soluble arabinoxylan, preparation method thereof, pharmaceutical composition and application |
| CN117903332B (en) * | 2024-01-11 | 2024-09-03 | 江西师范大学 | Distilled grain water-soluble arabinoxylan, preparation method thereof, pharmaceutical composition and application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107136317B (en) | 2020-05-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107136317A (en) | It is a kind of to comprehensively utilize the method that vinasse prepare xylo-oligosaccharide and protein feed simultaneously | |
| Ma et al. | Combination of biological pretreatment with mild acid pretreatment for enzymatic hydrolysis and ethanol production from water hyacinth | |
| US8658407B2 (en) | Compositions and methods for conversion of lignocellulosic material to fermentable sugars and products produced therefrom | |
| CN102203271B (en) | For being the materials and methods of biofuel by Wood Adhesives from Biomass | |
| CN101815788B (en) | For producing the method based on cellulase of alcohol and glucose from pretreated lignocellulosic material | |
| US8372609B2 (en) | Process for producing a sugar solution by combined chemical and enzymatic saccharification of polysaccharide enriched biomass | |
| JP2008537886A (en) | Concentration of separate supply streams in biomass processing and utilization | |
| CN102304550B (en) | Method for producing ethanol or acetone and butanol by taking lignocellulose as raw material | |
| CN104256086A (en) | Technology for preparing docosahexaenoic acid (DHA)-rich feed additive by grain dreg raw material through fermentation | |
| CN108902446A (en) | A kind of high protein lees feeds and preparation method thereof | |
| CN107259101A (en) | A kind of method of camellia seed meal ferment making feed | |
| Efeovbokhan et al. | Production of bioethanol from hybrid cassava pulp and peel using microbial and acid hydrolysis | |
| CN105000981A (en) | Carbonized particle fermented organic fertilizer and preparation method therefor | |
| CN104073533A (en) | Method for preprocessing biomass through thermal hydrolysis with low energy consumption and device thereof | |
| CN103992901A (en) | Processing method for sweet-potato wine | |
| CA2745382A1 (en) | Methods of processing ensiled biomass | |
| CN101700096A (en) | Method for preparing feed by rapidly hydrolyzing vegetal biomass | |
| Sun et al. | Production of single cell protein from brewer’s spent grain through enzymatic saccharification and fermentation enhanced by ammoniation pretreatment | |
| CN107494928A (en) | A kind of method of composite bacteria solid state fermentation mushroom bran production protein feed | |
| CN104593449B (en) | A kind of method for improveing alkaline process preprocessing lignocellulose biolobic material | |
| US20140273134A1 (en) | Barley-Based Biorefinery Process | |
| Liu et al. | Enzymatic degradation of polysaccharides in Chinese vinegar residue to produce alcohol and xylose. | |
| CN105273908A (en) | Preparation method for liquor or feed with corn straw as accessory material | |
| Zabed et al. | Tailoring whole slurry bioprocessing for sugary stovers to augment sugar production by integrating soluble and insoluble carbohydrates | |
| CN111218490A (en) | Method for pretreating lignocellulose by using ammonia and auxiliary agent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |