CN106399425A - Method using activated carbon absorption and ethanol desorption to synchronously produce different-quality xylooligosaccharide - Google Patents
Method using activated carbon absorption and ethanol desorption to synchronously produce different-quality xylooligosaccharide Download PDFInfo
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- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
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Abstract
The invention discloses a preparation method of xylooligosaccharide. The preparation method includes: soaking crushed corn straw with water and ethanol respectively to remove water-soluble and lipid-soluble non-structure components in the straw; using a sodium chlorite acid solution to remove the lignin of the degreased straw, and then using an alkali solution to perform extraction so as to obtain crude xylan liquid; removing part of salt of the crude xylan liquid, then performing enzymolysis, removing the residues of enzymatic hydrolysate, using activated carbon to perform absorption, using ethanol of different concentration gradients to perform step-by-step elution, and subjecting each eluent to freeze drying to obtain the xylooligosaccharide. The method has the advantages the different-quality xylooligosaccharide is produced synchronously by the simple-flow and low-cost method, and the method is good in industrial production potential.
Description
Technical field
The invention belongs to chemical industry, food technology field, particularly to a kind of system of oligomeric xylose food and feed additive
Preparation Method.
Background technology
Corn straw, as domestic most representational lignocellulosic material, develops its process and utilization technology meaning deep
Far.Meanwhile, as important composition composition in corn straw, its gross reserves in nature is only second to fiber to hemicellulose
Element, is the second in the world big class hydridization polysaccharide.Based on complicated and diversified architectural characteristic and its physiological active functionses that have so that
Hemicellulose has huge research and value.And the oligomeric wood as one of the most important conversion product of hemicellulose
Sugar, except the general specially good effect with functional oligose, such as efficient selective is bred bacillus bifiduss, the absorption promoting calcium, is reduced blood
Sugared content, dental caries etc., it is few also to have an effective dose, the peculiar property such as acid, heat stability are good.
In xylooligosaccharides production technique, the features such as activated carbon is due to its high adsorption, safety non-toxic, it is widely used in sugar
Loss of thick fluid color, the enterprise much manufacturing refined sugar both at home and abroad adopts activated carbon to process sugar liquid.China Agricultural University discloses " oligomeric xylose
Preparation method " (application number 01131171.1), the method with corn cob as raw material, through alkali hydroxide soln pretreatment
Afterwards, under weak-type catalyst action using directly-heated steaming and decocting cracking by the way of dissolution xylan, through enzymolysis gained oligomeric xylose molten
Liquid adopts decolorization activated carbon powder, finally high-purity oligoxylose product is obtained, but this method oligomeric xylose yield is relatively low, thus relatively
Economic benefit is low.Shandong Longli Biology Science and Technology Co., Ltd discloses " a kind of isolation and purification method of components for xylose oligomer "
(application number 200910017913.3), the method is adsorbed to oligomeric xylose liquid with activated-charcoal column, subsequently adopts 0-45% (v/
V) ethanol of concentration eluting step by step, each collection liquid is freeze-dried respectively to obtain high-purity 1,4-.beta.-Xylobiose-wood seven sugar, but the method behaviour
Cycle of making is longer, and ethanol maximum concentration is 45%, and high polymerization degree oligomeric xylose eluting does not thoroughly cause product yield relatively low.Overseas Chinese
Li Xialan of university et al. discloses " method that in wheat groove, ferulic acid and oligomeric xylose isolate and purify " (application number
201210331544.7), the method, by the wheat grain insoluble matter enzymolysis after Ethanol Treatment, subsequently adopts activated carbon adsorption, uses
Eluting obtains oligomeric xylose to the ethanol of 0-45% (v/v) concentration step by step, and the NaOH solution eluting of 2% (v/v) obtains ferulic acid, the method
Realize the oligomeric xylose in separated in synchronization wheat grain and ferulic acid, but experimental period is longer, equally exists high polymerization degree oligomeric xylose
The not thorough relatively low problem of yield of eluting, does not fully take into account the ethanol elution gained oligomeric xylose product of variable concentrations gradient simultaneously
Matter is different.
Content of the invention
It is contemplated that using variable concentrations graded ethanol step by step eluting synchronous production difference quality oligomeric xylose, provide
A kind of be suitable for, easy xylooligosaccharides production technique.Advantage of the invention is that feedstuff is met with easy technique synchronous production
The oligomeric xylose of the different qualities of additive and food additive quality standard；This technique productions cost is relatively low, Relative economy
Preferably, there is good commercial Application potential quality.
For achieving the above object, the present invention employs the following technical solutions：
(1) air-dry, pulverize after corn stalk powder soak through water and ethanol respectively, to remove water solublity and fat-soluble non-knot
Constitute and divide, subsequently adopt sodium chlorite acid solution to remove lignin, obtain holocellulose.Water soluble polysaccharide, starch and inorganic
The presence of the water-soluble macromolecules such as thing significantly increases the viscosity of sugar liquid, reduces solid-liquid separation speed；And waxiness in liposoluble substance
The presence of layer can make lignocellulose have hydrophobicity, hinders enzyme molecule contact hemicellulose surface；Phospholipid in lipoid exists
Facile hydrolysiss under heating or acid-base environment, form foam and emulsion, and the presence of pigment then can make the color and luster of xylan liquid add
Deep.Based on this, pretreatment need to be carried out to raw material, to reduce the impurity content in product and to reduce product colour.Lignocellulose
In raw material, hemicellulose is closely connected with covalent bond with lignin, in order to promote the dissolution of hemicellulose, using sodium chlorite acid
Property solution removal lignin.
(2) holocellulose is obtained thick xylan liquid with NaOH solution extracting.In numerous hemicellulose extracting method, alkali
Method extract can obtain extraction process degraded less, the degree of polymerization is higher, the higher hemicellulose of the accessibility of enzyme in hydrolytic process.
Conventional aqueous slkali has KOH, NaOH, due to Na+Aquation cation compared with K+Aquation cation big, therefore NaOH is to hemicellulose
Extracting ability is better than KOH.
(3) thick xylan liquid is digested using alkalescent xylanase after partial deionization, obtains oligomeric xylose enzymolysis solution, enzymolysis
Liquid adjusts pH to 4, and after standing, solid-liquor separation removes Production With Residue of Enzymatic Hydrolysis.Metal ion in salinity is often inhibitor or the promotion of enzyme
Agent, and each metal ion species have different action effects for different conditions, different types of enzyme.Suitable salt content pair
There is certain activation in xylanase, but the most suitable salt concentration is then relevant with xylanase species.Experimental result and literary composition
Offer analysis display xylan salinity contained by it need not be removed completely before enzymolysis, the salinity retaining debita spissitudo is on the contrary to wood
The enzymolysis of polysaccharide has certain facilitation.In this method, the salinity of 5-10mg/mL exists, and can be obviously promoted alkalescent xylanase
Activity.By enzymolysis solution pH regulator to 4.0, standing a period of time, residual lignin dissolution, sucking filtration removes the enzymes such as insoluble lignin
Solution slag.
(4) add 2%-4% (w/v) wooden powder activated carbon in the enzymolysis solution that removes slag, and wooden of 0-2% (w/v)
Grain activated carbon, initial pH 4-6, adsorbs 30-60min under 40-70 DEG C of stirring condition.Research finds the granularity of activated carbon to sugar liquid
Middle oligosaccharide adsorption rate and follow-up sucking filtration speed all have a significant impact.Powdered active carbon absorption property is better than granulated activated
Charcoal, with the minimizing of granularity of activated carbon, oligosaccharide adsorption rate is in rising trend, but the thing followed is exactly follow-up sucking filtration and ethanol
The speed issue of eluting.Through repeatedly optimizing, find the wooden powder's activity the use of 2%-4% (w/v) mesh number being 200-270 mesh
Charcoal, and the mesh number of 0-2% (w/v) be 5-10 mesh wood substance grain activated carbon, by powder different for granule size and seed activity
Charcoal mixes by a certain percentage, not only ensured preferably absorption property while but also preferable sucking filtration speed can be obtained.Investigate simultaneously and live
Property charcoal consumption, adsorption temp, the impact to adsorption effect of activated carbon in water of adsorption time and initial pH.
(5) after adsorption reaction terminates, in adsorption liquid, add 1%-3% (w/v) kieselguhr, filter, solid-liquid separation, make activity
Charcoal filter cake quality is in 0.3-0.6g/cm2, treat lower step eluting.For improving sucking filtration speed further, solve xylooligosaccharides production process
The slow-footed problem of middle activated carbon sucking filtration, this research, while adding filter aid diatomite, has probed into activated carbon filter cake thick again
The impact to sucking filtration speed for the degree.Expect to find a suitable filter cake thickness it is ensured that while sucking filtration effect, further speeding up and take out
Filtering velocity degree, shortens experimental period.Research finds that when filter cake amounts of activated carbon be 0.3-0.6g/cm2When, there is good sucking filtration effect
Really, both ensured that filtrate clarification no leaked charcoal phenomenon, had good sucking filtration speed concurrently.
(6) multiple ranks are used, ethanol water from low to high carries out step eluting to concentration successively, and first order ethanol is dense
Spend for 0-10% (v/v), afterbody concentration of alcohol is 70% (v/v), centre carries out eluting using 1-4 level, and concentration is in 0-
Increase successively between 70% (v/v), eluent, respectively through concentrating under reduced pressure, obtains oligomeric xylose product after lyophilization.Research finds,
The ethanol of variable concentrations can be with the oligomeric xylose of eluting different polymerization degree, and when oligomeric xylose molecular weight is higher, its degree of polymerization is got over
Greatly, the higher ethanol of concentration is needed could to elute it from activated carbon surface.This method uses 3-6 level concentration successively by low
Carry out step eluting, the oligomeric xylose of synchronous production difference quality to high ethanol water.High according to the quality of oligomeric xylose
Low make different purposes, front 1-2 level eluting gained oligomeric xylose purity is low, can be used as feed additive, rear 3-6 level eluting institute
Obtain oligomeric xylose purity more than 95%, can be used as functional food ingredient.
The invention has the characteristics that and advantage：
(1) wooden powder's activated carbon and wood substance grain activated carbon are mixed in proportion, and have both ensured that absorption property further carries
Adsorption conditionses are optimized simultaneously, significantly improve oligosaccharide adsorption rate in sugar liquid, and then improve oligomeric wood by high follow-up sucking filtration speed
Candy output；
(2) variable concentrations graded ethanol eluting step by step, the oligomeric xylose of synchronous production difference quality are adopted；
(3) this technique productions cost is relatively low, and preferably, flow process is simple and practical simultaneously for Relative economy, has good
Commercial Application potential quality.
Brief description
Fig. 1 xylooligosaccharides production technique
1, corn straw；2, holocellulose；3, enzymolysis solution；4, destaining solution；5, activated carbon；6, one-level eluent；7, one-level
Activity eluted charcoal；8, two grades of eluents；9, two grades of activity eluted charcoals；10, the activity eluted charcoal of Pyatyi；11, six grades of eluents；12,
Six grades of activity eluted charcoals；13, oligomeric xylose.
A, pretreatment (water extraction, alcohol extraction, delignification)；B, enzymolysis；C, activated carbon adsorption；D, one-level ethanol elution；E, two
Level ethanol elution；F, six grades of ethanol elutions；G, lyophilization.
Each composition quality fraction in Fig. 2 oligomeric xylose
The oligosaccharide response rate in Fig. 3 oligomeric xylose
Specific embodiment
Below by embodiment, the present invention will be further described.
Embodiment
Corn straw is pulverized with high speed mill after air-drying, and collection cut size is standby in the powder of straw of below 2mm；Will
100g powder of straw presses solid-to-liquid ratio 1 with deionized water:8 (g/mL) mixes, hot-water extraction 2h at 80 DEG C, and often changes after an hour
Deionized water, to remove the water solublity non-structural composition in straw, obtains the insoluble straw of water；Again by insoluble for water straw with
Solid-to-liquid ratio 1 pressed by the ethanol of 95% (w/v):5 (g/mL) mixes, and extracts 2h at 60 DEG C, and every ethanol of replacing after an hour,
To remove the fat-soluble non-structural composition in straw, obtain defat straw；By above-mentioned defat straw and 6% (w/v) sodium chlorite
Solution presses solid-to-liquid ratio 7.5:100 (g/mL) mixes, and sodium chlorite solution, with second acid for adjusting pH to 3.6-3.8, locates at 75 DEG C
2h is to remove the lignin in straw for reason, obtains holocellulose；Holocellulose is being consolidated with the NaOH solution of mass fraction 10%
Liquor ratio 1:10 (g/mL), extract 2h under the conditions of 90 DEG C, reaction terminates rear sucking filtration and makes solid-liquid separation, filtering residue be washed with deionized to
Dry cellulose after neutrality, the concentrated hydrochloric acid of the extracting solution (filtrate+cleaning mixture) after merging adjusts pH to 5.0 and thick xylan is obtained
Liquid；The film dialysis desalination that thick xylan liquid is 1000 using molecular cut off；Xylan liquid after desalination adjusts concentration to 2%
(w/v), salinity is 8mg/ml, using 1% (w/w) alkalescent xylanase in pH 8.0, temperature 50 C, digests under stirring condition
4h obtains enzymolysis solution；Enzymolysis solution adjusts pH to 4.0, and after standing a period of time, sucking filtration removes Production With Residue of Enzymatic Hydrolysis, adds 2.5% in enzymolysis solution
(w/v) after the wood activated charcoal powder of 200 mesh and 1% (m/v) mesh number are the wood activated charcoal granular absorption of 5 mesh, in initial pH
30min is adsorbed under 4,60 DEG C of stirring conditions.It is subsequently adding the kieselguhr of 2% (m/v), sucking filtration.During sucking filtration, according to funnel filtering surface
Long-pending, calculate the volume of enzymolysis solution, make filter cake quality be 0.3g/cm2.Using equal-volume concentration be respectively 10%, 30%, 50%,
70% (v/v) ethanol eluting step by step, eluent, respectively through concentrating under reduced pressure, obtains oligomeric xylose product after lyophilization.
Gained oligomeric xylose product measures its monosaccharide and oligomeric xylose content through high performance liquid chromatograph.As shown in Fig. 2
In the oligomeric xylose solid that 10% ethanol elution obtains, salt content is 30.59%, illustrates to use low-concentration ethanol activity eluted at first
During charcoal, salinity enters in eluent together with low polymerization degree oligosaccharide, and subsequent concentration of alcohol raises, the salt content eluting
Reduce, oligosaccharide purity raises.From Fig. 3 it is apparent that the 1,4-.beta.-Xylobiose being eluted and the xylotriose overwhelming majority are by 10%
With 30% ethanol elution.Meanwhile, in the oligomeric xylose that 30% ethanol elution obtains based on wooden pentasaccharides and wooden six sugar, and 50% second
In the oligomeric xylose that alcohol affords, main inclusion wood six sugar and wood seven are sugared, illustrate that different concentration ethanol eluting oligomeric xylose is polymerized
Degree is different, and molecular weight is higher, and the degree of polymerization is higher, needs high concentration ethanol eluting.Oligomeric using 10% and 30% ethanol elution
Xylose meets the quality standard of feedstuff oligomeric xylose after testing, and the oligomeric xylose final products of 50% and 70% ethanol elution
Meet the quality standard of food additive.
Claims (6)
1. a kind of activated carbon adsorption ethanol desorption synchronous production difference quality oligomeric xylose method it is characterised in that include with
Lower production craft step：
(1) corn stalk powder after pulverizing soaks through water and ethanol respectively, removes water solublity and fat-soluble non-structural composition, subsequently
Lignin is removed using sodium chlorite acid solution, obtains holocellulose；
(2) holocellulose aqueous slkali is extracted to obtain thick xylan extraction liquid, thick xylan extraction liquid uses after partial deionization
Alkalescent xylanase digests to obtain enzymolysis solution, and enzymolysis solution adjusts pH to 4, and after standing a period of time, sucking filtration removes Production With Residue of Enzymatic Hydrolysis；
(3) add wooden powder's activated carbon in the enzymolysis solution that removes slag and wood substance grain activated carbon is adsorbed, after the completion of absorption, add
Plus kieselguhr solid-liquor separation obtains activated carbon filter cake；
(4) using the ethanol solution activity eluted carbon filtration cake step by step being gradually increased concentration, eluent, respectively through concentrating under reduced pressure, is dried
Afterwards, synchronously obtain the oligomeric xylose product of different stage.
2. the side of a kind of activated carbon adsorption ethanol desorption synchronous production difference quality oligomeric xylose as claimed in claim 1
Method is it is characterised in that described activated carbon dosage is the wooden powder's activated carbon and 0- that 2%-4% (m/v) mesh number is 200-270
2% (m/v) mesh number is the wood substance grain activated carbon of 5-10, and it is 0.03-0.04g/mL that activated carbon amounts to addition, and adsorption time is
30-60min, adsorption temp is 40-70 DEG C.
3. the side of a kind of activated carbon adsorption ethanol desorption synchronous production difference quality oligomeric xylose as claimed in claim 1
Method is it is characterised in that described kieselguhr addition is 1%-3% (m/v).
4. the side of a kind of activated carbon adsorption ethanol desorption synchronous production difference quality oligomeric xylose as claimed in claim 1
Method is it is characterised in that described activated carbon filter cake quality is 0.3-0.6g/cm2.
5. the side of a kind of activated carbon adsorption ethanol desorption synchronous production difference quality oligomeric xylose as claimed in claim 1
It is characterised in that described ethanol solution first order concentration is 0-10% (v/v), afterbody concentration is 70% (v/v) to method, in
Between for 1-4 level concentration be 0%-70% (v/v) ethanol, common 3-6 level.
6. the side of a kind of activated carbon adsorption ethanol desorption synchronous production difference quality oligomeric xylose as claimed in claim 1
Method is it is characterised in that the oligomeric xylose of described different stage refers to meet the oligomeric of feed additive and food additive standard
Xylose.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109680020A (en) * | 2019-01-07 | 2019-04-26 | 中国科学院过程工程研究所 | A kind of method that synchronous realization the lignocellulosic high enzymatic hydrolyzation and high material utilization rate of detoxification technology is exempted from utilization |
| CN114984664A (en) * | 2022-06-09 | 2022-09-02 | 成都长力元生物科技有限公司 | Method for filtering viscous konjac flour enzymatic hydrolysate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101781669A (en) * | 2010-03-22 | 2010-07-21 | 苏州工业园区尚融科技有限公司 | Method for preparing high-purity xylo-oligosaccharide by adopting straws |
| CN105463040A (en) * | 2016-01-13 | 2016-04-06 | 中国科学院过程工程研究所 | Method for raising yield of xylooligosaccharide |
| CN105483184A (en) * | 2016-01-07 | 2016-04-13 | 中国科学院过程工程研究所 | Production method of high-yield xylooligosaccharide |
-
2016
- 2016-10-08 CN CN201610878650.5A patent/CN106399425A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781669A (en) * | 2010-03-22 | 2010-07-21 | 苏州工业园区尚融科技有限公司 | Method for preparing high-purity xylo-oligosaccharide by adopting straws |
| CN105483184A (en) * | 2016-01-07 | 2016-04-13 | 中国科学院过程工程研究所 | Production method of high-yield xylooligosaccharide |
| CN105463040A (en) * | 2016-01-13 | 2016-04-06 | 中国科学院过程工程研究所 | Method for raising yield of xylooligosaccharide |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109680020A (en) * | 2019-01-07 | 2019-04-26 | 中国科学院过程工程研究所 | A kind of method that synchronous realization the lignocellulosic high enzymatic hydrolyzation and high material utilization rate of detoxification technology is exempted from utilization |
| CN114984664A (en) * | 2022-06-09 | 2022-09-02 | 成都长力元生物科技有限公司 | Method for filtering viscous konjac flour enzymatic hydrolysate |
| CN114984664B (en) * | 2022-06-09 | 2023-12-15 | 成都长力元生物科技有限公司 | Method for filtering viscous konjaku flour enzymatic hydrolysate |
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Application publication date: 20170215 |