CN105463040A - Method for raising yield of xylooligosaccharide - Google Patents
Method for raising yield of xylooligosaccharide Download PDFInfo
- Publication number
- CN105463040A CN105463040A CN201610022194.4A CN201610022194A CN105463040A CN 105463040 A CN105463040 A CN 105463040A CN 201610022194 A CN201610022194 A CN 201610022194A CN 105463040 A CN105463040 A CN 105463040A
- Authority
- CN
- China
- Prior art keywords
- solid
- xylan
- oligosaccharide
- conducting
- xylo
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- 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
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/12—Disaccharides
Landscapes
- Organic Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Zoology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Microbiology (AREA)
- General Chemical & Material Sciences (AREA)
- Biotechnology (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention discloses a method for raising the yield of xylooligosaccharide and belongs to the fields of chemical engineering and food. The method comprises of treating corn straw as the raw material, firstly, sequentially conducting air drying and pulverization, conducting soaking treatment with water and ethyl alcohol for removing water soluble impurities and fat soluble impurities in the raw material, and then conducting lignin removal treatment through a sodium chlorite method; secondly, obtaining a xylan extracting solution through an alkaline extraction method, and after pH is adjusted to be neutral, conducting concentration for removing salt; finally, conducting depolymerization treatment on xylan through an enzymolysis method and an acidolysis method in sequence, and conducting centrifugation, activated carbon treatment and freeze-drying, so that a xylooligosaccharide product is obtained. The method has the following advantages that xylan liquid obtained through the method is subjected to a hydrolysis reaction, and the complex separating and drying steps in the preparation process are omitted; enzymolysis residues are subjected to acetic acid treatment at the high temperature, the yield of the xylooligosaccharide can be raised, and no excessive influence can be caused to the acidic and basic property of the product; the straw is utilized as the raw material, so that good economic benefits and ecological significance are achieved.
Description
Technical field
The present invention relates to a kind of method improving xylo-oligosaccharide productive rate, belong to chemical industry, food technology field.
Background technology
At present, be that the method for hydrolysis of xylo-oligosaccharide is mainly divided into enzymatic hydrolysis, Acid hydrolysis, from hydrolysis, chemical enzymolysis four kinds by hemicellulose degradation, wherein enzymatic hydrolysis is by feat of the reaction conditions of its gentleness and low stain, becomes the main stream approach preparing xylo-oligosaccharide.But the productive rate that current single enzyme process or Acid hydrolysis produce xylo-oligosaccharide is general not high, and major cause has: enzyme deactivation; In substrate, part xylan is connected with xylogen and closely cannot carries out enzymolysis; Enzyme and sugared binding site deficiency etc. in reaction process.Acid system degraded is comparatively thorough, but without scission of link specificity.Thus, a kind of if can find enzymolysis, acidolysis are organically combined and reach the method for higher xylo-oligosaccharide productive rate, industrial output being had to the meaning of essence.In addition, alcohol precipitating method is used to be separated obtained xylan in tradition leaching process, although this method can reach the content reducing residual lignin in xylan, but because ethanol exists obvious restraining effect to follow-up enzymolysis, therefore still need to use the modes such as drying to be removed by ethanol on separation basis, and follow-up hydrolytic process is all carried out in liquid state, thus this flow process is too loaded down with trivial details.If sloughed by xylogen at pretreatment stage, do not use alcohol precipitating method, and each processing step all completes in liquid situation, not only makes zytase in enzymolysis process more easily contact with xylan, and can significantly improve whole technique can be handling.
China Agricultural University discloses " preparation method of xylo-oligosaccharide " (application number 01131171.1), with all kinds of corn cob for raw material, under acidulous catalyst effect, direct pyrolysis is carried out after alkali metal hydroxide pre-treatment, enzyme process is used to carry out the preparation of xylo-oligosaccharide subsequently, final refining obtains high-purity oligoxylose product, but this invention productive rate is lower, and does not process further hydrolytic residue, causes the waste of part hemicellulose components.The people such as Li Xiufang disclose " utilizing biological straw to prepare the method for xylo-oligosaccharide, dissolving pulp and bio-fuel-oil ", residual Production With Residue of Enzymatic Hydrolysis after enzymolysis is carried out slurrying, washing screening, delignification, pre-treatment, bleaching prepared a series of process such as dissolving pulp, thus Production With Residue of Enzymatic Hydrolysis is utilized, this invented technology flow process is complicated, and energy consumption is larger.If Production With Residue of Enzymatic Hydrolysis to be carried out further degraded sugaring, not only flow process is simple, and agrees with mutually with integrated artistic flow process, directly can improve xylo-oligosaccharide productive rate and be about 6%-10%.
Summary of the invention
The invention provides a kind of method improving xylo-oligosaccharide productive rate, by the following technical solutions:
A raw material prepares: the air-dry rear use pulverizer of stalk is pulverized, to below particle diameter 2mm;
B Feedstock treating: above-mentioned corn stalk powder is put into thermally resistant container, boiling water is used to soak 1-3h, solid-liquid separation gets filter residue, reuse 75-95% (v/v) alcohol immersion 1-3h, to remove water-soluble in corn stalk raw material and oil-soluble impurities, filter residue is got by after mixture solid-liquid separation after process, at 40-80 DEG C, be dried to solid content be greater than 90%, 6% (w/v) Textone is added subsequently with 1:10-15 (w/v) solid-to-liquid ratio, and after using 8%-12% (w/v) vinegar acid for adjusting pH to 3.6-3.8, at 75 DEG C, process 2-4h;
Prepared by c xylan: by stalk after above-mentioned process, uses 8-15% (w/v) NaOH solution, with 1:5-10 (w/v) for solid-to-liquid ratio, processes 0.5-2h, get filtrate after solid-liquid separation at 90-160 DEG C;
After filtrate uses dense HCl to regulate pH to 6-8 by d, desalination after concentrated, obtains xylan extraction liquid;
E enzymic hydrolysis: above-mentioned xylan solid is dissolved in deionized water with 1.5-2.5% (w/v) concentration of substrate, the commercial xylanase preparation of 1% (w/w) is added by substrate weight, hydrolysis temperature 45-55 DEG C, enzymolysis 4-24h under agitation condition;
F acid treatment: by enzymolysis solution solid-liquor separation, is formulated as 1-2% (w/v) mixture as acid treatment substrate using Production With Residue of Enzymatic Hydrolysis, use 0.8-1.2% (v/v) acetic acid to react 60-120min at 140-160 DEG C;
G purifying: the acid hydrolysis solution of the enzymolysis solution of step e and f step is merged, pH regulator to 4.0, use 4% (w/v) charcoal absorption, then 15%, 30%, 60% ethanol of 1 times of volume is adopted to carry out wash-out successively, and concentrating under reduced pressure, obtain xylo-oligosaccharide liquid, after freeze-drying, namely obtain xylo-oligosaccharide product.
Compared with prior art, tool has the following advantages in the present invention:
1. the present invention is prepared into xylan liquid and is hydrolyzed reaction, eliminates separation loaded down with trivial details in preparation process and drying step, is more conducive to the unity of preparation flow;
2. under adopting high temperature, acetic acid process enzymolysis residue can improve xylo-oligosaccharide productive rate, can't cause too much impact, and the reduction of molecular weight of product is beneficial to its solubility property on product acid alkalescence, and in minimizing hydrolytic process, solid residue is residual;
3. complete removal that is water-soluble in stalk and oil-soluble impurities at pretreatment stage, and the removing of xylogen to a certain extent, reduce the impact being unfavorable for sequential hydrolysis empirical factor, and reduce xylan colour, be conducive to subsequent product purifying;
4. utilize agricultural wastes straw as raw material, there is good economic benefit and ecological significance;
Embodiment
Enzyme used herein is endo-xylanase; Xylo-oligosaccharide (xylo-bioses ~ wood six sugar) content is recorded by high performance liquid chromatography (HPLC); Xylo-oligosaccharide productive rate is for benchmark gained with hemicellulose level in raw material xylan.
Below by embodiment, the present invention will be further described, but do not limit its content.
Embodiment 1
Raw material prepares: the air-dry rear use high speed runner milling of maize straw is pulverized, to below particle diameter 2mm; Feedstock treating: above-mentioned corn stalk powder is put into thermally resistant container, boiling water is used to soak 2h, solid-liquid separation gets filter residue, reuse 80% alcohol immersion 2h, to remove water-soluble in corn stalk raw material and oil-soluble impurities, filter residue is got by after mixture solid-liquid separation after process, at 60 DEG C, be dried to solid content be greater than 90%, 6% (w/v) Textone is added subsequently with 1:10 (w/v) solid-to-liquid ratio, and after using 10% (w/v) HAc to regulate pH to 3.6-3.8, at 75 DEG C, process 4h; Prepared by xylan: by maize straw after above-mentioned process, uses 10% (w/v) NaOH solution, with 1:10 (w/v) for solid-to-liquid ratio, processes 2h, get filtrate after solid-liquid separation at 105 DEG C; After filtrate being used dense HCl to regulate pH to 6-8, desalination after concentrated, obtains xylan extraction liquid; Enzymic hydrolysis: above-mentioned xylan solid is dissolved in deionized water with 2% (w/v) concentration of substrate, adds the commercial xylanase preparation of 1% (w/w) by substrate weight, hydrolysis temperature 50 DEG C, enzymolysis 18h under agitation condition; Acid treatment: after enzymolysis solution solid-liquid separation, Production With Residue of Enzymatic Hydrolysis is formulated as 1% (w/v) mixture as acid treatment substrate, uses 1% (v/v) acetic acid to react 60min at 160 DEG C; Purifying: enzymolysis solution and acid hydrolysis solution are merged, pH regulator to 4.0, use 4% (w/v) charcoal absorption, then 15%, 30%, 60% ethanol of 1 times of volume is adopted to carry out wash-out successively, and concentrating under reduced pressure, obtain xylo-oligosaccharide liquid, after freeze-drying, namely obtain xylo-oligosaccharide product.
And sampling after each one-step hydrolysis completes, centrifugal, cross film use the oligosaccharides in efficient liquid phase chromatographic analysis hydrolyzed solution and monosaccharide concentration.After measured, enzymolysis process xylo-oligosaccharide productive rate is 42.6%, and acid hemolysis process xylo-oligosaccharide productive rate is 7.5%, and xylo-oligosaccharide overall yield reaches 50.1%.
Embodiment 2
In this example, xylan preparation, enzymolysis, purification step and correlation parameter are identical with embodiment 1, and in subsequent step, acidolysis uses 0.8% (v/v) acetic acid to react 60min at 140 DEG C.
After measured, under this condition, acid hemolysis process xylo-oligosaccharide productive rate is 6.4%, and xylo-oligosaccharide overall yield reaches 49%, and monose overall yield reaches 11.2% in addition, and namely total sugar yield is 60.2%.
Embodiment 3
In this example, xylan preparation, enzymolysis, purification step and correlation parameter are identical with embodiment 1, and in subsequent step, acidolysis uses 1% (v/v) acetic acid to react 120min at 160 DEG C.
After measured, under this condition, acid hemolysis process xylo-oligosaccharide productive rate is 9.7%, and xylo-oligosaccharide overall yield reaches 52.3%, and monose overall yield reaches 14.6% in addition, and namely total sugar yield is 66.9%.
Claims (2)
1. improve a method for xylo-oligosaccharide productive rate, it is characterized in that comprising following processing step:
A raw material prepares: the air-dry rear use pulverizer of stalk is pulverized, to below particle diameter 2mm;
B Feedstock treating: above-mentioned corn stalk powder is put into thermally resistant container, boiling water is used to soak 1-3h, solid-liquid separation gets filter residue, reuse 75-95% (v/v) alcohol immersion 1-3h, to remove water-soluble in corn stalk raw material and oil-soluble impurities, filter residue is got by after mixture solid-liquid separation after process, at 40-80 DEG C, be dried to solid content be greater than 90%, 6% (w/v) Textone is added subsequently with 1:10-15 (w/v) solid-to-liquid ratio, and after using 8%-12% (w/v) vinegar acid for adjusting pH to 3.6-3.8, at 75 DEG C, process 2-4h;
Prepared by c xylan: by stalk after above-mentioned process, uses 8-15% (w/v) NaOH solution, with 1:5-10 (w/v) for solid-to-liquid ratio, processes 0.5-2h, get filtrate after solid-liquid separation at 90-160 DEG C;
After filtrate uses dense HCl to regulate pH to 6-8 by d, desalination after concentrated, obtains xylan extraction liquid;
E enzymic hydrolysis: above-mentioned xylan solid is dissolved in deionized water with 1.5-2.5% (w/v) concentration of substrate, the commercial xylanase preparation of 1% (w/w) is added by substrate weight, hydrolysis temperature 45-55 DEG C, enzymolysis 4-24h under agitation condition;
F acid treatment: by enzymolysis solution solid-liquor separation, is formulated as 1-2% (w/v) mixture as acid treatment substrate using Production With Residue of Enzymatic Hydrolysis, use 0.8-1.2% (v/v) acetic acid to react 60-120min at 140-160 DEG C;
G purifying: the acid hydrolysis solution of the enzymolysis solution of step e and f step is merged, pH regulator to 4.0, use 4% (w/v) charcoal absorption, then 15%, 30%, 60% ethanol of 1 times of volume is adopted to carry out wash-out successively, and concentrating under reduced pressure, obtain xylo-oligosaccharide liquid, after freeze-drying, namely obtain xylo-oligosaccharide product.
2. a kind of method improving xylo-oligosaccharide productive rate as claimed in claim 1, is characterized in that described stalk refers to maize straw, wheat stalk, rice straw, broomcorn straw, sunflower stalk.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610022194.4A CN105463040A (en) | 2016-01-13 | 2016-01-13 | Method for raising yield of xylooligosaccharide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610022194.4A CN105463040A (en) | 2016-01-13 | 2016-01-13 | Method for raising yield of xylooligosaccharide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105463040A true CN105463040A (en) | 2016-04-06 |
Family
ID=55601196
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610022194.4A Pending CN105463040A (en) | 2016-01-13 | 2016-01-13 | Method for raising yield of xylooligosaccharide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105463040A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106399425A (en) * | 2016-10-08 | 2017-02-15 | 中国科学院过程工程研究所 | Method using activated carbon absorption and ethanol desorption to synchronously produce different-quality xylooligosaccharide |
| CN107226872A (en) * | 2017-06-09 | 2017-10-03 | 安徽赛澳生物工程有限公司 | A kind of method that utilization biological fermentation process processing stalk obtains high-purity xylan |
| CN109385455A (en) * | 2018-12-06 | 2019-02-26 | 齐鲁工业大学 | A kind of application of wheat stalk hemicellulose |
| CN114350723A (en) * | 2021-12-27 | 2022-04-15 | 海南拉风农业科技有限公司 | Method for preparing xylooligosaccharide by using black corncobs |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1403591A (en) * | 2001-09-05 | 2003-03-19 | 中国农业大学 | Prepn of oligoxylose |
| CN101003823A (en) * | 2006-12-30 | 2007-07-25 | 江南大学 | Method for preparing oligo xylose in high purity by using stalk as raw material, and using technique of enzyme and membrane |
| 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 |
| CN102559804A (en) * | 2010-12-16 | 2012-07-11 | 苏州工业园区尚融科技有限公司 | Method for preparing high-purity XOS by adopting straw and rice husk |
| CN102965454A (en) * | 2012-11-23 | 2013-03-13 | 北京林业大学 | Microwave-assisted xylo-oligosaccharide preparation method |
| CN104164520A (en) * | 2014-07-15 | 2014-11-26 | 南京林业大学 | Method using acetic acid for controlled catalysis of orientational hydrolysis of xylan to prepare multicomponent xylooligosaccharide |
-
2016
- 2016-01-13 CN CN201610022194.4A patent/CN105463040A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1403591A (en) * | 2001-09-05 | 2003-03-19 | 中国农业大学 | Prepn of oligoxylose |
| CN101003823A (en) * | 2006-12-30 | 2007-07-25 | 江南大学 | Method for preparing oligo xylose in high purity by using stalk as raw material, and using technique of enzyme and membrane |
| 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 |
| CN102559804A (en) * | 2010-12-16 | 2012-07-11 | 苏州工业园区尚融科技有限公司 | Method for preparing high-purity XOS by adopting straw and rice husk |
| CN102965454A (en) * | 2012-11-23 | 2013-03-13 | 北京林业大学 | Microwave-assisted xylo-oligosaccharide preparation method |
| CN104164520A (en) * | 2014-07-15 | 2014-11-26 | 南京林业大学 | Method using acetic acid for controlled catalysis of orientational hydrolysis of xylan to prepare multicomponent xylooligosaccharide |
Non-Patent Citations (1)
| Title |
|---|
| 孙军涛等: "玉米芯生产低聚木糖脱色工艺研究", 《粮油食品科技》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106399425A (en) * | 2016-10-08 | 2017-02-15 | 中国科学院过程工程研究所 | Method using activated carbon absorption and ethanol desorption to synchronously produce different-quality xylooligosaccharide |
| CN107226872A (en) * | 2017-06-09 | 2017-10-03 | 安徽赛澳生物工程有限公司 | A kind of method that utilization biological fermentation process processing stalk obtains high-purity xylan |
| CN107226872B (en) * | 2017-06-09 | 2019-08-27 | 安徽赛澳生物工程有限公司 | A method of high-purity xylan is obtained using biological fermentation process processing stalk |
| CN109385455A (en) * | 2018-12-06 | 2019-02-26 | 齐鲁工业大学 | A kind of application of wheat stalk hemicellulose |
| CN114350723A (en) * | 2021-12-27 | 2022-04-15 | 海南拉风农业科技有限公司 | Method for preparing xylooligosaccharide by using black corncobs |
| CN114350723B (en) * | 2021-12-27 | 2024-03-26 | 海南拉风农业科技有限公司 | Method for preparing xylo-oligosaccharide by using black corncob |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US8618280B2 (en) | Biorefinery process for extraction, separation, and recovery of fermentable saccharides, other useful compounds, and yield of improved lignocellulosic material from plant biomass | |
| JP4330839B2 (en) | Method for producing glucose and / or water-soluble cellooligosaccharide | |
| CN102585030B (en) | Method for extracting beta-glucan by using cereal | |
| CN101555293B (en) | Method for extracting beta- glucosans from bran of corn | |
| CN108411044B (en) | Ultrasonic-assisted purification method for xylose in eucalyptus hot water prehydrolysis liquid | |
| CN104757564B (en) | A kind of method utilizing Pericarppium arachidis hypogaeae to prepare dietary fiber | |
| CN105463040A (en) | Method for raising yield of xylooligosaccharide | |
| CN101838343A (en) | Method for preparing pectin by using waste sisal dregs | |
| CN107266609B (en) | Method for extracting pomegranate peel residue pectin by electrolytic water | |
| CN101851300A (en) | Process for extracting chondroitin sulfate | |
| CN105754015A (en) | Method for extracting chitin from oyster shell | |
| CN102492054B (en) | Preparation method of soybean episperm pectin gel polysaccharide | |
| CN103130904A (en) | High-valued utilization method for patinopecten yessoensis offal | |
| CN101628922B (en) | Oligosaccharide ferulic acid ester preparation method | |
| CN102532334B (en) | Method for producing flaxseed mucilage | |
| CN112175111B (en) | Method for efficiently separating wood fiber material to obtain high-purity components | |
| CN104387484A (en) | Method for extracting rapeseed polysaccharide from rape seed cake by bioenzyme process | |
| CN102925516A (en) | Xylo-oligosaccharide preparation method | |
| CN115466335B (en) | Process for extracting polysaccharide from wheat bran | |
| RU2422044C1 (en) | Method for production of pectin and food fibres of pumpkin cake | |
| CN104830927B (en) | A kind of method that forulic acid oligosaccharide syrup is prepared using wheat bran | |
| CN106883315A (en) | A kind of method that pectin is extracted from kiwifruit peel | |
| CN106883314A (en) | A kind of method that pectin is extracted in the slag from lemon peel | |
| CN108252143B (en) | Method for extracting plant salt and cellulose from suaeda salsa | |
| CN105483184A (en) | Production method of high-yield xylooligosaccharide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160406 |