CN105483184A - Production method of high-yield xylooligosaccharide - Google Patents
Production method of high-yield xylooligosaccharide Download PDFInfo
- Publication number
- CN105483184A CN105483184A CN201610009343.3A CN201610009343A CN105483184A CN 105483184 A CN105483184 A CN 105483184A CN 201610009343 A CN201610009343 A CN 201610009343A CN 105483184 A CN105483184 A CN 105483184A
- Authority
- CN
- China
- Prior art keywords
- solid
- xylan
- oligosaccharide
- xylooligosaccharide
- 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
-
- 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
- C12P2201/00—Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
Abstract
The invention discloses a production method of high-yield xylooligosaccharide, and belongs to the field of chemical engineering and food. The method includes the steps of firstly, conducting air-drying, smashing, and water and ethyl alcohol soaking with corn straw as the raw material so as to remove water-soluble and fat-soluble impurities in the corn straw; secondly, obtaining xylan through an alkaline extraction and alcohol precipitation method; thirdly, conducting depolymerization on xylan through an enzymolysis and acidolysis combined method to achieve the high xylooligosaccharide yield, and then conducting centrifuging, activated carbon decoloring and freeze-drying to obtain the xylooligosaccharide product. The method has the advantages that the xylooligosaccharide yield can be remarkably improved through the enzymolysis and acidolysis combined method, and the average molecular weight of the product is low; the xylan raw material structure is more thoroughly broken, and the catalytic hydrolysis upper limit is higher; the agricultural waste corn straw serves as the production raw material, no specific straw parts are particularly required, and good economic benefits and ecological meaning are achieved.
Description
Technical field
The present invention relates to a kind of production method of high yield xylo-oligosaccharide, belong to chemical industry, food technology field.
Background technology
Hemicellulose is the class carbohydrate in plant fiber material, and it is one of renewable resources abundant, the most cheap on the earth, is only second to Mierocrystalline cellulose.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, enzyme amount are not enough; In substrate, part xylan is connected with xylogen and closely cannot carries out enzymolysis etc.; In reaction process enzyme and sugared binding site not enough, react kinetic energy deficiency etc.And for enzyme process and Acid hydrolysis, enzyme process has relatively mild condition but power and undercapacity, acid system has stronger response intensity 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.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 relatively economical benefit is lower.
Summary of the invention
The invention provides a kind of production method of high yield xylo-oligosaccharide, the method adopting enzyme process and acid system to combine makes xylo-oligosaccharide yield significantly promote, and acidity used is strong simultaneously, can not destructive enzyme solution environment, thus directly again can carry out enzymolysis processing, with lasting raising productive rate.
For achieving the above object, the present invention is by the following technical solutions:
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 1-3h, solid-liquid separation gets filter residue, reuse 75-95% alcohol immersion 1-3h, to remove water-soluble in corn stalk raw material and oil-soluble impurities, get filter residue by after mixture solid-liquid separation after process, at 40-80 DEG C, be dried to solid content be greater than 90%; Prepared by xylan: by maize straw after above-mentioned process, uses 8-15% (w/v) NaOH solution, with 1:5-10 (w/v) for solid-to-liquid ratio, at 90-160 DEG C, processes 0.5-2h, get filtrate and be xylan extraction liquid after solid-liquid separation; After using dense HCl to regulate pH to 5-7, concentrated, add ethanol and make the alcohol concn of system be 50-75% (v/v), get filter residue after solid-liquid separation after leaving standstill 1-3h, 40-80 DEG C of drying, obtains solid xylan; 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 45-50 DEG C, enzymolysis 4-24h under agitation condition; Acid treatment: after above-mentioned enzymolysis solution without solid-liquid separation directly as acid treatment substrate, use 0.7-1% (v/v) acetic acid at 150-160 DEG C, react 60-120min; Secondary enzymic hydrolysis: be consistent with enzymatic hydrolysis condition first, the reaction times is 1-4h; Purifying: by product pH regulator to 4.0, uses 4% (w/v) charcoal absorption, then adopts 15%, 30%, 60% ethanol of 1 times of volume 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 inventive method can significantly improve xylo-oligosaccharide productive rate, and the molecular-weight average of product is lower, it is oligomeric to be more partial to;
2. pair xylan raw material mix interrupt more thorough, namely the catalytic hydrolysis upper limit is higher, thus gives larger space to the lifting of technique;
3. the present invention all can have the effect of reduction to product colour at pretreatment stage and acidolysis stage, refines advantageously follow-up;
4. acidity used is strong, can not destructive enzyme solution environment, directly again can carry out enzymolysis processing, with lasting raising productive rate;
5. utilize agricultural wastes maize straw as raw materials for production, and the concrete stalk position of not careful requirement, the stalk that agriculture can be given up directly pulverize air-dry after be for further processing, 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
Prepared by xylan: corn stalk powder is put into reactor after pulverizing by the air-dry rear use high speed runner milling of maize straw, boiling water is used to soak 2h, 95% alcohol immersion 2h is reused after removing waste water, thus water-soluble and oil-soluble impurities in removing corn stalk raw material, solid drying to solid content is 95% by mixture solid-liquid separation after processing.Maize straw after above-mentioned process, uses 10% (w/v) NaOH, with 1:10 (w/v) for solid-to-liquid ratio, at 121 DEG C, processes 2h, obtains xylan extraction liquid after solid-liquid separation; After using dense HCl to regulate pH to 5, concentrated, add ethanol and make system alcohol concn be 60% (v/v), solid-liquid separation after leaving standstill 2h also by filter residue, obtains xylan.Enzymic hydrolysis: be dissolved in deionized water with 2% (w/v) concentration of substrate by above-mentioned xylan solid, adds 1% (w/w) with substrate weight and adds commercial xylanase preparation, stirs enzymolysis 24h in a kettle., temperature control 50 DEG C.Acid hydrolysis: add 1% (v/v) acetic acid after above-mentioned enzymolysis completes in reactor, reaction 60min, temperature control 160 DEG C.Secondary enzymolysis: after above-mentioned acidolysis completes and temperature is returned and fallen, carries out enzyme digestion reaction, reaction 1h with enzymatic hydrolysis condition first again.Purifying: by product pH regulator to 4.0, uses 4% (w/v) charcoal absorption, then adopts 15%, 30%, 60% ethanol of 1 times of volume 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 6.7%, secondary enzymolysis process xylo-oligosaccharide productive rate is 13.4%, xylo-oligosaccharide overall yield reaches 62.7%, and monose overall yield reaches 26.3% in addition, and namely total sugar yield is 89.1%.
Embodiment 2
In this example, xylan preparation, enzymolysis, secondary 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 150 DEG C.
After measured, under this condition, acid hemolysis process xylo-oligosaccharide productive rate is 8.5%, and secondary enzymolysis process xylo-oligosaccharide productive rate is 11.1%, and xylo-oligosaccharide overall yield reaches 62.2%, and monose overall yield reaches 28.6% in addition, and namely total sugar yield is 90.8%.
Embodiment 3
In this example, xylan preparation, enzymolysis, acidolysis, purification step and correlation parameter are identical with embodiment 1, and in subsequent step, the secondary enzymolysis reaction times is 4h.
After measured, under this condition, secondary enzymolysis process xylo-oligosaccharide productive rate is 15.7%, and xylo-oligosaccharide overall yield reaches 65.0%, and monose overall yield reaches 26.1% in addition, and namely total sugar yield is 91.1%.
Claims (1)
1. a production method for high yield xylo-oligosaccharide, is characterized in that comprising following processing step: 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 1-3h, solid-liquid separation gets filter residue, reuse 75-95% alcohol immersion 1-3h, to remove water-soluble in corn stalk raw material and oil-soluble impurities, get filter residue by after mixture solid-liquid separation after process, at 40-80 DEG C, be dried to solid content be greater than 90%; Prepared by xylan: by maize straw after above-mentioned process, uses 8-15% (w/v) NaOH solution, with 1:5-10 (w/v) for solid-to-liquid ratio, at 90-160 DEG C, processes 0.5-2h, get filtrate and be xylan extraction liquid after solid-liquid separation; After using dense HCl to regulate pH to 5-7, concentrated, add ethanol and make the alcohol concn of system be 50-75% (v/v), get filter residue after solid-liquid separation after leaving standstill 1-3h, 40-80 DEG C of drying, obtains solid xylan; 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 45-50 DEG C, enzymolysis 4-24h under agitation condition; Acid treatment: after above-mentioned enzymolysis solution without solid-liquid separation directly as acid treatment substrate, use 0.7-1% (v/v) acetic acid at 150-160 DEG C, react 60-120min; Secondary enzymic hydrolysis: be consistent with enzymatic hydrolysis condition first, the reaction times is 1-4h; Purifying: by product pH regulator to 4.0, uses 4% (w/v) charcoal absorption, then adopts 15%, 30%, 60% ethanol of 1 times of volume to carry out wash-out successively, and concentrating under reduced pressure, obtain xylo-oligosaccharide liquid, after freeze-drying, namely obtain xylo-oligosaccharide product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610009343.3A CN105483184A (en) | 2016-01-07 | 2016-01-07 | Production method of high-yield xylooligosaccharide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610009343.3A CN105483184A (en) | 2016-01-07 | 2016-01-07 | Production method of high-yield xylooligosaccharide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105483184A true CN105483184A (en) | 2016-04-13 |
Family
ID=55670455
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610009343.3A Pending CN105483184A (en) | 2016-01-07 | 2016-01-07 | Production method of high-yield xylooligosaccharide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105483184A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106367449A (en) * | 2016-08-26 | 2017-02-01 | 唐山三友集团兴达化纤有限公司 | Method for preparing feed-grade xylooligosaccharide from waste liquid generated in a production process of viscose staple fibers |
| 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 |
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
- 2016-01-07 CN CN201610009343.3A patent/CN105483184A/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 (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106367449A (en) * | 2016-08-26 | 2017-02-01 | 唐山三友集团兴达化纤有限公司 | Method for preparing feed-grade xylooligosaccharide from waste liquid generated in a production process of viscose staple fibers |
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101285106B (en) | Process for preparing multicomponent liquid glucose and lignose while effectively hydrolyzing lignocellulosic biomass | |
| CN102153763B (en) | Lignocellulose acid/alkali coupling pretreatment method | |
| CN104223125B (en) | A kind of method preparing potato residues dietary fiber | |
| JP5322150B2 (en) | Method for saccharification of biomass containing cellulose | |
| US20110129886A1 (en) | Biorefinery Process for Extraction, Separation, and Recovery of Fermentable Saccharides, other Useful Compounds, and Yield of Improved Lignocellulosic Material from Plant Biomass | |
| JP7149332B2 (en) | Method for producing cellulose, low-dispersion hemicellulose and lignin-dissociated polyphenols from fibrous biomass | |
| CN104086667A (en) | Method for preparing pectin from citrus fruit peel residues by employing ultrasonic-assisted extraction | |
| MX2011001387A (en) | Process for the production of sugars from biomass. | |
| Tayeh et al. | Subcritical hydrothermal pretreatment of olive mill solid waste for biofuel production | |
| CN106702802B (en) | A kind of method that ionic liquid-sulfamic acid binary system extracts high pure cellulose from stalk | |
| CN102644210A (en) | Method for pretreating biomass through microwave coupling high boiling alcohol | |
| CN101628922B (en) | Oligosaccharide ferulic acid ester preparation method | |
| CN108117652B (en) | Extraction method of enzymatic hydrolysis lignin | |
| CN105463040A (en) | Method for raising yield of xylooligosaccharide | |
| CN104762419A (en) | Method for preparing xylooligosaccharide from corncobs through microwave-assisted hydrothermal treatment | |
| CN112321652B (en) | Method for efficiently separating high-quality lignin from biomass | |
| CN105483184A (en) | Production method of high-yield xylooligosaccharide | |
| CN106755198B (en) | Method for producing sugar by hydrolyzing agricultural and forestry biomass raw material thick mash | |
| CA2866826C (en) | Process for the production of organic compounds from plant species | |
| JP5861413B2 (en) | Continuous production method of furfural from biomass | |
| CN104928341A (en) | Preparation method for ferulic acid combining ultrasonic-assisted enzymolysis and microbial-fermented bran | |
| KR101216829B1 (en) | Method of manufacturing glucose comprising multistage process | |
| CN104403013A (en) | Bio-enzyme method for extracting rapeseed polysaccharide from rapeseed cake meal | |
| CN103880976A (en) | Microwave-assisted extraction method of beet pectin | |
| JP2014090707A (en) | Method for enzymatic saccharification of biomass containing lignocellulose and method of producing ethanol with biomass containing lignocellulose |
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 |
Application publication date: 20160413 |
|
| WD01 | Invention patent application deemed withdrawn after publication |