CN106636480A - Preparation method of xylooligosaccharide by corn - Google Patents
Preparation method of xylooligosaccharide by corn Download PDFInfo
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- CN106636480A CN106636480A CN201611036161.1A CN201611036161A CN106636480A CN 106636480 A CN106636480 A CN 106636480A CN 201611036161 A CN201611036161 A CN 201611036161A CN 106636480 A CN106636480 A CN 106636480A
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- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K13/00—Sugars not otherwise provided for in this class
- C13K13/002—Xylose
Abstract
The invention discloses a preparation method of xylooligosaccharide by corn; the preparation method includes steps of A, selecting qualified corn core, and crushing the corn core; B, immersing the corn core acquired in step A in the water and adding acetic acid; C, cooking the mixed in step B under high pressure and acquiring hydrolysate; D, cooling the hydrolysate in step C; E, preserving and saccharifying the hydrolysate processed in step D; F, heating and sterilizing the saccharification liquid acquired in step E; G, cooling the saccharification liquid acquired in step F; H, extruding and dewatering the saccharification liquid acquired in step G; J, performing the first decolorizing treatment on the liquid acquired in step H; K, performing membrane filtering and film concentration treatment on the liquid acquired in step J; L, purifying the liquid acquired in step K; M, evaporating and condensing the liquid acquired in step L; N, performing chromatograph on the liquid acquired in step M, and acquiring xylooligosaccharide. The technical scheme of the invention can make the corn core fully saccharify and acquire massive xylooligosaccharide.
Description
Technical field
The present invention relates to a kind of method for making xylo-oligosaccharide, more particularly to a kind of corncob makes xylo-oligosaccharide
Method.
Background technology
Xylo-oligosaccharide has good physiology characteristic, the such as multiplication capacity of Bifidobacterium, not digested characteristic, pre- preventing decayed tooth
Tooth, promotes calcium uptake etc..It is a kind of a kind of important functional oligose for being widely used in human food and animal feed.
The preparation of xylo-oligosaccharide is mainly by the plant resources rich in xylan, such as corncob, cotton seed hulls, peanut shell, sugarcane
Slag and rice husk etc. are raw material, are obtained by methods such as sour water solution, thermophilic digestion or enzyme hydrolysis.As a large agricultural country, corn
It is one of China's Three major grain crops, with abundant corncob raw material resources.At present China to the utilization of corncob relatively
It is few, the low-level primary process segment is substantially at, the overwhelming majority is burned off as farmers''s fuel.With corncob as raw material, system
Standby functional low polyxylose, not only can comprehensively utilize agricultural resource, while can also increase farmers' income, reduce environment dirty
Dye, with good market prospects.
The content of the invention
To solve the above problems, the present invention provides a kind of method that corncob makes xylo-oligosaccharide.
In order to realize object above, the present invention is adopted the following technical scheme that：
A kind of method for making xylo-oligosaccharide with corncob, comprises the steps：
The qualified corncob of A, selection, carries out pulverization process and obtains material to corncob, the corncob after pulverization process
The particle diameter of grain is 0.05～0.5mm；
B, the corncob that step A is obtained is inserted in water and soaks and add acetic acid, wherein corncob is with the volume ratio of water
1:7～1:9, acetic acid is 3 with the weight ratio of the corncob：200～5:200, soak time is 15～25min；
C, the mixture for obtaining step B carry out autoclaving and obtain hydrolyzate, and boiling temperature is 110～135 DEG C, boiling
Pressure is 0.8～1 MPa, and the time of boiling is 2.5～3.5h；
D, the hydrolyzate for obtaining step C cooling, make temperature be down to 45～75 DEG C；
E, in the hydrolyzate that step D was processed zytase is added to carry out insulation saccharification, wherein zytase and step A
Described in corncob weight ratio be 3：1000～5:1000, saccharification temperature control at 40～55 DEG C, saccharificatinn period is 17～
21h；
F, the saccharified liquid obtained to step E heat up and sterilize, and sterilising temp is 75～90 DEG C, and sterilization time is 20～50min；
G, the saccharified liquid that step F is obtained is lowered the temperature, make temperature control at 45～55 DEG C；
H, the saccharified liquid obtained to step G carry out extrusion dehydration, and the moisture content of the corn wheat bran after extrusion dehydration is 50%
～70%；
I, the corn wheat bran for obtaining step H carry out dextrine conversion, and feed grade xylooligosaccharide product is generated after dextrine conversion
Product；
J, the step H liquid that obtains of extruding is carried out into first time desolventing technology；
K, the liquid for obtaining step J carry out successively membrane filtration and film concentration, the liquid Jing after membrane filtration and film concentration
In xylo-oligosaccharide concentration be about 8.2%～10.5%.
L, the liquid for obtaining step K are purified using the method for ion exchange.
M, the liquid that step L is obtained is evaporated into concentration；
N, the liquid for obtaining step M carry out chromatographic isolation and obtain xylo-oligosaccharide.
It is described with corncob make xylo-oligosaccharide method the step of N include：
N1, the liquid for obtaining step M carry out secondary decolourization；
N2, the liquid for obtaining step N1 carry out Two-step ion-exchanging and three secondary ions are exchanged；
N3, the liquid for obtaining step N2 carry out hyperfiltration treatment；
N4, the liquid for obtaining step N3 carry out double evaporation-cooling concentration；
N5, the liquid for obtaining step N4 carry out chromatographic isolation and obtain xylo-oligosaccharide.
The particle diameter of the corn cob granule in step A after pulverization process is 0.1～0.3mm.
Corncob and the volume ratio of water are 1 in step B:8, acetic acid is 1 with the weight ratio of the corncob:50, leaching
The bubble time is 20min.
Boiling temperature is 125 DEG C in step C, and cooking pressure is 0.9 MPa, and the time of boiling is 3h.
By circulating cooling pond cooling water solution liquid in step D, hydrolysis liquid temp is set to be down to 60 DEG C, then will hydrolysis
Liquid sends into saccharifying tank.
Step E is：Insulation saccharification, wherein zytase are carried out by zytase is added in the hydrolyzate in saccharifying tank
It is 4 with the weight ratio of corncob described in step A：1000, saccharification temperature is controlled at 45～55 DEG C, and saccharificatinn period is 20h.
Step F is：Saccharified liquid is heated up and is sterilized, sterilising temp is 80 DEG C, sterilization time is 30～40min；
Step G is：Saccharified liquid is lowered the temperature by circulating water pool, temperature control is made at 48～52 DEG C.
Step I includes：
I1, by step H to corn wheat bran deliver in reactor, be passed through steam, plus acetic acid, control temperature, pressure and
Time, carry out high-temperature high-voltage reaction；
I2, the material for obtaining step I1 carry out spraying quick-fried process；
Xylo-oligosaccharide specific enzyme is added in I3, the material for obtaining step I2, material fermentation is made；
I4, the material that step I3 is obtained is dried；
I5, the material that step I4 is obtained is crushed and packed.
Step H is：Extrusion dehydration is carried out to saccharified liquid using screw extruder, the corn wheat bran after extrusion dehydration
Moisture content is 65%, and the press filtration water direct reuse Jing after screw extruder is in saccharification system.
Step K is：The liquid that step J is obtained carries out successively membrane filtration and film concentration, Jing membrane filtrations and film
Xylo-oligosaccharide concentration after concentration in liquid is about 9.2%.
Reactor temperature is controlled in 125～300 degrees Celsius, Stress control at 0.8～1 MPa in step I1, when
Between at 1～2 hour, the weight of added acetic acid is 2% of corncob weight in step A.
The temperature of the step I3 material fermentation is 60-90 degree Celsius, and fermentation time is 8-12 hours.
Material moisture after step I4 is processed is 6%-9%.
Material mesh number after step I5 is processed is controlled in 55～65 mesh, particularly 60 mesh.
Step I5 also includes carrying out dust removal process to the material after crushing.
It is described spray it is quick-fried process be：It is quick to open reactor, make material flow out reactor rapidly；The original for spraying quick-fried process
Reason：Because the pressure very little in reactor so that material inside and outside pressure difference becomes big, causes material inner high voltage vapor also drastically swollen
It is swollen, opening instantaneously popping for reactor.
Technical scheme makes corncob be fully saccharified, and makes full use of corncob to obtain more substantial oligomeric wood
Sugar, meanwhile, the waste of generation can be recycled mostly, and pollutant and gurry are less, energy-conserving and environment-protective.
Specific embodiment
Embodiment 1
A kind of method for making xylo-oligosaccharide with corncob that the present embodiment is provided, comprises the steps：
The qualified corncob of A, selection, carries out pulverization process and obtains material to corncob, the corncob after pulverization process
The particle diameter of grain is 0.05mm；
B, the corncob that step A is obtained is inserted in water and soaks and add acetic acid, wherein corncob is with the volume ratio of water
1:7, acetic acid is 3 with the weight ratio of the corncob：200, soak time is 15min；
C, the mixture for obtaining step B carry out autoclaving and obtain hydrolyzate, and boiling temperature is 110 DEG C, cooking pressure
For 0.8 MPa, the time of boiling is 2.5h；
D, the hydrolyzate for obtaining step C cooling, make temperature be down to 45 DEG C；
E, in the hydrolyzate that step D was processed zytase is added to carry out insulation saccharification, wherein zytase and step A
Described in corncob weight ratio be 3：1000, saccharification temperature is controlled at 40 DEG C, and saccharificatinn period is 17h；
F, the saccharified liquid obtained to step E heat up and sterilize, and sterilising temp is 75 DEG C, and sterilization time is 20min；
G, the saccharified liquid that step F is obtained is lowered the temperature, make temperature control at 45 DEG C；
H, the saccharified liquid obtained to step G carry out extrusion dehydration, and the moisture content of the corn wheat bran after extrusion dehydration is 50%；
I, the corn wheat bran for obtaining step H carry out dextrine conversion, and feed grade xylooligosaccharide product is generated after dextrine conversion
Product；
J, the step H liquid that obtains of extruding is carried out into first time desolventing technology；
K, the liquid for obtaining step J carry out successively membrane filtration and film concentration, the liquid Jing after membrane filtration and film concentration
In xylo-oligosaccharide concentration be about 8.2%.
L, the liquid for obtaining step K are purified using the method for ion exchange.
M, the liquid that step L is obtained is evaporated into concentration；
N, the liquid for obtaining step M carry out chromatographic isolation and obtain xylo-oligosaccharide.
It is described with corncob make xylo-oligosaccharide method the step of N include：
N1, the liquid for obtaining step M carry out secondary decolourization；
N2, the liquid for obtaining step N1 carry out Two-step ion-exchanging and three secondary ions are exchanged；
N3, the liquid for obtaining step N2 carry out hyperfiltration treatment；
N4, the liquid for obtaining step N3 carry out double evaporation-cooling concentration；
N5, the liquid for obtaining step N4 carry out chromatographic isolation and obtain xylo-oligosaccharide.
By circulating cooling pond cooling water solution liquid in step D, then hydrolyzate is sent into into saccharifying tank.
Zytase will be added in the hydrolyzate in saccharifying tank to carry out insulation saccharification in step E.
Saccharified liquid is lowered the temperature by circulating water pool in step G.
Step I includes：
I1, by step H to corn wheat bran deliver in reactor, be passed through steam, plus acetic acid, control temperature, pressure and
Time, carry out high-temperature high-voltage reaction；
I2, the material for obtaining step I1 carry out spraying quick-fried process；
Xylo-oligosaccharide specific enzyme is added in I3, the material for obtaining step I2, material fermentation is made；
I4, the material that step I3 is obtained is dried；
I5, the material that step I4 is obtained is crushed and packed.
Extrusion dehydration is carried out to saccharified liquid using screw extruder in step H.
Reactor temperature control is in 125 degrees Celsius, Stress control at 0.8 MPa in step I1, and the time is little 1
When, the weight of added acetic acid is 2% of corncob weight in step A.
The temperature of the step I3 material fermentation is 60 degrees Celsius, and fermentation time is 8 hours.
Material moisture after step I4 is processed is 6%.
Material mesh number after step I5 is processed is controlled in 55 mesh.
Step I5 also includes carrying out dust removal process to the material after crushing.
Embodiment 2
A kind of method for making xylo-oligosaccharide with corncob that the present embodiment is provided, comprises the steps：
The qualified corncob of A, selection, carries out pulverization process and obtains material to corncob, the corncob after pulverization process
The particle diameter of grain is 0.1mm；
B, the corncob that step A is obtained is inserted in water and soaks and add acetic acid, wherein corncob is with the volume ratio of water
1:9, acetic acid is 5 with the weight ratio of the corncob:200, soak time is 25min；
C, the mixture for obtaining step B carry out autoclaving and obtain hydrolyzate, and boiling temperature is 135 DEG C, cooking pressure
For 1 MPa, the time of boiling is 3.5h；
D, the hydrolyzate for obtaining step C cooling, make temperature be down to 75 DEG C；
E, in the hydrolyzate that step D was processed zytase is added to carry out insulation saccharification, wherein zytase and step A
Described in corncob weight ratio be 5:1000, saccharification temperature is controlled at 55 DEG C, and saccharificatinn period is 21h；
F, the saccharified liquid obtained to step E heat up and sterilize, and sterilising temp is 90 DEG C, and sterilization time is 50min；
G, the saccharified liquid that step F is obtained is lowered the temperature, make temperature control at 55 DEG C；
H, the saccharified liquid obtained to step G carry out extrusion dehydration, and the moisture content of the corn wheat bran after extrusion dehydration is 70%；
I, the corn wheat bran for obtaining step H carry out dextrine conversion, and feed grade xylooligosaccharide product is generated after dextrine conversion
Product；
J, the step H liquid that obtains of extruding is carried out into first time desolventing technology；
K, the liquid for obtaining step J carry out successively membrane filtration and film concentration, the liquid Jing after membrane filtration and film concentration
In xylo-oligosaccharide concentration be about 10.5%.
L, the liquid for obtaining step K are purified using the method for ion exchange.
M, the liquid that step L is obtained is evaporated into concentration；
N, the liquid for obtaining step M carry out chromatographic isolation and obtain xylo-oligosaccharide.
It is described with corncob make xylo-oligosaccharide method the step of N include：
N1, the liquid for obtaining step M carry out secondary decolourization；
N2, the liquid for obtaining step N1 carry out Two-step ion-exchanging and three secondary ions are exchanged；
N3, the liquid for obtaining step N2 carry out hyperfiltration treatment；
N4, the liquid for obtaining step N3 carry out double evaporation-cooling concentration；
N5, the liquid for obtaining step N4 carry out chromatographic isolation and obtain xylo-oligosaccharide.
By circulating cooling pond cooling water solution liquid in step D, then hydrolyzate is sent into into saccharifying tank.
Zytase will be added in the hydrolyzate in saccharifying tank to carry out insulation saccharification in step E.
Saccharified liquid is lowered the temperature by circulating water pool in step G.
Step I includes：
I1, by step H to corn wheat bran deliver in reactor, be passed through steam, plus acetic acid, control temperature, pressure and
Time, carry out high-temperature high-voltage reaction；
I2, the material for obtaining step I1 carry out spraying quick-fried process；
Xylo-oligosaccharide specific enzyme is added in I3, the material for obtaining step I2, material fermentation is made；
I4, the material that step I3 is obtained is dried；
I5, the material that step I4 is obtained is crushed and packed.
Extrusion dehydration is carried out to saccharified liquid using screw extruder in step H, the press filtration water Jing after screw extruder
Direct reuse is in saccharification system.
In the step I1 reactor temperature control in 300 degrees Celsius, Stress control at 1 MPa, the time at 2 hours,
The weight of added acetic acid is 2% of corncob weight in step A.
The temperature of the step I3 material fermentation is 90 degrees Celsius, and fermentation time is 12 hours.
Material moisture after step I4 is processed is 9%.
Material mesh number after step I5 is processed is controlled in 65 mesh.
Step I5 also includes carrying out dust removal process to the material after crushing.
Embodiment 3
A kind of method for making xylo-oligosaccharide with corncob that the present embodiment is provided, comprises the steps：
The qualified corncob of A, selection, carries out pulverization process and obtains material to corncob, the corncob after pulverization process
The particle diameter of grain is 0.5mm；
B, the corncob that step A is obtained is inserted in water and soaks and add acetic acid, wherein corncob is with the volume ratio of water
1:8, acetic acid is 1 with the weight ratio of the corncob:50, soak time is 20min；
C, the mixture for obtaining step B carry out autoclaving and obtain hydrolyzate, and boiling temperature is 125 DEG C, cooking pressure
For 0.9 MPa, the time of boiling is 3h；
D, the hydrolyzate for obtaining step C cooling, make temperature be down to 60 DEG C；
E, in the hydrolyzate that step D was processed zytase is added to carry out insulation saccharification, wherein zytase and step A
Described in corncob weight ratio be 1:250, saccharification temperature is controlled at 50 DEG C, and saccharificatinn period is 20h；
F, the saccharified liquid obtained to step E heat up and sterilize, and sterilising temp is 80 DEG C, and sterilization time is 35min；
G, the saccharified liquid that step F is obtained is lowered the temperature, make temperature control at 50 DEG C；
H, the saccharified liquid obtained to step G carry out extrusion dehydration, and the moisture content of the corn wheat bran after extrusion dehydration is 65%；
I, the corn wheat bran for obtaining step H carry out dextrine conversion, and feed grade xylooligosaccharide product is generated after dextrine conversion
Product；
J, the step H liquid that obtains of extruding is carried out into first time desolventing technology；
K, the liquid for obtaining step J carry out successively membrane filtration and film concentration, the liquid Jing after membrane filtration and film concentration
In xylo-oligosaccharide concentration be about 9.2%.
L, the liquid for obtaining step K are purified using the method for ion exchange.
M, the liquid that step L is obtained is evaporated into concentration；
N, the liquid for obtaining step M carry out chromatographic isolation and obtain xylo-oligosaccharide.
It is described with corncob make xylo-oligosaccharide method the step of N include：
N1, the liquid for obtaining step M carry out secondary decolourization；
N2, the liquid for obtaining step N1 carry out Two-step ion-exchanging and three secondary ions are exchanged；
N3, the liquid for obtaining step N2 carry out hyperfiltration treatment；
N4, the liquid for obtaining step N3 carry out double evaporation-cooling concentration；
N5, the liquid for obtaining step N4 carry out chromatographic isolation and obtain xylo-oligosaccharide.
By circulating cooling pond cooling water solution liquid in step D, then hydrolyzate is sent into into saccharifying tank.
Zytase will be added in the hydrolyzate in saccharifying tank to carry out insulation saccharification in step E.
Step F is：Saccharified liquid is heated up and is sterilized, sterilising temp is 80 DEG C, sterilization time is 30～40min；
Saccharified liquid is lowered the temperature by circulating water pool in step G.
Step I includes：
I1, by step H to corn wheat bran deliver in reactor, be passed through steam, plus acetic acid, control temperature, pressure and
Time, carry out high-temperature high-voltage reaction；
I2, the material for obtaining step I1 carry out spraying quick-fried process；
Xylo-oligosaccharide specific enzyme is added in I3, the material for obtaining step I2, material fermentation is made；
I4, the material that step I3 is obtained is dried；
I5, the material that step I4 is obtained is crushed and packed.
Step H is：Extrusion dehydration is carried out to saccharified liquid using screw extruder, the corn wheat bran after extrusion dehydration
Moisture content is 65%, and the press filtration water direct reuse Jing after screw extruder is in saccharification system.
Step K is：The liquid that step J is obtained carries out successively membrane filtration and film concentration, Jing membrane filtrations and film
Xylo-oligosaccharide concentration after concentration in liquid is about 9.2%.
Reactor temperature control is in 200 degrees Celsius, Stress control at 0.9 MPa in step I1, and the time is little 1.5
When, the weight of added acetic acid is 2% of corncob weight in step A.
The temperature of the step I3 material fermentation is 75 degrees Celsius, and fermentation time is 10 hours.
Material moisture after step I4 is processed is 8%.
Material mesh number after step I5 is processed is controlled in 60 mesh.
Step I5 also includes carrying out dust removal process to the material after crushing.
Making in the method for xylo-oligosaccharide of corncob described in the technical program, corncob is by feed belt in step A
Deliver to corncob crushing system to be crushed.
Acetic acid in step B can disconnect on the lignocellulosic chain in corncob as catalyst.Step B is and sizes mixing,
The purpose sized mixing is in order to catalyst (acetic acid), water and corncob are stirred, without caking phenomenon, in order to improve next step
The efficiency of boiling.Water used is mainly the indirect steam condensed water of subsequent evaporation and concentration section in sizing mixing, and is sized mixing with reaching
The recycling of required temperature and water.
Step C be hydrolyzing process, hydrolyzing process is one of important workshop section of xylose production, be related to wood sugar quality and after
The key of sequence manufacturing procedure difficulty or ease.The workshop section is that the slurries that will be sized mixing are placed in autoclaving tank and carry out autoclaving.
Hydrolyzate after the completion of hydrolysis is cooled down by circulating cooling pond, and saccharifying tank is sent into after cooling.
Zytase carries out chain rupture by diastatic fermentation to polysaccharide more than 7 sugar, makes xylo-oligosaccharide more with 2 sugar to 7 sugar
Form occurs.
Corn wheat bran is feed grade xylooligosaccharide product Jing after adding the drying of zytase secondary fermentation.500 tons of production
2000 tons of feed grade xylooligosaccharide products (moisture content about 10%) can be produced while food-grade xylooligosaccharide product.
Bleaching process is the master operation of xylooligosaccharides production, and the pigment in liquid glucose has the natural colouring matter in raw material and giving birth to
The pigment generated in product, these pigments deepen the color and luster of liquid glucose, affect the quality of xylo-oligosaccharide product, it is necessary to decolourized
Process.The decolouring of xylo-oligosaccharide liquid glucose substantially belongs to adsorption bleaching, and adsorbent uses the larger powdery of porous, specific surface area
Activated carbon, pigment that not only can be in adsorption of hydrolyzation liquid using powdered activated carbon, and to the impurity in liquid glucose, colloid and albumen
Matter class material etc. also has stronger removal ability.Because colloidal substance present in xylo-oligosaccharide solution is more, xylo-oligosaccharide is molten
The viscosity of liquid itself is larger, when being decolourized must heating stirring make solution be decolourized again after being uniformly dispersed.By saccharified liquid
Filtered with filter press, sloughed sugar residue therein and waste active carbon, with filter cloth as medium, liquid is by filter cloth, and solid is useless
Thing is trapped within filter cloth.
Bleaching workshop section can produce a certain amount of steam condensate (SC), and condensed water collecting pit is back to workshop section of sizing mixing after collecting.
In solution after decolouring sugared dense relatively low (about 2.747% or so), main component has：Wood sugar, arabinose, wood
Disaccharides, xylotriose, the homologue of high polymerization degree and a small amount of inorganic salts etc..Membrane separation technique is exactly according to intermolecular radial dimension
Difference, using molecular level membrane treatment appts retain macromolecular, pass through hydrone.The Organic substance in water concentration that membrane filtration is produced
It is higher, enter Sewage Disposal and processed.Liquid glucose purity after Jing membrane filtrations is higher, is dense, the work that further improves its sugar
Skill designs Jing films concentration again, and the transmission water colorless of film concentration, COD value are low, and temperature is higher, and a portion is recyclable to be used for
Size mixing workshop section, another part is recycled to Purified Water Station recycling.Sugared concentration is about 9.2% Jing after membrane filtration and film concentration.
Xylo-oligosaccharide slurry purity after membrane filtration and film concentration than relatively low, and containing a small amount of pigment miscellaneous, ash
Part (gypsum etc.), sour, nitrogenous thing (protein, amino acid etc.), colloid etc., it is necessary to which xylo-oligosaccharide slurry is adopted into the side of ion exchange
Method is purified, to improve the quality of product.Xylo-oligosaccharide slurry, uniformly through ion exchange column, is used with certain speed and pressure
Cationic, anionic exchange resin is refined, and liquid glucose is flowed into from ion exchange column top, and per cube of exchanger resin can be exchanged about
15 cubes of liquid glucose.The purpose of ion exchange is further to improve liquid glucose purity, removes protein, the amino remained after decolourizing
Acid, coloring matter and ash grade.It is sun-male-female ion exchange that this technology primary ions exchange operation：
Cation exchange：Using strong acid positive resin the neutral salt in destainer is decomposed, exchanged, reduced neutral salt
Concentration in destainer.
Anion exchange：Liquid glucose contains a certain amount of acetate after decolouring, in solution.Anion exchange primarily to
The acetate in liquid glucose is removed, while adsorbable remove many colloidal impurities and pigment.
Cation exchange：Contain a small amount of deleterious cations, mainly iron, magnesium, calcium and cation ash in liquid glucose simultaneously.Sun
The purpose of ion exchange is exactly to remove ash and cation.
Resin regeneration is washed：Need to backwash resin after ion exchange, regenerate and drip washing, wherein positive resin is used
3% regeneration of hydrochloric acid, negative resin is regenerated with 3% NaOH.
It is sugared dense by being concentrated by evaporation further raising xylo-oligosaccharide content Jing after primary ions are exchanged, under being conducive to
The carrying out of one step ion-exchange process.This technology is evaporated concentration, part of heat energy to liquid glucose using triple effect used heat plate evaporation
Using the used heat of hydrolysis workshop section, the purpose of energy saving is reached, the content of xylo-oligosaccharide can be carried in the liquid glucose being concentrated by evaporation
It is high to 25.7% or so.
Be concentrated by evaporation workshop section can produce part evaporating waste water, the waste water can direct reuse in workshop section of sizing mixing.
After concentration and evaporation, moisture content is reduced in concentrated mother liquor, but ion concentration also increased, therefore female to concentration
Liquid carries out process again, and processing method is mainly secondary decolourization filtration, charcoal post and decolourizes and the exchange of two, three secondary ions.
Secondary decolourization：Decolorising agent is grain active carbon, after being decolourized using grain active carbon first with 3% caustic soda and
3% hydrochloric acid is regenerated.The workshop section can produce a certain amount of steam condensate (SC), and direct reuse is in workshop section of sizing mixing.
Two-step ion-exchanging：For male-female, negative resin mainly removes pigment, adsorbs a small amount of vinegar the exchange process for adopting
Acid group.Positive resin mainly swaps the cation in evaporation mother liquor, while adjusting pH, controls pH for 3～4.Three times from
Son is exchanged：The exchange process for adopting is sun-cloudy, positive resin mainly adjustment pH value, and the purpose of negative resin is that removing part is micro
Acetate.Mainly there are backwashing wastewater, regeneration and wastewater eluting in the workshop section.
Liquid glucose after ion exchange is further carried out ultrafiltration, primarily to remove liquid glucose in bacterium, virus,
The particulates such as colloid, macromolecular, to improve the purity of liquid glucose.
Double evaporation-cooling concentration is further to be concentrated the xylose solution after ion exchange, in order to the knot of next workshop section
Crystalline substance, double evaporation-cooling adopts MVR plate evaporation systems, the concentration of total reducing sugar in hydrolyzate can be brought up to into 40% or so.
The workshop section can produce part evaporating waste water, the waste water in addition to a small amount of lower boiling volatilizable organic acid, impurity
Less, heat is more, can direct reuse in workshop section of sizing mixing.
The concentrate after evaporation and concentration is separated by chromatographic separation technology, to isolate 95% Icing Sugar.According to this skill
Art is designed and Counseling Technique personnel, and the chromatographic separation technology used by this technology is thin layer chromatography method, using each component in chromatographic column
In migration rate difference come realize separate.
The chromatographic separation technology that this technology is adopted, it is oligomeric using 95% by the use of resin dedicated as fixing phase in chromatographic column
The difference of xylose powder and raffinate wood molasses to resin dedicated absorption affinity, wherein 95% xylo-oligosaccharide powder is than raffinate wood molasses
Resin dedicated absorption affinity is eager to excel, thus 95% xylo-oligosaccharide powder migration rate in the chromatography column is than raffinate wood molasses
It is little.Using the principle, due to migration velocity of 95% xylo-oligosaccharide powder with raffinate wood molasses in the chromatography column it is different, therefore
95% xylo-oligosaccharide powder and raffinate wood molasses are also different by the time of chromatographic column, and 95% xylo-oligosaccharide powder is by chromatographic column
Time is shorter, first separates out from discharging opening；Raffinate wood molasses is separated out within a period of time after the precipitation of 95% xylo-oligosaccharide powder, so as to
Complete the separation of 95% xylo-oligosaccharide powder and raffinate wood molasses.
Chromatographic isolation uses resin dedicated, needs in use for some time to backwash it, regenerated and drenched
Wash.
Technical scheme makes corncob be fully saccharified, and makes full use of corncob to obtain more substantial oligomeric wood
Sugar, meanwhile, the waste of generation can be recycled mostly, and pollutant and gurry are less, energy-conserving and environment-protective.
Claims (10)
1. it is a kind of with corncob make xylo-oligosaccharide method, it is characterised in that comprise the steps：
The qualified corncob of A, selection, to corncob pulverization process is carried out, and the particle diameter of the corn cob granule after pulverization process is
0.05～0.5mm；
B, the corncob that step A is obtained is inserted in water and soaks and add acetic acid, wherein corncob and the volume ratio of water are 1:7～
1:9, acetic acid is 3 with the weight ratio of the corncob：200～5:200, soak time is 15～25min；
C, the mixture for obtaining step B carry out autoclaving and obtain hydrolyzate, and boiling temperature is 110～135 DEG C, cooking pressure
For 0.8～1 MPa, the time of boiling is 2.5～3.5h；
D, the hydrolyzate for obtaining step C cooling, make temperature be down to 45～75 DEG C；
E, in the hydrolyzate that step D was processed zytase is added to carry out insulation saccharification, wherein zytase and institute in step A
The weight ratio for stating corncob is 3：1000～5:1000, at 40～55 DEG C, saccharificatinn period is 17～21h for saccharification temperature control；
F, the saccharified liquid obtained to step E heat up and sterilize, and sterilising temp is 75～90 DEG C, and sterilization time is 20～50min；
G, the saccharified liquid that step F is obtained is lowered the temperature, make temperature control at 45～55 DEG C；
H, the saccharified liquid obtained to step G carry out extrusion dehydration, and the moisture content of the corn wheat bran after extrusion dehydration is 50%～
70%；
I, the corn wheat bran for obtaining step H carry out dextrine conversion, and feed grade xylooligosaccharide product is generated after dextrine conversion；
J, the step H liquid that obtains of extruding is carried out into first time desolventing technology；
K, the liquid for obtaining step J carry out successively membrane filtration and film concentration, Jing after membrane filtration and film concentration in liquid
Xylo-oligosaccharide concentration is about 8.2%～10.5%；
L, the liquid for obtaining step K are purified using the method for ion exchange, that is, carry out primary ions exchange；
M, the liquid that step L is obtained is evaporated into concentration；
N, the liquid for obtaining step M carry out chromatographic isolation and obtain xylo-oligosaccharide.
2. it is according to claim 1 it is a kind of with corncob make xylo-oligosaccharide method, it is characterised in that：It is described to use corn
The step of core makes the method for xylo-oligosaccharide N includes：
N1, the liquid for obtaining step M carry out secondary decolourization；
N2, the liquid for obtaining step N1 carry out Two-step ion-exchanging and three secondary ions are exchanged；
N3, the liquid for obtaining step N2 carry out hyperfiltration treatment；
N4, the liquid for obtaining step N3 carry out double evaporation-cooling concentration；
N5, the liquid for obtaining step N4 carry out chromatographic isolation and obtain xylo-oligosaccharide.
3. it is according to claim 1 it is a kind of with corncob make xylo-oligosaccharide method, it is characterised in that：Step A
The particle diameter of the corn cob granule after middle pulverization process is 0.1～0.3mm.
4. it is according to claim 1 it is a kind of with corncob make xylo-oligosaccharide method, it is characterised in that：Step B
Middle corncob is 1 with the volume ratio of water:8, acetic acid is 1 with the weight ratio of the corncob:50, soak time is 20min.
5. it is according to claim 1 it is a kind of with corncob make xylo-oligosaccharide method, it is characterised in that：Step C
Middle boiling temperature is 125 DEG C, and cooking pressure is 0.9 MPa, and the time of boiling is 3h.
6. it is according to claim 1 it is a kind of with corncob make xylo-oligosaccharide method, it is characterised in that：Step D
In by circulating cooling pond cooling water solution liquid, make hydrolysis liquid temp be down to 60 DEG C, then hydrolyzate is sent into into saccharifying tank.
7. according to claim 1 or 6 it is a kind of with corncob make xylo-oligosaccharide method, it is characterised in that：The step
Suddenly E is：Zytase will be added in hydrolyzate in saccharifying tank to carry out insulation saccharification, wherein zytase with described in step A
The weight ratio of corncob is 4：1000, saccharification temperature is controlled at 45～55 DEG C, and saccharificatinn period is 20h.
8. it is according to claim 1 it is a kind of with corncob make xylo-oligosaccharide method, it is characterised in that：Step F
For：Saccharified liquid is heated up and is sterilized, sterilising temp is 80 DEG C, sterilization time is 30～40min；Step G is：It is logical to saccharified liquid
Cross circulating water pool to be lowered the temperature, make temperature control at 48～52 DEG C.
9. it is according to claim 1 it is a kind of with corncob make xylo-oligosaccharide method, it is characterised in that：Step I includes：
I1, by step H to corn wheat bran deliver in reactor, be passed through steam, plus acetic acid, control temperature, pressure and time,
Carry out high-temperature high-voltage reaction；
I2, the material for obtaining step I1 carry out spraying quick-fried process；
Xylo-oligosaccharide specific enzyme is added in I3, the material for obtaining step I2, material fermentation is made；
I4, the material that step I3 is obtained is dried；
I5, the material that step I4 is obtained is crushed and packed.
10. it is according to claim 1 it is a kind of with corncob make xylo-oligosaccharide method, it is characterised in that：Step H
For：Extrusion dehydration is carried out to saccharified liquid using screw extruder, the moisture content of the corn wheat bran after extrusion dehydration is 65%, Jing spiral shells
Press filtration water direct reuse after rotation extruder is in saccharification system.
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| CN111647694A (en) * | 2020-07-14 | 2020-09-11 | 焦作市华康糖醇科技有限公司 | Method for extracting xylose from corncobs |
| CN113088582A (en) * | 2021-04-15 | 2021-07-09 | 南京林业大学 | Method for preparing xylo-oligosaccharide by two-step lactic acid catalytic hydrolysis |
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