CN112458133B - Method for preparing xylo-oligosaccharide from corn bran - Google Patents
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Abstract
The invention discloses a method for preparing xylo-oligosaccharide from corn bran, which comprises the steps of adding acetic acid and water into the corn bran to be stirred and mixed into suspension, adjusting the pH value to 4.5-5.5, conveying the suspension into a pressurizing ejector by a pump, passing the suspension through a laminar flow tank, rapidly releasing pressure by a gas-liquid separator, recycling secondary steam for heating subsequent materials, conveying liquid into a saccharifying tank, cooling, and then adding xylanase and saccharifying enzyme, wherein the light transmittance of saccharified feed liquid is =3%, the conductivity is low (< 3000 mu s/cm), the solid content is 3-5%, the purity of xylo-oligosaccharide is more than 70%, the product quality is improved, the sewage amount is greatly reduced, the waste heat of gas-liquid separation is convenient to recycle, and the energy consumption is reduced.
Description
Technical Field
The invention belongs to the technical field of biochemical engineering, and particularly relates to a method for preparing xylo-oligosaccharide from corn bran.
Background
Xylo-oligosaccharide is also called xylo-oligosaccharide, and is a functional polysaccharide formed by combining 2-7 xylose molecules by beta-1,4 glycosidic bonds. Compared with the commonly used soybean oligosaccharide, fructo-oligosaccharide, isomaltose hypgather and the like, the bifidobacterium propagation activity in intestinal tracts can be selectively promoted. The bifidus factor function is 10-20 times of other polymeric saccharides.
The preparation method of xylo-oligosaccharide generally comprises the following steps:
1. firstly, cooking the raw material containing xylan at high temperature, and then further performing enzymolysis on the raw material to obtain xylo-oligosaccharide;
2. hydrolyzing the raw material directly by steam, water or dilute inorganic acid to generate xylo-oligosaccharide.
The raw materials for producing xylo-oligosaccharide in the industry at present are corncob powder, rice hulls or wood hemicellulose and other agricultural and forestry wastes. The production process of xylo-oligosaccharide in the industry is that corncob powder is pretreated by acid, then is subjected to intermittent high-pressure cooking, and finally is subjected to enzymolysis to obtain the xylo-oligosaccharide.
In the prior art, the problems are that: the corn cob powder is cooked intermittently, waste heat steam is not easy to recover, an evaporator is used for material concentration, steam consumption is high, acid and alkali consumption is high due to multiple enzymolysis purification, decoloring cost is high, and sewage discharge is large; the saccharified feed liquid has low light transmittance (less than 1 percent), high conductivity (more than 5000 mu s/cm) and low solid content (less than 3 percent), and the purity of the produced xylo-oligosaccharide can only reach about 70 percent to the maximum extent.
Disclosure of Invention
Aiming at the situation, in order to overcome the defects of the prior art, the invention provides a method for preparing xylo-oligosaccharide from corn husks.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for preparing xylo-oligosaccharide from corn bran comprises the following steps:
(1) Mixing corn bran with water according to the mass ratio of 1:8-10, adding acid to adjust the pH value to 4.5-5.5, then heating to 80-90 ℃, and stirring and mixing uniformly to form a suspension of the corn bran;
(2) Conveying the suspension of the corn husks to a pressurizing ejector, allowing the suspension to enter a laminar flow tank through the ejector, allowing the materials to stay in the laminar flow tank for 50-70min, and finally allowing the suspension to enter a gas-liquid separator for gas-liquid separation; recovering waste heat of the flash evaporated secondary steam of the gas-liquid separator;
(3) The liquid after vapor-liquid separation enters a saccharification tank, the temperature is controlled at 50 +/-1 ℃, and the concentration is 1m 3 Adding 0.05-0.1kg of xylanase and 0.05-0.1kg of saccharifying enzyme into the materials, and carrying out enzymolysis for 10 hours;
(4) After enzymolysis, detecting the purity of the xylo-oligosaccharide, then heating to 80-90 ℃ to inactivate enzyme, keeping the temperature of inactivating enzyme for 30-40min, and filtering;
(5) Adding activated carbon into the filtrate for decolorization and filtration treatment, wherein the light transmittance is more than 20%;
(6) The filtrate after decolorization passes through a cation exchange column, calcium and magnesium are controlled to be zero, and then ultrafiltration is carried out, wherein the discharge light transmittance is more than 40%.
(7) Concentrating the ultrafiltered filtrate with membrane to obtain filtrate with refractive index higher than 18%;
(8) The waste heat recovered in the step (2) is used for concentrating the material obtained in the step (7), and the discharge refractive index is more than 30%;
(9) Decolorizing the concentrated material obtained in the step (8) again, wherein the light transmittance after decolorization and filtration is more than 50%;
(10) Performing ion exchange on the material subjected to secondary decolorization in the step (9), wherein the conductivity after the ion exchange is less than 20 mu s/cm, the pH value is 4-7, and the light transmittance is more than 95%; respectively regenerating the cation exchange column and the anion exchange column by using hydrochloric acid and liquid alkali, wherein the mass concentrations of the hydrochloric acid and the liquid alkali are 3-4%, leaching by using reverse osmosis pure water, and the conductivity of the reverse osmosis pure water is less than 30 mu s/cm;
(11) And (4) carrying out secondary concentration on the sugar solution subjected to ion exchange in the step (10), and filling a finished product of the concentrated material.
Furthermore, in the step (7), a nanofiltration membrane is adopted during membrane concentration.
Further, in the step (2), after the suspension of the corn husks enters the pressure increasing ejector, a steam valve of the pressure increasing ejector is opened at the same time, the materials are heated by steam, the pressure is 0.6-0.7MPa, and the temperature of the materials is kept at 160-170 ℃. In the laminar flow tank, the steam pressure is also kept at 0.6-0.7MPa, and the material temperature is kept at 160-170 ℃.
Further, in the step (1), acetic acid is added to adjust the pH.
The invention has the beneficial effects that:
(1) According to the invention, corn bran is adopted as a raw material, acetic acid and water are added firstly and stirred to form a suspension, the pH value is adjusted to 4.5-5.5, then the suspension is conveyed into a pressurizing ejector by a pump, then the suspension passes through a laminar flow tank, pressure is rapidly released through a gas-liquid separator, secondary steam is recycled for heating subsequent materials, liquid enters a saccharification tank, xylanase and saccharifying enzyme are added after the liquid is cooled, the light transmittance of saccharified feed liquid is more than =3%, the conductivity is low (less than 3000 mu s/cm), the solid content is 3-5%, the purity of xylo-oligosaccharide is more than 70%, the product quality is improved, the sewage quantity is greatly reduced, the waste heat of gas-liquid separation is convenient to recycle, and the energy consumption is reduced.
(2) The invention expands the raw materials for preparing the xylo-oligosaccharide and verifies the effectiveness of the process for producing the xylo-oligosaccharide from the corn bran; the problem of utilization of waste heat of cooking is solved; the waste heat of steam explosion can be used for concentrating the materials after membrane concentration, and 2t steam is saved when 1t syrup is produced.
(3) The invention adopts the membrane technology, reduces the consumption of the active carbon by two times of ultrafiltration, can save 200kg of the active carbon for producing 1t of syrup, reduces the steam consumption by the nanofiltration concentration membrane, and saves 5t of steam for producing 1t of syrup.
(4) The preparation method can improve the quality of the xylo-oligosaccharide liquid glucose; the purity of the xylo-oligosaccharide prepared by the original process can only reach about 70 percent (70-72 percent), and the purity of the xylo-oligosaccharide prepared by the method can reach over 75 percent.
(5) The preparation method can reduce acid and alkali consumption and sewage discharge. Compared with the traditional process, the preparation method reduces one-time ion exchange, and can reduce the acid and alkali consumption and the sewage discharge by about 20 percent.
Drawings
FIG. 1 is a flow chart of the present invention for preparing xylo-oligosaccharide.
Detailed Description
The technical solutions of the present invention are further described in detail below with reference to the accompanying drawings, and it should be noted that the detailed description is only for describing the present invention, and should not be construed as limiting the present invention.
Example 1
A method for preparing xylo-oligosaccharide from corn bran comprises the following steps:
(1) Firstly, syrup tank (full volume 25 m) 3 ) Adding 18m of process water 3 Then adding 2t of corn bran (the water content is less than 12%), adding acid to adjust the pH value to 4.5, heating to 80 ℃, and stirring and mixing uniformly; obtaining a suspension of corn husks; in this embodiment, the acid added is acetic acid, and the addition of other acids affects the purity of the xylooligosaccharide after enzymolysis. Corn husks are commercially available. The moisture content of the corn bran was 10% and the ash content was less than 2%, in this example, the ash content was 1%.
(2) And (2) starting a delivery pump, delivering the corn bran suspension obtained in the step (1) to a pressurizing ejector, simultaneously opening a steam valve of the pressurizing ejector, performing steam heating on the material, ensuring that the steam pressure of the ejector is 0.6MPa, keeping the temperature of the material at 160 ℃, delivering the material to a laminar flow tank, ensuring that the material stays in the laminar flow tank for 50min, and finally, delivering the material to a gas-liquid separator. The retention time of the materials in the laminar flow tank has certain influence on the yield and the purity. The long retention time can increase the content of monosaccharide and reduce the purity of xylo-oligosaccharide. In laminar flow tanks, it is also necessary to maintain: the steam pressure is 0.6MPa, and the material temperature is 160 ℃.
(3) And (3) recovering waste heat of the secondary steam of the material subjected to flash evaporation by the gas-liquid separator (the recovered waste heat can be used for concentrating the material in a waste heat evaporator after membrane concentration), and enabling the material to enter a collecting tank of the gas-liquid separator. Steam explosion has an effect on yield and purity. The better the steam explosion effect is, the better the enzymolysis effect can be promoted, and the yield and the purity of the xylo-oligosaccharide can be improved.
(4) The material collected in the step (3) is input into a saccharification tank (25 m) through a pump 3 ) Then, when the liquid level reaches 80%, closing the feed valve and opening the feed valve of another saccharification tank at the same time, then cooling to 50 ℃, and then adding1.0kg of xylanase and 1.0kg of saccharifying enzyme, and carrying out enzymolysis for 10h. Both xylanase and glucoamylase are purchased from commercial sources, wherein the xylanase model SP25 has the enzyme activity of more than or equal to 75000U/g, and the glucoamylase (glucoamylase compounded with 10 ten thousand U/ml).
(5) And after the enzymolysis is finished, detecting the content of xylo-oligosaccharide in the sugar solution in the enzymolysis tank, determining the purity of the xylo-oligosaccharide, and then heating to the temperature of more than 80 ℃ for enzyme deactivation. In this example, the temperature was raised to 85 ℃.
(6) Keeping the enzyme deactivation temperature for more than half an hour, then conveying the materials to a candle filter and a plate-and-frame filter, adding powdered activated carbon into filtrate, and carrying out decolorization and removal treatment, wherein the light transmittance is more than 20%; in this example, the enzyme deactivation temperature was maintained for 35min. Adding activated carbon in proportion: the addition amount is 1m based on light transmission 3 3kg of activated carbon was added to the filtrate.
(7) Passing the decolorized filtrate through cation exchange column at ion exchange temperature of less than 45 deg.C and flow rate of 2 times of resin volume/hr (specifically, the volume of resin is 5 m) 3 The material flow is 10m 3 And/h), controlling the content of calcium ions and magnesium ions to be zero, then carrying out ultrafiltration, wherein the discharge light transmittance is more than 40%, and then passing through a nanofiltration membrane, wherein the discharge refractive index is more than 18%. The molecular weight intercepted by the ultrafiltration membrane is 10000 Dalton, and the molecular weight intercepted by the nanofiltration membrane is 300 Dalton.
(8) The feed liquid after membrane concentration is concentrated by a waste heat evaporator (heated by secondary steam of continuous cooking flash evaporation), and the discharge concentration is more than 30%.
(9) And (4) carrying out secondary decolorization on the concentrated material in the step (8), wherein after decolorization and filtration, the light transmittance of the material is more than 50%. Here, the secondary decoloring is the same as the above-mentioned activated carbon decoloring, and the addition amounts are: 1m 3 3kg of activated carbon was added to the filtrate.
(10) Performing ion exchange on the material subjected to secondary decolorization, wherein the conductivity after the ion exchange is less than 20 mu s/cm, the pH value is 4, and the light transmittance is more than 95%; ion exchange here means: adopting cation and anion exchange combination, adopting 001 × 7 cation exchange resin and D301 anion exchange resin, and the ion exchange treatment temperature is lessThe flow rate of the ion exchange treatment was 2 times the volume of the resin per hour at 45 deg.C (specifically, the volume of the resin was 5 m) 3 The material flow is 10m 3 /h)。
After ion exchange is finished, the materials are ejected out by water until the refractive index is less than 1 percent, and sugar liquor loss is avoided. Then regenerating, soaking the cation exchange column with hydrochloric acid and the anion exchange column with liquid alkali for 3h, discharging waste acid and alkali, then leaching with pure water, wherein the leaching end point of the cation column is 3-3.5, the leaching end point of the anion column is 9.5-10, and the solution is reserved after leaching; hydrochloric acid and liquid alkali for regeneration, the mass concentration of which is 3 percent, and the conductivity of the leached pure water is less than 30 mu s/cm.
(11) And (3) ultrafiltering the sugar solution after ion exchange, returning filtrate to a secondary decolorizing tank, carrying out secondary concentration on the permeate, and filling the concentrated material into a finished product, wherein the discharge mass concentration is 76%. The ultrafiltration membrane used herein has a molecular weight cut-off of 1000-2000 daltons. The secondary concentration refers to: concentrating by adopting a triple-effect plate evaporator, wherein the single-effect vacuum degree is-0.01 to-0.03 Mpa, and the temperature is 95-105 ℃; the secondary vacuum degree is-0.04 to-0.06 Mpa, and the temperature is 80 to 85 ℃; the triple effect vacuum degree is-0.01 to-0.03 Mpa, and the temperature is 65-75 ℃.
Example 2
A method for preparing xylo-oligosaccharide from corn bran comprises the following steps:
(1) Firstly, syrup tank (full volume 25 m) 3 ) Adding process water, adding corn bran (the water content is less than 12 percent), wherein the mass ratio of the corn bran to the water is 1:9, adding acid to adjust the pH value to 5, heating to 85 ℃, and stirring and mixing uniformly; obtaining a suspension of corn husks; in this embodiment, the acid added is acetic acid, and the addition of other acids affects the purity of the xylooligosaccharide after enzymolysis. Corn husks are commercially available. The moisture content of the corn bran was 8% and the ash content was less than 2%, in this example, the ash content was 0.5%.
(2) And (2) starting a delivery pump, delivering the corn bran suspension obtained in the step (1) to a pressurizing ejector, simultaneously opening a steam valve of the pressurizing ejector, performing steam heating on the material, delivering the material to a laminar flow tank, ensuring the steam pressure of the ejector to be 0.7MPa, keeping the temperature of the material to be about 165 ℃, ensuring the material to stay in the laminar flow tank for 60min, and finally entering a gas-liquid separator. The length of time that the material stays in the laminar flow tank has an influence on the yield and purity. In laminar flow tanks, it is also necessary to maintain: the steam pressure is 0.7MPa, and the material temperature is 165 ℃.
(3) And (3) recovering waste heat of the secondary steam of the material subjected to flash evaporation by the gas-liquid separator (the recovered waste heat can be used for concentrating the material in a waste heat evaporator after membrane concentration), and enabling the material to enter a collecting tank of the gas-liquid separator.
(4) The material collected in the step (3) is input into a saccharification tank (25 m) through a pump 3 ) Then, when the liquid level reaches 80%, closing the feeding valve, simultaneously opening the feeding valve of the other saccharification tank, then cooling to 50 ℃, then adding xylanase and saccharifying enzyme, and carrying out enzymolysis for 10 hours; every 1m 3 0.07kg of xylanase and 0.07kg of glucoamylase were added to the batch. Both xylanase and glucoamylase are purchased from commercial sources, wherein the xylanase model SP25 has the enzyme activity of more than or equal to 75000U/g, and the glucoamylase (glucoamylase Glumael) has the enzyme activity of 10 ten thousand U/ml.
(5) And (3) detecting the content of xylo-oligosaccharide in the sugar solution in the enzymolysis tank after enzymolysis is finished, confirming the purity of the xylo-oligosaccharide, and then heating to the temperature of more than 80 ℃ to inactivate enzyme. In this example, the temperature was raised to 90 ℃ to inactivate the enzyme.
(6) Keeping the enzyme deactivation temperature for more than half an hour, then conveying the materials to a candle filter and a plate-and-frame filter, adding powdered activated carbon into filtrate, and carrying out decolorization and removal treatment, wherein the light transmittance is more than 30%; in this example, the enzyme deactivation temperature was maintained for 35min. Adding activated carbon in proportion: the addition amount is 1m based on light transmission 3 3kg of activated carbon was added to the filtrate.
(7) Passing the decolorized filtrate through cation exchange column at ion exchange temperature of less than 45 deg.C and flow rate of 2 times of resin volume/hr (specifically, the volume of resin is 5 m) 3 The material flow is 10m 3 And/h), controlling the content of calcium ions and magnesium ions to be zero, then carrying out ultrafiltration, wherein the discharge light transmittance is more than 40%, and then passing through a nanofiltration membrane, wherein the discharge refractive index is more than 18%. The ultrafiltration membrane adopted has a molecular weight cut-off of 10000 Dalton and adopts sodiumThe molecular weight retained by the filter was 300 daltons.
(8) The feed liquid after membrane concentration is concentrated by a waste heat evaporator (heated by secondary steam of continuous cooking flash evaporation), and the discharge concentration is more than 30%.
(9) And (4) carrying out secondary decolorization on the concentrated material in the step (8), wherein after decolorization and filtration, the light transmittance of the material is more than 50%. Here, the secondary decoloring is the same as the above-mentioned activated carbon decoloring, and the addition amounts are: 1m 3 3kg of active carbon is added into the filtrate;
(10) Performing ion exchange on the material subjected to secondary decolorization, wherein the conductivity after the ion exchange is less than 20 mu s/cm, the pH value is 5, and the light transmittance is more than 95%; ion exchange here means: adopting cation and anion exchange combination, adopting 001 × 7 cation exchange resin and D301 anion exchange resin, wherein the ion exchange treatment temperature is less than 45 deg.C, and the flow rate of the ion exchange treatment is 2 times of the resin volume/hr, specifically, the resin volume is 5m 3 The material flow is 10m 3 /h。
After ion exchange is finished, the materials are ejected out by water, and the loss of sugar liquor is avoided on the basis that the refractive index is less than 1%. Then regenerating, soaking the cation exchange column with hydrochloric acid and the anion exchange column with liquid alkali for 3h, discharging waste acid and alkali, then leaching with pure water, wherein the leaching end point of the cation column is 3-3.5, the leaching end point of the anion column is 9.5-10, and the solution is reserved after leaching; hydrochloric acid and liquid alkali for regeneration, the mass concentration of which is 3 percent, and the conductivity of the leached pure water is less than 30 mu s/cm.
(11) And (3) performing ultrafiltration on the sugar liquor after ion exchange, returning filtrate to a secondary decoloring tank, performing secondary concentration on the permeate, and filling the concentrated material into a finished product, wherein the mass concentration of the discharged material is 78%. The ultrafiltration membrane used herein has a molecular weight cut-off of 1000-2000 daltons. The secondary concentration means: concentrating by adopting a triple-effect plate evaporator, wherein the single-effect vacuum degree is-0.01 to-0.03 Mpa, and the temperature is 95-105 ℃; the secondary vacuum degree is-0.04 to-0.06 Mpa, and the temperature is 80 to 85 ℃; the triple effect vacuum degree is-0.01 to-0.03 Mpa, and the temperature is 65-75 ℃.
Other embodiments in this example are the same as example 1.
Example 3
A method for preparing xylo-oligosaccharide from corn bran comprises the following steps:
(1) Firstly, syrup tank (full volume 25 m) 3 ) Adding process water, then adding corn bran (the water content is less than 12%), wherein the mass ratio of the corn bran to the water is 1; obtaining a suspension of corn husks; in this embodiment, the acid added is acetic acid, and the addition of other acids affects the purity of the xylooligosaccharide after enzymolysis. Corn husks are commercially available. The moisture content of the corn bran was 5% and the ash content was less than 2%, in this example, the ash content was 0.5%.
(2) And (2) starting a delivery pump, delivering the corn bran suspension obtained in the step (1) to a pressurizing ejector, simultaneously opening a steam valve of the pressurizing ejector, performing steam heating on the material, delivering the material to a laminar flow tank, ensuring the steam pressure of the ejector to be 0.7MPa, keeping the temperature of the material to be 170 ℃, ensuring the material to stay in the laminar flow tank for 70min, and finally entering a gas-liquid separator. In laminar flow tanks, it is also necessary to maintain: the steam pressure is 0.7MPa, and the material temperature is 170 ℃.
(3) And (3) recovering waste heat of the secondary steam of the material subjected to flash evaporation by the gas-liquid separator (the recovered waste heat can be used for concentrating the material in a waste heat evaporator after membrane concentration), and enabling the material to enter a collecting tank of the gas-liquid separator.
(4) The material collected in the step (3) is input into a saccharification tank (25 m) through a pump 3 ) Then, when the liquid level reaches 80%, closing the feeding valve, simultaneously opening the feeding valve of the other saccharification tank, then cooling to 50 ℃, then adding xylanase and saccharifying enzyme, and carrying out enzymolysis for 10 hours; every 1m 3 0.1kg of xylanase and 0.1kg of glucoamylase were added to the batch. Xylanase and glucoamylase are purchased from commercial sources, wherein the xylanase model SP25 has the enzyme activity of more than or equal to 75000U/g, and the glucoamylase (glucoamylase Glumastel compounded) has the enzyme activity of 10 ten thousand U/ml.
(5) And after the enzymolysis is finished, detecting the content of xylo-oligosaccharide in the sugar solution in the enzymolysis tank, determining the purity of the xylo-oligosaccharide, and then heating to the temperature of more than 80 ℃ for enzyme deactivation. In this example, the temperature was raised to 90 ℃ to inactivate the enzyme.
(6) Keeping the enzyme deactivation temperature for more than half an hour, then conveying the materials to a candle filter and a plate-and-frame filter, adding powdered activated carbon into filtrate, and carrying out decolorization and removal treatment, wherein the light transmittance is more than 30%; in this example, the enzyme deactivation temperature was maintained for 40min. Adding activated carbon in proportion: the addition amount is 1m based on light transmission 3 3kg of activated carbon was added to the filtrate.
(7) Passing the decolorized filtrate through cation exchange column at ion exchange temperature of less than 45 deg.C and flow rate of 2 times of resin volume/hr (specifically, the volume of resin is 5 m) 3 The material flow is 10m 3 And/h), controlling the content of calcium ions and magnesium ions to be zero, performing ultrafiltration, wherein the discharge light transmittance is more than 40%, and then concentrating by using a nanofiltration membrane, wherein the discharge refractive index is more than 18%. The molecular weight intercepted by the ultrafiltration membrane is 10000 Dalton, and the molecular weight intercepted by the nanofiltration membrane is 300 Dalton.
(8) The feed liquid after membrane concentration is concentrated by a waste heat evaporator (heated by secondary steam of continuous cooking flash evaporation), and the discharge concentration is more than 30%.
(9) And (4) carrying out secondary decolorization on the concentrated material in the step (8), wherein after decolorization and filtration, the light transmittance of the material is more than 50%. Here, the secondary decoloring is the same as the above-mentioned activated carbon decoloring, and the addition amounts are: 1m 3 3kg of active carbon is added into the filtrate;
(10) Performing ion exchange on the material subjected to secondary decolorization, wherein the conductivity after the ion exchange is less than 20 mu s/cm, the pH value is 6, and the light transmittance is more than 95%; ion exchange here means: adopting cation and anion exchange combination, adopting 001 × 7 cation exchange resin and D301 anion exchange resin, wherein the ion exchange treatment temperature is less than 45 deg.C, and the flow rate of the ion exchange treatment is 2 times of the resin volume/hr (specifically, the volume of the resin is 5 m) 3 The material flow is 10m 3 /h)。
After ion exchange is finished, the materials are ejected out by water, and the loss of sugar liquor is avoided on the basis that the refractive index is less than 1%. Then regenerating, soaking the cation exchange column with hydrochloric acid and the anion exchange column with liquid alkali for 3h, discharging waste acid and alkali, then leaching with pure water, wherein the leaching end point of the cation column is 3-3.5, the leaching end point of the anion column is 9.5-10, and the solution is reserved after leaching; hydrochloric acid and liquid alkali for regeneration, the mass concentration of which is 3 percent, and the conductivity of the leached pure water is less than 30 mu s/cm.
(11) And (3) performing ultrafiltration on the sugar liquor after ion exchange, returning filtrate to a secondary decoloring tank, performing secondary concentration on the permeate, and filling the concentrated material into a finished product, wherein the mass concentration of the discharged material is 75%. The ultrafiltration membrane used herein has a molecular weight cut-off of 1000-2000 daltons. The secondary concentration means: concentrating by adopting a triple-effect plate evaporator, wherein the single-effect vacuum degree is-0.01 to-0.03 Mpa, and the temperature is 95-105 ℃; the secondary vacuum degree is-0.04 to-0.06 Mpa, and the temperature is 80 to 85 ℃; the triple effect vacuum degree is-0.01 to-0.03 Mpa, and the temperature is 65-75 ℃.
Other embodiments in this example are the same as example 1.
Comparative example 1
In the present embodiment, the steam explosion step, i.e. the step (2), is not present, and the steam explosion step directly enters the gas-liquid separator.
Other embodiments in this example are the same as example 1.
Comparative example 2
In this example, only one enzyme (xylanase) was used, and the other steps were the same as in example 1.
Comparative example 3
In this example, only one enzyme (saccharifying enzyme) was used, and the other steps were the same as in example 1.
Table 1 shows the detection results of xylo-oligosaccharide in the sugar solution after the completion of the enzymatic hydrolysis in the examples and comparative examples
TABLE 2 examination results of the final xylo-oligosaccharide products obtained in examples and comparative examples
As can be seen from Table 1, the purity of the xylo-oligosaccharide obtained after the enzymolysis in the examples is high (> 70%), the light transmittance of the feed liquid is less than 10%, and the conductivity is 2000-3300 mus/cm. Compared with the prior art, the saccharified feed liquid obtained by the preparation method has the advantages of increased light transmittance, reduced conductivity and increased purity of xylo-oligosaccharide. In comparative examples 1-3, the purity of the xylo-oligosaccharide obtained after the enzymolysis is not high (less than 70%), and the light transmittance of the feed liquid is less than 10%. As the comparative example 1 has no steam explosion step, the purity of the xylo-oligosaccharide in the prepared sugar solution is lower, and the comparative examples 2-3 only adopt one enzyme for enzymolysis, so that the purity of the xylo-oligosaccharide in the prepared sugar solution is lower.
As can be seen from Table 2, the purity of the xylooligosaccharide finally obtained in examples 1-3 was high (= 75%), the transmittance of the feed liquid was > 90%, and the conductivity was low (= < 25. Mu.s/cm). Compared with the examples, the comparative example 1 lacks a steam explosion step, is not beneficial to the preparation of the xylo-oligosaccharide, and the obtained xylo-oligosaccharide has lower purity and the differences of the conductivity and the light transmittance with the data in the examples are not large. In comparative example 2 and comparative example 3, only one enzyme is used for enzymolysis, which is not beneficial to the preparation of high-purity xylo-oligosaccharide, the purity of the prepared xylo-oligosaccharide is low, the light transmittance is not much different from that of the feed liquid in the examples, and the electric conductivity is slightly smaller than that in the examples.
It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (2)
1. The method for preparing xylo-oligosaccharide from corn bran is characterized by comprising the following steps:
(1) Mixing corn bran with water according to the mass ratio of 1:8-10, adding acetic acid to adjust the pH value to 4.5-5.5, then heating to 80-90 ℃, and stirring and mixing uniformly to form a suspension of the corn bran;
(2) Conveying the suspension of the corn husks to a pressurizing ejector, allowing the suspension to enter a laminar flow tank through the ejector, allowing the materials to stay in the laminar flow tank for 50-70min, and finally allowing the suspension to enter a gas-liquid separator for gas-liquid separation; recovering waste heat of the flash evaporated secondary steam of the gas-liquid separator; after the suspension liquid of the corn husks enters a pressurizing ejector, simultaneously opening a steam valve of the pressurizing ejector to perform steam heating on the materials, so that the pressure is 0.6-0.7MPa, and the temperature of the materials is kept at 160-170 ℃;
(3) The liquid after vapor-liquid separation enters a saccharification tank, the temperature is controlled at 50 +/-1 ℃, and the concentration is 1m 3 Adding 0.05-0.1kg of xylanase and 0.05-0.1kg of saccharifying enzyme into the materials, and carrying out enzymolysis for 10 hours;
(4) After enzymolysis, detecting the purity of the xylo-oligosaccharide, then heating to 80-90 ℃ to inactivate enzyme, keeping the temperature of inactivating enzyme for 30-40min, and filtering;
(5) Adding activated carbon into the filtrate for decolorization and filtration treatment, wherein the light transmittance is more than 20%;
(6) The filtrate after decolorization passes through a cation exchange column, the content of calcium ions and magnesium ions is controlled to be zero, and then ultrafiltration is carried out, and the discharge light transmittance is more than 40 percent.
(7) Concentrating the ultrafiltered filtrate with membrane to obtain filtrate with refractive index higher than 18%;
(8) The waste heat recovered in the step (2) is used for concentrating the material obtained in the step (7), and the discharge refractive index is more than 30%;
(9) Decolorizing the concentrated material obtained in the step (8) again, wherein the light transmittance after decolorization and filtration is more than 50%;
(10) Performing ion exchange on the material subjected to secondary decolorization in the step (9), wherein the conductivity after the ion exchange is less than 20 mu s/cm, the pH value is 4-7, and the light transmittance is more than 95%; respectively regenerating the cation exchange column and the anion exchange column by using hydrochloric acid and liquid alkali, wherein the mass concentrations of the hydrochloric acid and the liquid alkali are 3-4%, leaching by using reverse osmosis pure water, and the conductivity of the reverse osmosis pure water is less than 30 mu s/cm;
(11) And (4) carrying out secondary concentration on the sugar solution subjected to ion exchange in the step (10), and filling the concentrated material into finished products.
2. The method for preparing xylo-oligosaccharide from corn husks as claimed in claim 1, wherein in the step (7), nanofiltration membranes are used for membrane concentration.
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| CN1680415A (en) * | 2004-04-05 | 2005-10-12 | 山东龙力生物科技有限公司 | Preparation of oligo-wood sugar |
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