CN112458125B - Method for preparing xylo-oligosaccharide from corncob powder - Google Patents
Method for preparing xylo-oligosaccharide from corncob powder Download PDFInfo
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- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
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Abstract
The invention discloses a method for preparing xylo-oligosaccharide from corncob powder, which comprises the steps of adding acid and water, stirring and mixing to obtain a 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 vapor-liquid separator, recycling secondary steam for heating subsequent materials, conveying liquid into a saccharification tank, cooling, and then adding xylanase and saccharifying enzyme, wherein a multi-stage membrane system is additionally arranged in the production process, the conductivity of saccharified feed liquid is lower than 5000 mu s/cm, the purity of xylo-oligosaccharide is 70-80%, the quality of products is improved, the sewage amount is greatly reduced, the waste heat of vapor-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 corncob meal.
Background
The 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 promoter has unique advantages and can selectively promote the proliferation activity of intestinal bifidobacteria. 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. the raw material is directly hydrolyzed by steam, water or dilute inorganic acid to generate the xylo-oligosaccharide.
In the prior art, the traditional process for producing the xylo-oligosaccharide in the industry adopts intermittent high-pressure cooking and carries out enzymolysis twice 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 times of enzymolysis and purification, the 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, the invention provides a method for preparing xylo-oligosaccharide from corncob meal to overcome the defects of the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for preparing xylo-oligosaccharide from corncob meal comprises the following steps:
(1) mixing the corncob meal and 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 corncob meal suspension;
(2) conveying the suspension of the corncob powder to a pressurizing ejector, allowing the suspension to enter a laminar flow tank through the ejector, allowing the material to stay in the laminar flow tank for 50-60min, and finally allowing the suspension to enter a vapor-liquid separator for vapor-liquid separation; recovering waste heat of the flash evaporated secondary steam of the steam-liquid separator;
(3) the liquid after vapor-liquid separation enters a saccharification tank, and the saccharification tank is used for saccharifying every 1m 3 Adding 0.05-0.3kg of xylanase and 0.05-0.3kg of saccharifying enzyme into the material, controlling the temperature at 50 +/-1 ℃, 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 10 percent;
(6) the decolorized filtrate is ultrafiltered, and the discharge light transmittance is more than 30 percent;
(7) concentrating the ultrafiltered filtrate by a membrane, wherein the discharge refractive index is more 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 30%;
(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) performing secondary concentration on the sugar solution subjected to ion exchange in the step (10), wherein the mass concentration of discharged materials is 70-75%, and filling finished products of the concentrated materials; or concentrating the syrup subjected to ion exchange in the step (10) until the refractive index is 40-60%, performing chromatographic purification until the content is increased to over 96%, adding an excipient, and performing spray granulation to produce granular xylo-oligosaccharide. Or if granulation is needed, controlling the refractive index of the sugar solution obtained by secondary concentration to be 40-60%, then adding various excipients, and producing granular xylo-oligosaccharide through spray granulation.
Furthermore, in the step (7), a nanofiltration membrane is adopted during membrane concentration.
Further, in the step (2), after the suspension of the corncob meal enters the pressurizing ejector, a steam valve of the pressurizing ejector is opened simultaneously to perform steam heating on the material, so that the pressure is 0.6-0.7MPa, and the temperature of the material is kept at 160-170 ℃. In the laminar flow tank, the steam pressure is also kept between 0.6 and 0.7MPa, and the material temperature is kept between 160 ℃ and 170 ℃.
Further, in the step (12), the excipient is at least one of maltodextrin and corncob residue.
The invention has the beneficial effects that:
(1) in the invention, acid and water are added and stirred to form 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, the pressure is rapidly released by a vapor-liquid separator, secondary steam is recycled for heating subsequent materials, liquid enters a saccharifying tank, xylanase and saccharifying enzyme are added after the temperature is reduced, a multi-stage membrane system is additionally arranged in the production process, the conductivity of saccharified feed liquid is lower than 5000 mus/cm, the solid content (4-6%), the purity of xylo-oligosaccharide is 70-80%, the product quality is improved, the sewage quantity is greatly reduced, the waste heat of vapor-liquid separation is convenient to recycle, and the energy consumption is reduced.
(2) The invention adopts steam explosion and double enzymolysis methods, adds a membrane technology and can effectively produce xylo-oligosaccharide. The problem of utilization of waste heat of cooking is solved; waste heat after intermittent cooking is directly discharged, waste heat of steam explosion is used for material concentration after membrane concentration, and steam is expected to be saved by 2t for each 1t of syrup produced.
(3) The invention adopts the membrane technology, reduces the consumption of active carbon by ultrafiltration, can save 200kg of active carbon when producing 1t of syrup, reduces the steam consumption by the nanofiltration concentration membrane, and saves 5t of steam when producing 1t of syrup.
(4) The preparation method of the invention improves the quality of xylo-oligosaccharide liquid glucose; in the prior art, the purity of the produced xylo-oligosaccharide can only reach about 70 percent, and the purity of the xylo-oligosaccharide syrup finally obtained by adopting the preparation method can reach more than 72 percent.
(5) The preparation method can reduce acid and alkali consumption and sewage discharge. Compared with the traditional process, the method can reduce the acid and alkali consumption and the sewage discharge by about 20 percent by reducing one-time ion exchange.
Drawings
FIG. 1 is a flow chart of the present invention for preparing xylooligosaccharide.
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
As shown in figure 1, the method for preparing xylo-oligosaccharide from corncob meal comprises the following steps:
(1) firstly, syrup tank (full volume 25 m) 3 ) Adding 18m of process water 3 Then adding 2t of corn cob powder (water content is less than 12%), adding acetic acid to adjust pH to 4.5, heating to 85 deg.C, stirring and mixing uniformlyHomogenizing to obtain suspension of half corncob powder; the corncob meal used in the present invention is commercially available.
(2) And (2) starting a delivery pump, delivering the suspension of the corncob powder obtained in the step (1) to a pressurizing ejector, simultaneously opening a steam valve of the pressurizing ejector, carrying out steam heating on the material, then delivering the material to a laminar flow tank, ensuring that the steam pressure of the liquefying ejector is 0.6MPa, keeping the temperature of the material at about 160 ℃, ensuring that the material stays in the laminar flow tank for 50min, and finally entering a gas-liquid separator. The retention time of the materials in the laminar flow tank has certain influence on the yield and the purity. Too long a residence time increases the purity of the monosaccharides and decreases the purity of the xylo-oligosaccharides. 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 flash-evaporated secondary steam of the material in the vapor-liquid separator, (the recovered waste heat can be used for concentrating the material in a waste heat evaporator after membrane concentration), and the material enters a collecting tank of the vapor-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 conveyed into a saccharification tank (25 m) through a pump 3 ) And 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 1.0kg of xylanase and 1.0kg of saccharifying enzyme, and carrying out enzymolysis for 10 hours. Both xylanase and glucoamylase are purchased from commercial sources, wherein the xylanase model SP25 has enzyme activity of more than or equal to 75000U/g, and the glucoamylase (glucoamylase Glumael) has 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 85 ℃.
(6) Keeping the enzyme deactivation temperature for more than half an hour, then conveying the materials to a turbid filter and a plate-frame filter, adding powdered activated carbon into the filtrate, and carrying out decolorization and dehydration treatment, wherein the light transmittance is more than 10%. In this example, the enzyme deactivation temperature was maintained for 32 min. Adding activated carbon in proportion: based on light transmission, the addition amount is1m 3 3kg of activated carbon was added to the filtrate.
(7) The decolorized filtrate is ultrafiltered to obtain material with light transmittance higher than 30%, and then is passed through a nanofiltration concentration membrane to obtain material with refractive index higher 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 (5) performing secondary decolorization on the concentrated material obtained in the step (8), wherein after decolorization and filtration, the light transmittance of the material is more than 50%. Here, the secondary decolorization is the same as the above-mentioned activated carbon decolorization, 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 percent; 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, ejecting the material by using water until refraction is less than 1%, then regenerating, using hydrochloric acid for a cation exchange column, using liquid alkali for an anion exchange column, soaking for 3 hours, then discharging waste acid and alkali, then leaching by using pure water, wherein the leaching end point of a positive column is 3-3.5, the leaching end point of a negative column is 9.5-10, and reserving after leaching; hydrochloric acid and liquid alkali are used for regeneration, the mass concentration is 3-4%, and the conductivity of the eluted pure water is less than 30 mu s/cm.
(11) And (4) 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 discharge mass concentration is 72%. The ultrafiltration membrane used here retained a molecular weight of 1000-. 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 ℃.
(12) If granulation is needed, the refractive index of the sugar solution obtained by secondary concentration is controlled at 50 percent, then various excipients are added, and the granular xylo-oligosaccharide is produced by spray granulation. The excipient is at least one of maltodextrin and corncob residue, and in this embodiment, maltodextrin is used.
Example 2
As shown in figure 1, the method for preparing xylo-oligosaccharide from corncob meal comprises the following steps:
(1) firstly, syrup tank (full volume 25 m) 3 ) Adding process water, adding corncob powder (water content is less than 12%), wherein the mass ratio of the corncob powder to the water is 1:9, adding acid to adjust the pH value to 4.5, heating to 85 ℃, and stirring and mixing uniformly to obtain a semi-corncob powder suspension;
(2) and (2) starting a delivery pump, delivering the suspension of the corncob powder obtained in the step (1) to a pressurizing ejector, simultaneously opening a steam valve of the pressurizing ejector, carrying out steam heating on the material, delivering the material to a laminar flow tank, ensuring that the steam pressure of the liquefying ejector is 0.6MPa, keeping the temperature of the material at about 165 ℃, ensuring that the material stays in the laminar flow tank for 55min, and finally entering 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 165 ℃.
(3) And (3) recovering waste heat of the flash-evaporated secondary steam of the material in the vapor-liquid separator, (the recovered waste heat can be used for concentrating the material in a waste heat evaporator after membrane concentration), and the material enters a collecting tank of the vapor-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 materials collected in the step (3) are conveyed into a saccharification tank (25 m) through a pump 3 ) Then, when the liquid level reaches 80%, closing the feeding valve and simultaneously opening the feeding valve of the other saccharification tank, then cooling to 50 ℃, and then coolingAdding xylanase and diastase, and performing enzymolysis for 10 h; every 1m 3 0.2kg of xylanase and 0.2kg of glucoamylase were added to the batch. Both xylanase and glucoamylase are purchased from commercial sources, wherein the xylanase model SP25 has enzyme activity of more than or equal to 75000U/g, and the glucoamylase (glucoamylase compounded with 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 85 ℃ for enzyme deactivation.
(6) Keeping enzyme deactivation temperature for 35 minutes, then conveying the materials to a turbid filter and a plate-and-frame filter, adding powdered activated carbon into the filtrate, and carrying out decolorization and removal treatment, wherein the light transmittance is more than 10%. In this example, the enzyme deactivation temperature was maintained for 35 min. 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) The decolorized filtrate is ultrafiltered to obtain material with light transmittance higher than 30%, and then is passed through a nanofiltration concentration membrane to obtain material with refractive index higher 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 30%. 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 5, and the light transmittance is more than 95 percent; 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, firstly ejecting the materials by using water until refraction is less than 1%, then regenerating, soaking a cation exchange column by using hydrochloric acid and an anion exchange column by using liquid alkali for 3h, then discharging waste acid and alkali, then leaching by using pure water, wherein the leaching end point of a positive column is 3-3.5, the leaching end point of a negative column is 9.5-10, and reserving after leaching is finished; the regenerated hydrochloric acid and liquid alkali are used, the mass concentration is 3-4%, and the conductivity of the eluted pure water is less than 30 mu s/cm.
(11) And (4) 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 74%. The ultrafiltration membrane used here retained a molecular weight of 1000-. 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 three-effect vacuum degree is-0.01 to-0.03 Mpa, and the temperature is 65-75 ℃.
(12) If granulation is needed, the refractive index of the sugar solution obtained by secondary concentration is controlled to be 55 percent, then various excipients are added, and the granular xylo-oligosaccharide is produced by spray granulation. The excipient is at least one of maltodextrin and corncob residue, and in this embodiment, corncob residue is used.
Other embodiments in this example are the same as example 1.
Example 3
As shown in figure 1, the method for preparing xylo-oligosaccharide from corncob meal comprises the following steps:
(1) firstly, syrup tank (full volume 25 m) 3 ) Adding process water, adding corncob powder (water content is less than 12%), wherein the mass ratio of the corncob powder to the water is 1:10, adding acid to adjust the pH value to 4.5, heating to 85 ℃, and stirring and mixing uniformly to obtain a semi-corncob powder suspension;
(2) and (2) starting a delivery pump, delivering the suspension of the corncob powder obtained in the step (1) to a pressurizing ejector, simultaneously opening a steam valve of the pressurizing ejector, carrying out steam heating on the material, then delivering the material to a laminar flow tank, ensuring that the steam pressure of the liquefying ejector is 0.7MPa, keeping the temperature of the material at about 170 ℃, ensuring that the material stays in the laminar flow tank for 60min, and finally entering a gas-liquid separator. The retention time of the materials in the laminar flow tank has certain influence on the yield and the purity. Too long a residence time increases the monosaccharide content and reduces the purity of the xylo-oligosaccharides. 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 flash-evaporated secondary steam of the material in the vapor-liquid separator, (the recovered waste heat can be used for concentrating the material in a waste heat evaporator after membrane concentration), and the material enters a collecting tank of the vapor-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 conveyed into a saccharification tank (25 m) through a pump 3 ) And 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 0.3kg of xylanase and 0.3kg of glucoamylase were added to the batch. Both xylanase and glucoamylase are purchased from commercial sources, wherein the xylanase model SP25 has 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.
(6) Keeping the enzyme deactivation temperature for more than half an hour, then conveying the materials to a turbid filter and a plate-frame filter, adding powdered activated carbon into the filtrate, and carrying out decolorization and dehydration treatment, wherein the light transmittance is more than 10%. In this example, the enzyme deactivation temperature was maintained for 40 min. 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) The decolorized filtrate is ultrafiltered to obtain material with light transmittance higher than 30%, and then passed through a nanofiltration concentration membrane to obtain material with refractive index higher 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 30%. 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 6, and the light transmittance is more than 95%; the 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, ejecting the material by using water until refraction is less than 1%, then regenerating, using hydrochloric acid for a cation exchange column, using liquid alkali for an anion exchange column, soaking for 3 hours, then discharging waste acid and alkali, then leaching by using pure water, wherein the leaching end point of a positive column is 3-3.5, the leaching end point of a negative column is 9.5-10, and reserving after leaching; hydrochloric acid and liquid alkali are used for regeneration, the mass concentration is 3-4%, and the conductivity of the eluted 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 76%. The ultrafiltration membrane used here retained a molecular weight of 1000-. 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 ℃.
(12) If granulation is needed, the refractive index of the sugar solution obtained by secondary concentration is controlled at 60%, then various excipients are added, and the granular xylo-oligosaccharide is produced by spray granulation. The excipient is at least one of maltodextrin and corncob residue, and in this embodiment, maltodextrin is used.
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 detection results of xylo-oligosaccharide in sugar solution after enzymolysis in examples and comparative examples
TABLE 2 examination results of the final xylo-oligosaccharide products obtained in the examples and comparative examples
As can be seen from Table 1, in the examples, the purity of the xylooligosaccharide obtained after the enzymolysis is finished is higher (> 70%), the transmittance of the feed liquid is less than 15%, and the conductivity is 2000-3300 μ s/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 the comparative example, the purity of the xylo-oligosaccharide obtained after the enzymolysis is finished is not high (less than 70%), the light transmittance of the feed liquid is less than 10%, and the conductivity is slightly smaller than that in the example. 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 the examples was high (═ 73%), the transmittance of the feed liquid was 90% and the conductivity was low (═ 21. 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, slightly larger conductivity and light transmittance which is not much different from that in the examples. 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, and the prepared xylo-oligosaccharide has low purity, the light transmittance is not much different from that of the feed liquid in the examples, and the electric conductivity is slightly larger 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 (4)
1. A method for preparing xylo-oligosaccharide from corncob meal is characterized by comprising the following steps:
(1) mixing the corncob meal and 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 corncob meal suspension;
(2) conveying the suspension of the corncob powder to a pressurizing ejector, allowing the suspension to enter a laminar flow tank through the ejector, allowing the material to stay in the laminar flow tank for 50-60min, and finally allowing the suspension to enter a vapor-liquid separator for vapor-liquid separation; recovering waste heat of the flash evaporated secondary steam of the steam-liquid separator;
(3) the liquid after vapor-liquid separation enters a saccharification tank, and the saccharification tank is used for saccharifying every 1m 3 Adding 0.05-0.3kg of xylanase and 0.05-0.3kg of saccharifying enzyme into the materials, controlling the temperature at 50 +/-1 ℃, 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 10%;
(6) the filtrate after decolorization is ultrafiltered, and the discharge light transmittance is more than 30 percent;
(7) concentrating the ultrafiltered filtrate with membrane to obtain material 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 30%;
(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; ion exchange here means: cation and anion exchange combination is adopted, 001 multiplied by 7 cation exchange resin and D301 anion exchange resin are adopted, the temperature of ion exchange treatment is less than 45 ℃, and the flow rate of the ion exchange treatment is 2 times of the volume of the resin per hour; after ion exchange is finished, firstly ejecting the materials by using water until refraction is less than 1%, then regenerating, soaking a cation exchange column by using hydrochloric acid and an anion exchange column by using liquid alkali for 3h, then discharging waste acid and alkali, then leaching by using pure water, wherein the leaching end point of a positive column is 3-3.5, the leaching end point of a negative column is 9.5-10, and reserving after leaching is finished; regenerating hydrochloric acid and liquid alkali, wherein the mass concentration of the hydrochloric acid and the liquid alkali is 3-4%, and the conductivity of the eluted pure water is less than 30 mu s/cm;
(11) 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; 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 ℃;
(12) if granulation is needed, controlling the refractive index of sugar solution obtained by secondary concentration to be 40-60%, carrying out chromatographic purification, increasing the content to be more than 96%, then adding excipient, and carrying out spray granulation to produce granular xylo-oligosaccharide; or if granulation is needed, controlling the refractive index of the sugar solution obtained by secondary concentration to be 40-60%, then adding an excipient, and producing granular xylo-oligosaccharide through spray granulation.
2. The method for preparing xylo-oligosaccharide from corncob meal as claimed in claim 1, wherein in the step (7), a nanofiltration membrane is used for membrane concentration.
3. The method as claimed in claim 1, wherein in the step (2), after the suspension of the corncob meal enters the pressure increasing injector, the steam valve of the pressure increasing injector is opened to heat the material with steam, so that the pressure is 0.6-0.7MPa, and the temperature of the material is kept at 160-170 ℃.
4. The method for preparing xylo-oligosaccharide from hemicellulose according to claim 1, wherein in the step (12), the excipient is at least one of maltodextrin and corncob residue.
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