CN112679558A - Method for separating and preparing high-purity xylobiose from lignocellulose hydrolysate - Google Patents
Method for separating and preparing high-purity xylobiose from lignocellulose hydrolysate Download PDFInfo
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Abstract
The invention discloses a method for separating and preparing high-purity xylobiose from lignocellulose hydrolysate. Firstly, the active carbon is adopted to selectively adsorb sugar in the hydrolysate, then the simple water washing method is adopted to remove monosaccharide, buffer salt and other impurities with weak combination, finally the low-concentration organic solvent is adopted to desorb and recover xylobiose, and the desorption solution is subjected to reduced pressure distillation and freeze drying to obtain high-purity xylobiose powder. The separation preparation process has the advantages of simple steps, low treatment cost, environmental protection and the like. In addition, the adopted activated carbon has good recycling performance after being dried, so the method has good industrial application prospect. The invention solves the problems of complicated steps, high cost and the like in the existing technology for preparing high-purity xylobiose.
Description
Technical Field
The invention relates to the field of preparation of glycosyl compounds, in particular to a method for separating and preparing high-purity xylobiose from lignocellulose hydrolysate.
Background
Xylo-oligosaccharide is functional oligosaccharide consisting of 2-7 xylo-oligosaccharides, can selectively promote the growth of beneficial bacteria, inhibit the growth of other harmful bacteria, and further enhance the immune system of an organism. With the increasing demand of industries such as food, health care products, medicine and the like on xylo-oligosaccharide, the requirement of the market on the quality of the xylo-oligosaccharide is continuously improved. The enzymatic hydrolysis method is a main method for producing xylo-oligosaccharide by using lignocellulose raw materials such as bagasse, corncobs, straws and the like, and the xylo-oligosaccharide-rich lignocellulose enzymatic hydrolysate contains substances such as saccharides (monosaccharides and xylo-oligosaccharides with various polymerization degrees), proteins (endo-xylanase), salts (buffer salts), pigments and the like. The refining process of xylo-oligosaccharide usually comprises the steps of ultrafiltration (removing macromolecular zymoprotein and undegraded xylan), activated carbon adsorption (decolorization), nanofiltration (removing monosaccharides such as xylose and arabinose) and ion exchange (desalination), and the like, so that the xylo-oligosaccharide product with better quality can be obtained. Xylobiose is the main effective component in xylo-oligosaccharide, and because the physical and chemical properties of xylobiose, xylose and other xylo-oligosaccharides are similar, the difficulty in separating xylobiose from xylo-oligosaccharide is high, and in addition, the decolorization and desalination process in the refining process of xylo-oligosaccharide is complex and has high cost. Gel chromatography is a common method for separating and preparing xylobiose, and patent CN 106046066B proposes a method for purifying and preparing xylobiose, which comprises the steps of firstly removing protein from xylanase hydrolysate through ultrafiltration, then utilizing resin to desalt, and then utilizing a sephadex chromatographic column to purify and prepare the xylobiose, wherein the steps are relatively complicated, and the adopted resin and sephadex chromatography have relatively high cost. In patent CN 1847254A, an ultrafiltration membrane is adopted to intercept undegraded high polymers, and then polyacrylamide gel chromatography is used to separate xylooligosaccharide with polymerization degree of 2-8, wherein the purity can reach more than 90%, but the gel is expensive and difficult to regenerate, so that the industrial application is limited. In patent CN 103319545B, xylobiose with higher purity can be obtained by ethanol precipitation, washing, decoloring and impurity removal, enzyme hydrolysis in a membrane enzyme reactor and purification in a simulated moving bed, but the cost of repeated washing and impurity removal of ethanol is high, and specific equipment is required for subsequent hydrolysis and purification, so that large-scale popularization and application are difficult.
Disclosure of Invention
The invention aims to provide a method for separating and preparing high-purity xylobiose from lignocellulose hydrolysate, and the separation and preparation process has the advantages of simple steps, low treatment cost, environmental friendliness and the like.
The invention is realized by the following technical scheme:
a method for separating and preparing high-purity xylobiose from lignocellulose hydrolysate comprises the following steps:
(1) adsorption: adding active carbon into the lignocellulose enzyme hydrolysate rich in xylo-oligosaccharide, adsorbing for 5-60 min at 20-60 ℃, and performing solid-liquid separation after the reaction is finished to obtain an active carbon filter cake;
(2) removing impurities: washing the activated carbon filter cake with water with 2-5 times volume of hydrolysate until no monosaccharide or buffer salt is detected;
(3) desorption: eluting the impurity-removed active carbon filter cake by using a low-concentration organic solvent aqueous solution with the volume of 2-5 times that of the hydrolysate, and collecting the eluent;
(4) concentration and freeze-drying: and removing and recovering the organic solvent in the eluent by reduced pressure distillation, pre-freezing the xylobiose solution, and freeze-drying the xylobiose solution into powder in a freeze dryer to obtain the high-purity xylobiose.
Preferably, the adding amount of the active carbon is 8-20% of the mass of the lignocellulose hydrolysate.
Preferably, the volume fraction of the organic solvent in the organic solvent aqueous solution is 2.5-10%.
Preferably, the organic solvent is selected from one of methanol, ethanol and acetone.
The invention has the technical effects that:
(1) the separation and purification of high-purity xylobiose from lignocellulose hydrolysate requires the removal of pigments, proteins, buffer salts, monosaccharides and other xylooligosaccharide components. According to the method, the high-purity xylobiose can be obtained by removing proteins and pigments by using the activated carbon, selectively adsorbing xylobiose components, and then removing impurities by using simple water washing and eluting by using a low-concentration organic solvent.
(2) The active carbon adopted by the invention can be recycled, and the adsorption performance can be kept stable after 5 times of recycling, so that the method has a good industrial application prospect.
Drawings
FIG. 1 is a process flow diagram for separating and preparing high-purity xylobiose from lignocellulose hydrolysate.
FIG. 2 is a high performance liquid chromatogram of the process for separating and preparing high-purity xylobiose from lignocellulose hydrolysate. Wherein 1, the lignocellulose hydrolysate 2, the adsorption solution 3, the washing impurity removal solution 4, the desorption solution (eluent) 5 and the xylobiose concentrated solution are washed with water.
FIG. 3 is an evaluation of the cycling performance of activated carbon.
Detailed Description
The following examples are further illustrative of the present invention and are not intended to be limiting thereof.
The process flow chart of the process for separating and preparing high-purity xylobiose from lignocellulose hydrolysate in the following example is shown in figure 1, and the high performance liquid chromatogram is shown in figure 2.
Example 1:
weighing 8 parts by weight of active carbon, adding 100 parts by weight of lignocellulose hydrolysate rich in xylo-oligosaccharide, adsorbing in a shaking table at 60 ℃ for 60min, taking out, carrying out solid-liquid separation to obtain an active carbon filter cake, washing the active carbon filter cake with 200 parts by weight of water until no monosaccharide or buffer salt is detected, then washing the active carbon filter cake with 200 parts by weight of 5% ethanol water solution by volume fraction, collecting eluent, carrying out reduced pressure distillation to remove organic solvent, and freeze-drying to obtain a xylobiose sample with purity of more than 95% and yield of 46.53%.
Example 2:
weighing 8 parts by weight of active carbon, adding 100 parts by weight of lignocellulose hydrolysate rich in xylo-oligosaccharide, adsorbing in a shaking table at 20 ℃ for 5min, taking out, carrying out solid-liquid separation to obtain an active carbon filter cake, washing the active carbon filter cake with 200 parts by weight of water until no monosaccharide or buffer salt is detected, washing the active carbon filter cake with 200 parts by weight of 5% ethanol water solution by volume fraction, collecting eluent, carrying out reduced pressure distillation to remove organic solvent, and freeze-drying to obtain a xylobiose sample with purity of more than 95% and yield of 48.14%.
Example 3:
weighing 12 parts by weight of activated carbon, adding 100 parts by weight of lignocellulose hydrolysate rich in xylo-oligosaccharide, adsorbing in a shaking table at 20 ℃ for 10min, taking out, carrying out solid-liquid separation to obtain an activated carbon filter cake, washing the activated carbon filter cake with 500 parts by weight of water until no monosaccharide or buffer salt is detected, washing the activated carbon filter cake with 500 parts by weight of 5% ethanol water solution by volume fraction, collecting eluent, carrying out reduced pressure distillation to remove organic solvent, and freeze-drying to obtain a xylobiose sample with purity of more than 95% and yield of 52.93%.
Example 4:
weighing 20 parts by weight of activated carbon, adding 100 parts by weight of lignocellulose hydrolysate rich in xylo-oligosaccharide, adsorbing in a shaking table at 20 ℃ for 10min, taking out, carrying out solid-liquid separation to obtain an activated carbon filter cake, washing the activated carbon filter cake with 500 parts by weight of water until no monosaccharide or buffer salt is detected, washing the activated carbon filter cake with 500 parts by weight of 5% ethanol water solution by volume fraction, collecting eluent, carrying out reduced pressure distillation to remove organic solvent, and freeze-drying to obtain a xylobiose sample with purity of more than 95% and yield of 75.09%.
Example 5:
weighing 12 parts by weight of active carbon, adding 100 parts by weight of lignocellulose hydrolysate rich in xylo-oligosaccharide, adsorbing in a shaking table at 20 ℃ for 10min, taking out, carrying out solid-liquid separation to obtain an active carbon filter cake, washing the active carbon filter cake with 200 parts by weight of water until no monosaccharide or buffer salt is detected, then washing the active carbon filter cake with 300 parts by weight of acetone aqueous solution with volume fraction of 5%, collecting eluent, carrying out reduced pressure distillation to remove organic solvent, and freeze-drying to obtain a xylobiose sample with purity of more than 95% and yield of 70.39%.
Example 6:
weighing 16 parts by weight of activated carbon, adding 100 parts by weight of lignocellulose hydrolysate rich in xylo-oligosaccharide, adsorbing in a shaking table at 20 ℃ for 10min, taking out, carrying out solid-liquid separation to obtain an activated carbon filter cake, washing the activated carbon filter cake with 300 parts by weight of water until no monosaccharide or buffer salt is detected, washing the activated carbon filter cake with 500 parts by weight of 5% methanol aqueous solution by volume fraction, collecting eluent, carrying out reduced pressure distillation to remove organic solvent, and freeze-drying to obtain a xylobiose sample with the purity of more than 95% and the yield of 49.34%.
Example 7:
weighing 16 parts by weight of activated carbon, adding 100 parts by weight of lignocellulose hydrolysate rich in xylo-oligosaccharide, adsorbing in a shaking table at 20 ℃ for 10min, taking out, carrying out solid-liquid separation to obtain an activated carbon filter cake, washing the activated carbon filter cake with 300 parts by weight of water until no monosaccharide or buffer salt is detected, washing the activated carbon filter cake with 500 parts by weight of 2.5% ethanol water solution by volume fraction, collecting eluent, carrying out reduced pressure distillation to remove organic solvent, and freeze-drying to obtain a xylobiose sample with purity of more than 95% and yield of 64.38%.
Example 8:
weighing 16 parts by weight of activated carbon, adding 100 parts by weight of lignocellulose hydrolysate rich in xylo-oligosaccharide, adsorbing in a shaking table at 20 ℃ for 10min, taking out, carrying out solid-liquid separation to obtain an activated carbon filter cake, washing the activated carbon filter cake with 300 parts by weight of water until no monosaccharide or buffer salt is detected, washing the activated carbon filter cake with 500 parts by weight of 10% ethanol aqueous solution by volume fraction, collecting eluent, carrying out reduced pressure distillation to remove organic solvent, and freeze-drying to obtain a xylobiose sample with purity of more than 85% and yield of 75.62%.
Example 9:
referring to the procedure of example 1, the activated carbon was recovered and recycled 5 times to evaluate the recycling performance of the activated carbon, and the results are shown in FIG. 3. As can be seen from FIG. 3, the xylobiose adsorbing efficiency of the activated carbon after being recycled for 5 times is still more than 95%, which shows that the xylobiose prepared by the activated carbon adsorption and separation method has stable properties and good industrial application prospects.
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.
Claims (4)
1. A method for separating and preparing high-purity xylobiose from lignocellulose hydrolysate is characterized by comprising the following steps:
(1) adsorption: adding active carbon into the lignocellulose enzyme hydrolysate rich in xylo-oligosaccharide, adsorbing for 5-60 min at 20-60 ℃, and performing solid-liquid separation after the reaction is finished to obtain an active carbon filter cake;
(2) removing impurities: washing the activated carbon filter cake with water with 2-5 times volume of hydrolysate until no monosaccharide or buffer salt is detected;
(3) desorption: eluting the impurity-removed active carbon filter cake by using a low-concentration organic solvent aqueous solution with the volume of 2-5 times that of the hydrolysate, and collecting the eluent;
(4) concentration and freeze-drying: and removing and recovering the organic solvent in the eluent by reduced pressure distillation, pre-freezing the xylobiose solution, and freeze-drying the xylobiose solution into powder in a freeze dryer to obtain the high-purity xylobiose.
2. The method according to claim 1, wherein the amount of the activated carbon added is 8-20% of the mass of the lignocellulose hydrolysate.
3. The method according to claim 1, wherein the volume fraction of the organic solvent in the aqueous solution of the organic solvent is 2.5% to 10%.
4. The method according to claim 1 or 3, wherein the organic solvent is selected from one of methanol, ethanol and acetone.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101632877A (en) * | 2009-08-17 | 2010-01-27 | 山东龙力生物科技有限公司 | Method for separating and purifying components of xylo-oligosaccharide |
| CN103789376A (en) * | 2014-02-21 | 2014-05-14 | 青岛博智汇力生物科技有限公司 | Method of extracting xylo-oligosaccharide from bamboo shoot shells and separating to obtain xylo-oligosaccharide monomer |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101632877A (en) * | 2009-08-17 | 2010-01-27 | 山东龙力生物科技有限公司 | Method for separating and purifying components of xylo-oligosaccharide |
| CN103789376A (en) * | 2014-02-21 | 2014-05-14 | 青岛博智汇力生物科技有限公司 | Method of extracting xylo-oligosaccharide from bamboo shoot shells and separating to obtain xylo-oligosaccharide monomer |
Non-Patent Citations (2)
| Title |
|---|
| 候丽芬 等: "树脂和活性炭法分离纯化低聚木糖的研究", 《农产品加工•学刊》 * |
| 石波 等: "低聚木糖的制备与分离", 《食品工业科技》 * |
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