CN113151614A - Method for preparing xylooligosaccharide from agricultural and forestry waste through two-step acetic acid hydrolysis - Google Patents
Method for preparing xylooligosaccharide from agricultural and forestry waste through two-step acetic acid hydrolysis Download PDFInfo
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title claims abstract description 153
- HEBKCHPVOIAQTA-NGQZWQHPSA-N d-xylitol Chemical compound OC[C@H](O)C(O)[C@H](O)CO HEBKCHPVOIAQTA-NGQZWQHPSA-N 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000002699 waste material Substances 0.000 title claims abstract description 40
- 238000005903 acid hydrolysis reaction Methods 0.000 title claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 35
- 239000007787 solid Substances 0.000 claims abstract description 22
- 229920001221 xylan Polymers 0.000 claims abstract description 19
- 150000004823 xylans Chemical class 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 5
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- 239000002994 raw material Substances 0.000 claims description 8
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- 235000021307 Triticum Nutrition 0.000 claims description 7
- LGQKSQQRKHFMLI-SJYYZXOBSA-N (2s,3r,4s,5r)-2-[(3r,4r,5r,6r)-4,5,6-trihydroxyoxan-3-yl]oxyoxane-3,4,5-triol Chemical compound O[C@@H]1[C@@H](O)[C@H](O)CO[C@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O)OC1 LGQKSQQRKHFMLI-SJYYZXOBSA-N 0.000 claims description 6
- JCSJTDYCNQHPRJ-UHFFFAOYSA-N 20-hydroxyecdysone 2,3-acetonide Natural products OC1C(O)C(O)COC1OC1C(O)C(O)C(OC2C(C(O)C(O)OC2)O)OC1 JCSJTDYCNQHPRJ-UHFFFAOYSA-N 0.000 claims description 6
- LGQKSQQRKHFMLI-UHFFFAOYSA-N 4-O-beta-D-xylopyranosyl-beta-D-xylopyranose Natural products OC1C(O)C(O)COC1OC1C(O)C(O)C(O)OC1 LGQKSQQRKHFMLI-UHFFFAOYSA-N 0.000 claims description 6
- SQNRKWHRVIAKLP-UHFFFAOYSA-N D-xylobiose Natural products O=CC(O)C(O)C(CO)OC1OCC(O)C(O)C1O SQNRKWHRVIAKLP-UHFFFAOYSA-N 0.000 claims description 6
- FTTUBRHJNAGMKL-UHFFFAOYSA-N Xylohexaose Natural products OC1C(O)C(O)COC1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(OC4C(C(O)C(OC5C(C(O)C(O)OC5)O)OC4)O)OC3)O)OC2)O)OC1 FTTUBRHJNAGMKL-UHFFFAOYSA-N 0.000 claims description 6
- LFFQNKFIEIYIKL-UHFFFAOYSA-N Xylopentaose Natural products OC1C(O)C(O)COC1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(OC4C(C(O)C(O)OC4)O)OC3)O)OC2)O)OC1 LFFQNKFIEIYIKL-UHFFFAOYSA-N 0.000 claims description 6
- JVZHSOSUTPAVII-UHFFFAOYSA-N Xylotetraose Natural products OCC(OC1OCC(OC2OCC(OC3OCC(O)C(O)C3O)C(O)C2O)C(O)C1O)C(O)C(O)C=O JVZHSOSUTPAVII-UHFFFAOYSA-N 0.000 claims description 6
- JCSJTDYCNQHPRJ-FDVJSPBESA-N beta-D-Xylp-(1->4)-beta-D-Xylp-(1->4)-D-Xylp Chemical compound O[C@@H]1[C@@H](O)[C@H](O)CO[C@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O)C(O)OC2)O)OC1 JCSJTDYCNQHPRJ-FDVJSPBESA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- KPTPSLHFVHXOBZ-BIKCPUHGSA-N xylotetraose Chemical compound O[C@@H]1[C@@H](O)[C@H](O)CO[C@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O)[C@H](O[C@H]3[C@@H]([C@@H](O)C(O)OC3)O)OC2)O)OC1 KPTPSLHFVHXOBZ-BIKCPUHGSA-N 0.000 claims description 6
- ABKNGTPZXRUSOI-UHFFFAOYSA-N xylotriose Natural products OCC(OC1OCC(OC2OCC(O)C(O)C2O)C(O)C1O)C(O)C(O)C=O ABKNGTPZXRUSOI-UHFFFAOYSA-N 0.000 claims description 6
- 229920002488 Hemicellulose Polymers 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- 238000001125 extrusion Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 239000007788 liquid Substances 0.000 description 11
- 229910001220 stainless steel Inorganic materials 0.000 description 11
- 239000010935 stainless steel Substances 0.000 description 11
- 229920001542 oligosaccharide Polymers 0.000 description 9
- 239000002253 acid Substances 0.000 description 7
- 238000001816 cooling Methods 0.000 description 7
- 238000007789 sealing Methods 0.000 description 7
- 235000018185 Betula X alpestris Nutrition 0.000 description 6
- 235000018212 Betula X uliginosa Nutrition 0.000 description 6
- 241000219000 Populus Species 0.000 description 6
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 5
- 238000010828 elution Methods 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 239000002893 slag Substances 0.000 description 5
- 239000001632 sodium acetate Substances 0.000 description 5
- 235000017281 sodium acetate Nutrition 0.000 description 5
- 238000005571 anion exchange chromatography Methods 0.000 description 4
- 239000000413 hydrolysate Substances 0.000 description 4
- 238000004255 ion exchange chromatography Methods 0.000 description 4
- 230000008961 swelling Effects 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 108010009736 Protein Hydrolysates Proteins 0.000 description 3
- 229920002522 Wood fibre Polymers 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000002025 wood fiber Substances 0.000 description 3
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 238000000703 high-speed centrifugation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 235000013406 prebiotics Nutrition 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 230000000378 dietary effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000003599 food sweetener Nutrition 0.000 description 1
- 235000013376 functional food Nutrition 0.000 description 1
- 230000007413 intestinal health Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000013615 non-nutritive sweetener Nutrition 0.000 description 1
- 150000002482 oligosaccharides Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000003765 sweetening agent Substances 0.000 description 1
- 125000000969 xylosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)CO1)* 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K13/00—Sugars not otherwise provided for in this class
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K13/00—Sugars not otherwise provided for in this class
- C13K13/002—Xylose
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Organic Chemistry (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention provides a method for preparing xylo-oligosaccharide from agricultural and forestry waste by two-step acetic acid hydrolysis, which comprises the following steps: mixing the agricultural and forestry wastes rich in xylan with acetic acid, heating at low temperature for reaction, and separating to obtain a first xylo-oligosaccharide solution and residual solid residues; cleaning the residual solid residues to be neutral, adding acetic acid, mixing, heating for reaction, and separating to obtain a second xylo-oligosaccharide solution; and collecting the first xylo-oligosaccharide solution and the second xylo-oligosaccharide solution. The invention adopts a two-step acidolysis method to efficiently convert xylan components of agricultural and forestry wastes into xylo-oligosaccharide, obtains higher xylo-oligosaccharide yield, and highly utilizes inert xylan components of the agricultural and forestry wastes.
Description
Technical Field
The invention belongs to the technical field of xylo-oligosaccharide preparation, and particularly relates to a method for preparing xylo-oligosaccharide from agricultural and forestry waste through two-step acetic acid hydrolysis.
Background
Xylo-oligosaccharide is functional oligosaccharide formed by connecting xylose units through beta-1, 4-glycosidic bonds, has prebiotic properties of reducing cholesterol, increasing calcium absorption, maintaining intestinal health and the like, is widely applied to the feed industry and the medical care industry, and has extremely high market value due to the low-dose prebiotic effect in human bodies and animal bodies. In addition, xylo-oligosaccharide is a low calorie sweetener with stable properties, which makes xylo-oligosaccharide an ideal component for functional food and dietary sweetener. The wood fiber raw material rich in xylan component is mainly used as the raw material for producing xylo-oligosaccharide in industry. Since the wood fiber raw material is the most abundant agricultural and forestry waste available in the world, the wood fiber raw material serving as the production raw material of the xylo-oligosaccharide with high added value helps to promote the sustainable development and the economic utilization of the agricultural and forestry waste. Currently, various methods for producing xylo-oligosaccharides are widely used, wherein the most popular method is an organic acid pretreatment method, the acetic acid pretreatment method can convert most of hemicellulose xylan components in agricultural and forestry wastes into xylo-oligosaccharides, however, about 30% of inert xylan remained after the one-step method treatment is generally carried out, and the hemicellulose components of the agricultural and forestry wastes are not fully utilized.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made in view of the above-mentioned technical drawbacks.
Therefore, as one aspect of the invention, the invention overcomes the defects in the prior art and provides a method for preparing xylooligosaccharide by two-step acetic acid hydrolysis of agricultural and forestry waste.
In order to solve the technical problems, the invention provides the following technical scheme: a method for preparing xylo-oligosaccharide from agricultural and forestry waste by two-step acetic acid hydrolysis comprises the steps of mixing the agricultural and forestry waste rich in xylan with acetic acid, heating at low temperature for reaction, and separating to obtain a first xylo-oligosaccharide solution and residual solid residues; cleaning the residual solid residues to be neutral, adding acetic acid, mixing, heating for reaction, and separating to obtain a second xylo-oligosaccharide solution; and collecting the first xylo-oligosaccharide solution and the second xylo-oligosaccharide solution.
As a preferred scheme of the method for preparing xylo-oligosaccharide by two-step acetic acid hydrolysis of agricultural and forestry waste, the method comprises the following steps: the low-temperature heating reaction is carried out, wherein the heating temperature is 120-170 ℃, and the time is 20-60 min.
As a preferred scheme of the method for preparing xylo-oligosaccharide by two-step acetic acid hydrolysis of agricultural and forestry waste, the method comprises the following steps: the heating temperature is 170-190 ℃ and the time is 5-30 min.
As a preferred scheme of the method for preparing xylo-oligosaccharide by two-step acetic acid hydrolysis of agricultural and forestry waste, the method comprises the following steps: according to volume fraction, the concentration of the acetic acid in the low-temperature heating reaction is 5% -25%, and the concentration of the acetic acid in the temperature-rising heating reaction is 2.5% -20%.
As a preferred scheme of the method for preparing xylo-oligosaccharide by two-step acetic acid hydrolysis of agricultural and forestry waste, the method comprises the following steps: the agricultural and forestry waste comprises one or more of wheat straw and corncobs.
As a preferred scheme of the method for preparing xylo-oligosaccharide by two-step acetic acid hydrolysis of agricultural and forestry waste, the method comprises the following steps: the separation method is centrifugal filtration or extrusion filtration.
As a preferred scheme of the method for preparing xylo-oligosaccharide by two-step acetic acid hydrolysis of agricultural and forestry waste, the method comprises the following steps: the first xylo-oligosaccharide solution or the second xylo-oligosaccharide solution comprises one or more of xylobiose, xylotriose, xylotetraose, xylopentaose and xylohexaose.
As a preferred scheme of the method for preparing xylo-oligosaccharide by two-step acetic acid hydrolysis of agricultural and forestry waste, the method comprises the following steps: the total xylo-oligosaccharide yield of the first xylo-oligosaccharide solution and the second xylo-oligosaccharide solution can reach 61-64%, and the removal rate of hemicellulose xylan from agricultural and forestry waste can reach more than 90%.
The invention has the beneficial effects that:
the invention adopts a two-step acetic acid hydrolysis method to convert xylan components of agricultural and forestry waste into xylo-oligosaccharide with high added value, can obtain high-concentration xylo-oligosaccharide products, and can realize high utilization of hemicellulose xylan components of the agricultural and forestry waste.
Description of the drawings:
in order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 is a flow chart of a production process in example 1;
FIG. 2 is the composition distribution of the acidolysis solution after the two-step acetic acid acidolysis in example 1;
FIG. 3 shows the composition distribution of the acidolysis solution after two steps of acetic acid acidolysis in example 2.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1:
in 30mLAdding 1.5g of oven-dried corncob powder and 15mL of 21.2% (volume fraction) acetic acid solution into a stainless steel high-temperature reaction kettle, sealing, swelling at normal temperature for 1h, and immersing in a constant-temperature oil tank at 140 ℃ for heat preservation for 60 min; after the reaction is finished, placing the stainless steel high-temperature reaction kettle in cold water for rapid cooling; separating xylo-oligosaccharide solution and residual solid residue obtained in the first step of acidolysis by high-speed centrifugation (3000rpm, 5 min); washing the residual solid slag to neutrality, squeezing water, and balancing water in refrigerator at 4 deg.C. And the second step of acidolysis is still carried out in a 30mL stainless steel high-temperature reaction kettle, the residual solid residue after water washing and 2.5 percent acetic acid solution are added according to the solid-to-liquid ratio of 1:10, the mixture is sealed and immersed in a constant-temperature oil tank at 190 ℃ for heat preservation for 5min, and after the reaction is finished, the cooled hydrolysate and the solid residue are separated through high-speed centrifugation to obtain the xylo-oligosaccharide solution. The obtained xylo-oligosaccharide solution adopts high-efficiency anion exchange chromatography to analyze the sugar concentration and the components, and the chromatographic conditions are as follows: american Saimer fly ICS-3000 type ion chromatography, configured with CarboPacTMPA200(3mm × 250mm) chromatographic column, PAD integrated ampere detector, column temperature 30 deg.C, sample volume 20 μ L; and (3) carrying out binary gradient elution by using 100mmol/L sodium hydroxide and 500mmol/L sodium acetate as mobile phases at the flow rate of 0.3 mL/min. The analytical map is shown in FIG. 2, and xylose (X1), xylobiose (X2), xylotriose (X3), xylotetraose (X4), xylopentaose (X5) and xylohexaose (X6) can be simultaneously detected. As shown in figure 2, after two steps of acetic acid hydrolysis, 13.15g/L xylo-oligosaccharide can be obtained after the first step of acidolysis, 6.84g/L xylo-oligosaccharide can be obtained after the second step of acidolysis, 63.14% of total xylo-oligosaccharide yield can be obtained by finally converting the corncob powder, and the xylan removal rate of the corncobs reaches 91.84%.
In addition, the specific procedure of the binary gradient elution with 100mmol/L sodium hydroxide (NaOH) and 500mmol/L sodium acetate (NaAc) as mobile phase is shown in the following table:
| Time(min) | 100mmol/L NaOH(％) | 500mmol/L NaAc(％) |
| -2.3 | 100 | 0 |
| 7 | 100 | 0 |
| 45 | 65 | 35 |
| 50 | 65 | 35 |
| 50 | 100 | 0 |
| 65 | 100 | 0 |
example 2:
adding 1.5g of oven-dried wheat straw particles and 15mL of 24.9% (volume fraction) acetic acid solution into a 30mL stainless steel high-temperature reaction kettle, sealing, swelling at normal temperature for 1h, and immersing in a constant-temperature oil tank at 140 ℃ for heat preservation for 60 min; after the reaction is finished, placing the reaction kettle in cold water for rapid cooling, taking out acid hydrolysate, centrifugally separating acid hydrolysate from residual solid slag, and collecting xylo-oligosaccharide solution; the remaining solid residue was washed to neutrality, drained and equilibrated at 4 ℃ in a refrigerator. Second acidolysis with first acidolysisMixing the residual solid residues of the wheat straws as a raw material with 4.5% of acetic acid solution in a 30mL stainless steel high-temperature reaction kettle according to a solid-to-liquid ratio of 1:10, sealing, immersing in a 190 ℃ constant-temperature oil tank, preserving the temperature for 5min, taking out after the reaction is finished, immersing in cold water, rapidly cooling, and centrifugally separating acid hydrolysis liquid and the solid residues to obtain xylo-oligosaccharide liquid. The obtained xylo-oligosaccharide solution adopts high-efficiency anion exchange chromatography to analyze the sugar concentration and the components, and the chromatographic conditions are as follows: american Saimer fly ICS-3000 type ion chromatography, configured with CarboPacTMPA200(3mm × 250mm) chromatographic column, PAD integrated ampere detector, column temperature 30 deg.C, sample volume 20 μ L; and (3) carrying out binary gradient elution by using 100mmol/L sodium hydroxide and 500mmol/L sodium acetate as mobile phases at the flow rate of 0.3 mL/min. The xylo-oligosaccharides obtained by the two-step acidolysis all comprise xylobiose (X2), xylotriose (X3), xylotetraose (X4), xylopentaose (X5) and xylohexaose (X6) components, as shown in figure 3, the distribution rule of the xylo-oligosaccharides obtained by the two-step acidolysis is consistent, wherein 7.96g/L xylo-oligosaccharides can be obtained after the first-step acidolysis, 6.10g/L xylo-oligosaccharides can be obtained after the second-step acidolysis, 61.44% of total xylo-oligosaccharides yield can be obtained after the wheat straw particles are subjected to the two-step acetic acid acidolysis, and the removal rate of the xylo-oligosaccharides components in the wheat straw can reach 92.58%.
Example 3:
adding 1.5g of oven-dried poplar wood chips and 15mL of 5% (volume fraction) acetic acid solution into a 30mL stainless steel high-temperature reaction kettle, sealing, swelling at normal temperature for 1h, and immersing in a constant-temperature oil tank at 170 ℃ for heat preservation for 30 min; after the reaction is finished, placing the mixture into cold water for rapid cooling, taking out acid hydrolysate, centrifugally separating acid hydrolysate from poplar solid residues, and collecting xylo-oligosaccharide solution; fully washing the residual poplar solid slag to be neutral, squeezing water, and storing in a refrigerator at 4 ℃ to balance water; mixing the residual solid residue of the poplar and 3.34% acetic acid solution in a 30mL stainless steel high-temperature reaction kettle in a solid-to-liquid ratio of 1:10, sealing, immersing in a 190 ℃ constant-temperature oil tank for a second-step acidolysis reaction for 10min, taking out the stainless steel high-temperature reaction kettle after the reaction is finished, immersing in cold water for rapid cooling, and centrifugally separating acid hydrolysis liquid and solid residue to obtain xylo-oligosaccharide liquid. The obtained xylo-oligosaccharideThe liquid adopts high-efficiency anion exchange chromatography to analyze the sugar concentration and the components, and the chromatographic conditions are as follows: american Saimer fly ICS-3000 type ion chromatography, configured with CarboPacTMPA200(3mm × 250mm) chromatographic column, PAD integrated ampere detector, column temperature 30 deg.C, sample volume 20 μ L; and (3) carrying out binary gradient elution by using 100mmol/L sodium hydroxide and 500mmol/L sodium acetate as mobile phases at the flow rate of 0.3 mL/min. The xylo-oligosaccharide obtained by the two-step acidolysis comprises xylobiose (X2), xylotriose (X3), xylotetraose (X4), xylopentaose (X5) and xylohexaose (X6) which are uniformly distributed, 6.02g/L xylo-oligosaccharide can be obtained by first-step acidolysis of poplar chips, 1.26g/L xylo-oligosaccharide can be obtained by second-step acidolysis, and 40.88% of total xylo-oligosaccharide yield can be obtained by two-step acetic acid hydrolysis.
Example 4
Adding 1.5g of oven-dried birch sawdust and 15mL of 5% (volume fraction) acetic acid solution into a 30mL stainless steel high-temperature reaction kettle, sealing, swelling at normal temperature for 1h, immersing in a constant-temperature oil tank at 160 ℃, and keeping the temperature for 30 min; after the reaction is finished, placing the mixture into cold water for rapid cooling, taking out acid hydrolysate, centrifugally separating acid hydrolysate from birch solid slag, and collecting xylo-oligosaccharide solution; fully washing the residual birch solid slag to be neutral, squeezing water, and storing in a refrigerator at 4 ℃ to balance water; mixing the residual solid residues of the birch and 3.42% acetic acid solution in a 30mL stainless steel high-temperature reaction kettle according to the solid-to-liquid ratio of 1:10, sealing, immersing in a 190 ℃ constant-temperature oil groove for a second-step acidolysis reaction for 12min, taking out the stainless steel high-temperature reaction kettle after the reaction is finished, immersing in cold water for rapid cooling, and centrifugally separating acid hydrolysis liquid and solid residues to obtain xylo-oligosaccharide liquid. The obtained xylo-oligosaccharide solution adopts high-efficiency anion exchange chromatography to analyze the sugar concentration and the components, and the chromatographic conditions are as follows: american Saimer fly ICS-3000 type ion chromatography, configured with CarboPacTMPA200(3mm × 250mm) chromatographic column, PAD integrated ampere detector, column temperature 30 deg.C, sample volume 20 μ L; and (3) carrying out binary gradient elution by using 100mmol/L sodium hydroxide and 500mmol/L sodium acetate as mobile phases at the flow rate of 0.3 mL/min. Xylo-oligosaccharide obtained by two-step acidolysis comprises xylobiose (X2), xylotriose (X3), xylotetraose (X4), xylopentaose (X5) and xylohexaose (X6) components, is uniformly distributed,5.77g/L xylo-oligosaccharide can be obtained from birch sawdust through the first acidolysis, 2.37g/L xylo-oligosaccharide can be obtained through the second acidolysis, and 49.09% of total xylo-oligosaccharide yield can be obtained through the two acetic acid acidolysis.
The invention directly degrades and converts the xylan component of the agricultural and forestry waste into xylo-oligosaccharide by a two-step acetic acid hydrolysis method, and fully utilizes the inert xylan component in the agricultural and forestry waste; the method has high technical universality, is suitable for corncobs, wheat straws, poplar, birch and other straws and broad-leaved wood raw materials, and is also suitable for other organic acids; the reaction temperature, the acetic acid concentration and the heat preservation time of the two-step acetic acid hydrolysis are strictly controlled to avoid excessive degradation of xylan components of agricultural and forestry wastes, the first-step acid hydrolysis process is preferably low-temperature acid hydrolysis and can ensure that fast xylan is preferentially degraded, and the second-step acid hydrolysis process is carried out under the conditions of high temperature, low acid concentration and short time and can gradually hydrolyze inert xylan components. The invention adopts a two-step acetic acid hydrolysis method, so that the xylan component of the agricultural and forestry waste can be highly utilized, and higher-concentration xylooligosaccharide can be obtained compared with a one-step method.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (8)
1. A method for preparing xylo-oligosaccharide from agricultural and forestry waste by two-step acetic acid hydrolysis is characterized by comprising the following steps: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
mixing the agricultural and forestry wastes rich in xylan with acetic acid, heating at low temperature for reaction, and separating to obtain a first xylo-oligosaccharide solution and residual solid residues;
cleaning the residual solid residues to be neutral, adding acetic acid, mixing, heating for reaction, and separating to obtain a second xylo-oligosaccharide solution;
and collecting the first xylo-oligosaccharide solution and the second xylo-oligosaccharide solution.
2. The method for preparing xylo-oligosaccharide from agricultural and forestry waste by two-step acetic acid hydrolysis as claimed in claim 1, wherein: the low-temperature heating reaction is carried out, wherein the heating temperature is 120-170 ℃, and the time is 20-60 min.
3. The method for preparing xylo-oligosaccharide from agricultural and forestry waste by two-step acetic acid hydrolysis as claimed in claim 1, wherein: the heating temperature is 170-190 ℃ and the time is 5-30 min.
4. The method for preparing xylo-oligosaccharide from agricultural and forestry waste by two-step acetic acid hydrolysis as claimed in claim 1, wherein: according to volume fraction, the concentration of the acetic acid in the low-temperature heating reaction is 5% -25%, and the concentration of the acetic acid in the temperature-rising heating reaction is 2.5% -20%.
5. The method for preparing xylo-oligosaccharide from agricultural and forestry waste by two-step acetic acid hydrolysis as claimed in any one of claims 1 to 4, wherein: the agricultural and forestry waste comprises one or more of wheat straw and corncobs.
6. The method for preparing xylo-oligosaccharide from agricultural and forestry waste by two-step acetic acid hydrolysis as claimed in claim 5, wherein: the separation method is centrifugal filtration or extrusion filtration.
7. The method for preparing xylo-oligosaccharide from agricultural and forestry waste by two-step acetic acid hydrolysis as claimed in claim 1, wherein: the first xylo-oligosaccharide solution or the second xylo-oligosaccharide solution comprises one or more of xylobiose, xylotriose, xylotetraose, xylopentaose and xylohexaose.
8. The method for preparing xylo-oligosaccharide from agricultural and forestry waste by two-step acetic acid hydrolysis as claimed in claim 1, wherein: the total xylo-oligosaccharide yield of the first xylo-oligosaccharide solution and the second xylo-oligosaccharide solution can reach 61-64%, and the removal rate of hemicellulose xylan from agricultural and forestry waste can reach more than 90%.
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