CN114736249B - Method for preparing functional xylo-oligosaccharide by using agricultural and forestry waste bamboo powder - Google Patents
Method for preparing functional xylo-oligosaccharide by using agricultural and forestry waste bamboo powder Download PDFInfo
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- CN114736249B CN114736249B CN202210440213.0A CN202210440213A CN114736249B CN 114736249 B CN114736249 B CN 114736249B CN 202210440213 A CN202210440213 A CN 202210440213A CN 114736249 B CN114736249 B CN 114736249B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
- C07H3/04—Disaccharides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
- C07H3/06—Oligosaccharides, i.e. having three to five saccharide radicals attached to each other by glycosidic linkages
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0057—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Xylans, i.e. xylosaccharide, e.g. arabinoxylan, arabinofuronan, pentosans; (beta-1,3)(beta-1,4)-D-Xylans, e.g. rhodymenans; Hemicellulose; Derivatives thereof
Abstract
The invention discloses a method for preparing functional xylo-oligosaccharide by utilizing agricultural and forestry waste bamboo powder. The method comprises the steps of taking bamboo powder as a raw material, extracting under the catalysis of low-concentration inorganic acid to obtain crude sugar solution, purifying the crude sugar solution, and finally spray-drying to obtain the xylooligosaccharide powder. The residue produced during extraction of the crude sugar solution can be used in the fields of papermaking, fuel and the like through a digestion pulping or compression molding technology. Byproducts such as calcium phosphate and the like are generated in the purification process of the crude sugar solution, and the byproducts can be recycled, so that the cost investment is reduced. The reaction condition is that the temperature is 100-140 ℃. The time is 70-120 min, and the stirring speed is 500r/min. The production process is simple, has strong practicability, not only improves the economic value of the product, but also better solves the problem of utilizing the bamboo powder of the agricultural and forestry waste, and can not produce wastewater, only has low-concentration brine, avoids the extra energy input and economy caused by wastewater treatment, and the whole production process is cleaner and environment-friendly.
Description
Technical Field
The invention belongs to the field of biochemistry, and particularly relates to a method for preparing functional xylo-oligosaccharide and purifying the functional xylo-oligosaccharide by utilizing agricultural and forestry waste bamboo powder.
Background
Bamboo chips are waste resources rich in cellulose and xylan, wherein the content of the cellulose and the xylan is about 40% and about 20% respectively. The waste resources are deeply processed by adopting a biotechnology method, so that high-added-value sugar engineering products, biological energy sources, bulk chemicals and the like can be produced, the resource utilization rate and the economic value can be improved, and the method has important significance for relieving the energy shortage problem in China, saving energy, reducing emission and developing rural economy. The xylooligosaccharide is oligosaccharide composed of 2-7 xylose units, is derived from hemicellulose rich in xylan, is connected through beta-1, 4 glycosidic bonds, and is an important functional food. The xylooligosaccharide has a plurality of functional characteristics, has obvious high selective proliferation effect on beneficial intestinal bacteria (bifidobacteria and lactobacillus), has obvious inhibition effect on pathogenic bacteria such as escherichia coli, enterococcus, clostridium and the like, can provide excellent intestinal protection effect, and is called as super-strong bifidus factor. In addition, it has immunomodulating activity, anticancer activity, antimicrobial activity, antiallergic, anti-infective and anti-inflammatory properties, immunomodulating effect, anti-hyperlipidemia effect, and can be used for growth regulation in aquaculture and poultry. Therefore, the functional xylo-oligosaccharide has great market potential.
Disclosure of Invention
In view of the background, the invention provides a method for preparing functional xylo-oligosaccharide by using agricultural and forestry waste bamboo powder.
The invention provides a method for preparing functional xylo-oligosaccharide by utilizing agricultural and forestry waste bamboo powder, which is characterized by comprising the following steps:
firstly, mixing raw material bamboo powder with an aqueous solution of a phosphoric acid catalyst by taking agricultural and forestry waste bamboo powder as a raw material, heating and stirring at a high temperature, cooling, and performing filter pressing to obtain a crude sugar solution;
secondly, adding calcium oxide to regulate the pH, adding activated carbon to decolorize, filtering to obtain sugar solution after decolorization, and concentrating the sugar solution by a membrane;
and thirdly, spray drying the sugar solution to obtain the product, namely the xylooligosaccharide powder.
In a preferred embodiment, the aqueous catalyst solution is a phosphoric acid solution having a phosphoric acid concentration of 0.08% to 0.12% (w/v).
In a specific embodiment, in the first step, the high temperature is used for heating and stirring, the temperature is 90-140 ℃ (preferably 100-120 ℃), the time is 60-100min (preferably 70-90 min), and the stirring speed is 400-500 r/min.
In the second step, preferably, the crude sugar solution is treated, and 0.37 to 0.4 percent (w/v) of calcium oxide is added for neutralization, so that the pH value of the solution is adjusted to 4 to 5; then adding 0.2% -0.4% (w/v) 200-mesh food-grade sugar activated carbon into the solution.
Further preferably, in the second step, the membrane concentration is ultrafiltration or nanofiltration, and the ultrafiltration membrane has a molecular weight cut-off of 2500 daltons; ultrafiltering under the conditions of operation pressure of 1.5-2.5 MPa and membrane temperature at room temperature; nanofiltration membrane with molecular weight cut-off of 150Dalton is carried out under the conditions of operating pressure of 1.5MPa-2.5MPa and membrane temperature at room temperature.
And the third step also comprises adding maltodextrin into the obtained xylooligosaccharide concentrated sugar solution, stirring, and then performing spray drying to obtain the functional xylooligosaccharide powder.
Preferably, in the third step, the obtained xylooligosaccharide concentrated sugar solution is prepared according to the mass ratio of 1:0.5-2, adding maltodextrin, stirring, and spray drying.
The invention provides xylooligosaccharide powder obtained by the method for preparing functional xylooligosaccharide by utilizing agricultural and forestry waste bamboo powder. Wherein the xylooligosaccharide powder contains one or more of xylobiose, xylotriose, xylotetraose, xylopentaose, xylohexaose and xyloheptaose.
The invention takes agriculture and forestry waste bamboo powder as raw material, crude sugar liquid is obtained by extraction under the catalysis of phosphoric acid with lower concentration, and residues generated during the extraction of the obtained crude sugar liquid can be used in the fields of papermaking, fuel and the like through a digestion pulping or compression molding technology. And byproducts such as calcium phosphate and the like are generated in the purification process of the crude sugar solution, and the byproducts can be recycled, so that the cost investment is reduced, and finally, the xylooligosaccharide powder is obtained through spray drying. The catalyst has the advantages of low concentration, short reaction time and strong practicability, not only improves the economic value of the product, but also better solves the problem of utilizing the bamboo powder of the agricultural and forestry waste, and the production process can not generate waste water, avoids the extra energy input and economy caused by waste water treatment, and is cleaner and environment-friendly and easy for industrialized production.
Drawings
FIG. 1 is a process flow diagram of a process for preparing functional xylo-oligosaccharides from bamboo powder.
FIG. 2 is a liquid chromatogram of a bamboo powder for preparing functional xylo-oligosaccharide.
Figure 3 XRD spectrum of solid precipitate.
FIG. 4 shows the comparison of sugar solutions before and after decolorization of xylooligosaccharide sugar solutions.
Detailed Description
The invention is further illustrated with reference to examples. Unless otherwise specified, the reagents and equipment used in the examples below, except for the ball-type reactors, were developed on their own and the rest were commercially available products. The specific implementation cases are as follows:
example 1
Preparation of the catalyst: taking 1g of 99% phosphoric acid solution in a 200ml beaker, adding 100 deionized water, and stirring for 30 min.
In the first step, 5g of bamboo powder and 0.5g of prepared H are mixed 3 PO 4 (mixing aqueous solution with concentration of 0.1% (w/v) and solid-liquid ratio of 1:10; loading into high-pressure reaction tank, heating to 100deg.C for reaction for 90min, and vacuum filtering to separate sugar solution, and performing qualitative and quantitative analysis by liquid phase mass spectrometry (HPLC, agilent) to obtain xylooligosaccharide yield of 25.2%.
Secondly, ultrafiltration is carried out at the membrane temperature of about 2MPa of operating pressure and at the room temperature by using an ultrafiltration membrane with the molecular weight cutoff of 2500Dalton; the molecular weight cut-off of the nanofiltration membrane is 150Dalton, ultrafiltration is carried out at the operating pressure of about 2MPa and the membrane temperature at room temperature, and the result is that: the yield of the xylooligosaccharide is 20.4%.
Thirdly, the xylooligosaccharide concentrated sugar solution obtained in the step is prepared according to the mass ratio of 1:1 adding maltodextrin, stirring and then spray drying. The result is that: the yield of the xylooligosaccharide powder is 24.8%.
Example 2
Preparation of the catalyst: taking 1g of sulfuric acid solution with the mass fraction of 99% in a 200ml beaker, adding 100 deionized water, and stirring for 30 min.
In the first step, 5g of bamboo powder and 0.5g of prepared H are mixed 2 SO 4 (mixing aqueous solution with concentration of 0.1% (w/v) and solid-liquid ratio of 1:10; loading into high-pressure reaction tank, heating to 100deg.C for reaction for 90min, and vacuum filtering to separate sugar solution, and performing qualitative and quantitative analysis by liquid phase mass spectrometry (HPLC, agilent) to obtain xylooligosaccharide with yield of 20.2%.
Secondly, ultrafiltration is carried out at the membrane temperature of about 2MPa of operating pressure and at the room temperature by using an ultrafiltration membrane with the molecular weight cutoff of 2500Dalton; the molecular weight cut-off of the nanofiltration membrane is 150Dalton, ultrafiltration is carried out at the operating pressure of about 2MPa and the membrane temperature at room temperature, and the result is that: the yield of the xylooligosaccharide is 16.4%.
Thirdly, the xylooligosaccharide concentrated sugar solution obtained in the step is prepared according to the mass ratio of 1:1 adding maltodextrin, stirring and then spray drying. The result is that: the yield of the xylooligosaccharide powder is 19.8%.
Example 3
The reaction was carried out as in example 1, except that the reaction temperature was 110 ℃. The reaction gave the following results: the yield of the xylooligosaccharide is 40.8%. The second step, the result is: the yield of the xylooligosaccharide is 35.2%. The third step, the result is: the yield of the xylooligosaccharide powder is 40.5%.
Example 4
The reaction was carried out as in example 1, except that the reaction temperature was 120 ℃. The reaction gave the following results: the yield of the xylooligosaccharide is 55.2%. The second step, the result is: the yield of the xylooligosaccharide is 50.1%. The third step, the result is: the yield of the xylooligosaccharide powder is 55.2%.
Example 5
The reaction was carried out as in example 1, except that the reaction temperature was 130 ℃. The reaction gave the following results: the yield of the xylooligosaccharide is 45.5%. The second step, the result is: the yield of the xylooligosaccharide is 35.2%. The third step, the result is: the yield of the xylooligosaccharide powder is 44.6%.
Example 6
The reaction was carried out as in example 1 except that the reaction temperature was 140 ℃. The reaction gave the following results: the yield of the xylooligosaccharide is 40.3%. The second step, the result is: the yield of the xylooligosaccharide is 35.8%. The third step, the result is: the yield of the xylooligosaccharide powder is 39.5%.
Example 7
The reaction was carried out as in example 1 except that the reaction temperature was 120℃and the catalyst concentration was 0.08% (w/v). The reaction gave the following results: the yield of xylo-oligosaccharide is 44.7%. The second step, the result is: the yield of the xylooligosaccharide is 40.5%. The third step, the result is: the yield of the xylooligosaccharide powder is 47.2%.
Example 8
The reaction was carried out as in example 1 except that the reaction temperature was 120℃and the catalyst concentration was 0.12% (w/v). The reaction gave the following results: the yield of the xylooligosaccharide is 50.8%. The second step, the result is: the yield of the xylooligosaccharide is 45.2%. The third step, the result is: the yield of the xylooligosaccharide powder is 50.2%.
Example 9
The reaction was carried out as in example 1 except that the reaction temperature was 120℃and the time was 70 minutes. The reaction gave the following results: the yield of the xylooligosaccharide is 49.6%. The second step, the result is: the yield of the xylooligosaccharide is 45.2%. The third step, the result is: the yield of the xylooligosaccharide powder is 49.2%.
Example 10
The reaction was carried out as in example 1 except that the reaction temperature was 120℃and the time was 80 minutes. The reaction gave the following results: the yield of the xylooligosaccharide is 52.7%. The second step, the result is: the yield of xylo-oligosaccharide is 47.2%. The third step, the result is: the yield of the xylooligosaccharide powder is 51.8%.
Example 11
The reaction was carried out as in example 1 except that the reaction temperature was 120℃and the time was changed to 100 minutes. The reaction gave the following results: the yield of the xylooligosaccharide is 54.2%. The second step, the result is: the yield of the xylooligosaccharide is 50.8%. The third step, the result is: the yield of the xylooligosaccharide powder is 53.5%.
Example 12
The reaction was carried out as in example 1 except that the reaction temperature was 120℃and the time was 110 minutes. The reaction gave the following results: the yield of the xylooligosaccharide is 46.2%. The second step, the result is: the yield of the xylooligosaccharide is 40.8%. The third step, the result is: the yield of the xylooligosaccharide powder is 45.8%.
The results are summarized in the following table:
TABLE 1 influence of the yield of xylo-oligosaccharides under different conditions
According to the results of the above embodiment, 0.1% H 3 PO 4 In order to obtain better yield of the xylo-oligosaccharide by the catalyst, the yield of the crude sugar solution obtained by direct acid extraction and the yield of the xylo-oligosaccharide obtained by spray drying after maltose is added are basically kept unchanged. Under the optimal conditions, namely the reaction temperature is 120 ℃, the reaction time is 90min, the catalyst concentration is 0.1% (w/v), and the yield of the xylooligosaccharide powder is 55.2%.
The specific examples of the present invention are for illustrative purposes only, and the catalyst is applicable to the conversion of lignocellulosic biomass to xylooligosaccharides. It is not intended to limit the scope of the invention in any way, and a person skilled in the art can modify or change the invention according to the description above, all such modifications and changes being intended to fall within the scope of the appended claims.
Claims (6)
1. A method for preparing functional xylo-oligosaccharide by using agricultural and forestry waste bamboo powder is characterized by comprising the following steps:
firstly, mixing raw material bamboo powder with aqueous solution of phosphoric acid catalyst by taking agricultural and forestry waste bamboo powder as raw material, heating and stirring at a high temperature of 90-140 ℃, cooling and pressure-filtering to obtain crude sugar solution; wherein, the concentration of phosphoric acid is 0.08% -0.12% (w/v);
secondly, treating the crude sugar solution, adding 0.37% -0.4% (w/v) of calcium oxide for neutralization, and adjusting the pH value of the solution to 4-5; then adding 0.2% -0.4% (w/v) 200-mesh food-grade active carbon for sugar into the solution, decoloring, filtering to obtain sugar solution, and concentrating by a membrane;
and thirdly, adding maltodextrin into the sugar solution after membrane concentration, stirring and spray drying to obtain the xylooligosaccharide powder.
2. The method for preparing functional xylo-oligosaccharide by using agricultural and forestry waste bamboo powder according to claim 1, which is characterized by comprising the following steps: in the first step, the high temperature heating and stirring are carried out for 60-100min at a stirring speed of 400-500 r/min.
3. The method for preparing functional xylo-oligosaccharide by using agricultural and forestry waste bamboo powder according to claim 1, which is characterized by comprising the following steps: in the second step, membrane concentration is ultrafiltration or nanofiltration, and the molecular weight cut-off of an ultrafiltration membrane is 2500Dalton; ultrafiltering under the conditions of operation pressure of 1.5-2.5 MPa and membrane temperature at room temperature; nanofiltration membrane with molecular weight cut-off of 150Dalton is carried out under the conditions of operating pressure of 1.5MPa-2.5MPa and membrane temperature at room temperature.
4. The method for preparing functional xylo-oligosaccharide by using agricultural and forestry waste bamboo powder according to claim 1, which is characterized by comprising the following steps: and thirdly, the obtained xylooligosaccharide concentrated sugar solution is subjected to a mass ratio of 1:0.5-2, adding maltodextrin, stirring, and spray drying.
5. The xylooligosaccharide powder obtained by the method for preparing functional xylooligosaccharide by using agricultural and forestry waste bamboo powder according to any one of claims 1 to 4.
6. The xylooligosaccharide powder as claimed in claim 5, wherein: it contains one or more of xylobiose, xylotriose, xylotetraose, xylopentaose, xylohexaose and xyloheptaose.
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Citations (4)
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CN102286571A (en) * | 2011-06-16 | 2011-12-21 | 北京化工大学 | Clean and high-efficiency production process for preparing xylose and L-arabinose |
CN103320548A (en) * | 2013-06-24 | 2013-09-25 | 稼禾生物股份有限公司 | Method for preparing xylooligosaccharide and cellulose by using crop straws |
CN107116654A (en) * | 2017-06-20 | 2017-09-01 | 博莱维(厦门)生物科技有限公司 | A kind of bamboo wood full constituent comprehensive utilization process |
CN111004827A (en) * | 2019-12-27 | 2020-04-14 | 山东百龙创园生物科技股份有限公司 | Preparation method of xylo-oligosaccharide |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN102286571A (en) * | 2011-06-16 | 2011-12-21 | 北京化工大学 | Clean and high-efficiency production process for preparing xylose and L-arabinose |
CN103320548A (en) * | 2013-06-24 | 2013-09-25 | 稼禾生物股份有限公司 | Method for preparing xylooligosaccharide and cellulose by using crop straws |
CN107116654A (en) * | 2017-06-20 | 2017-09-01 | 博莱维(厦门)生物科技有限公司 | A kind of bamboo wood full constituent comprehensive utilization process |
CN111004827A (en) * | 2019-12-27 | 2020-04-14 | 山东百龙创园生物科技股份有限公司 | Preparation method of xylo-oligosaccharide |
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