CN112877482A - Method for extracting xylooligosaccharide from camellia oleifera shells - Google Patents
Method for extracting xylooligosaccharide from camellia oleifera shells Download PDFInfo
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- 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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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F5/00—Fertilisers from distillery wastes, molasses, vinasses, sugar plant or similar wastes or residues, e.g. from waste originating from industrial processing of raw material of agricultural origin or derived products thereof
- C05F5/006—Waste from chemical processing of material, e.g. diestillation, roasting, cooking
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
- Y02A40/20—Fertilizers of biological origin, e.g. guano or fertilizers made from animal corpses
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Abstract
The invention provides a method for extracting xylo-oligosaccharide from oil-tea camellia shells, which takes the oil-tea camellia shells as raw materials and obtains filtrate and filter residue through crushing, presoaking, steam flash explosion, enzymolysis and filtration; performing integrated membrane separation, decoloring, desalting and concentrating on the obtained filtrate to obtain xylo-oligosaccharide; the water obtained by reverse osmosis treatment of the reclaimed water generated in the extraction procedures such as membrane separation and concentration is recycled; and performing biological fermentation treatment on the filter residue to obtain the organic fertilizer. The xylo-oligosaccharide is extracted by combining the steam flash explosion technology, the biological enzyme technology and the integrated membrane separation technology, so that the extraction rate is high; no organic reagent is added in the whole process, the reclaimed water is recycled, and the waste residues are prepared into organic fertilizer for planting the oil tea; no waste water and waste residue are discharged in the whole process, zero discharge is realized, and the method is economical and environment-friendly.
Description
Technical Field
The invention relates to the technical field of resource utilization of agricultural and forestry wastes, in particular to a method for extracting xylooligosaccharide from camellia oleifera shells.
Background
The kernels of the oil tea are used for processing into the oil tea, and the shells are usually discarded or burned as waste, so that not only is the resource seriously wasted, but also the solid waste pollution is increased. The camellia oleifera shells generally account for 50-60% of the whole fresh tea fruit by mass, and contain abundant cellulose, hemicellulose, lignin, procyanidine and other substances, wherein the content of procyanidine is 4%, the content of cellulose is 15%, the content of hemicellulose is 25% and the content of lignin is 30%, and the hemicellulose is mainly xylan and is an ideal raw material for preparing xylo-oligosaccharide.
The traditional process uses an alkaline method to extract low-xylan, and introduces a large amount of impurities while extracting xylan, which increases the difficulty of subsequent separation and purification. Meanwhile, the alkaline extraction method can generate a large amount of alkaline wastewater, so that the method does not meet the future environmental protection requirement, and the sewage treatment cost is increased; the treated waste residue contains rich organic matters and is a good organic resource. Therefore, it is a future trend to find an environmentally friendly and efficient method for extracting xylooligosaccharide.
Disclosure of Invention
The invention aims to provide a method for extracting xylo-oligosaccharide from oil-tea camellia shells, which takes the oil-tea camellia shells as raw materials, adopts an advanced steam flash explosion technology, a biological enzyme technology and an integrated membrane separation technology, does not add any organic reagent in the whole process, reuses the generated reclaimed water in an extraction process through reverse osmosis treatment, recycles the reclaimed water, biologically ferments waste residues into organic fertilizers, does not discharge waste water and waste residues in the whole process, is efficient in utilization, and is economic and environment-friendly.
In order to achieve the purpose, the method for extracting the camellia oleifera shell xylo-oligosaccharide provided by the invention comprises the following steps: taking oil tea shells as raw materials, and obtaining filtrate and filter residues through crushing, presoaking, steam flash explosion, enzymolysis and filtering; the filtrate is subjected to integrated membrane separation, decoloration, desalination and concentration to obtain xylo-oligosaccharide; returning water obtained by performing reverse osmosis treatment on reclaimed water generated in the extraction process to the extraction process for recycling; and performing biological fermentation treatment on the filter residue to obtain the organic fertilizer.
Further, crushing the camellia oleifera shells to 10-20 meshes of granularity.
Furthermore, the pre-immersion liquid is 0.2% dilute hydrochloric acid, the pre-immersion conditions are that the material-liquid ratio is 1:8-15(W/W), and the pre-immersion time is 6-12 h.
Further, the steam flash explosion condition is that the steam pressure is 1.8-2.5Mpa, and the pressure maintaining time is 2-4 min.
Further, the enzyme adding amount in the enzymolysis is 3-5%, the enzymolysis temperature is 48-62 ℃, the time is 5-7h, the enzyme inactivation temperature is 100 ℃, and the enzyme inactivation time is 18-30 min.
Further, the membrane separation adopts a 50nm ceramic membrane and an ultrafiltration membrane for filtration.
Further, activated carbon is adopted for primary decolorization, and the addition amount of the activated carbon is 25-40% of the solid content.
Furthermore, the desalting procedure adopts D301, and the adsorption time is 10-16 h.
Further, the biological fermentation takes the filter residue after enzymolysis as a raw material, auxiliary materials and zymophyte are added, the mixture is uniformly mixed, the pile height is 1.5-3m, the mixture is fermented for 45-60 days, and the pile is turned when the temperature of the material exceeds 65 ℃ during the fermentation.
Further, the xylo-oligosaccharide is type 70 xylo-oligosaccharide syrup.
The invention has the beneficial effects that: the invention adopts advanced steam flash explosion technology, biological enzyme technology and integrated membrane separation technology, no organic reagent is added in the whole process, and the reclaimed water generated in the extraction process is reused in the extraction process through reverse osmosis treatment and is recycled; the waste residues are biologically fermented into organic fertilizer which can be used for planting the oil tea; no waste water and waste residue are discharged in the whole process, so that zero discharge is realized; meanwhile, the extraction rate of the obtained xylo-oligosaccharide syrup is up to more than 7%, and the additional value of the camellia oleifera shell is improved; the cyclic and efficient utilization of the oil tea fruit shells is realized, and the method is economical and environment-friendly.
Drawings
FIG. 1 is a process flow diagram of the practice of the present invention.
Detailed Description
The invention is further explained with reference to the drawings and the embodiments.
The endonuclease used by the invention is provided by a Jinan Bailong organism; the content detection method of 70 type xylooligosaccharide syrup adopts high performance liquid chromatography. The 70-type xylo-oligosaccharide syrup is 70-type syrup with physicochemical indexes meeting the national standard of GB/T35545-2017 xylo-oligosaccharide.
Example 1
The embodiment provides a method for extracting camellia oleifera shell xylo-oligosaccharide, as shown in fig. 1, comprising the following steps:
1. crushing: crushing 10kg of oil tea fruit shell to 10 meshes of granularity for later use;
2. pre-dipping: adding 100kg of 0.2% dilute hydrochloric acid water into the crushed oil tea fruit shell, soaking for 8 hours, and fishing out dry residues for later use;
3. steam flash explosion: placing the pre-soaked oil-tea camellia shell in a blasting cavity of steam explosion equipment, opening an air inlet valve, introducing saturated steam, keeping the steam pressure at 2Mpa for 3min, and completing steam explosion to obtain steam exploded oil-tea camellia shell for later use;
4. enzymolysis: and (3) adding 160kg of water into the steam exploded oil tea fruit shell obtained in the step (3), fully and uniformly mixing, adjusting the pH value to 6.0, then adding 600g of endonuclease, and keeping the temperature of 50 ℃ for enzymolysis for 6 hours. After the enzymolysis reaction is finished, inactivating enzyme for 20min at the temperature of 100 ℃, and then filtering the enzymolysis liquid to obtain filtrate and filter residue for later use.
5. Membrane separation: filtering the filtrate obtained in the step 4 by using a 50nm ceramic membrane and an ultrafiltration membrane to obtain a filtrate;
6. and (3) decoloring: adding activated carbon with the solid content of 25% into the filtrate obtained in the step 5 for primary decolorization, and separating to obtain a filtrate;
7. desalting: adsorbing the filtrate obtained in the step 5 for 10 hours by using D301 resin to obtain feed liquid;
8. concentration: concentrating the feed liquid treated in the step (7) to 40% concentration in vacuum, and sending to a spray dryer for spraying sugar powder; then concentrated by a central circulating tube evaporator, and discharged when the solid content reaches 70 percent. The product is 70 type xylo-oligosaccharide syrup.
9. Reverse osmosis: the reclaimed water generated in the step is intensively sent into a reverse osmosis treatment system for treatment, and the obtained water enters an extraction process for reuse;
10. biological fermentation: and (4) adding auxiliary materials and fermentation strains into the filter residue obtained in the step (4), uniformly mixing, piling up to 1.5m for fermentation for 55d, turning the pile when the temperature of the materials exceeds 65 ℃ during fermentation, and obtaining the organic fertilizer after fermentation.
As a result: in the embodiment, 0.72kg of 70-type xylo-oligosaccharide syrup is obtained, the reclaimed water in the extraction process is recycled, and the filter residue is prepared into an organic fertilizer which can be used for planting the camellia oleifera.
Example 2
The embodiment provides a method for extracting camellia oleifera shell xylo-oligosaccharide, as shown in fig. 1, comprising the following steps:
1. crushing: crushing 20kg of oil tea fruit shell to 15 meshes for later use;
2. pre-dipping: adding 160kg of 0.2% dilute hydrochloric acid water into the crushed oil tea fruit shell, soaking for 7 hours, and fishing out dry residues for later use;
3. steam flash explosion: placing the pre-soaked oil tea fruit shell in a blasting cavity of steam explosion equipment, opening an air inlet valve, introducing saturated steam, keeping the steam pressure at 2.5Mpa for 3.5min, and completing steam explosion to obtain steam exploded oil tea fruit shell for later use;
4. enzymolysis: and (3) adding 300kg of water into the steam exploded oil tea fruit shell obtained in the step 3, fully and uniformly mixing, adjusting the pH value to 6.0, then adding 1000g of endonuclease, and keeping the temperature of 55 ℃ for enzymolysis for 6.5 hours. After the enzymolysis reaction is finished, inactivating enzyme for 25min at the temperature of 100 ℃, and then filtering the enzymolysis liquid to obtain filtrate and filter residue for later use.
5. Membrane separation: filtering the filtrate obtained in the step 4 by using a 50nm ceramic membrane and an ultrafiltration membrane to obtain a filtrate;
6. and (3) decoloring: adding active carbon with the solid content of 30% into the filtrate obtained in the step 5 for primary decolorization, and separating to obtain a filtrate;
7. desalting: and (5) adsorbing the filtrate in the step (5) for 12 hours by using D301 resin to obtain feed liquid.
8. Concentration: concentrating the feed liquid treated in the step (7) to 40% concentration in vacuum, and sending to a spray dryer for spraying sugar powder; then concentrated by a central circulating tube evaporator, and discharged when the solid content reaches 70 percent. The product is 70 type xylo-oligosaccharide syrup.
9. Reverse osmosis: and (3) the reclaimed water generated in the step is intensively sent into a reverse osmosis treatment system for treatment, and the obtained water can enter an extraction process for reuse.
10. Biological fermentation: and (4) adding auxiliary materials and fermentation strains into the filter residue obtained in the step (4), uniformly mixing, piling up for 2m for fermentation for 50d, turning the piles when the temperature of the materials exceeds 65 ℃ during fermentation, and completing fermentation to obtain the organic fertilizer.
As a result: in the embodiment, 1.4kg of 70-type xylo-oligosaccharide syrup is obtained, the reclaimed water in the extraction process is recycled, and the filter residue is prepared into an organic fertilizer which can be used for planting the camellia oleifera.
Example 3
The embodiment provides a method for extracting camellia oleifera shell xylo-oligosaccharide, as shown in fig. 1, comprising the following steps:
1. crushing: crushing 30kg of oil tea fruit shell to 18 meshes for later use.
2. Pre-dipping: adding 400kg of 0.2% dilute hydrochloric acid water into the crushed oil tea fruit shell, soaking for 10 hours, and fishing out dry residues for later use.
3. Steam flash explosion: and (3) placing the pre-soaked oil-tea camellia shells in a blasting cavity of steam explosion equipment, opening an air inlet valve, introducing saturated steam, keeping the steam pressure at 2.5Mpa for 4min, and completing steam explosion to obtain the steam exploded oil-tea camellia shells for later use.
4. Enzymolysis: and (3) adding 400kg of water into the steam exploded oil tea fruit shell obtained in the step (3), fully and uniformly mixing, adjusting the pH value to 6.0, then adding 1500g of endonuclease, and keeping the temperature of 60 ℃ for enzymolysis for 7 hours. After the enzymolysis reaction is finished, inactivating enzyme for 30min at the temperature of 100 ℃, and then filtering the enzymolysis liquid to obtain filtrate and filter residue for later use.
5. Membrane separation: and (4) filtering the filtrate obtained in the step (4) by using a 50nm ceramic membrane and an ultrafiltration membrane to obtain a filtrate.
6. And (3) decoloring: and (5) adding activated carbon with the solid content of 35% into the filtrate obtained in the step (5) for primary decolorization, and separating to obtain the filtrate.
7. Desalting: and (5) adsorbing the filtrate in the step (5) for 16h by using D301 resin to obtain feed liquid.
8. Concentration: concentrating the feed liquid treated in the step (7) to 40% concentration in vacuum, and sending to a spray dryer for spraying sugar powder; then concentrated by a central circulating tube evaporator, and discharged when the solid content reaches 70 percent. The product is 70 type xylo-oligosaccharide syrup.
9. Reverse osmosis: and (3) the reclaimed water generated in the step is intensively sent into a reverse osmosis treatment system for treatment, and the obtained water can enter an extraction process for reuse.
10. Biological fermentation: and (4) adding auxiliary materials and fermentation strains into the filter residue obtained in the step (4), uniformly mixing, piling up to 2.5m, fermenting for 48d, turning the piles when the temperature of the materials exceeds 65 ℃ during fermentation, and obtaining the organic fertilizer after fermentation.
As a result: in the embodiment, 2.2kg of 70-type xylo-oligosaccharide syrup is obtained, the reclaimed water in the extraction process is recycled, and the filter residue is prepared into an organic fertilizer which can be used for planting the camellia oleifera.
Comparative example 1
The method for extracting the camellia oleifera shell xylooligosaccharide in the comparative example comprises the following steps:
1. crushing: crushing 10kg of oil tea fruit shell to 10 meshes of granularity for later use;
2. pre-dipping: adding 100L of 60% ethanol aqueous solution with volume fraction into the crushed oil tea fruit shell, performing reflux extraction for 3 hours, and taking out dry residues for later use;
3. enzymolysis: and (3) adding 160kg of water into the oil tea fruit shell obtained in the step (2), fully and uniformly mixing, adjusting the pH value to 6.0, adding 1000g of endonuclease, and keeping the temperature of 50 ℃ for enzymolysis for 6 hours. After the enzymolysis reaction is finished, inactivating enzyme for 20min at the temperature of 100 ℃, and then filtering the enzymolysis liquid to obtain filtrate for later use.
4. Membrane separation: filtering the filtrate obtained in the step 3 by using a 50nm ceramic membrane and an ultrafiltration membrane to obtain a filtrate;
5. desalting: adsorbing the filtrate obtained in the step 4 for 10 hours by using D301 resin to obtain feed liquid;
6. concentration: concentrating the feed liquid treated in the step 5 to 40% concentration in vacuum, and sending to a spray dryer for spraying sugar powder; then concentrated by a central circulating tube evaporator, and discharged when the solid content reaches 70 percent. The product is 70 type xylo-oligosaccharide syrup.
As a result: this comparative example yielded 0.46kg of a type 70 oligoxylose syrup, the filter residue and waste liquid of the extraction process not being treated.
Comparative example 2
The method for extracting the camellia oleifera shell xylooligosaccharide in the comparative example comprises the following steps:
1. crushing: crushing 10kg of oil tea fruit shell to 10 meshes of granularity for later use;
2. pre-dipping: adding 100L of 60% ethanol aqueous solution with volume fraction into the crushed oil tea fruit shell, performing reflux extraction for 3 hours, and taking out dry residues for later use;
3. alkali extraction: and (3) adding 100L of 10% NaOH solution into the dry residue obtained in the step (2), stirring, extracting for 1h, and performing suction filtration to obtain an extracting solution.
4. Separation: and (3) adjusting the pH value of the extract in the step (3) to 5, adding 1 volume of absolute ethyl alcohol for alcohol precipitation, standing for 10 hours, and centrifuging to obtain a precipitate.
5. Concentration: and (4) concentrating the precipitate obtained in the step (4) by using a central circulating tube evaporator, and discharging when the solid content reaches 70%. The product is 70 type xylo-oligosaccharide syrup.
As a result: this comparative example yielded 0.28kg of a type 70 oligoxylose syrup, the filter residue and waste liquid of the extraction process not being treated.
TABLE 1 extraction yield of each example and comparative example
From the table 1, the extraction rate of the 70-type xylo-oligosaccharide syrup extracted by the scheme of the invention is up to more than 7%, while the comparative example 1 does not adopt a steam flash explosion technology, the comparative example 2 adopts a conventional alkali extraction method, the extraction rates are relatively low, and waste liquid and waste residue are not treated.
Finally, it should be emphasized that the above-described preferred embodiments of the present invention are merely examples of implementations, rather than limitations, and that many variations and modifications of the invention are possible to those skilled in the art, without departing from the spirit and scope of the invention.
Claims (10)
1. A method for extracting xylo-oligosaccharide from oil tea fruit shells is characterized in that the oil tea fruit shells are taken as raw materials, and filtrate and filter residue are obtained through crushing, presoaking, steam flash explosion, enzymolysis and filtering;
performing integrated membrane separation, decoloring, desalting and concentrating on the filtrate to obtain xylo-oligosaccharide;
the reclaimed water produced in the extraction procedure is recycled after reverse osmosis treatment;
and performing biological fermentation treatment on the filter residue to obtain the organic fertilizer.
2. The method for extracting camellia oleifera shell xylo-oligosaccharide according to claim 1, wherein the camellia oleifera shell is crushed to a particle size of 10-20 meshes.
3. The method for extracting camellia oleifera shell xylo-oligosaccharide according to claim 1, wherein the pre-soaking solution is 0.2% dilute hydrochloric acid, the pre-soaking condition is that the material-liquid ratio is 1:8-15(W/W), and the pre-soaking time is 6-12 h.
4. The method for extracting camellia oleifera shell xylo-oligosaccharide according to claim 1, wherein the steam pressure of the steam flash explosion is 1.8-2.5Mpa, and the pressure holding time is 2-4 min.
5. The method for extracting camellia oleifera shell xylo-oligosaccharide according to claim 1, wherein the amount of endonuclease added in the enzymolysis is 3-5%, the enzymolysis temperature is 48-62 ℃, the time is 5-7h, the enzyme deactivation temperature is 100 ℃, and the enzyme deactivation time is 18-30 min.
6. The method for extracting camellia oleifera shell xylo-oligosaccharide according to claim 1, wherein the membrane separation is performed by adopting a 50nm ceramic membrane and an ultrafiltration membrane.
7. The method for extracting camellia oleifera shell xylo-oligosaccharide according to claim 1, wherein the decolorization is performed by activated carbon at one time, and the added amount of the activated carbon is 25-40% of the solid content.
8. The method for extracting camellia oleifera shell xylo-oligosaccharide according to claim 1, wherein D301 is adopted in the desalting process, and the adsorption time is 10-16 h.
9. The method for extracting camellia oleifera shell xylo-oligosaccharide according to claim 1, wherein the biological fermentation takes filter residues obtained after enzymolysis as a raw material, auxiliary materials and fermentation bacteria are added, the mixture is uniformly mixed, the pile height is 1.5-3m, the mixture is fermented for 45-60 days, and the pile is turned when the temperature of the material exceeds 65 ℃ during the fermentation.
10. The method for extracting camellia oleifera shell xylooligosaccharide according to any one of claims 1 to 9, wherein the xylooligosaccharide is type 70 xylooligosaccharide syrup.
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Application publication date: 20210601 |