CN109206539B - Method for extracting bagasse hemicellulose by microwave-assisted double-aqueous-phase separation - Google Patents
Method for extracting bagasse hemicellulose by microwave-assisted double-aqueous-phase separation Download PDFInfo
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- CN109206539B CN109206539B CN201810907364.6A CN201810907364A CN109206539B CN 109206539 B CN109206539 B CN 109206539B CN 201810907364 A CN201810907364 A CN 201810907364A CN 109206539 B CN109206539 B CN 109206539B
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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 extracting bagasse hemicellulose by microwave-assisted double-aqueous phase separation, which comprises the steps of weighing inorganic salt, placing the inorganic salt in water for ultrasonic dissolution, adding polyethylene glycol, standing and carrying out phase separation to obtain a polyethylene glycol/inorganic salt double-aqueous phase system; extracting bagasse in a double-water-phase system under the conditions of microwave power of 600-; the method overcomes the defect that lignin needs to be separated firstly and then hemicellulose needs to be extracted in the traditional extraction method, so that the hemicellulose is directly extracted in a double-aqueous-phase system, and the double-aqueous-phase system has the characteristics of high phase separation speed, low energy consumption and high extraction rate, and is suitable for extracting the hemicellulose.
Description
Technical Field
The invention relates to a method for extracting bagasse hemicellulose by microwave-assisted aqueous two-phase separation, and belongs to the field of biomass refining and extraction.
Background
Bagasse is a main byproduct after sugar production of sugarcane, mainly comprises cellulose, hemicellulose and lignin, wherein the content of the hemicellulose and the content of the lignin are both 20-30%, and the hemicellulose is easy to degrade and difficult to extract due to inherent multicomponent of the hemicellulose, special chemical structures of multiple branches and chemical chain connection with the lignin and a structure which is tightly combined with the cellulose.
Compared with other medicinal plants, the bagasse in the process of extracting hemicellulose can be directly used without grinding, and the double-aqueous phase system is a mutually insoluble double-aqueous phase system formed spontaneously by mixing two different water-soluble substances in water at a certain concentration. With the development of the aqueous two-phase extraction technology, a new system of hydrophilic organic solvent/inorganic salt, mixed surfactant, ionic liquid and the like appears. The hydrophilic organic solvent/inorganic salt system is mostly lower alcohol/inorganic salt, such as ethanol, propanol and the like, and compared with the conventional high polymer system, the hydrophilic organic solvent/inorganic salt system has the advantages of cheaper and easily obtained phase forming matter, small interfacial tension and viscosity, low mass transfer resistance and simple sample post-treatment. The double-aqueous phase extraction realizes separation according to the selective distribution of a target object in the double-aqueous phase, has the characteristics of good selectivity, mild extraction conditions, simple and convenient operation and the like, and is widely applied to the extraction and separation of bioactive substances such as protein, enzyme and the like. With the development of a novel double-aqueous phase system, active ingredients in some metal and natural biomass resources can be extracted and separated quickly and effectively through the novel double-aqueous phase system.
Disclosure of Invention
The method adopts microwave-assisted double-aqueous phase separation to extract the bagasse hemicellulose, can separate the bagasse hemicellulose at one time, and has quick reaction.
The technical scheme of the invention is as follows:
a method for extracting bagasse hemicellulose by microwave-assisted double-aqueous-phase separation comprises the following specific steps:
(1) preparation of a two-aqueous phase system: weighing inorganic salt, placing the inorganic salt in water for ultrasonic dissolution, adding polyethylene glycol, standing and carrying out phase separation to obtain a polyethylene glycol/inorganic salt double-water-phase system;
(2) microwave-assisted extraction of hemicellulose: adding bagasse into the aqueous two-phase system in the step (1), extracting for 10-30min under the conditions of microwave power of 600-1000W and temperature of 40-80 ℃, taking supernatant, adjusting the pH value of the supernatant to 2-4 by using 2mol/L hydrochloric acid, adding ethanol with the volume concentration of 3-5 times of that of the supernatant being 95%, then carrying out centrifugal separation at the rotating speed of 4000-7000r/min at-5 ℃, washing products after the centrifugal separation to be neutral by using absolute ethanol and acetone respectively, and drying to obtain bagasse hemicellulose.
In the polyethylene glycol/inorganic salt aqueous two-phase system in the step (1), the mass percent of polyethylene glycol is 20-40%, the mass percent of inorganic salt is 15-30%, and the balance is water.
The inorganic salt in the step (1) is ammonium sulfate, sodium carbonate, sodium hydrogen phosphate, potassium hydrogen phosphate or dipotassium hydrogen phosphate.
The mass-volume ratio g: mL of the bagasse to the aqueous two-phase system in the step (2) is 1: 5-10.
The invention has the beneficial effects that:
the invention has the characteristics of fast phase separation, short reaction time, one-time extraction of hemicellulose, uniform and fast microwave heating, easy temperature control and huge application prospect of the microwave two-aqueous-phase extraction technology.
Detailed Description
The present invention will be described in further detail with reference to examples, but the scope of the present invention is not limited to the examples.
Example 1
A method for extracting bagasse hemicellulose by microwave-assisted double-aqueous-phase separation comprises the following specific steps:
(1) preparation of a two-aqueous phase system: weighing 5g of ammonium sulfate in a 50mL conical flask, adding 15mL of water, ultrasonically dissolving, adding 10g of polyethylene glycol, standing, and carrying out phase separation to obtain a polyethylene glycol/ammonium sulfate double-water-phase system;
(2) and (3) microwave-assisted extraction of bagasse hemicellulose: weighing bagasse according to the mass-to-volume ratio g: mL of 1:5 of the bagasse to the aqueous two-phase system, adding the bagasse into the aqueous two-phase system in the step (1), extracting for 30min under the conditions of microwave power of 1000W and temperature of 80 ℃, taking supernatant, adjusting the pH value to 2 by using 2mol/L hydrochloric acid, adding ethanol with the volume concentration of 95% and the volume of 5 times that of the supernatant, then carrying out centrifugal separation at-5 ℃ at the rotating speed of 7000r/min, washing products after the centrifugal separation to be neutral by using absolute ethanol and acetone respectively, and drying to obtain bagasse hemicellulose.
In this example, the bagasse hemicellulose yield is 58.2%.
Example 2
A method for extracting bagasse hemicellulose by microwave-assisted double-aqueous-phase separation comprises the following specific steps:
(1) preparation of a two-aqueous phase system: weighing 8g of sodium hydrogen phosphate into a 50mL conical flask, adding 20mL of water, ultrasonically dissolving, adding 12g of polyethylene glycol, standing, and carrying out phase separation to obtain a polyethylene glycol/sodium hydrogen phosphate two-aqueous-phase system;
(2) and (3) microwave-assisted extraction of bagasse hemicellulose: weighing bagasse according to the mass-volume ratio g: mL of the bagasse to the aqueous two-phase system of 1:6, adding the bagasse into the aqueous two-phase system in the step (1), extracting for 20min at the temperature of 70 ℃ under the microwave power of 900W, taking supernatant, adjusting the pH value to 2 by using 2mol/L hydrochloric acid, adding ethanol with the volume concentration of 95% 4 times the volume of the supernatant, then carrying out centrifugal separation at the rotating speed of 6000r/min at-5 ℃, washing products after the centrifugal separation to be neutral by using absolute ethanol and acetone respectively, and drying to obtain bagasse hemicellulose.
In this example, the yield of bagasse hemicellulose was 61.1%.
Example 3
A method for extracting bagasse hemicellulose by microwave-assisted double-aqueous-phase separation comprises the following specific steps:
(1) preparation of a two-aqueous phase system: weighing 6g of sodium carbonate into a 50mL conical flask, adding 10mL of water, ultrasonically dissolving, adding 4g of polyethylene glycol, standing, and carrying out phase separation to obtain a polyethylene glycol/sodium carbonate double-water-phase system;
(2) and (3) microwave-assisted extraction of bagasse hemicellulose: weighing bagasse according to the mass-to-volume ratio g: mL of 1:7 of the bagasse to the aqueous two-phase system, adding the bagasse into the aqueous two-phase system in the step (1), extracting for 25min under the conditions of microwave power of 800W and temperature of 60 ℃, taking supernatant, adjusting the pH value to 3 by using 2mol/L hydrochloric acid, adding ethanol with the volume concentration of 95% and the volume of 3 times that of the supernatant, then carrying out centrifugal separation at the rotating speed of 5000r/min at-5 ℃, washing products after the centrifugal separation to be neutral by using absolute ethanol and acetone respectively, and drying to obtain bagasse hemicellulose.
In this example, the bagasse hemicellulose yield is 62.9%.
Example 4
A method for extracting bagasse hemicellulose by microwave-assisted double-aqueous-phase separation comprises the following specific steps:
(1) preparation of a two-aqueous phase system: weighing 3g of potassium hydrogen phosphate into a 50mL conical flask, adding 10mL of water, ultrasonically dissolving, adding 7g of polyethylene glycol, standing, and carrying out phase separation to obtain a polyethylene glycol/potassium hydrogen phosphate double-aqueous-phase system;
(2) and (3) microwave-assisted extraction of bagasse hemicellulose: weighing bagasse according to the mass-to-volume ratio g: mL of 1:10 of the bagasse to the aqueous two-phase system, adding the bagasse into the aqueous two-phase system in the step (1), extracting for 10min at the temperature of 50 ℃ under the microwave power of 700W, taking supernatant, adjusting the pH value to 4 by using 2mol/L hydrochloric acid, adding ethanol with the volume concentration of 95% and the volume of 3 times that of the supernatant, performing centrifugal separation at the temperature of minus 5 ℃ at the rotating speed of 4000r/min, washing products after the centrifugal separation to be neutral by using absolute ethanol and acetone respectively, and drying to obtain bagasse hemicellulose.
In this example, the bagasse hemicellulose yield is 57.4%.
Example 5
A method for extracting bagasse hemicellulose by microwave-assisted double-aqueous-phase separation comprises the following specific steps:
(1) preparation of a two-aqueous phase system: weighing 10g of dipotassium phosphate into a 50mL conical flask, adding 20mL of water, ultrasonically dissolving, adding 20g of polyethylene glycol, standing, and carrying out phase separation to obtain a polyethylene glycol/dipotassium phosphate double-aqueous-phase system;
(2) and (3) microwave-assisted extraction of bagasse hemicellulose: weighing bagasse according to the mass-to-volume ratio g: mL of 1:9 of the bagasse to the aqueous two-phase system, adding the bagasse into the aqueous two-phase system in the step (1), extracting for 30min at the temperature of 40 ℃ under the microwave power of 600W, taking supernatant, adjusting the pH value to 2 by using 2mol/L hydrochloric acid, adding ethanol with the volume concentration of 95% 4 times the volume of the supernatant, then carrying out centrifugal separation at the temperature of minus 5 ℃ at the rotating speed of 4500r/min, washing products after the centrifugal separation to be neutral by using absolute ethanol and acetone respectively, and drying to obtain bagasse hemicellulose.
In this example, the bagasse hemicellulose yield is 58.4%.
Example 6
A method for extracting bagasse hemicellulose comprises the following specific steps:
weighing bagasse, extracting for 50min under the conditions of microwave power of 1000W, temperature of 100 ℃ and alkali concentration of 14%, taking out an extracting solution, centrifuging for 5min at the rotating speed of 3000r/min, taking a supernatant, adjusting the pH value of the supernatant to 2 by using 2mol/L hydrochloric acid, centrifugally separating lignin, taking the supernatant after lignin separation, adding ethanol with the volume concentration of 95% and the volume concentration of 3 times that of the supernatant, then carrying out centrifugal separation at the rotating speed of 5000r/min at-5 ℃, washing products after centrifugal separation to be neutral by using absolute ethanol and acetone respectively, and drying to obtain bagasse hemicellulose.
In the non-two-aqueous-phase extraction of the embodiment, the bagasse hemicellulose yield is 58.9%, and the difference between the bagasse hemicellulose yield and the embodiment 1-5 is not large, but the embodiment adds a step of lignin separation, and the two-aqueous-phase extraction of the bagasse hemicellulose in the embodiment 1-5 is one-time extraction, so that the speed is improved.
Example 7
Extracting hemicellulose by a traditional alkaline method: mixing bagasse and a NaOH solution according to a mass-volume ratio of kg: L of 1:7, wherein the mass percentage concentration of the NaOH solution is 14%, carrying out alkaline extraction on hemicellulose at 100 ℃ for 4 hours, filtering and collecting supernatant after the reaction is finished, adjusting the pH value to 2 by using 2mol/L hydrochloric acid, filtering to remove acid-insoluble lignin, adjusting the pH value of filtrate to 4.5, adding 3 times of volume of ethanol for flocculation and separation of flocculate, washing precipitates to be neutral by using ethanol and acetone, and drying at 50 ℃ to obtain the hemicellulose.
In this example, the bagasse hemicellulose yield was 32.6%, which was much lower than that in examples 1-5.
Claims (2)
1. A method for extracting bagasse hemicellulose by microwave-assisted double-aqueous-phase separation is characterized by comprising the following specific steps:
(1) preparation of a two-aqueous phase system: weighing inorganic salt, placing the inorganic salt in water for ultrasonic dissolution, adding polyethylene glycol, standing and carrying out phase separation to obtain a polyethylene glycol/inorganic salt double-water-phase system; the inorganic salt is ammonium sulfate, sodium carbonate, sodium hydrogen phosphate, potassium hydrogen phosphate or dipotassium hydrogen phosphate;
(2) microwave-assisted extraction of hemicellulose: adding bagasse into the aqueous two-phase system in the step (1), wherein the mass volume ratio g: mL of the bagasse to the aqueous two-phase system is 1:5-10, extracting for 10-30min under the conditions of microwave power of 600-.
2. The microwave-assisted aqueous two-phase separation method for extracting bagasse hemicellulose according to claim 1, wherein the mass percent of polyethylene glycol in the polyethylene glycol/inorganic salt aqueous two-phase system in the step (1) is 30-50%, the mass percent of inorganic salt is 15-40%, and the balance is water.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS541778B1 (en) * | 1968-08-22 | 1979-01-29 | ||
| KR20020006559A (en) * | 2000-07-04 | 2002-01-23 | 조봉희 | Seperation method of dietary hemicellulose-fiber from plant |
| CN101063114A (en) * | 2007-05-11 | 2007-10-31 | 陕西科技大学 | Method for pectic enzyme separating purification by double aqueous phase extraction system |
| CN101735648B (en) * | 2010-01-25 | 2013-09-18 | 青岛鹏远康华天然产物有限公司 | Method for separating and purifying beet red pigment by two aqueous phase extraction system |
| CN104072504A (en) * | 2014-06-16 | 2014-10-01 | 南京泽朗医药科技有限公司 | Method for extracting and purifying hernandia nymphaeifolia alkali from hernandia nymphaeifolia |
| CN105111332A (en) * | 2015-09-27 | 2015-12-02 | 常州市奥普泰科光电有限公司 | Method for extracting hemicellulose from wheat straw |
| CN107641082A (en) * | 2017-09-30 | 2018-01-30 | 浙江树人学院（浙江树人大学） | A kind of method of microwave cooperating double-aqueous phase system extraction sweet potato leaves chlorogenic acid |
-
2018
- 2018-08-10 CN CN201810907364.6A patent/CN109206539B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS541778B1 (en) * | 1968-08-22 | 1979-01-29 | ||
| KR20020006559A (en) * | 2000-07-04 | 2002-01-23 | 조봉희 | Seperation method of dietary hemicellulose-fiber from plant |
| CN101063114A (en) * | 2007-05-11 | 2007-10-31 | 陕西科技大学 | Method for pectic enzyme separating purification by double aqueous phase extraction system |
| CN101735648B (en) * | 2010-01-25 | 2013-09-18 | 青岛鹏远康华天然产物有限公司 | Method for separating and purifying beet red pigment by two aqueous phase extraction system |
| CN104072504A (en) * | 2014-06-16 | 2014-10-01 | 南京泽朗医药科技有限公司 | Method for extracting and purifying hernandia nymphaeifolia alkali from hernandia nymphaeifolia |
| CN105111332A (en) * | 2015-09-27 | 2015-12-02 | 常州市奥普泰科光电有限公司 | Method for extracting hemicellulose from wheat straw |
| CN107641082A (en) * | 2017-09-30 | 2018-01-30 | 浙江树人学院（浙江树人大学） | A kind of method of microwave cooperating double-aqueous phase system extraction sweet potato leaves chlorogenic acid |
Non-Patent Citations (2)
| Title |
|---|
| Extraction and characterization of hemicelluloses from flax shives by different methods;Anvar U.Buranov et al.;《Carbohydrate Polymers》;20090625;第79卷;第17-25页 * |
| 双水相萃取在中药活性成分提取分离中的应用进展;刘磊磊等;《中草药》;20151231;第46卷(第5期);第766-773页 * |
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