CN112143835A - Method for extracting multiple polysaccharide substances from biomass material - Google Patents

Method for extracting multiple polysaccharide substances from biomass material Download PDF

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Publication number
CN112143835A
CN112143835A CN202010861440.1A CN202010861440A CN112143835A CN 112143835 A CN112143835 A CN 112143835A CN 202010861440 A CN202010861440 A CN 202010861440A CN 112143835 A CN112143835 A CN 112143835A
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CN
China
Prior art keywords
biomass materials
polysaccharide substances
biomass
heating
filtering
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Pending
Application number
CN202010861440.1A
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Chinese (zh)
Inventor
沈贤德
王猛
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Changchun Xinruide New Material Technology Development Co ltd
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Changchun Xinruide New Material Technology Development Co ltd
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Priority to CN202010861440.1A priority Critical patent/CN112143835A/en
Publication of CN112143835A publication Critical patent/CN112143835A/en
Pending legal-status Critical Current

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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
    • C13K1/00—Glucose; Glucose-containing syrups
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/10—Organic substances
    • A23K20/163—Sugars; Polysaccharides
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
    • C05F11/00—Other organic fertilisers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
    • 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
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials

Abstract

The invention relates to a method for extracting various polysaccharide substances from biomass materials, which comprises the following steps: step 1, crushing biomass materials, placing the crushed biomass materials in a stainless steel high-pressure reaction kettle, introducing nitrogen as protective gas, and adding water and CaCl2Stirring, heating to 180 ℃ and 200 ℃, keeping for 1.5-3 hours, stopping heating, and cooling to room temperature; step 2, taking out the reactant and filtering to obtain a black solid and a light yellow liquid; step 3, directly returning black solidObtaining cellulose and lignin by soil or separation; distilling and concentrating the liquid part to obtain viscous fluid containing multiple polysaccharides, and directly utilizing; or dripping the viscous fluid into 99% ethanol for reprecipitation, and filtering to obtain yellowish solid powder containing multiple polysaccharides. The method effectively extracts and separates various polysaccharide substances from the biomass material by using the high-pressure reaction kettle and the unique processing technology, is simple, and realizes effective comprehensive utilization of the waste biomass material.

Description

Method for extracting multiple polysaccharide substances from biomass material
Technical Field
The invention belongs to the technical field of biomass conversion processing, and particularly relates to a method for extracting various polysaccharide substances from biomass materials.
Background
Aiming at the treatment work of biomass materials (straws and branches of various crops), burning prohibition is taken as an important work by governments at all levels in China, various administrative management measures are taken to supervise and guide the effective comprehensive utilization of the biomass materials, five-material comprehensive utilization research projects of the biomass materials such as fertilizer, feed, raw material, base material and fuel are developed, and the comprehensive utilization efficiency of the straws is greatly improved. But the problems of immature process technology, low production efficiency, high energy consumption, missing industrial standard, poor economic benefit and the like exist, and a plurality of phenomena of waste in half way occur in the aspect of practical application and popularization, so that the process cannot be continuously developed.
Disclosure of Invention
In view of the above technical problems and disadvantages, the present invention provides a method for extracting various polysaccharides from biomass materials, which effectively extracts and separates various polysaccharides from biomass materials by using a high pressure reactor and a unique processing technology, and further separates cellulose and lignin from the extracted intermediate product, thereby realizing effective comprehensive utilization of waste biomass materials and achieving the purpose of sustainable development.
In order to realize the purpose, the invention is realized by adopting the following technical scheme:
a method for extracting multiple polysaccharide substances from biomass materials specifically comprises the following steps:
step 1, crushing biomass materials, placing the crushed biomass materials in a stainless steel high-pressure reaction kettle, introducing nitrogen as protective gas, and adding water and CaCl2Stirring, heating to 180 ℃ and 200 ℃, keeping for 1.5-3 hours, stopping heating, and cooling to room temperature under the stirring state;
step 2, taking out the reactant and filtering to obtain a black solid and a light yellow liquid;
step 3, directly returning the black solid to the soil or separating to obtain cellulose and lignin; distilling and concentrating the liquid part to obtain viscous fluid containing multiple polysaccharides, and directly utilizing; or dripping viscous fluid into ethanol for reprecipitation, and filtering to obtain yellowish solid powder containing multiple polysaccharides.
As the optimization of the invention, the biomass material is straw, including corn straw and wheat straw.
As the optimization of the invention, the crushed particles in the step 1 are controlled to be 10mm to 30mm, CaCl2The adding amount is 2% -3% of the biomass material, and then the temperature is raised to 180 ℃ at the heating rate of 4 ℃/minute, and the temperature is kept for 2 hours.
In a preferred embodiment of the present invention, in the step 3, the method for obtaining cellulose and lignin by black solid separation comprises: putting the black solid into a mixed solution system of butanol and water with the volume ratio of 1:1, stirring and heating at 180-200 ℃ for 1-2 hours, and stopping heating; then distilling the butanol phase obtained after filtration to obtain lignin; filtering and drying the water phase to obtain the cellulose.
Preferably, the polysaccharide substances in step 3 include glucose, xylose, arabinose, mannose, xylose pool and fiber pool.
The invention has the advantages and beneficial effects that:
(1) the method for extracting various polysaccharide substances from the biomass material provided by the invention utilizes the high-pressure reaction kettle and a unique processing technology to effectively extract and separate various polysaccharide substances from the biomass material, and can further separate cellulose and lignin by utilizing the extracted intermediate product, thereby realizing effective comprehensive utilization of the waste biomass material and achieving the purpose of sustainable development.
(2) The method for extracting various polysaccharide substances provided by the invention is simple to operate, the process conditions are easy to control, the extraction yield is high, and the faint yellow solid powder with the polysaccharide substance content of more than 99% can be obtained after alcohol precipitation, so that the faint yellow solid powder is convenient to store and utilize; in addition, black solids generated in the middle of extracting polysaccharide substances can be directly returned to the soil to achieve the purpose of increasing the fertilizer.
(3) The polysaccharide substances extracted by the invention comprise glucose, xylose, arabinose, mannose, xylose-xylose.
Drawings
FIG. 1 is a light yellow solid powder of example 1 of the present invention1H-NMR(D2O, 500 MHz).
Fig. 2 is a partially enlarged view of fig. 1.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
Example 1
A method for extracting multiple polysaccharide substances from biomass materials specifically comprises the following steps:
step 1, 20g of biomass material (corn straw) is crushed (within the range of 10mm to 30 mm) and then placed in a stainless steel high-pressure reaction kettle, and 150ml of water and 0.5g of CaCl are added2Stirring (introducing nitrogen as protective gas) for 2 minutes, heating to 180 ℃ at the heating rate of 4 ℃/minute, keeping for 2 hours, stopping heating, and cooling to room temperature under the stirring state;
step 2, taking out the reactant and filtering to obtain a black solid and a light yellow liquid;
step 3, the black solid can be directly returned to the soil, so that the purpose of increasing the fertilizer is achieved; or further separating to obtain cellulose and lignin; the liquid part is distilled and concentrated to obtain viscous fluid containing various polysaccharide substances, which can be directly utilized; or dripping into 99% ethanol for reprecipitation, and filtering to obtain 2g of yellowish solid powder containing multiple polysaccharides for storage and utilization.
More than 99 percent of the faint yellow solid powder is a mixture of polysaccharide substances; as can be seen from FIGS. 1 and 2, strong peaks of absorption of hydrogen atoms in polysaccharide substances (glucose, xylose, arabinose, mannose, xylose pool, fiber pool) appear in the range of 2.0 to 5.5 ppm.
Further, the process of separating cellulose and lignin is as follows: putting the black solid into 150ml of a butanol-water (1:1) mixed solution system, stirring and heating at 200 ℃ for 1 hour, and stopping heating; the butanol phase obtained after filtration was distilled to obtain 4g of lignin with a purity of 99%, and the aqueous phase was filtered and dried to obtain 12g of cellulose with a purity of 60%.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application.

Claims (5)

1. A method for extracting various polysaccharide substances from biomass materials is characterized by comprising the following steps:
step 1, crushing biomass materials, placing the crushed biomass materials in a stainless steel high-pressure reaction kettle, introducing nitrogen as protective gas, and adding water and CaCl2Stirring, heating to 180 ℃ and 200 ℃, keeping for 1.5-3 hours, stopping heating, and cooling to room temperature under the stirring state;
step 2, taking out the reactant and filtering to obtain a black solid and a light yellow liquid;
step 3, directly returning the black solid to the soil or separating to obtain cellulose and lignin; distilling and concentrating the liquid part to obtain viscous fluid containing multiple polysaccharides, and directly utilizing; or dripping viscous fluid into ethanol for reprecipitation, and filtering to obtain yellowish solid powder containing multiple polysaccharides.
2. The method for extracting a plurality of polysaccharide substances from biomass materials as claimed in claim 1, wherein the biomass materials are straws including corn straws and wheat straws.
3. The method for extracting multiple polysaccharide substances from biomass material as claimed in claim 1, wherein the pulverized particles of step 1 are controlled to 10mm to 30mm, CaCl2The adding amount is 2% -3% of the biomass material, and then the temperature is raised to 180 ℃ at the heating rate of 4 ℃/minute, and the temperature is kept for 2 hours.
4. The method for extracting a plurality of polysaccharide substances from biomass materials as claimed in claim 1, wherein the method for separating black solids to obtain cellulose and lignin in step 3 is as follows: putting the black solid into a mixed solution system of butanol and water with the volume ratio of 1:1, stirring and heating at 180-200 ℃ for 1-2 hours, and stopping heating; then distilling the butanol phase obtained after filtration to obtain lignin; filtering and drying the water phase to obtain the cellulose.
5. The method of claim 1, wherein the polysaccharide comprises glucose, xylose, arabinose, mannose, xylose, and cellulose in step 3.
CN202010861440.1A 2020-08-25 2020-08-25 Method for extracting multiple polysaccharide substances from biomass material Pending CN112143835A (en)

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Application Number Priority Date Filing Date Title
CN202010861440.1A CN112143835A (en) 2020-08-25 2020-08-25 Method for extracting multiple polysaccharide substances from biomass material

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CN112143835A true CN112143835A (en) 2020-12-29

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4018620A (en) * 1975-05-19 1977-04-19 Biocel Corporation Method of hydrolyzing cellulose to monosaccharides
US4699124A (en) * 1985-06-28 1987-10-13 Power Alcohol, Inc. Process for converting cellulose to glucose and other saccharides
CN102660587A (en) * 2012-05-07 2012-09-12 中国科学院过程工程研究所 Method for pretreating lignocellulose raw material continuously/intermittently under normal pressure by using calcium chloride solution
CN106319100A (en) * 2015-06-30 2017-01-11 名京实业集团有限公司 Biomass resource utilization method
CN109504527A (en) * 2018-11-02 2019-03-22 石首市博锐德生物科技有限公司 Microalgae based biomass method for refining and the system for implementing it

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4018620A (en) * 1975-05-19 1977-04-19 Biocel Corporation Method of hydrolyzing cellulose to monosaccharides
US4699124A (en) * 1985-06-28 1987-10-13 Power Alcohol, Inc. Process for converting cellulose to glucose and other saccharides
CN102660587A (en) * 2012-05-07 2012-09-12 中国科学院过程工程研究所 Method for pretreating lignocellulose raw material continuously/intermittently under normal pressure by using calcium chloride solution
CN106319100A (en) * 2015-06-30 2017-01-11 名京实业集团有限公司 Biomass resource utilization method
CN109504527A (en) * 2018-11-02 2019-03-22 石首市博锐德生物科技有限公司 Microalgae based biomass method for refining and the system for implementing it

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Application publication date: 20201229