CN112726253A - Method for efficiently separating plant fibers by acidic eutectic solvent/metal salt multi-component system - Google Patents
Method for efficiently separating plant fibers by acidic eutectic solvent/metal salt multi-component system Download PDFInfo
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- CN112726253A CN112726253A CN202110073880.5A CN202110073880A CN112726253A CN 112726253 A CN112726253 A CN 112726253A CN 202110073880 A CN202110073880 A CN 202110073880A CN 112726253 A CN112726253 A CN 112726253A
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- eutectic solvent
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- 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
- D21C3/00—Pulping cellulose-containing materials
- D21C3/20—Pulping cellulose-containing materials with organic solvents or in solvent environment
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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
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
Abstract
The invention relates to a method for pretreating lignocellulose by using an acidic eutectic solvent/metal salt Lewis acid multi-component solvent system. The method can be carried out at low temperature and normal pressure, and particularly can degrade and separate hemicellulose and partial lignin in plant fibers, so that the cellulose is efficiently reserved. The method can realize that the removal rate of hemicellulose reaches 97.26 percent, the retention rate of cellulose reaches 97.26 percent, and the high-efficiency separation of wood fiber components can be realized. The solvent is easy to prepare, green, pollution-free, recyclable, low in pretreatment energy consumption, low in requirements on environment and equipment, and good in industrial application prospect.
Description
Technical Field
The invention belongs to the technical field of biomass refining, and particularly relates to effective separation of three major components, namely cellulose, hemicellulose and lignin in plant fibers, wherein low-temperature, quick and effective separation is realized through a novel green solvent-acidic eutectic solvent/metal salt multi-element system.
Background
Lignocellulose is one of the main components of plant cell walls, the total amount of lignocellulose produced by photosynthesis on the earth can reach 1000 million tons every year, for example, the total amount of lignocellulose which can be collected in the United states every year can reach 10 million tons, China can also reach 8 million tons, however, only a small part of lignocellulose is effectively utilized by human beings. The main components of the lignocellulose, namely cellulose, hemicellulose and lignin, have the potential of replacing fossil fuels such as petroleum to prepare materials, chemicals and energy. However, during the long-term evolution of lignocellulose, more complex biological structures have evolved to prevent microbial and animal threats, known as "recalcitrance" of lignocellulose. During the conversion process of biomass, the complex chemical components and physical and chemical structures of the wood fibers can affect the permeation and mass transfer of the liquid medicine into the wood fiber raw material and the accessibility and activity of the cellulase. Therefore, separation of its components is essential before biomass conversion with lignocellulose.
In recent years, ABBOTT finds a novel natural ionic liquid-eutectic solvent, and attracts more and more students' attention. The eutectic solvent is a mixed solvent which is formed by mixing and heating a hydrogen bond acceptor and a hydrogen bond donor in a certain stoichiometric ratio for a certain time and is in a liquid state at room temperature. Generally, two or three solid high melting point reagents are mixed and heated for a certain time to form a stable solvent in a liquid state. Has a series of advantages of simple preparation process, low toxicity, biodegradability, environmental protection, recyclable use, low price of raw materials and the like. Since the eutectic solvent has similar physicochemical properties to ionic liquids, such as low volatility, incombustibility, etc., it is also called "ionic liquid-like".
Although a few eutectic solvents have been reported for separating and purifying lignocellulose, the separation of lignocellulose is not very effective. Especially, the removal effect on hemicellulose is not obvious. The presence of hemicellulose in lignocellulose has a higher effect on cellulase hydrolysis than lignin. On the basis of the research on the eutectic solvent, the metal salt with selective degradation effect on the hemicellulose is introduced into the low eutectic solvent reaction system, so that the hemicellulose in the wood fiber is rapidly separated at low temperature, and the cellulose with high yield and purity is obtained. The method realizes the high-efficiency separation of the lignocellulose components and lays a foundation for the subsequent high-added-value application of the lignocellulose components.
Disclosure of Invention
In order to overcome the problems and effectively separate components of lignocellulose in a low-temperature and normal-pressure environment, the invention provides a novel eutectic solvent for preparing a multi-hydrogen bond donor by introducing metal salt Lewis acid into the eutectic solvent. The prepared novel eutectic solvent is utilized to pretreat the wood fiber raw material, so that the effective separation of three major elements under normal pressure and low temperature is realized.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows:
step 1): mixing the hydrogen bond donor lactic acid, the hydrogen bond acceptor and metal salt Lewis acid, and reacting at 60-80 ℃ until uniform transparent liquid is formed;
step 2): uniformly mixing a lignocellulose raw material and the prepared eutectic solvent in the step 1), and reacting for 30-180min at normal pressure;
step 3): cooling the pretreatment mixture obtained in the step 2), and then carrying out solid-liquid separation to obtain solid pretreatment cellulose residues and pretreatment liquid;
step 4): analyzing the component composition of the solid residue obtained in the step 3) by utilizing an acid two-step hydrolysis method, and using the solid residue for subsequent utilization.
Preferably, the hydrogen bond acceptor is at least one of choline chloride, betaine hydrochloride and urea.
Preferably, the metal chloride lewis acid is at least one of potassium chloride, sodium chloride, magnesium chloride, copper chloride, aluminum chloride, ferric sulfate, copper sulfate, ammonium sulfate and magnesium sulfate.
Preferably, the plant fiber is needle-leaved wood, broad-leaved wood, and Gramineae raw material, and the size includes wood chip with length of 2-4cm and width of 1-2cm, grass raw material with length of 102cm, and 40-80 mesh pulverized granule.
Preferably, the ratio of the pretreatment solid to the liquid is 1: 3-1: 10, the temperature is 90-120 ℃, the pressure is normal, and the time is 30-180 min.
Has the advantages that: compared with the prior art, the invention has the remarkable advantages that:
1) the method introduces metal salt Lewis acid into a eutectic solvent system to form a multi-hydrogen bond donor system, pretreats the lignocellulose raw material at low temperature and normal pressure, effectively separates out cellulose, hemicellulose and lignin in the lignocellulose raw material, and particularly improves the recovery of hemicellulose monosaccharide. The prepared DES solvent is green and pollution-free and can be recycled. The pretreatment is carried out at normal pressure and low temperature, and has the advantages of low requirements on environment and equipment, strong operability, low energy consumption and the like.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It is to be understood that the described embodiments are merely a few, and not all embodiments of the invention. The present invention may be appropriately modified or supplemented by those skilled in the art, and all of them fall within the scope of the claims set forth herein.
Example 1
1) Preparation of eutectic solvent:
mixing the dried lactic acid and choline chloride according to the molar ratio of 2: 1, heating and stirring for 2 hours at the temperature of 60 ℃ until all solids are completely dissolved to form a uniform and transparent solution;
pre-treating plant fibers:
adding the eucalyptus powder with particle size of 40-80 mesh, which is obtained by pulverizing and sieving with plant pulverizer, into the obtained solution, mixing at solid-to-liquid ratio of 1: 10, and heating at 120 deg.C for 3 hr. After the reaction, the mixture was centrifuged at high speed to separate the pretreated solid residue and the pretreated liquid.
3) Chemical composition analysis of pretreated solid residue
Washing the pretreatment residue obtained in the step 2) with deionized water to be neutral, filtering, air-drying the solid, and taking part of the solid to measure the contents of cellulose, hemicellulose and lignin in the solid.
Example 2
1) Preparing a eutectic solvent:
mixing dried lactic acid and betaine hydrochloride according to a molar ratio of 6: 1, heating and stirring at 80 ℃ for 2 hours until all solids are completely dissolved to form a uniform transparent solution;
2) pre-treating plant fibers:
adding the eucalyptus powder with particle size of 40-80 mesh, which is obtained by pulverizing and sieving with plant pulverizer, into the obtained solution, mixing at solid-to-liquid ratio of 1: 10, and heating at 120 deg.C for 3 hr. After the reaction, the mixture was centrifuged at high speed to separate the pretreated solid residue and the pretreated liquid.
3) Chemical composition analysis of pretreated solid residue
Washing the pretreatment residue obtained in the step 2) with deionized water to be neutral, filtering, air-drying the solid, and taking part of the solid to measure the contents of cellulose, hemicellulose and lignin in the solid.
Example 3
1) Preparing a eutectic solvent:
mixing dried lactic acid and betaine according to a molar ratio of 2: 1, heating and stirring at 80 ℃ for 2 hours until all solids are completely dissolved to form a uniform and transparent solution;
2) pre-treating plant fibers:
adding the eucalyptus powder with particle size of 40-80 mesh, which is obtained by pulverizing and sieving with plant pulverizer, into the obtained solution, mixing at solid-to-liquid ratio of 1: 10, and heating at 120 deg.C for 3 hr. After the reaction, the mixture was centrifuged at high speed to separate the pretreated solid residue and the pretreated liquid.
3) Chemical component analysis of the pretreated solid residue: washing the pretreatment residue obtained in the step 2) with deionized water to be neutral, filtering, air-drying the solid, and taking part of the solid to measure the contents of cellulose, hemicellulose and lignin in the solid.
Example 4
1) Preparation of a solvent:
mixing dried lactic acid, betaine hydrochloride and ferric chloride at a molar ratio of 14.5: 1: 0.2, heating and stirring at 80 deg.C until all solids are completely dissolved to form uniform transparent solution;
2) DES pretreatment of plant fibers
Adding the obtained DES solution into eucalyptus powder of 40-80 mesh size which is pulverized and sieved by plant pulverizer, mixing at solid-to-liquid ratio of 1: 10, and heating at 105 deg.C for 145 min. After the reaction, the mixture was centrifuged at high speed to separate the pretreated solid residue and the pretreated liquid.
3) Chemical component analysis of the pretreated solid residue: washing the pretreatment residue obtained in the step 2) with deionized water to be neutral, filtering, air-drying the solid, and taking part of the solid to measure the contents of cellulose, hemicellulose and lignin in the solid.
Example 5
1) Preparation of a solvent:
mixing dried lactic acid, betaine hydrochloride and magnesium chloride at a molar ratio of 14.5: 1: 0.2, heating and stirring at 80 deg.C until all solids are completely dissolved to form uniform transparent solution;
2) DES pretreatment of plant fibers
Adding the obtained DES solution into eucalyptus powder of 40-80 mesh size which is pulverized and sieved by plant pulverizer, mixing at solid-to-liquid ratio of 1: 10, and heating at 105 deg.C for 145 min. After the reaction, the mixture was centrifuged at high speed to separate the pretreated solid residue and the pretreated liquid.
3) Chemical composition analysis of pretreated solid residue
Washing the pretreatment residue obtained in the step 2) with deionized water to be neutral, filtering, air-drying the solid, and taking part of the solid to measure the contents of cellulose, hemicellulose and lignin in the solid.
The analysis of the cellulose, hemicellulose and lignin contents of the pretreated solid residue obtained in examples 1-5 was compared and the results are shown in Table 1.
TABLE 1 analysis of the chemical composition of the pretreated solid residue
Claims (7)
1. The method for efficiently separating the plant fibers by using the acid eutectic solvent/metal salt ternary system is characterized by comprising the following steps of:
step (1): preparation of an acidic eutectic solvent (DES), characterized in that: mixing dry acid as Hydrogen Bond Donor (HBD) and different hydrogen bond acceptors in a certain proportion into a round-bottom flask, heating and stirring at 60-80 ℃ until the suspension in the round-bottom flask becomes a homogeneous transparent solution, and storing at room temperature;
step (2): preparation of an acidic eutectic solvent/metal salt (DES/MClx) solvent, characterized in that: adding a certain amount of metal salt into the prepared DES solvent, heating and stirring until a uniform and transparent solution is formed;
and (3): adding the vegetable fiber raw material into the DES solvent prepared in the step (1) or the DES/MClx solvent prepared in the step (2), and adding the solid-liquid mixture into a normal-pressure reaction kettle for pretreatment;
and (4): carrying out high-speed centrifugation on the solid-liquid mixture obtained in the step (3), and separating to obtain a pretreatment solid and a pretreatment liquid;
and (5): and (4) carrying out chemical component analysis on the pretreated solid obtained in the step (4), and analyzing and comparing the separation effect of each DES solvent and DES/MClx on plant fiber components.
2. The method for efficiently separating three major components of plant fiber by using the acidic eutectic solvent/metal salt ternary system as claimed in claim 1, wherein the three major components comprise: the hydrogen bond donor acid is one or more of lactic acid, acetic acid, sulfuric acid, formic acid and the like.
3. The method for efficiently separating three major components of plant fiber by using the acidic eutectic solvent/metal salt ternary system as claimed in claim 1, wherein the three major components comprise: the hydrogen bond receptor is one or a mixture of choline chloride, betaine hydrochloride and urea.
4. The method for efficiently separating three major components of plant fiber by using the acidic eutectic solvent/metal salt ternary system as claimed in claim 1, wherein the three major components comprise: the metal salt added into the DES/MClx solvent is one or more of ferric chloride, magnesium chloride, zinc chloride, copper chloride, sodium chloride, aluminum chloride, potassium chloride, ferric sulfate, copper sulfate, ammonium sulfate and magnesium sulfate.
5. The method for efficiently separating three major components of plant fiber by using the acidic eutectic solvent/metal salt ternary system as claimed in claim 1, wherein the three major components comprise: and (3) preparing a DES solvent, wherein the mass ratio of the hydrogen bond acceptor donor substances is 1: 1-1: 20, the reaction temperature is 60-80 ℃, and the reaction time is 0.5-10 h.
6. The method for efficiently separating three major components of plant fiber by using the acidic eutectic solvent/metal salt ternary system as claimed in claim 1, wherein the three major components comprise: the plant fiber raw material is selected from needle-leaved wood, broad-leaved wood, and herbaceous plant, and is wood chip with length of 2-4cm and width of 1-2cm, grass with length of 2-4cm, or 40-80 mesh granule obtained by pulverizing with plant pulverizer.
7. The method for efficiently separating three major components of plant fiber by using the acidic eutectic solvent/metal salt ternary system as claimed in claim 1, wherein the three major components comprise: in the step (3), the solid-liquid ratio is 1: 3-1: 10, the pretreatment temperature is 90-120 ℃, and the time is 30-180 min.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113215860A (en) * | 2021-05-12 | 2021-08-06 | 东北林业大学 | Lignin/cellulose composite film and preparation method thereof |
| CN113388653A (en) * | 2021-08-06 | 2021-09-14 | 南京林业大学 | Method for improving yield of moso bamboo holocellulase hydrolysis glucose |
| CN113862318A (en) * | 2021-09-28 | 2021-12-31 | 北京化工大学 | Green and efficient refining system and method for lignocellulose |
| CN113880887A (en) * | 2021-10-11 | 2022-01-04 | 浙江理工大学 | Method for extracting multifunctional active biological polyphenol from waste wood fiber and application |
| CN114351493A (en) * | 2021-12-08 | 2022-04-15 | 华南理工大学 | Method for removing intercellular layer lignin |
| CN114774147A (en) * | 2022-04-28 | 2022-07-22 | 华南农业大学 | Method for promoting oriented conversion of lignocellulose into intermediate chemicals and application |
| CN115368486A (en) * | 2022-07-20 | 2022-11-22 | 淮阴工学院 | Ternary eutectic solvent and application thereof in extraction of procambarus clarkia shell chitin |
| CN116814990A (en) * | 2023-08-31 | 2023-09-29 | 中国科学院过程工程研究所 | Method for extracting and separating vanadium in vanadium-arsenic solution by utilizing hydrophobic eutectic solvent |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113215860A (en) * | 2021-05-12 | 2021-08-06 | 东北林业大学 | Lignin/cellulose composite film and preparation method thereof |
| CN113388653A (en) * | 2021-08-06 | 2021-09-14 | 南京林业大学 | Method for improving yield of moso bamboo holocellulase hydrolysis glucose |
| CN113388653B (en) * | 2021-08-06 | 2023-07-25 | 南京林业大学 | Method for improving glucose hydrolysis yield of moso bamboo heald cellulase |
| CN113862318B (en) * | 2021-09-28 | 2023-12-15 | 北京化工大学 | Lignocellulose refining system and method |
| CN113862318A (en) * | 2021-09-28 | 2021-12-31 | 北京化工大学 | Green and efficient refining system and method for lignocellulose |
| CN113880887A (en) * | 2021-10-11 | 2022-01-04 | 浙江理工大学 | Method for extracting multifunctional active biological polyphenol from waste wood fiber and application |
| CN114351493A (en) * | 2021-12-08 | 2022-04-15 | 华南理工大学 | Method for removing intercellular layer lignin |
| CN114774147A (en) * | 2022-04-28 | 2022-07-22 | 华南农业大学 | Method for promoting oriented conversion of lignocellulose into intermediate chemicals and application |
| CN114774147B (en) * | 2022-04-28 | 2023-06-20 | 华南农业大学 | Method for promoting directional conversion of lignocellulose into intermediate chemicals and application |
| CN115368486A (en) * | 2022-07-20 | 2022-11-22 | 淮阴工学院 | Ternary eutectic solvent and application thereof in extraction of procambarus clarkia shell chitin |
| CN115368486B (en) * | 2022-07-20 | 2023-12-22 | 淮阴工学院 | Ternary eutectic solvent and application thereof in procambarus clarkia shell chitin extraction |
| CN116814990B (en) * | 2023-08-31 | 2023-11-10 | 中国科学院过程工程研究所 | Method for extracting and separating vanadium in vanadium-arsenic solution by utilizing hydrophobic eutectic solvent |
| CN116814990A (en) * | 2023-08-31 | 2023-09-29 | 中国科学院过程工程研究所 | Method for extracting and separating vanadium in vanadium-arsenic solution by utilizing hydrophobic eutectic solvent |
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Application publication date: 20210430 |