CN109722932B - Method for extracting cellulose from agricultural straw waste - Google Patents
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Abstract
The invention discloses a method for extracting cellulose from agricultural straw waste, which comprises the following steps: washing, drying and crushing the agricultural straw wastes into 40-60 meshes of materials; the materials are uniformly mixed with a high-boiling-point organic solvent-water, and under the action of a catalyst Lewis acid metal salt, the materials are stirred and react at normal pressure and a temperature of 130-160 ℃ to obtain crude cellulose. The method utilizes agricultural straw wastes which can be recycled, has mild conditions, can efficiently and selectively separate lignocellulose by short-time treatment at normal pressure and low temperature, and realizes 100 percent recovery of the cellulose in the agricultural straw wastes; the method has low requirement on a processing device and high safety.
Description
Technical Field
The invention belongs to the technical field of crop straw biomass chemical industry, relates to a method for extracting cellulose from agricultural straw waste, and particularly relates to a method for extracting cellulose from agricultural straw waste by using a high-boiling-point organic solvent and metal salt as catalysts.
Background
With the promotion of agricultural mechanization in China, crop planting production modes are gradually planted by small-crop planting transformation farms, and accompanying crop wastes are increased year by year. The crop waste is mainly straw biomass, such as rice straw, wheat straw, corn straw, cotton straw, rape straw, soybean straw and the like. In 2016, the amount of crop straw waste reaches 8 hundred million tons in China. However, crop straw waste is a renewable sustainable biomass resource, and domestic treatment methods are mostly used for burning or producing solid formed fuel on site, and a few of the waste is also used for returning straws to fields. In short, the treatment of the crop straw waste has the defects of environmental pollution, low-valued utilization, high treatment cost and the like, and the resource is greatly wasted.
The inventors have discovered that biorefinery technologies that achieve bio-energy and high value-added bio-based products from lignocellulosic biomass face a number of bottleneck problems, of which the problem of separation of the lignocellulosic feedstock components of the lignocellulosic-sugar platform (i.e., lignocellulosic biomass pretreatment) is particularly acute. Studies have shown that lignocellulosic feedstocks have complex chemical compositions and rather compact structures that are difficult to directly degrade by cellulase enzymes without pretreatment. Therefore, the lignocellulose raw material needs to be subjected to component separation treatment to realize efficient recovery of cellulose, so that the lignocellulose raw material can be used for enzymolysis of lignocellulose biomass.
At present, the separation method of components of lignocellulose raw materials comprises the following steps: dilute acid, dilute base, and steam/ammonia explosion, among others. However, these methods are often carried out under high temperature and high pressure conditions, and have various problems, such as large cellulose loss, high quality requirements for equipment, and the like, and are difficult to meet the requirements for separating components of biorefinery of lignocellulosic raw materials. In response to this problem, some high boiling point organic solvents are attracting increasing attention of researchers at home and abroad by virtue of their thermal stability and solubility (lignin), such as glycerol and ethylene glycol (L i sias et al, Bioresource Technol,2011,102: 10040-. Wheat straw was treated with commercial glycerol as a solvent at 220 ℃ for 3h, achieving high recovery of cellulose (-98%) (Sun et al, BioresourceTechnol,2015,187: 354-. Martin C et al by addition of H to glycerol solution2SO4Bagasse was treated as a catalyst at 190 ℃ for 1h to achieve a purity of 72% of cellulose in the treated matrix (Martin et al, Cell ChemTechnol,2011,45: 487-. The method adopts the high-boiling-point organic solvent to treat the biomass, so that the loss of cellulose can be effectively avoided, but the biomass needs to be treated at high temperature for a longer time, and the treatment cost is increased.
Disclosure of Invention
The invention aims to solve the problems of high requirement on treatment conditions and high treatment cost of the existing lignocellulose raw material component separation method, and provides a method for extracting cellulose from agricultural straw waste.
The purpose of the invention is realized by the following technical scheme:
a method for extracting cellulose from agricultural straw waste comprises the following steps: washing, drying and crushing the agricultural straw wastes into 40-60 meshes of materials; the material is uniformly mixed with a high boiling point organic solvent-water, and is heated under the action of a catalyst to obtain crude cellulose.
The agricultural straw waste is one or more of rice straw, wheat straw, corn straw, cotton straw, rape straw and soybean straw.
The agricultural straw waste is dried to the water content of 10-15%.
The agricultural straw waste is mechanically crushed to 40-60 meshes, so that the structural change of cellulose, such as the reduction of crystallinity, is avoided, and the complete recovery of the cellulose is ensured.
In addition to considering the solubility of the high-boiling organic solvent in lignin, it is necessary to avoid the problem that the heating temperature cannot be reached due to the change in boiling point affecting the reaction system when the proportion of water is too large. Therefore, the volume ratio (v/v) of the high boiling point organic solvent to water is controlled to be 60: 40-95: 5. The high boiling point organic solvent is one of glycerol and glycol.
The catalyst is Lewis acid metal salt; the metal Lewis acid salt is FeCl3、Fe2(SO4)3、AlCl3、CuCl2And CuSO4Preferably FeCl3、AlCl3。
The concentration of the catalyst in the high-boiling-point organic solvent-water is 0.015-0.2 mol/L, preferably 0.03-0.12 mol/L. Specifically, the catalyst is AlCl3、FeCl3In the case of the catalyst, the concentration of the catalyst in the high boiling point organic solvent-water is 0.015 to 0.1mol/L, preferably 0.03 to 0.06 mol/L. The catalyst is Fe2(SO4)3、CuCl2Or CuSO4When the catalyst is in a high-boiling-point organic solvent-The concentration of the water is 0.1-0.12 mol/L.
The dosage ratio of the agricultural straw wastes to the catalyst is 1g: 0.0003-0.004 mol, and preferably 1g: 0.0006-0.0024 mol.
The heating treatment is stirring reaction at the normal pressure and the temperature of 130-160 ℃ for 0.2-1 h.
Preferably, the heating treatment is that the temperature is raised from room temperature to 130-160 ℃ at the temperature raising rate of 12-16 ℃/min while stirring at normal pressure, the temperature is kept for 0.2-1 h, and then the temperature is cooled to about 50 ℃ at the temperature lowering rate of 5-10 ℃/min.
Specifically, the method for extracting the cellulose from the agricultural straw waste comprises the following steps:
washing and desanding soil by using agricultural straw wastes, naturally drying the soil until the water content is 10-15%, and crushing the soil into short and thin materials of 40-60 meshes;
and (2) uniformly mixing the material obtained in the step (1) with a high-boiling-point organic solvent-water, adding a catalyst, heating, filtering to obtain a solid, and washing to be neutral to obtain the crude cellulose.
The crude cellulose prepared by the method can be further hydrolyzed into fermentable sugar (glucose and xylose) by cellulase, and is used for producing biofuel such as biodiesel, microbial oil, cellulosic ethanol, butanediol and the like.
The invention has the beneficial effects that:
1. the invention takes agricultural straw waste as raw material and is renewable sustainable resource;
2. the invention adopts high boiling point organic solvent and water as reaction medium, the water is used for dissolving catalyst, so that the high boiling point organic solvent-water-catalyst becomes homogeneous phase; in addition, in the lignocellulosic structure, hemicellulose is mainly present between cellulose and lignin, and the metal lewis acid salt is acidic after dissolving in water, generating hydronium ions (H)3O+) The catalyst can break hydrogen bonds and partial ionic bonds in lignocellulose without decomposing the cellulose, thereby selectively removing a large amount of lignin and hemicellulose, and dissolving products of hemicellulose degradation products, such as monosaccharide, furfural, acetic acid, formic acid and the likeDissolving lignin in high boiling point organic solvent in water, and retaining cellulose; in the heating treatment process, the high-boiling-point organic solvent is not easy to lose, and can be recycled.
3. The method disclosed by the invention is mild in condition, lignocellulose can be efficiently and selectively separated by short-time treatment at normal pressure and low temperature, the recovery rate of cellulose in agricultural straw waste is 90-100%, the removal rate of hemicellulose is 80-95%, and the removal rate of lignin is 80-90%. The content of cellulose in the prepared crude cellulose is 50-80%, the content of hemicellulose is 3-15%, and the content of lignin is 5-12%. The specific surface area of the coarse cellulose is 5-15 m2The pore volume is 0.01-0.035 cm3The pore diameter is 1.6-2 nm.
4. The method has low requirement on a processing device and high safety.
Drawings
FIG. 1 is an electron microscope scanning picture of original rice straw.
FIG. 2 is an electron microscope scanning image of coarse cellulose of example 4.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the present invention will be further described in detail with reference to the specific embodiments. Those skilled in the art can implement appropriate modifications of the process parameters under the teachings of the present invention. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be included within the invention.
Example 1
Washing and desanding soil by rice straws (containing 34% of cellulose, 20% of hemicellulose and 26% of lignin), naturally drying until the water content is 10%, and crushing into short and thin materials of 40-60 meshes. 5g of crushed rice straws, 100mL of ethylene glycol-water solution (v/v,90:10) and aluminum chloride hexahydrate are filled in a three-hole flask (500mL), the concentration of the aluminum chloride hexahydrate in the ethylene glycol-water solution is 0.006mol/L, the three-hole flask is placed in an intelligent temperature control digital display heating jacket (ZNHW-500mL, Shanghai Yunshong instruments and equipment company), and the whole process is mechanically stirred (150rpm) to ensure uniform mixing. Monitoring the temperature by a thermocouple inserted below the liquid level, raising the temperature from room temperature (25-30 ℃) to 150 ℃ within 8-10min, and preserving the temperature for 30 min; removing the heating sleeve, cooling to about 50 ℃ within 15-20min, taking out the three-hole flask, and performing vacuum filtration by using a sand core funnel (G1-100mL) to obtain a solid; the solid is washed 3 times with deionized water (200 mL of deionized water each time) until the filtrate is neutral, and crude cellulose is obtained.
Example 2
5g of crushed rice straws (same as example 1), 100mL of ethylene glycol-water solution (v/v,90:10) and aluminum chloride hexahydrate are placed in a three-hole flask (500mL), the concentration of the aluminum chloride hexahydrate in the ethylene glycol-water solution is 0.017mol/L, the three-hole flask is placed in an intelligent temperature control digital display heating jacket, and the whole process is mechanically stirred (150rpm) to ensure uniform mixing. Monitoring the temperature by a thermocouple inserted below the liquid level, raising the temperature from room temperature (25-30 ℃) to 150 ℃ within 8-10min, and preserving the temperature for 30 min; removing the heating sleeve, cooling to about 50 ℃ within 15-20min, taking out the three-hole flask, and performing vacuum filtration by using a sand core funnel to obtain a solid; washing the solid with deionized water until the filtrate is neutral to obtain the crude cellulose.
Example 3
5g of crushed rice straws (same as example 1), 100mL of ethylene glycol-water solution (v/v,90:10) and aluminum chloride hexahydrate are placed in a three-hole flask (500mL), the concentration of the aluminum chloride hexahydrate in the ethylene glycol-water solution is 0.039mol/L, the three-hole flask is placed in an intelligent temperature control digital display heating jacket, and the whole process is mechanically stirred (150rpm) to ensure uniform mixing. Monitoring the temperature by a thermocouple inserted below the liquid level, raising the temperature from room temperature (25-30 ℃) to 150 ℃ within 8-10min, and preserving the temperature for 30 min; removing the heating sleeve, cooling to about 50 ℃ within 15-20min, taking out the three-hole flask, and performing vacuum filtration by using a sand core funnel to obtain a solid; washing the solid with deionized water until the filtrate is neutral to obtain the crude cellulose.
Example 4
5g of crushed rice straw (same as example 1), 100mL of ethylene glycol-water solution (v/v,90:10) and aluminum chloride hexahydrate are placed in a three-hole flask (500mL), the concentration of the aluminum chloride hexahydrate in the ethylene glycol-water solution is 0.055mol/L, the three-hole flask is placed in an intelligent temperature control digital display heating jacket, and the whole process is mechanically stirred (150rpm) to ensure uniform mixing. Monitoring the temperature by a thermocouple inserted below the liquid level, raising the temperature from room temperature (25-30 ℃) to 150 ℃ within 8-10min, and preserving the temperature for 30 min; removing the heating sleeve, cooling to about 50 ℃ within 15-20min, taking out the three-hole flask, and performing vacuum filtration by using a sand core funnel to obtain a solid; washing the solid with deionized water until the filtrate is neutral to obtain the crude cellulose. The results show that the cellulose content in the crude fiber reaches 76%, and the hemicellulose and lignin contents are respectively reduced to 4% and 7%, namely the cellulose in the rice straw is recovered by 100%, and 90% of hemicellulose and 88% of lignin are respectively removed.
After the treatment of ethylene glycol-aluminum chloride, the original compact and smooth surface of the rice straw (as shown in figure 1) is broken, and the rice straw is in a loose structure (as shown in figure 2). In addition, the crystallinity of the crude cellulose was 64.2%, and the specific surface area, pore volume and pore diameter reached 9.8m, respectively2/g,26.3×10-3cm3G and 1.9 nm.
Example 5
5g of crushed rice straw (same as example 1), 100mL of ethylene glycol-water solution (v/v,90:10) and aluminum chloride hexahydrate, wherein the concentration of the aluminum chloride hexahydrate in the ethylene glycol-water solution is 0.083mol/L, the mixture is placed in an intelligent temperature control digital display heating jacket, and the whole process is mechanically stirred (150rpm) to ensure uniform mixing. Monitoring the temperature by a thermocouple inserted below the liquid level, raising the temperature from room temperature (25-30 ℃) to 150 ℃ within 8-10min, and preserving the temperature for 30 min; removing the heating sleeve, cooling to about 50 ℃ within 15-20min, taking out the three-hole flask, and performing vacuum filtration by using a sand core funnel to obtain a solid; washing the solid with deionized water until the filtrate is neutral to obtain the crude cellulose.
Example 6
In a three-hole flask (500mL), 5g of pulverized rice straw (same as in example 1), 100mL of an ethylene glycol-water solution (v/v,90:10) and FeCl were charged3,FeCl3The concentration of the mixture in glycol-water solution is 0.06mol/L, the mixture is placed in an intelligent temperature control digital display heating jacket, the mixture is uniformly mixed by mechanical stirring (150rpm) in the whole process, the temperature is increased from room temperature (25 ℃ to 30 ℃) to 150 ℃ within 8 to 10min, and the temperature is kept for 30 min; removing the heating sleeve, cooling to about 50 ℃ within 15-20min, taking out the three-hole flask, and performing vacuum filtration by using a sand core funnel to obtain a solid; fixing deviceWashing the filtrate with deionized water to neutralize to obtain coarse fiber.
Example 7
In a three-hole flask (500mL), 5g of pulverized rice straw (same as in example 1), 100mL of an ethylene glycol-water solution (v/v,90:10), and 0.1mol/L Fe were charged2(SO4)3,Fe2(SO4)3The concentration of the mixture in glycol-water solution is 0.1mol/L, the mixture is placed in an intelligent temperature control digital display heating jacket, the mixture is uniformly mixed by mechanical stirring (150rpm) in the whole process, the temperature is increased from room temperature (25 ℃ to 30 ℃) to 150 ℃ within 8 to 10min, and the temperature is kept for 30 min; removing the heating sleeve, cooling to about 50 ℃ within 15-20min, taking out the three-hole flask, and performing vacuum filtration by using a sand core funnel to obtain a solid; the solid is neutralized with deionized water to obtain crude fiber.
Example 8
In a three-hole flask (500mL), 5g of pulverized rice straw (same as in example 1), 100mL of an ethylene glycol-water solution (v/v,90:10), and 0.1mol/L of CuSO were placed4,CuSO4The concentration of the mixture in glycol-water solution is 0.1mol/L, the mixture is placed in an intelligent temperature control digital display heating jacket, the mixture is uniformly mixed by mechanical stirring (150rpm) in the whole process, the temperature is increased from room temperature (25 ℃ to 30 ℃) to 150 ℃ within 8 to 10min, and the temperature is kept for 30 min; removing the heating sleeve, cooling to about 50 ℃ within 15-20min, taking out the three-hole flask, and performing vacuum filtration by using a sand core funnel to obtain a solid; the solid is washed by deionized water until the filtrate is neutral, and crude fiber is obtained.
Comparative example 1
5g of crushed rice straws (same as example 1) and 100mL of ethylene glycol-water solution (v/v,90:10) are filled in a three-hole flask (500mL), the three-hole flask is placed in an intelligent temperature control digital display heating jacket, the whole process is mechanically stirred (150rpm) to ensure uniform mixing, the temperature is raised from room temperature (25 ℃ -30 ℃) to 150 ℃ within 8-10min, and the temperature is kept for 30 min; removing the heating sleeve, cooling to about 50 ℃ within 15-20min, taking out the three-hole flask, and performing vacuum filtration by using a sand core funnel to obtain a solid; the solid is washed by deionized water until the filtrate is neutral, and crude fiber is obtained.
Table 1: treatment effect of different catalysts
Claims (5)
1. A method for extracting cellulose from agricultural straw waste is characterized by comprising the following steps: washing, drying and crushing the agricultural straw wastes into 40-60 meshes of materials; uniformly mixing the material with a high-boiling-point organic solvent-water, and heating under the action of a catalyst to obtain crude cellulose; the volume ratio of the high-boiling-point organic solvent to the water in the high-boiling-point organic solvent-water is 60: 40-95: 5; the high-boiling-point organic solvent is one of glycerol and glycol; the catalyst is FeCl3、Fe2(SO4)3、AlCl3One or more of the above; the concentration of the catalyst in the high-boiling-point organic solvent-water is 0.015-0.2 mol/L; the dosage ratio of the agricultural straw wastes to the catalyst is 1g: 0.0003-0.004 mol; the heating treatment is stirring reaction at the normal pressure and the temperature of 130-160 ℃ for 0.2-1 h.
2. The method for extracting the cellulose from the agricultural straw waste according to claim 1, wherein the agricultural straw waste is one or more of rice straw, wheat straw, corn straw, cotton straw, rape straw and soybean straw.
3. The method for extracting the cellulose from the agricultural straw waste according to claim 1, wherein the concentration of the catalyst in the high-boiling-point organic solvent-water is 0.03-0.12 mol/L.
4. The method for extracting the cellulose from the agricultural straw waste according to claim 1, wherein the using amount ratio of the agricultural straw waste to the catalyst is 1g: 0.0006-0.0024 mol.
5. The method for extracting the cellulose from the agricultural straw waste according to claim 1, wherein the operation of obtaining the crude cellulose by heating treatment under the action of the catalyst comprises: adding a catalyst, heating, filtering to obtain a solid, and washing to neutrality to obtain the crude cellulose.
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CN114717278A (en) * | 2021-01-06 | 2022-07-08 | 江南大学 | Agricultural and forestry biomass pretreatment method |
CN114197233B (en) * | 2021-12-17 | 2022-12-02 | 大连理工大学 | Method for separating and extracting cellulose nanofibers from agricultural and forestry solid wastes |
CN115196998A (en) * | 2022-07-19 | 2022-10-18 | 东华大学 | Method for enhancing hydrothermal humification of cellulose waste biomass |
CN115928479A (en) * | 2022-11-17 | 2023-04-07 | 安徽工程大学 | Method for efficiently deconstructing lignocellulose raw material by coupling carbon dioxide with organic solvent |
CN115785035B (en) * | 2023-02-03 | 2023-04-21 | 中国农业科学院农业环境与可持续发展研究所 | Method for preparing furfural and 5-hydroxymethylfurfural from straw |
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