CN114438152A - Biomass pretreatment method and application - Google Patents
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- CN114438152A CN114438152A CN202210088975.9A CN202210088975A CN114438152A CN 114438152 A CN114438152 A CN 114438152A CN 202210088975 A CN202210088975 A CN 202210088975A CN 114438152 A CN114438152 A CN 114438152A
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- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
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Abstract
The invention provides a pretreatment method and application of biomass, wherein the method comprises the following steps: 1) crushing and screening the biomass raw material; 2) extracting benzene alcohol; 3) pretreating biomass by using the mixed solution; 4) and carrying out vacuum filtration to realize solid-liquid two-phase separation. The application mainly comprises the application of the pretreatment method of the biomass in the aspects of lignin recovery and cellulose conversion. The invention provides a pretreatment method and application of biomass, which can realize high-efficiency separation of biomass components under normal pressure and mild conditions, and simultaneously achieve the purposes of environmental friendliness and reduction of cost and energy consumption. The invention provides a biomass pretreatment method based on a green solvent, which has the remarkable advantages of environmental friendliness, mild conditions, high lignin removal rate and yield, stable solvent, high cellulase hydrolysis and saccharification efficiency, easy cellulose defibration and the like.
Description
Technical Field
The invention belongs to the technical field of biomass treatment, and particularly relates to a biomass pretreatment method and application.
Background
The conversion of lignocellulosic biomass is considered to be one of the most promising ways to address the growing fossil fuel shortages and environmental issues caused by combustion. Through the biomass refining technology, liquid fuels such as bioethanol and butanol, or biomass derived materials such as nanocellulose and holocellulose with high added values can be obtained from agricultural and forestry biomass such as wood, corncobs, bagasse, straws, waste paper and wood chips. However, there are many obstacles to the efficient utilization of lignocellulosic biomass due to the overall structural complexity of the lignocellulosic biomass components. Thus, pretreatment is a key step in deconstructing biomass and fractionating cellulose, hemicellulose and lignin for downstream high value utilization.
Conventional pretreatment techniques such as steam explosion, acid pretreatment and alkaline pretreatment methods use large amounts of energy and chemicals, such that the pretreatment step typically accounts for 20% to 30% of the total biofuel production cost. In addition, compared with extensive acid or alkali pretreatment, the organic solvent pretreatment can well maintain the structure of lignin, and is beneficial to converting the lignin into more valuable chemicals, thereby realizing the full utilization of biomass. Thus, there is increasing interest in the pretreatment of lignocellulosic biomass using low cost, environmentally friendly and non-toxic bio-based green solvents.
Disclosure of Invention
The first purpose of the present invention is to provide a method for pretreating biomass, which overcomes the disadvantages of the prior art.
Therefore, the above purpose of the invention is realized by the following technical scheme:
a method for pretreating biomass, which is characterized by comprising the following steps: the method comprises the following steps:
1) crushing and screening the biomass raw material:
crushing a biomass raw material, and sieving to obtain biomass powder;
2) and extraction of benzene alcohol:
extracting the biomass powder obtained by screening in the step 1) for 8 hours by using a toluene-ethanol mixed reagent, and then drying the biomass powder in a drying oven at 40 ℃;
3) and pretreating biomass by using the mixed solution:
weighing a certain amount of biomass powder obtained in the step 2) into a pressure-resistant bottle, adding a mixed solution into the pressure-resistant bottle according to the solid-to-liquid ratio of 1: 10-1: 20(m/v), wherein the volume ratio of isosorbide dimethyl ether or isosorbide acetate to water in the mixed solution is 10:0-8:2(v/v), and finally adding a certain amount of acid catalyst into the pressure-resistant bottle to enable the final concentration of the acid catalyst in the mixed solution to be 25-75 mM;
the whole reaction system is placed at the temperature of 100-120 ℃, the reaction lasts for 10-100min, and continuous magnetic stirring is carried out;
4) and carrying out vacuum filtration to realize solid-liquid two-phase separation:
after the reaction in the step 3) is finished, placing a pressure-resistant bottle in cold water for cooling, performing suction filtration by using a vacuum suction filtration device to realize solid-liquid two-phase separation, continuously washing the cellulose-rich slurry (solid phase) by using a mixed solution with the same volume and ratio as those in the step 3), and collecting filtrate; and finally, cleaning the solid-phase slurry by using ultrapure water with the volume 10 times that of the solid-phase slurry to remove the residual organic solvent on the surface of the solid-phase slurry.
While adopting the technical scheme, the invention can also adopt or combine the following technical scheme:
as a preferred technical scheme of the invention: the biomass is one of coniferous wood, broadleaf wood or grass.
As a preferred technical scheme of the invention: the acid catalyst is a Bronsted acid or a Lewis acid or acetic acid or oxalic acid or toluenesulfonic acid.
As a preferred technical scheme of the invention: in the step 1), the screen is 60-100 meshes.
As a preferred technical scheme of the invention: in the step 2), the volume ratio of the toluene to the ethanol is 2: 1.
A second object of the present invention is to provide the use of the method for pretreating biomass according to the above in the recovery of lignin, in view of the disadvantages of the prior art.
Therefore, the above purpose of the invention is realized by the following technical scheme:
use of a method of pretreatment of biomass according to the preamble for lignin recovery, comprising: and (3) dropwise adding the filtrate obtained by suction filtration into an aqueous solution containing 5-10% of NaCl to realize precipitation of lignin, and finally recovering the lignin by vacuum suction filtration.
A third object of the present invention is to provide the use of the pretreatment method of biomass according to the above in the conversion of cellulose, in view of the disadvantages of the prior art.
Therefore, the above purpose of the invention is realized by the following technical scheme:
use of a method of pretreatment of biomass as hereinbefore described for cellulose conversion, the use comprising: and (3) carrying out enzymatic hydrolysis on the solid-phase slurry obtained by suction filtration, adding 20-60 FPU (fermented glutinous rice) cellulase into each gram of cellulose component, and carrying out enzymatic saccharification for 72-96 h in a constant-temperature shaking table at 50 ℃ to obtain hydrolysate.
A fourth object of the present invention is to provide, in view of the drawbacks of the prior art, another application of the pretreatment method of biomass according to the preamble in cellulose conversion.
Therefore, the above purpose of the invention is realized by the following technical scheme:
use of a method of pretreatment of biomass as hereinbefore described for cellulose conversion, the use comprising: and (3) defibrating the solid-phase slurry obtained by suction filtration, and defibrating in a ball mill for 60-240 min according to the solid content ratio of 0.1-2%.
The invention provides a pretreatment method and application of biomass, which can realize high-efficiency separation of biomass components under normal pressure and mild conditions, and simultaneously achieve the purposes of environmental friendliness and reduction of cost and energy consumption. The invention provides a biomass pretreatment method based on a green solvent, which has the remarkable advantages of environmental friendliness, mild conditions, high lignin removal rate and recovery rate, stable solvent, high cellulase hydrolysis and saccharification efficiency, easy cellulose defibration and the like.
Drawings
FIG. 1 is a two-dimensional nuclear magnetic spectrum (aroma region) of eucalyptus native lignin (MWL) and lignin treated with isosorbide dimethyl ether or a mixed solution of isosorbide dimethyl ether/water.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited thereto.
The eucalyptus used in the invention is eucalyptus grandis, and the components of the eucalyptus grandis are 50.3% of cellulose, 16.0% of hemicellulose, 31.1% of lignin and 2.6% of others.
The calculation formula of the lignin removal rate and the lignin yield is as follows:
the chemical structure of isosorbide dimethyl ether is as follows:
the chemical structure of isosorbide acetate is as follows:
in the following examples, isosorbide dimethyl ether is used as an example, but since isosorbide acetate and isosorbide dimethyl ether have similar chemical structures and the Relative Energy Difference between the isosorbide acetate and the isosorbide dimethyl ether calculated by hansen solubility parameters is less than 1(Relative Energy Difference <1), isosorbide acetate should be effective for biomass pretreatment if dimethyl isosorbide can be effective for biomass pretreatment.
Example 1
A method of pretreating biomass comprising the steps of:
1) and crushing and screening the eucalyptus raw material:
crushing a eucalyptus raw material, and screening with a 60-100 mesh screen to obtain eucalyptus powder;
2) and extracting benzene alcohol:
extracting 60-100-mesh eucalyptus powder obtained after screening in the step 1) for 8 hours by using toluene-ethanol (2:1, v/v), and then putting the powder into an oven to dry at 40 ℃;
3) and pretreating biomass by using an isosorbide dimethyl ether/water mixed solution:
weighing 1.5g of the eucalyptus powder obtained in the step 2) into a pressure-resistant bottle, adding 15ml of isosorbide dimethyl ether into the pressure-resistant bottle according to the solid-to-liquid ratio of 1:10(m/v), and adding a certain amount of 67.5 mul of 72% H into the pressure-resistant bottle2SO4And (3) solution. The whole reaction system is placed at 100 ℃ for reaction for 60min, and continuous magnetic stirring is carried out.
4) And carrying out vacuum filtration to realize solid-liquid two-phase separation:
and (3) after the reaction in the step 3) is finished, putting the pressure-resistant bottle into cold water for cooling. And after 5min, performing suction filtration by using a vacuum suction filtration device to realize solid-liquid two-phase separation, taking 15ml of isosorbide dimethyl ether solution to wash the pulp (solid phase) rich in cellulose, and collecting filtrate together. Finally, the slurry was washed with 300ml of ultrapure water to remove the residual organic solvent on the surface of the slurry.
And (3) recovering lignin:
dropwise adding the filtrate obtained by filtering in the step 4) into 300ml of 5% NaCl aqueous solution to precipitate and separate out lignin. Finally, the lignin is recovered by vacuum filtration. The weight of the recovered lignin is 0.073g, and the removal rate of the obtained lignin is 52.2 percent and the yield is 15.6 percent by calculation.
Cellulose conversion and utilization:
carrying out enzyme hydrolysis on the pulp which is rich in cellulose and is obtained by separation in the step 4). Adding 20FPU cellulase per gram of cellulose component
Carrying out enzymolysis and saccharification for 72h in a constant-temperature shaking table at 50 ℃ to obtain hydrolysate, wherein the hydrolysis and saccharification efficiency is 6.8%.
Another application is to defibrate the cellulose-rich pulp separated in step 4). Defibrating in a ball mill for 60min according to the solid content ratio of 0.5%. The pretreated pulp is more likely to produce microfibrils than the pulp in which the raw material has been subjected to a bleaching treatment.
Example 2
When the temperature in step 3) of example 1 is raised to 120 ℃ and other conditions are not changed, the mass of the recovered lignin is 0.205g, and the calculated removal rate of the lignin is 79.4%, and the yield is 43.8%.
The cellulose hydrolysis saccharification efficiency in the cellulose conversion and utilization is 8.1 percent.
Example 3
When the temperature in the step 3) of the embodiment 1 is raised to 120 ℃, the volume ratio of the isosorbide dimethyl ether to the water is changed to 9:1(v/v), and other conditions are not changed, the mass of the recovered lignin is 0.237g, the removal rate of the lignin is 91.2 percent by calculation, and the yield is 50.6 percent.
The cellulose hydrolysis saccharification efficiency in the cellulose conversion and utilization is 82.1 percent.
Example 4
When the temperature in the step 3) of the embodiment 1 is increased to 120 ℃, the volume ratio of the isosorbide dimethyl ether to the water is changed to 8:2(v/v), and other conditions are not changed, the mass of the recovered lignin is 0.182g, the removal rate of the lignin is 71.3 percent by calculation, and the yield is 38.8 percent.
The cellulose hydrolysis saccharification efficiency in the cellulose conversion and utilization is 53.5 percent.
Example 5
The temperature in step 3) of example 1 was raised to 120 ℃ and the volume ratio of dimethyl isosorbide to water was changed to 9:1 (v/v). Performing enzyme hydrolysis on the cellulose-rich pulp obtained by separation in the step 4), and adding 60FPU cellulase into each gram of cellulose component
The other conditions are unchanged, and the cellulose hydrolysis saccharification efficiency in the cellulose conversion and utilization is 97.5 percent.
Example 6
The temperature in step 3) of example 1 was raised to 120 ℃ and the volume ratio of dimethyl isosorbide to water was changed to 9:1 (v/v). Performing enzyme hydrolysis on the cellulose-rich pulp obtained by separation in the step 4), and adding 60FPU cellulase into each gram of cellulose component
The enzyme hydrolysis time is adjusted to 96h, other conditions are not changed, and the cellulose hydrolysis saccharification efficiency in the cellulose conversion and utilization is 93.7 percent.
Example 7
The temperature in step 3) of example 1 was increased to 120 ℃, the reaction time was reduced from 60min to 20min, and the volume ratio of dimethyl isosorbide to water was changed to 9:1 (v/v). Performing enzyme hydrolysis on the cellulose-rich pulp obtained by separation in the step 4), and adding 60FPU cellulase into each gram of cellulose component
When the enzyme hydrolysis time is adjusted to 96 hours, the mass of the recovered lignin is 0.154g, the removal rate of the obtained lignin is 69.8 percent by calculation, and the yield is 32.9 percent.
The cellulose hydrolysis saccharification efficiency in the cellulose conversion and utilization is 48.3 percent.
The above examples are part of the embodiment of the invention, wherein the comparison between the reaction temperature of example 1 and example 2 shows that the removal rate and recovery rate of lignin are remarkably increased along with the increase of the temperature; the comparison of different volume ratios of isosorbide dimethyl ether and water in examples 2, 3 and 4 shows that the removal rate and recovery rate of lignin and the enzymolysis efficiency of cellulose are remarkably increased with the addition of a small amount of water, and as shown in fig. 1, the 2D HSQC NMR characterization shows that the condensation polymerization of lignin is reduced with the increase of water amount, which means that the recovered lignin is closer to the original lignin of eucalyptus wood and the structure of lignin is kept more completely in the pretreatment process; example 3 is compared with example 5 by different addition amounts of cellulase, and the result shows that the hydrolysis efficiency of cellulose is increased along with the increase of the addition amount of the cellulase; the results of comparing the enzyme hydrolysis time in example 5 with that in example 6 show that the cellulose hydrolysis time is increased from 72h to 96h, and the cellulose hydrolysis saccharification efficiency is not greatly changed; example 6 is a comparison of different reaction times with example 7, and the results show that the longer the reaction time, the higher the lignin removal rate, the lignin yield, and the enzymatic saccharification efficiency of cellulose.
The above-described embodiments are intended to illustrate the present invention, but not to limit the present invention, and any modifications, equivalents, improvements, etc. made within the spirit of the present invention and the scope of the claims fall within the scope of the present invention.
Claims (8)
1. A method for pretreating biomass, which is characterized by comprising the following steps: the method comprises the following steps:
1) crushing and screening the biomass raw material:
crushing a biomass raw material, and sieving to obtain biomass powder;
2) and extracting benzene alcohol:
extracting the screened biomass powder for a certain time by using a toluene-ethanol mixed reagent and then drying;
3) and pretreating biomass by using the mixed solution:
weighing a certain amount of biomass powder obtained in the step 2) into a pressure-resistant bottle, adding a mixed solution into the pressure-resistant bottle according to a solid-to-liquid ratio of 1: 10-1: 20, wherein the volume ratio of isosorbide dimethyl ether or isosorbide acetate to water in the mixed solution is 10:0-8:2, and finally adding a certain amount of acid catalyst into the pressure-resistant bottle to enable the final concentration of the acid catalyst in the solution to be 25-75 mM;
the whole reaction system is placed at 100-120 ℃, and is reacted for 10-100min, and continuous magnetic stirring is carried out;
4) and carrying out vacuum filtration to realize solid-liquid two-phase separation:
and (3) after the reaction in the step 3) is finished, placing the pressure-resistant bottle in cold water for cooling, performing suction filtration by using a vacuum filtration device to realize solid-liquid two-phase separation, continuously washing the solid-phase slurry subjected to vacuum filtration by using a mixed solution with the same volume and ratio as those in the step 3), simultaneously collecting filtrate, and finally cleaning the solid-phase slurry by using ultrapure water to remove the residual organic solvent on the surface of the solid-phase slurry.
2. The method for pretreating biomass according to claim 1, wherein: the biomass is one of coniferous wood, broadleaf wood or grass.
3. The method for pretreating biomass according to claim 1, wherein: the acid catalyst is a Bronsted acid or a Lewis acid or acetic acid or oxalic acid or toluenesulfonic acid.
4. The method for pretreating biomass according to claim 1, wherein: in the step 1), the screen is 60-100 meshes.
5. The method for pretreating biomass according to claim 1, wherein: in the step 2), the volume ratio of the toluene to the ethanol is 2: 1.
6. Use of the method for the pretreatment of biomass according to claim 1 for the recovery of lignin, characterized in that: the application comprises the following steps: and (3) dropwise adding the filtrate obtained by suction filtration into an aqueous solution containing 5-10% of NaCl to realize precipitation of lignin, and finally recovering the lignin by vacuum suction filtration.
7. Use of the method for the pretreatment of biomass according to claim 1 for the conversion of cellulose, characterized in that: the application comprises the following steps: and (3) carrying out enzymatic hydrolysis on the solid-phase slurry obtained by suction filtration, adding 20-60 FPU (fermented glutinous rice) cellulase into each gram of cellulose component, and carrying out enzymatic saccharification for 72-96 h in a constant-temperature shaking table at 50 ℃ to obtain hydrolysate.
8. Use of the method for the pretreatment of biomass according to claim 1 for the conversion of cellulose, characterized in that: the application comprises the following steps: and (3) defibrating the solid-phase slurry obtained by suction filtration, and defibrating in a ball mill for 60-240 min according to the solid content ratio of 0.1-2%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115678945A (en) * | 2022-10-27 | 2023-02-03 | 西湖大学 | Application of sulfuric acid-aluminum trichloride co-catalyst in promotion of lignocellulose enzymatic hydrolysis and saccharification |
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| JP2018039779A (en) * | 2016-06-27 | 2018-03-15 | 国立大学法人北海道大学 | Production method of alcohol |
| JP2018153140A (en) * | 2017-03-17 | 2018-10-04 | 三菱ケミカル株式会社 | Manufacturing method of carbohydrate solution for furfural manufacturing raw material and manufacturing method of furfural |
| US20200399549A1 (en) * | 2018-02-16 | 2020-12-24 | A.P. Møller - Mærsk A/S | A biofuel composition comprising lignin |
| CN113789355A (en) * | 2021-10-20 | 2021-12-14 | 浙江理工大学 | Method for improving lignocellulose enzymolysis saccharification efficiency through green high-efficiency pretreatment |
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Patent Citations (6)
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| WO2011050424A1 (en) * | 2009-10-27 | 2011-05-05 | Katholieke Universiteit Leuven | Catalytic process for the production of alcohols from biomass-related feedstock |
| US20170159076A1 (en) * | 2015-12-04 | 2017-06-08 | Arbiom Inc. | Method for fractionating a lignocellulosic biomass |
| JP2018039779A (en) * | 2016-06-27 | 2018-03-15 | 国立大学法人北海道大学 | Production method of alcohol |
| JP2018153140A (en) * | 2017-03-17 | 2018-10-04 | 三菱ケミカル株式会社 | Manufacturing method of carbohydrate solution for furfural manufacturing raw material and manufacturing method of furfural |
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