CN115976116A - Green and efficient biomass pretreatment method - Google Patents
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Abstract
The invention discloses a green and efficient biomass pretreatment method, which comprises the steps of soaking biomass fragments in water to obtain wet biomass fragments, carrying out steam explosion treatment on the wet biomass fragments to obtain biomass residues, adding the biomass residues into a eutectic solvent, reacting, and collecting solid residues; the eutectic solvent is a mixed solvent consisting of choline chloride and formic acid. According to the invention, steam explosion and the eutectic solvent are coupled, and the lignocellulose-containing biomass is pretreated under mild conditions, so that lignin and hemicellulose can be efficiently removed, a cellulose product with high purity and less loss is produced, wherein the structure and the composition of the cellulose are not greatly changed, and the method can be applied to the field of production of various large celluloses.
Description
Technical Field
The invention belongs to the technical field of biomass pretreatment, and particularly relates to a green and efficient biomass pretreatment method.
Background
With the excessive consumption of fossil resources and the inevitable trend of sustainability development roads, the concept of actively developing and applying environmentally-friendly renewable resources becomes a consensus, and industrial chemicals developed based on biomass have attracted the active attention of researchers. Lignocellulose has the advantages of wide source and abundant reserves, and can be effectively converted into various fossil resource substitutes for use in various fields as a renewable biomass resource with the most development potential. For example, the separated and purified lignin is made into nano lignin for application and various functional materials, the cellulose is subjected to enzymolysis and fermentation to produce bioethanol or is catalytically converted into ethylene glycol, and a hemicellulose product can become an optimal raw material for producing furfural.
However, lignocellulosic biomass, which is composed of hemicellulose, cellulose, lignin and a small amount of ash, is a main component constituting plant cell walls, and they are connected to each other by hydrogen bonds and anisole bonds, and are bonded together by intermolecular forces such as van der waals force, etc., to form a complex three-dimensional structure (anti-depolymerization barrier), which makes it difficult to convert lignocellulose into lignocellulose. If biomass is directly used as a raw material, the process cost is high, the products are easy to be complicated and varied, and most of cellulose is lost, so that the lignocellulose biomass is required to be pretreated for subsequent conversion and utilization in the current industrial production. Conventional pretreatment uses an acid treatment method, an alkali treatment method, an ionic liquid treatment method, a physical treatment method, a hydrothermal method, a eutectic solvent treatment method, and the like. Wherein the acid and alkali treatment corrodes equipment, causes additional environmental pollution, is difficult to recover a treatment solvent, has high cost in an ionic liquid treatment method and low physical method efficiency, and has high requirements on equipment due to high temperature and high pressure required by a hydrothermal method. However, the eutectic solvent treatment time is long but the solvent recovery is easy, but usually the solvent system is complicated, the reaction conditions are harsh, and the damage to equipment is large, for example, in patent (CN 115261219A), a biomass pretreating agent is an organic acid-based eutectic solvent, which includes organic acid, choline chloride and lewis acid, the lewis acid used includes one or more of aluminum chloride, ferric chloride and manganese chloride, wherein too many chloride ions in the lewis acid have large damage to the equipment, and meanwhile, the defects of inhibition of metal ions on the activity of cellulase and the like exist, and in addition, the residue yield is only about 44%, and the yield is low.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a green and efficient biomass pretreatment method, which comprises the steps of soaking treatment, steam explosion and eutectic solvent pretreatment on wood waste. Can remove most lignin and obtain high-quality raw materials with high cellulose retention rate for biomass energy production. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention provides a green and efficient biomass pretreatment method, which comprises the steps of soaking biomass fragments in water to obtain wet biomass fragments, carrying out steam explosion treatment on the wet biomass fragments to obtain biomass residues, adding the biomass residues into a eutectic solvent, reacting, and collecting solid residues; the eutectic solvent is a mixed solvent composed of choline chloride and formic acid.
The pretreatment method adopts steam explosion and eutectic solvent for synergistic treatment, firstly adopts steam explosion, introduces high-pressure steam and quickly releases pressure to promote the degradation of poplar hemicellulose into monosaccharide and cellulose, so that the cellulose is expanded and fractured, the cellulose crystallinity is changed, and partial lignin conversion is induced, so that the compact three-dimensional network structure of biomass is destroyed, and then utilizes the eutectic solvent to treat explosion residues, so as to destroy beta-O-4 connecting bonds between lignin, benzyl ether bonds of lignin and hemicellulose and other connecting bonds. Because the cohesive energy of the cellulose is too strong, the strength of hydrogen bonds in a eutectic solvent (DES) is weaker than the acting force between the cellulose, and the cellulose cannot be dissociated in a DES system, so that the DES can selectively separate lignin and the cellulose.
In the invention, the mixed solvent consisting of choline chloride and formic acid is only used as the eutectic solvent, so that the excellent pretreatment effect can be obtained, and the yield greatly higher than that of the prior art can be obtained.
According to the invention, steam explosion and the eutectic solvent are coupled, and the biomass containing lignocellulose is pretreated under mild conditions, so that lignin and hemicellulose can be efficiently removed, a cellulose product with high purity and less loss is produced, wherein the structure and the composition of cellulose are not greatly changed, and the method can be applied to the field of production of various large celluloses.
Further, the particle size of the biomass crumbs is 4-10 meshes.
Further, the time for soaking the biomass fragments in water is 12-24h.
Further, the pressure of the steam explosion treatment is 1.6-1.8MPa, and the pressure maintaining time is 180-240s.
In the invention, the pressure of the steam explosion treatment is controlled within the range, the cooperative treatment effect with DES is optimal finally, if the pressure of the steam explosion is too high, the hemicellulose is excessively hydrolyzed, harmful substances such as 5-hydroxymethylfurfural and the like which influence the enzymolysis effect are generated, and in addition, the crystallization area of cellulose is damaged by severe explosion conditions, so that the production of some functional materials based on the cellulose is not favorable. In actual operation, the wet biomass chips are placed in a steam explosion machine for treatment.
Further, performing steam explosion treatment on the wet biomass chips to obtain a product, and airing the product in the natural environment to obtain biomass residues.
Further, in the eutectic solvent, the molar ratio of choline chloride to formic acid is 1.8-2.5.
In the invention, the eutectic solvent selects a hydrogen bond acceptor as choline chloride and a hydrogen bond donor as formic acid, and in the actual exploration process, the inventor tries a large number of hydrogen bond donors, and finally finds that the optimal effect can be obtained by adopting the mutual matching of the formic acid and the choline chloride.
Further, the method for obtaining the eutectic solvent comprises the following steps: choline chloride is reacted with formic acid at 75-85 ℃ for 1.5-2h until a clear homogeneous solution is formed.
Further, the solid-liquid mass volume ratio of the biomass residue to the eutectic solvent is 1g.
Furthermore, the reaction temperature is 100-120 ℃, and the reaction time is 2-4h.
By adopting the eutectic solvent, excellent pretreatment effect can be obtained at lower temperature.
Further, after the reaction is finished, carrying out vacuum filtration to carry out solid-liquid separation on the mixture obtained by the reaction, washing the obtained solid phase to be neutral by using an ethanol water solution, and collecting solid residues; namely the separated and purified cellulose product.
Furthermore, the ethanol aqueous solution is a mixed solution prepared by mixing ethanol and ultrapure water according to a volume ratio of 1.
Advantageous effects
The method optimizes the prior biomass pretreatment technology, avoids excessive crushing processing of biomass waste in the whole process, reduces the requirements on the biomass raw material, has mild reaction conditions, short production period, high efficiency and yield greatly higher than that of the prior treatment technology, and also has the advantages of meeting the removal effect of hemicellulose after blasting by carrying out water soaking treatment on the biomass raw material before blasting, avoiding the defects of inhibiting the activity of cellulase and the like because dilute acid or dilute alkali is not necessary to be used, reducing environmental pollution and equipment corrosion and simultaneously not using metal ions.
As the biomass material with larger grain size is adopted as the raw material, the processing difficulty is reduced, and the raw material can fully utilize wood processing leftover materials and waste materials.
The green and efficient biomass pretreatment method provided by the invention can effectively improve the utilization efficiency of each component of the lignocellulose by separating the lignocellulose and produce cleaner and more environment-friendly green chemicals.
The invention optimizes the wood processing technology, reduces the particle size requirement of the biomass raw material, can fully utilize the waste wood, has mild reaction conditions in the whole preparation process, can recycle the eutectic solvent, has simple process, is easy to scale and has low requirement on equipment materials.
Drawings
FIG. 1: a comparison graph of the content of each component of the lignocellulose before and after pretreatment,
FIG. 2: a comparison graph of cellulose retention rate, hemicellulose removal rate and lignin removal rate before and after pretreatment,
FIG. 3: the medium pressure time in steam explosion influences the content of each component of lignocellulose,
FIG. 4: the blasting pressure in the steam blasting influences the content of each component of the lignocellulose,
FIG. 5: the treatment temperature in the eutectic solvent influences the content of each component of the lignocellulose,
FIG. 6: the treatment time in the eutectic solvent influences the content of each component of the lignocellulose.
Detailed Description
The following is a detailed description of specific embodiments of the present invention by way of specific examples. The examples are given solely for the purpose of illustration and are not intended to limit the scope of the invention. The starting materials used in the examples are either commercially available or prepared by conventional methods.
Determining the contents of cellulose, hemicellulose and lignin in poplar raw materials and pretreated poplar residues by an analysis method of a renewable energy laboratory (NREL) in the United states, and calculating the cellulose retention rate, the hemicellulose removal rate and the lignin removal rate, wherein the specific calculation formula is as follows:
in the formula: m is the product yield after pretreatment, M 0 、m 1 The solid mass (g) before and after pretreatment; c 1 、H 1 And L 1 The content (%) of cellulose, hemicellulose and lignin in the raw material; c 2 、H 2 And L 2 The content (%) of cellulose, hemicellulose and lignin in the pretreated poplar residue.
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 invention.
Example 1:
the green high-efficiency biomass pretreatment method comprises the following steps:
1) And (3) steam explosion treatment: soaking 4-6 mesh biomass chips in water for 24h, and treating in a steam explosion machine with explosion pressure of 1.6MPa and pressure maintaining time of 180s. Collecting residues after blasting, and airing in a natural environment;
2) Preparing a eutectic solvent: choline chloride was reacted with formic acid at 80 ℃ for 2h until a clear homogeneous solution was formed.
3) Pretreatment of eutectic solvent: adding a eutectic solvent into the dried biomass residue according to a solid-to-liquid ratio of 1 (g/ml) to 20, and carrying out oil bath for 2h at 120 ℃;
4) Washing: and (3) performing solid-liquid separation on the mixture after the pretreatment reaction is finished by vacuum filtration, washing the solid residue with an ethanol water solution (v: v = 1) until the solid residue is neutral, and collecting the solid residue, namely the separated and purified cellulose product.
In the solid residue obtained after pretreatment, the residue yield is 62.74%, the cellulose content is 75.97%, the removal rates of hemicellulose and lignin are 75.77% and 86.94% respectively, and the cellulose retention rate is 96.67%.
Example 2:
the green high-efficiency biomass pretreatment method comprises the following steps:
1) And (3) steam explosion treatment: soaking 4-6 mesh biomass chips in water for 24h, and treating in a steam explosion machine with explosion pressure of 1.6MPa and pressure maintaining time of 180s. Collecting residues after blasting, and airing in a natural environment;
2) Preparing a eutectic solvent: choline chloride was reacted with formic acid at 80 ℃ for 2h until a clear homogeneous solution was formed.
3) Pretreatment of eutectic solvent: and (3) adding the dried biomass residues into the mixture according to the solid-to-liquid ratio of 1:20 (g/ml) adding a eutectic solvent, and carrying out oil bath for 4h at 120 ℃;
4) Washing: and (3) performing solid-liquid separation on the mixture after the pretreatment reaction is finished by adopting vacuum filtration, washing the solid residue with an ethanol water solution (v: v = 1) until the solid residue is neutral, and collecting the solid residue, namely the separated and purified cellulose product.
In the solid residue obtained after pretreatment, the yield of the residue is 55.00%, the cellulose content is 81.35%, the removal rates of hemicellulose and lignin are respectively 83.50% and 85.47%, and the retention rate of cellulose is 90.75%.
Comparative example 1:
the green high-efficiency biomass pretreatment method comprises the following steps:
1) Simple soaking treatment: soaking 4-6 mesh biomass chips in water for 24h, and airing in a natural environment;
2) Preparing a eutectic solvent: choline chloride was reacted with formic acid at 80 ℃ for 2h until a clear homogeneous solution was formed.
3) Pretreatment of eutectic solvent: adding a eutectic solvent into the dried biomass residue according to a solid-to-liquid ratio of 1 (g/ml) to 20, and carrying out oil bath at 120 ℃ for 4h;
4) Washing: and (3) performing solid-liquid separation on the mixture after the pretreatment reaction is finished by vacuum filtration, washing the solid residue with an ethanol water solution (v: v = 1) until the solid residue is neutral, and collecting the solid residue, namely the separated and purified cellulose product.
In the solid residue obtained after pretreatment, the residue yield is 40.98%, the cellulose content is 86.48%, the removal rates of hemicellulose and lignin are respectively 95.69% and 95.09%, and the cellulose retention rate is 71.88%; therefore, although most of hemicellulose and lignin can be removed without blasting treatment, most of cellulose is hydrolyzed due to chemical bonding of components of lignocellulose, so that great loss is caused.
Comparative example 2:
the green high-efficiency biomass pretreatment method comprises the following steps:
1) And (3) steam explosion treatment: soaking 4-6 mesh biomass chips in water for 24h, and treating in a steam explosion machine with explosion pressure of 1.6MPa and pressure maintaining time of 180s. Collecting residues after blasting;
2) Washing: and (3) performing solid-liquid separation on the blasting residue by adopting vacuum filtration, washing the solid residue with an ethanol water solution (v: v = 1).
In the solid residue obtained after pretreatment, the residue yield is 90.00 percent, the cellulose content is 47.19 percent, the removal rates of hemicellulose and lignin are respectively 21.82 percent and 4.96 percent, and the cellulose retention rate is 86.03 percent;
the steam explosion treatment can only effectively destroy the fiber structure, and the high-efficiency separation of lignocellulose cannot be realized. In the process, due to the high-temperature and high-pressure action of steam explosion, hemicellulose is hydrolyzed, the compact structure of lignocellulose is damaged, and the lignocellulose components need to be further treated to be efficiently separated.
Comparative example 3:
the green high-efficiency biomass pretreatment method comprises the following steps:
1) And (3) steam explosion treatment: soaking 4-6 mesh biomass chips in water for 24h, and treating in a steam explosion machine with explosion pressure of 1.8MPa and pressure maintaining time of 180s. Collecting residues after blasting, and airing in a natural environment;
2) Preparing a eutectic solvent: choline chloride was reacted with formic acid at 80 ℃ for 2h until a clear homogeneous solution was formed.
3) Pretreatment of eutectic solvent: adding a eutectic solvent into the dried biomass residue according to a solid-to-liquid ratio of 1 (g/ml) to 20, and carrying out oil bath at 120 ℃ for 4h;
4) Washing: and (3) performing solid-liquid separation on the mixture after the pretreatment reaction is finished by adopting vacuum filtration, washing the solid residue with an ethanol water solution (v: v = 1) until the solid residue is neutral, and collecting the solid residue, namely the separated and purified cellulose product.
In the solid residue obtained after pretreatment, the residue yield is 49.42 percent, the cellulose content is 79.63 percent, the removal rates of hemicellulose and lignin are respectively 86.42 percent and 85.13 percent, and the cellulose retention rate is 79.81 percent;
therefore, the excessively violent steam explosion conditions not only increase the energy consumption and the danger, but also lose part of cellulose and reduce the utilization rate of the cellulose.
Comparative example 4:
the green high-efficiency biomass pretreatment method comprises the following steps:
1) And (3) steam explosion treatment: soaking 4-6 mesh biomass chips in water for 24h, and treating in a steam explosion machine with explosion pressure of 1.6MPa and pressure maintaining time of 300s. Collecting residues after blasting, and airing in a natural environment;
2) Preparing a eutectic solvent: choline chloride was reacted with formic acid at 80 ℃ for 2h until a clear homogeneous solution was formed.
3) Pretreatment of eutectic solvent: adding a eutectic solvent into the dried biomass residue according to a solid-to-liquid ratio of 1 (g/ml) to 20, and carrying out oil bath at 120 ℃ for 4h;
4) Washing: and (3) performing solid-liquid separation on the mixture after the pretreatment reaction is finished by vacuum filtration, washing the solid residue with an ethanol water solution (v: v = 1) until the solid residue is neutral, and collecting the solid residue, namely the separated and purified cellulose product.
In the solid residue obtained after pretreatment, the residue yield is 54.61%, the cellulose content is 73.41%, the removal rates of hemicellulose and lignin are 71.85% and 75.55% respectively, and the cellulose retention rate is 81.31%;
the separation effect of the eutectic solvent can be effectively enhanced by prolonging the pressing time, but the too long pressing time can cause the amorphous area of the cellulose to be seriously damaged, so that the yield and the purity of the cellulose are reduced.
Comparative example 5:
the green high-efficiency biomass pretreatment method comprises the following steps:
1) And (3) steam explosion treatment: soaking 4-6 mesh biomass chips in water for 24h, and treating in a steam explosion machine with explosion pressure of 1.6MPa and pressure maintaining time of 180s. Collecting residues after blasting, and airing in a natural environment;
2) Preparing a eutectic solvent: choline chloride was reacted with formic acid at 80 ℃ for 2h until a clear homogeneous solution was formed.
3) Pretreatment of eutectic solvent: adding a eutectic solvent into the dried biomass residue according to a solid-to-liquid ratio of 1 (g/ml) to 20, and performing oil bath for 4 hours at 100 ℃ and 140 ℃ respectively;
4) Washing: and (3) performing solid-liquid separation on the mixture after the pretreatment reaction is finished by vacuum filtration, washing the solid residue with an ethanol water solution (v: v = 1) until the solid residue is neutral, and collecting the solid residue, namely the separated and purified cellulose product.
In the solid residue obtained after pretreatment at 100 ℃, the residue yield is 57.96 percent, the cellulose content is 70.85 percent, the removal rates of hemicellulose and lignin are 67.95 percent and 70.78 percent respectively, and the cellulose retention rate is 83.29 percent; the cellulose content of the cellulose raw material obtained after pretreatment at 140 ℃ is 85.33 percent, the product yield is 41.74 percent, the removal rates of hemicellulose and lignin are respectively 90.75 percent and 92.98 percent, and the cellulose retention rate is 72.23 percent;
therefore, the proper temperature condition can effectively exert the removing effect of the eutectic solvent, and the excessively low temperature cannot effectively remove lignin and hemicellulose, so that the content of the pretreated cellulose product is low; too high a treatment temperature will seriously affect the yield of the pretreated product, and the yield of the cellulose product is greatly reduced.
Comparative example 6:
the green high-efficiency biomass pretreatment method comprises the following steps:
1) And (3) steam explosion treatment: soaking 4-6 mesh biomass chips in water for 24h, and treating in a steam explosion machine with explosion pressure of 1.6MPa and pressure maintaining time of 180s. Collecting residues after blasting, and airing in a natural environment;
2) Preparing a eutectic solvent: choline chloride was reacted with acetic acid at 80 ℃ for 2h until a clear homogeneous solution was formed.
3) Pretreatment of eutectic solvent: adding a eutectic solvent into the dried biomass residue according to a solid-to-liquid ratio of 1 (g/ml) to 20, and performing oil bath for 4 hours at 100 ℃ and 140 ℃ respectively;
4) Washing: and (3) performing solid-liquid separation on the mixture after the pretreatment reaction is finished by vacuum filtration, washing the solid residue with an ethanol water solution (v: v = 1) until the solid residue is neutral, and collecting the solid residue, namely the separated and purified cellulose product.
In the solid residue obtained after pretreatment, the residue yield is 60.21%, the cellulose content is 62.84%, the removal rates of hemicellulose and lignin are 55.05% and 59.49% respectively, and the cellulose retention rate is 76.74%;
when choline chloride and acetic acid are used as eutectic solvents, the effect of removing hemicellulose and lignin is poor.
The above-described embodiments are merely illustrative of several embodiments of the invention and are not to be construed as limiting. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
The technical features related to the above embodiments can be combined arbitrarily, and this specification only selects specific combinations to describe, and does not describe all possible combinations of the technical features in the above embodiments, which is intended to explain the principle and practical application of the present invention more concisely. However, as long as there is no contradiction between combinations of these technical features, the scope of the present specification should be considered as being described.
Claims (10)
1. A green and efficient biomass pretreatment method is characterized by comprising the following steps: soaking the biomass fragments in water to obtain wet biomass fragments, performing steam explosion treatment on the wet biomass fragments to obtain biomass residues, adding the biomass residues into a eutectic solvent, reacting, and collecting solid residues; the eutectic solvent is a mixed solvent consisting of choline chloride and formic acid.
2. The green and efficient biomass pretreatment method according to claim 1, wherein: the particle size of the biomass crumbs is 4-10 meshes.
3. The green and efficient biomass pretreatment method according to claim 1, characterized by comprising the following steps: the time for soaking the biomass scraps in water is 12-24h.
4. The green and efficient biomass pretreatment method according to claim 1, characterized by comprising the following steps: the pressure of the steam explosion treatment is 1.6-1.8MPa, and the pressure maintaining time is 180-240s.
5. The green and efficient biomass pretreatment method according to claim 1 or 4, characterized in that: and (3) carrying out steam explosion treatment on the wet biomass chips to obtain a product, and airing the product in the natural environment to obtain biomass residues.
6. The green and efficient biomass pretreatment method according to claim 1, characterized by comprising the following steps: in the eutectic solvent, the molar ratio of choline chloride to formic acid is 1.8-2.5.
7. The green and efficient biomass pretreatment method according to claim 1 or 6, wherein: the method for obtaining the eutectic solvent comprises the following steps: choline chloride is reacted with formic acid at 75-85 ℃ for 1.5-2h until a clear homogeneous solution is formed.
8. The green and efficient biomass pretreatment method according to claim 1 or 6, characterized in that: the solid-liquid mass volume ratio of the biomass residue to the eutectic solvent is 1g.
9. The green and efficient biomass pretreatment method according to claim 1 or 6, characterized in that: the reaction temperature is 100-120 ℃, and the reaction time is 2-4h.
10. The green and efficient biomass pretreatment method according to claim 1 or 6, wherein: after the reaction is finished, performing vacuum filtration to separate the solid from the liquid of the mixture obtained by the reaction, washing the obtained solid phase to be neutral by adopting ethanol water solution, and collecting solid residues; namely the separated and purified cellulose product.
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