CN114920952A - Lignin nanowire and preparation method and application thereof - Google Patents
Lignin nanowire and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a lignin nanowire and a preparation method and application thereof, wherein the preparation method comprises the following steps: adding lignin into water, then adding a cosolvent, finally adding electrolyte with strong complexing ability, uniformly mixing, and dialyzing to obtain a lignin nanowire; or mixing water and the cosolvent to form a cosolvent aqueous solution, then adding lignin, adding electrolyte with strong complexing ability, uniformly mixing, and dialyzing to obtain the lignin nanowire. The invention regulates the appearance of the lignin nanowires by regulating the cosolvent, the types and the content of the electrolyte and dialysis parameters, can prepare the lignin nanowires in a large scale and store the lignin nanowires stably, and provides a new way for high-added-value utilization of lignin products.
Description
Technical Field
The invention relates to the technical field of lignin, in particular to a lignin nanowire and a preparation method and application thereof.
Background
Lignin is the only renewable natural aromatic polymer in the nature, the source of the lignin is wide, the lignin accounts for 15-30% of various agriculture and forestry biomass resources, in addition, the pulping and papermaking industry can also generate a large amount of lignin wastes, and most of the lignin wastes are consumed as low-value fuels or fillers, so that the resource waste is caused. The lignin has the functions of antibiosis, antioxidation, ultraviolet absorption and the like, contains a large number of phenolic hydroxyl functional groups, and can be assembled into a stable nano structure by means of pi-pi interaction and hydrogen bond interaction of benzene rings of the lignin. However, most of the existing nano lignin is in the form of nano particles, and the research reports of lignin nanowires are few. The natural polymer lignin nanowire is a functional fiber with the advantages of good mechanical property, good thermal stability, large length-diameter ratio, antibiosis, ultraviolet absorption and the like, and can be used for preparing high-performance and functionalized composite materials; in addition, the large specific surface area and the good surface property of lignin enable the lignin to be used as a treatment material for adsorbing heavy metals and organic pollutants; furthermore, the lignin nano-fiber is activated and carbonized under proper conditions to obtain an activated carbon fiber material used as a high-performance catalyst carrier and the like. The nano-morphology of the lignin plays a critical role in the functions of the lignin, so that the development of the preparation method of the lignin nanowire with simple process and low cost is of great significance.
Disclosure of Invention
In order to solve the above defects in the prior art, the present invention aims to provide a lignin nanowire, a preparation method and an application thereof.
The technical scheme for solving the technical problems is as follows: the preparation method of the lignin nanowires comprises the following steps:
adding lignin into water, then adding a cosolvent, finally adding electrolyte with strong complexing power, uniformly mixing, and dialyzing to obtain a lignin nanowire; or
Mixing water and a cosolvent to form a cosolvent aqueous solution, then adding lignin, adding electrolyte with strong complexing ability, uniformly mixing, and dialyzing to obtain a lignin nanowire;
wherein, the electrolyte with strong complexing ability is formed by the following anions and cations:
the cation being Fe 3+ Or Al 3+ ；
The anion being Cl - 、Br - 、I - 、NO 3 - 、SO 4 2- 、HSO 4 - 、PO 4 3- 、HPO 4 2- And HPO 3 2- Any one of them.
The invention has the beneficial effects that: the lignin is added into water, and then the cosolvent is added, or the water and the cosolvent are mixed to form a cosolvent aqueous solution, the dissolution speed of the lignin in the water can be accelerated in such a reaction system, so that the lignin is uniformly dispersed in the water, and then the electrolyte solution with strong complexing ability is added, the electrolyte with strong complexing ability can be complexed with groups on the lignin, and the lignin can be effectively promoted to form the nano-wire by self-assembly in the dialysis process. The size of the lignin nanowires can be regulated and controlled by factors such as electrolyte, cosolvent and dialysis. The electrolyte species plays a very critical role in the formation of lignin nanowires when strong electrolytes such as those containing Fe as described above are added 3+ 、Al 3+ The cationic substance can effectively promote the formation of lignin nanowires, and the added electrolyte does not have strong complexing ability, for example, the electrolyte with weak complexing ability such as Fe-containing electrolyte is added 2+ The cationic species do not form lignin nanowires. The preparation method is simple in preparation process, and can be prepared in batches and stored stably.
On the basis of the technical scheme, the invention can be further improved as follows:
further, lignin is a pure lignin reagent such as dealkalized lignin, sodium lignosulfonate and the like.
Further, the mass concentration of the lignin in the reaction system is 1-20%.
The beneficial effect of adopting the further technical scheme is as follows: adding lignin into water, then adding a cosolvent or mixing water and the cosolvent to form a cosolvent aqueous solution, then adding the lignin, and finally enabling the mass concentration of the lignin to reach 1-20%, so that the lignin can be quickly dissolved under the cosolvent condition and is combined with electrolyte with strong complexing ability to form a relatively pure lignin nanowire, and if the concentration is too high, the dissolution and the combination with the electrolyte can be influenced, and the formation rate and the purity of the lignin nanowire are finally influenced.
Furthermore, the cosolvent is alcohols, aprotic solvents, protic solvents, deep eutectic solvents or ionic liquids.
Further, the alcohol is methanol, ethanol or ethylene glycol; the aprotic solvent is tetrahydrofuran or dioxane; the protic solvent is N, N-dimethylformamide; the deep eutectic solvent is choline chloride/citric acid, choline chloride/acetic acid; the ionic liquid is [ Amim ] Cl, [ Bmim ] Cl and DMSO/TBAH.
The beneficial effects of adopting the further technical scheme are as follows: the cosolvent is added to accelerate the dissolution speed of lignin in water, and the formation of lignin nanowires can be effectively promoted after the cosolvent is matched with electrolyte with strong complexing ability.
The above-mentioned partial cosolvents are only listed, for example, the alcohol substance as the cosolvent can be not only methanol, ethanol or ethylene glycol as the cosolvent in the technical scheme, but also other alcohol substances as long as the alcohol substance can play the same solubilizing role, which is not listed here.
Further, after adding the cosolvent, the volume concentration of the cosolvent in the reaction system is 10-90%; or the volume concentration of the cosolvent in the cosolvent water solution is 10-90%. The effect of the cosolvent not only influences the dissolution rate of lignin in water, but also influences the yield of the formed lignin nanowires due to the content of the added cosolvent.
Further, adding electrolyte solution with strong complexing ability to ensure that the concentration of the electrolyte with strong complexing ability in a reaction system is 0.01-0.1 mol/L; the preferred concentration is 0.05 mol/L.
The beneficial effects of adopting the further technical scheme are as follows: only when the concentration of the added electrolyte with strong complexing ability in the reaction system is 0.01-0.1mol/L, the electrolyte can be effectively combined with lignin to form the lignin nanowire, if the concentration is higher than the concentration, the dosage of the electrolyte is too much to form good combination with the lignin, the purity and the yield of the lignin nanowire can be influenced, and if the concentration is lower than the concentration, the yield of the lignin nanowire can be influenced.
Further, the dialysis temperature is 20-60 deg.C, and the dialysis time is 2-4 days; preferably, the dialysis temperature is 30 ℃ and the dialysis time is 2 days.
The beneficial effects of adopting the further technical scheme are as follows: during the dialysis process, lignin can be self-assembled to form lignin nanowires, and the length of the nanowires can be influenced by the dialysis temperature, so that the dialysis temperature is increased and the length is shortened.
The prepared lignin nanowire can be used for preparing adsorbing materials, shape memory materials, energy storage materials, slow release materials, ultraviolet protection materials, antibacterial materials, antioxidant materials and the like.
The invention has the following beneficial effects:
the invention provides a preparation method of a lignin nanowire with high efficiency and low cost, the morphology of the lignin nanowire is regulated and controlled by regulating and controlling the cosolvent, the types and the content of electrolytes and dialysis parameters, the lignin nanowire can be prepared in a large scale and stably stored, and a new way is provided for high-added-value utilization of lignin products.
Drawings
Fig. 1 is an SEM topography of the lignin nanowires prepared in example 1.
Fig. 2 is an SEM topography of the lignin nanowires prepared in example 2.
Detailed Description
The following examples are given for the purpose of illustration only and are not intended to limit the scope of the invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1:
a lignin nanowire is prepared by the following steps:
adding dealkalized lignin into water, then adding a cosolvent Tetrahydrofuran (THF), wherein the mass concentration of the lignin in the system is 1%, the volume concentration of the THF is 20%, then adding ferric chloride to enable the concentration of ferric chloride to be 0.05mol/L, and dialyzing for 48h at 30 ℃ after fully dissolving the dealkalized lignin and the ferric chloride to obtain the lignin nanowire.
Example 2:
a lignin nanowire is prepared by the following steps:
adding dealkalized lignin into water, then adding a cosolvent Tetrahydrofuran (THF), wherein the mass concentration of the lignin in the system is 1%, the volume concentration of N, N-dimethylformamide is 20%, then adding ferric chloride to enable the concentration of ferric chloride to be 0.1mol/L, and dialyzing for 48h at 30 ℃ after fully dissolving the dealkalized lignin and the ferric chloride to obtain the lignin nanowire.
Example 3:
a lignin nanowire is prepared by the following steps:
adding dealkalized lignin into water, then adding a cosolvent Tetrahydrofuran (THF), wherein the mass concentration of the lignin in the system is 1%, the volume concentration of N, N-dimethylformamide is 20%, then adding ferric chloride to enable the concentration of ferric chloride to be 0.2mol/L, and dialyzing for 48h at 30 ℃ after fully dissolving the dealkalized lignin and the ferric chloride to obtain the lignin nanowire.
Example 4:
a lignin nanowire is prepared by the following steps:
adding dealkalized lignin into water, then adding a cosolvent Tetrahydrofuran (THF), wherein the mass concentration of the lignin in the system is 5%, the volume concentration of the THF is 40%, then adding ferric chloride to ensure that the concentration of ferric chloride is 0.05mol/L, and dialyzing for 4 days at 20 ℃ after fully dissolving the dealkalized lignin and the ferric chloride to obtain the lignin nanowire.
Example 5:
a lignin nanowire is prepared by the following steps:
adding dealkalized lignin into water, then adding a cosolvent Tetrahydrofuran (THF), wherein the mass concentration of the lignin in the system is 10%, the volume concentration of the THF is 50%, then adding ferric chloride to ensure that the concentration of ferric chloride is 0.06mol/L, and dialyzing at 40 ℃ for 2 days after fully dissolving the dealkalized lignin and the ferric chloride to obtain the lignin nanowire.
Example 6:
a lignin nanowire is prepared by the following steps:
adding dealkalized lignin into water, then adding a cosolvent Tetrahydrofuran (THF), wherein the mass concentration of the lignin in the system is 20%, the volume concentration of the THF is 80%, then adding ferric chloride to enable the concentration of ferric chloride to be 0.1mol/L, and dialyzing for 2 days at 60 ℃ after fully dissolving the dealkalized lignin and the ferric chloride to obtain the lignin nanowire.
Example 7:
a lignin nanowire is prepared by the following steps:
adding dealkalized lignin into water, then adding a cosolvent N, N-Dimethylformamide (DMF), wherein the mass concentration of the lignin in the system is 1%, the volume concentration of the N, N-dimethylformamide is 20%, then adding ferric chloride to enable the concentration of the ferric chloride to be 0.2mol/L, and dialyzing for 48h at 30 ℃ after fully dissolving the dealkalized lignin and the ferric chloride to obtain the lignin nanowire.
Example 8:
a lignin nanowire is prepared by the following steps:
adding dealkalized lignin into water, then adding a cosolvent N, N-Dimethylformamide (DMF), wherein the mass concentration of the lignin in the system is 1%, the volume concentration of the N, N-dimethylformamide is 20%, then adding ferric chloride to enable the concentration of the ferric chloride to be 0.1mol/L, and dialyzing for 48h at 30 ℃ after fully dissolving the dealkalized lignin and the ferric chloride to obtain the lignin nanowire.
Example 9:
a lignin nanowire is prepared by the following steps:
adding dealkalized lignin into water, then adding cosolvent ethanol, wherein the mass concentration of the lignin in the system is 1%, the volume concentration of the ethanol is 20%, then adding ferric chloride to enable the concentration of the ferric chloride to be 0.1mol/L, and dialyzing for 48h at 30 ℃ after fully dissolving the dealkalized lignin and the ferric chloride to obtain the lignin nanowire.
Example 10:
a lignin nanowire is prepared by the following steps:
adding dealkalized lignin into water, then adding cosolvent ethanol, wherein the mass concentration of the lignin in the system is 1%, the volume concentration of the ethanol is 20%, then adding ferric chloride to enable the concentration of the ferric chloride to be 0.2mol/L, and dialyzing for 48h at 30 ℃ after fully dissolving the dealkalized lignin and the ferric chloride to obtain the lignin nanowire.
Example 11:
a lignin nanowire is prepared by the following steps:
adding dealkalized lignin into water, then adding a cosolvent tetrahydrofuran, wherein the mass concentration of the lignin in the system is 1%, the volume concentration of the tetrahydrofuran is 20%, then adding aluminum chloride to ensure that the concentration of the aluminum chloride is 0.05mol/L, and dialyzing for 48h at 30 ℃ after fully dissolving the dealkalized lignin and the aluminum chloride to prepare the lignin nanowire.
Example 12:
a lignin nanowire is prepared by the following steps:
adding dealkalized lignin into water, then adding a cosolvent tetrahydrofuran, wherein the mass concentration of the lignin in the system is 5%, the volume concentration of the tetrahydrofuran is 40%, then adding aluminum chloride to ensure that the concentration of the aluminum chloride is 0.01mol/L, and dialyzing at 20 ℃ for 4 days after the dealkalized lignin and the aluminum chloride are fully dissolved to prepare the lignin nanowire.
Example 13:
a lignin nanowire is prepared by the following steps:
adding dealkalized lignin into water, then adding a cosolvent tetrahydrofuran, wherein the mass concentration of the lignin in the system is 10%, the volume concentration of the tetrahydrofuran is 50%, then adding aluminum chloride to ensure that the concentration of the aluminum chloride is 0.06mol/L, and dialyzing at 40 ℃ for 2 days after the dealkalized lignin and the aluminum chloride are fully dissolved to prepare the lignin nanowire.
Example 14:
a lignin nanowire is prepared by the following steps:
adding dealkalized lignin into water, then adding a cosolvent tetrahydrofuran, wherein the mass concentration of the lignin in the system is 20%, the volume concentration of the tetrahydrofuran is 80%, then adding aluminum chloride to ensure that the concentration of the aluminum chloride is 0.1mol/L, and dialyzing at 60 ℃ for 1 day after fully dissolving the dealkalized lignin and the aluminum chloride to prepare the lignin nanowire.
Example 15:
a lignin nanowire is prepared by the following steps:
adding dealkalized lignin into water, then adding a cosolvent N, N-dimethylformamide, wherein the mass concentration of the lignin in a system is 1%, the volume concentration of the N, N-dimethylformamide is 20%, then adding aluminum chloride to ensure that the concentration of the aluminum chloride is 0.05mol/L, and dialyzing for 48h at 30 ℃ after the dealkalized lignin and the aluminum chloride are fully dissolved to prepare the lignin nanowire.
Example 16:
a lignin nanowire is prepared by the following steps:
adding dealkalized lignin into water, then adding a cosolvent N, N-dimethylformamide, wherein the mass concentration of the lignin in a system is 5%, the volume concentration of the N, N-dimethylformamide is 40%, then adding aluminum chloride to ensure that the concentration of the aluminum chloride is 0.01mol/L, and dialyzing at 20 ℃ for 4 days after the dealkalized lignin and the aluminum chloride are fully dissolved to prepare the lignin nanowire.
Example 17:
a lignin nanowire is prepared by the following steps:
adding dealkalized lignin into water, then adding a cosolvent N, N-dimethylformamide, wherein the mass concentration of the lignin in the system is 10%, the volume concentration of the N, N-dimethylformamide is 50%, then adding aluminum chloride to enable the concentration of the aluminum chloride to be 0.06mol/L, and dialyzing for 2 days at 40 ℃ after the dealkalized lignin and the aluminum chloride are fully dissolved to obtain the lignin nanowire.
Example 18:
a lignin nanowire is prepared by the following steps:
adding dealkalized lignin into water, then adding a cosolvent N, N-dimethylformamide, wherein the mass concentration of the lignin in the system is 20%, the volume concentration of the N, N-dimethylformamide is 80%, then adding aluminum chloride to enable the concentration of the aluminum chloride to be 0.1mol/L, and dialyzing at 60 ℃ for 2 days after the dealkalized lignin and the aluminum chloride are fully dissolved to obtain the lignin nanowire.
During the preparation process, the lignin nano wire can be prepared by adding the lignin into water, then adding the cosolvent, and finally adding the electrolyte for dissolving and dialyzing, or by mixing the water and the cosolvent to form a cosolvent aqueous solution, then adding the lignin into the cosolvent aqueous solution, then adding the electrolyte for dissolving and dialyzing.
The above examples 1 to 18 can all obtain good lignin nanowire morphologies, and the result graphs of some examples are given, taking example 1 and example 2 as examples, and the SEM morphology graphs are specifically shown in fig. 1 and fig. 2.
As can be seen from FIGS. 1 and 2, the diameter of the obtained lignin nanowire is less than 100nm, the length is greater than 100 μm, the diameter of the nanotube is 100-600nm, and the length is greater than 100 nm.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The preparation method of the lignin nanowires is characterized by comprising the following steps:
adding lignin into water, then adding a cosolvent, finally adding electrolyte with strong complexing ability, uniformly mixing, and dialyzing to obtain a lignin nanowire; or
Mixing water and a cosolvent to form a cosolvent aqueous solution, then adding lignin, adding electrolyte with strong complexing ability, uniformly mixing, and dialyzing to obtain a lignin nanowire;
wherein, the electrolyte with strong complexing ability is formed by the following anions and cations:
the cation being Fe 3+ Or Al 3+ ；
The anion being Cl - 、Br - 、I - 、NO 3 - 、SO 4 2- 、HSO 4 - 、PO 4 3- 、HPO 4 2- And HPO 3 2- Any one of them.
2. The method for preparing lignin nanowires according to claim 1, wherein the mass concentration of lignin in the co-solvent aqueous solution is 1-20%.
3. The method for preparing lignin nanowires according to claim 1, wherein the cosolvent is added to the reaction system so that the volume concentration of the cosolvent in the reaction system is 10-90%.
4. The method for preparing the lignin nanowires according to claim 1 or 3, wherein the cosolvent is an alcohol, an aprotic solvent, a protic solvent, a deep eutectic solvent or an ionic liquid.
5. The method for preparing lignin nanowires according to claim 4, wherein the alcohol is methanol, ethanol or ethylene glycol; the aprotic solvent is tetrahydrofuran or dioxane; the protic solvent is N, N-dimethylformamide.
6. The preparation method of the lignin nanowires according to claim 4, wherein the deep eutectic solvent is choline chloride/citric acid or choline chloride/acetic acid; the ionic liquid is [ Amim ] Cl, [ Bmim ] Cl or DMSO/TBAH.
7. The method for preparing lignin nanowires according to claim 1, wherein the concentration of the electrolyte with strong complexing power in the reaction system is 0.01-0.1mol/L after the electrolyte with strong complexing power is added.
8. The method for preparing lignin nanowires according to claim 1, wherein the dialysis temperature is 20-60 ℃ and the dialysis time is 2-4 days.
9. Lignin nanowires produced by the production method according to any one of claims 1 to 8.
10. The application of the lignin nanowires of claim 9 in preparing adsorption materials, shape memory materials, energy storage materials, slow release materials, ultraviolet protection materials, antibacterial materials and antioxidant materials.
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| CN112080022A (en) * | 2020-09-25 | 2020-12-15 | 齐鲁工业大学 | Preparation method of lignin nanoparticles, product and application thereof |
| CN112265981A (en) * | 2020-10-23 | 2021-01-26 | 中南林业科技大学 | Method for preparing carbon nano tube by lignin nano micelle |
| CN113527711A (en) * | 2021-08-27 | 2021-10-22 | 西南交通大学 | Method for preparing lignin nanotubes by using agriculture and forestry biomass raw materials |
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| CN112080022A (en) * | 2020-09-25 | 2020-12-15 | 齐鲁工业大学 | Preparation method of lignin nanoparticles, product and application thereof |
| CN112265981A (en) * | 2020-10-23 | 2021-01-26 | 中南林业科技大学 | Method for preparing carbon nano tube by lignin nano micelle |
| CN113527711A (en) * | 2021-08-27 | 2021-10-22 | 西南交通大学 | Method for preparing lignin nanotubes by using agriculture and forestry biomass raw materials |
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