CN114920952B - Lignin nanowire and preparation method and application thereof - Google Patents

Lignin nanowire and preparation method and application thereof Download PDF

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CN114920952B
CN114920952B CN202210637059.6A CN202210637059A CN114920952B CN 114920952 B CN114920952 B CN 114920952B CN 202210637059 A CN202210637059 A CN 202210637059A CN 114920952 B CN114920952 B CN 114920952B
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lignin
cosolvent
nanowire
electrolyte
concentration
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CN114920952A (en
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姜曼
胡翔洲
徐汪杰
王峰
陆远
潘宇
周昱帆
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Southwest Jiaotong University
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2397/00—Characterised by the use of lignin-containing materials
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    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
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    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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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 cosolvent, finally adding electrolyte with strong complexing ability, uniformly mixing, and dialyzing to obtain lignin nanowire; or mixing water and cosolvent to form cosolvent water solution, adding lignin, adding strong complexing electrolyte, mixing, and dialyzing to obtain lignin nanowire. The morphology of the lignin nanowire is regulated and controlled by regulating and controlling the cosolvent, the electrolyte type and the electrolyte content and the dialysis parameter, and the lignin nanowire can be prepared in a large scale and stably stored, so that a new way is provided for the high added value utilization of lignin products.

Description

Lignin nanowire and preparation method and application thereof
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 nature, and has wide sources, and accounts for 15-30% of various agriculture and forestry biomass resources, and besides, the pulping and papermaking industry can generate a large amount of lignin wastes, and most of the lignin wastes are consumed as low-value fuel or filler, so that the resource waste is caused. 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. However, the morphology of the nano lignin is mostly nano particles at present, and the research report of lignin nanowires is less. 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 functional composite materials; in addition, the lignin can be used as a treatment material for adsorbing heavy metals and organic pollutants due to the large specific surface area and good surface property of the lignin; furthermore, the lignin nanofiber is activated and carbonized under proper conditions to obtain the active carbon fiber material which is used as a high-performance catalyst carrier and the like. The nano morphology of lignin plays a key role in the function of the lignin, so that the development of a preparation method of lignin nanowires with simple process and low cost has important significance.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide a lignin nanowire, a preparation method and application thereof, wherein the lignin nanowire is simple in preparation method and can be prepared in batches and stably stored.
The technical scheme for solving the technical problems is as follows: the preparation method of the lignin nanowire comprises the following steps:
adding lignin into water, then adding cosolvent, finally adding electrolyte with strong complexing ability, uniformly mixing, and dialyzing to obtain lignin nanowire; or (b)
Mixing water and a cosolvent to form a cosolvent aqueous solution, then adding lignin, adding an electrolyte with strong complexing ability, uniformly mixing, and dialyzing to obtain lignin nanowires;
among them, the strong complexing ability electrolyte is a substance formed by the following anions and cations:
the cation is 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 the following.
The beneficial effects of the invention are as follows: adding lignin into water, and adding cosolvent, or mixing water and cosolvent to form cosolvent water solution, wherein lignin isIn the reaction system of the sample, the dissolution speed of lignin in water can be increased, so that lignin is uniformly dispersed in water, then, electrolyte solution with strong complexing ability is added, the electrolyte solution with strong complexing ability can be complexed with groups on lignin, and the lignin self-assembly can be effectively promoted to form nanowires in the dialysis process. The size of lignin nanowires can be regulated by factors such as electrolytes, cosolvents, dialysis, and the like. The electrolyte species play a very critical role in lignin nanowire formation when strong electrolytes such as those described above are added 3+ 、Al 3+ The cationic substance can effectively promote the formation of lignin nanowire, while the added electrolyte does not have strong complexing ability, such as the electrolyte with weak complexing ability, such as Fe 2+ The cationic species does not form lignin nanowires. The preparation method is simple in preparation process, and can be used for batch preparation and stable storage.
Based on the technical scheme, the invention can also be improved as follows:
further, lignin is a pure lignin reagent such as dealkalized lignin, sodium lignin sulfonate and the like.
Further, the mass concentration of lignin in the reaction system is 1-20%.
The beneficial effects of adopting the further technical scheme are as follows: adding lignin into water, adding cosolvent or mixing water and cosolvent to form cosolvent water solution, adding lignin to make the mass concentration of lignin reach 1-20%, so that lignin can be quickly dissolved under the cosolvent condition and combined with electrolyte with strong complexing ability to form relatively pure lignin nanowire, if the concentration is too high, the dissolution and the combination with electrolyte can be influenced, and the formation rate and purity of lignin nanowire can be finally influenced.
Further, the cosolvent is an alcohol, an aprotic solvent, a protic solvent, a deep eutectic solvent, or an ionic liquid.
Further, the alcohol is methanol, ethanol or ethylene glycol; the aprotic solvent is tetrahydrofuran or dioxane; the proton solvent is N, N-dimethylformamide; the deep eutectic solvent is choline chloride/citric acid, choline chloride/acetic acid; the ionic liquid is [ ami ] Cl, [ Bmim ] Cl, DMSO/TBAH.
The beneficial effects of adopting the further technical scheme are as follows: the cosolvent is added to accelerate the dissolution rate of lignin in water, and the cosolvent can effectively promote the formation of lignin nanowires after being matched with electrolyte with strong complexing capacity.
The above-mentioned only partial cosolvent, for example, the alcohol as the cosolvent may be not only methanol, ethanol or ethylene glycol as the cosolvent in the technical solution, but also other alcohols as long as the same cosolvent can be achieved, and this is not necessarily exemplified herein.
Further, after the cosolvent is added, 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 co-solvent not only affects the dissolution rate of lignin in water, but the amount of co-solvent added also affects the yield of lignin nanowires formed.
Further, the concentration of the strong complexing electrolyte in the reaction system is 0.01-0.1mol/L after the strong complexing electrolyte solution is added; the concentration is preferably 0.05mol/L.
The beneficial effects of adopting the further technical scheme are as follows: the electrolyte with strong complexing ability can be effectively combined with lignin only when the concentration of the electrolyte in a reaction system is 0.01-0.1mol/L, so that lignin nanowires are formed, if the concentration is higher than the concentration, the electrolyte is excessively used and cannot be well combined with lignin, the purity and the yield of the lignin nanowires can be influenced, and if the concentration is lower than the concentration, the yield of the lignin nanowires can be influenced.
Further, the dialysis temperature is 20-60 ℃, 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: lignin can self-assemble to form lignin nanowires in the dialysis process, and the dialysis temperature can influence the length of the nanowires, so that the dialysis temperature is increased and the length is shortened.
The lignin nanowire prepared by the method can be used for preparing adsorption 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 lignin nanowires with high efficiency and low cost, the morphology of the lignin nanowires is regulated and controlled by regulating and controlling the types and the content of cosolvent and electrolyte and dialysis parameters, and the lignin nanowires can be prepared in a large scale and stably stored, so that a new way is provided for the high added value utilization of lignin products.
Drawings
Fig. 1 is an SEM morphology of the lignin nanowires produced in example 1.
Fig. 2 is an SEM morphology of the lignin nanowires produced in example 2.
Detailed Description
The examples given below are only intended to illustrate the invention and are not intended to limit the scope thereof. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1:
a lignin nanowire, the method of making comprising the steps of:
adding dealkalized lignin into water, then adding cosolvent Tetrahydrofuran (THF), wherein the mass concentration of lignin in the system is 1%, the volume concentration of tetrahydrofuran is 20%, then adding ferric chloride to enable the concentration of ferric chloride to be 0.05mol/L, and dialyzing at 30 ℃ for 48 hours after the dealkalized lignin and the ferric chloride are fully dissolved, so as to obtain the lignin nanowire.
Example 2:
a lignin nanowire, the method of making comprising the steps of:
adding dealkalized lignin into water, then adding cosolvent Tetrahydrofuran (THF), wherein the mass concentration of 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 at 30 ℃ for 48 hours after the dealkalized lignin and the ferric chloride are fully dissolved, so as to obtain the lignin nanowire.
Example 3:
a lignin nanowire, the method of making comprising the steps of:
adding dealkalized lignin into water, then adding cosolvent Tetrahydrofuran (THF), wherein the mass concentration of 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 at 30 ℃ for 48 hours after the dealkalized lignin and the ferric chloride are fully dissolved, so as to obtain the lignin nanowire.
Example 4:
a lignin nanowire, the method of making comprising the steps of:
adding dealkalized lignin into water, then adding cosolvent Tetrahydrofuran (THF), wherein the mass concentration of lignin in the system is 5%, the volume concentration of tetrahydrofuran is 40%, then adding ferric chloride to enable the concentration of ferric chloride to be 0.05mol/L, and dialyzing for 4 days at 20 ℃ after the dealkalized lignin and the ferric chloride are fully dissolved, so as to obtain the lignin nanowire.
Example 5:
a lignin nanowire, the method of making comprising the steps of:
adding dealkalized lignin into water, then adding cosolvent Tetrahydrofuran (THF), wherein the mass concentration of lignin in the system is 10%, the volume concentration of tetrahydrofuran is 50%, then adding ferric chloride to make the concentration of ferric chloride be 0.06mol/L, and dialyzing at 40 ℃ for 2 days after dealkalized lignin and ferric chloride are fully dissolved, so as to obtain lignin nanowires.
Example 6:
a lignin nanowire, the method of making comprising the steps of:
adding dealkalized lignin into water, then adding cosolvent Tetrahydrofuran (THF), wherein the mass concentration of lignin in the system is 20%, the volume concentration of tetrahydrofuran is 80%, then adding ferric chloride to make the concentration of ferric chloride be 0.1mol/L, and dialyzing at 60 ℃ for 2 days after the dealkalized lignin and ferric chloride are fully dissolved, so as to obtain the lignin nanowire.
Example 7:
a lignin nanowire, the method of making comprising the steps of:
adding dealkalized lignin into water, then adding cosolvent N, N-Dimethylformamide (DMF), wherein the mass concentration of 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 at 30 ℃ for 48 hours after the dealkalized lignin and the ferric chloride are fully dissolved, so as to obtain the lignin nanowire.
Example 8:
a lignin nanowire, the method of making comprising the steps of:
adding dealkalized lignin into water, then adding cosolvent N, N-Dimethylformamide (DMF), wherein the mass concentration of 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 at 30 ℃ for 48 hours after the dealkalized lignin and the ferric chloride are fully dissolved, so as to obtain the lignin nanowire.
Example 9:
a lignin nanowire, the method of making comprising the steps of:
adding dealkalized lignin into water, adding cosolvent ethanol, wherein the mass concentration of lignin in the system is 1%, the volume concentration of ethanol is 20%, adding ferric chloride to make the concentration of ferric chloride be 0.1mol/L, and dialyzing at 30deg.C for 48h after dealkalized lignin and ferric chloride are fully dissolved to obtain lignin nanowire.
Example 10:
a lignin nanowire, the method of making comprising the steps of:
adding dealkalized lignin into water, adding cosolvent ethanol, wherein the mass concentration of lignin in the system is 1%, the volume concentration of ethanol is 20%, adding ferric chloride to make the concentration of ferric chloride be 0.2mol/L, and dialyzing at 30deg.C for 48h after dealkalized lignin and ferric chloride are fully dissolved to obtain lignin nanowire.
Example 11:
a lignin nanowire, the method of making comprising the steps of:
adding dealkalized lignin into water, then adding cosolvent tetrahydrofuran, wherein the mass concentration of lignin in the system is 1%, the volume concentration of tetrahydrofuran is 20%, then adding aluminum chloride to enable the concentration of aluminum chloride to be 0.05mol/L, and dialyzing at 30 ℃ for 48 hours after the dealkalized lignin and the aluminum chloride are fully dissolved, so as to obtain the lignin nanowire.
Example 12:
a lignin nanowire, the method of making comprising the steps of:
adding dealkalized lignin into water, adding cosolvent tetrahydrofuran, wherein the mass concentration of lignin in the system is 5%, the volume concentration of tetrahydrofuran is 40%, adding aluminum chloride to make the concentration of aluminum chloride be 0.01mol/L, and dialyzing at 20 ℃ for 4 days after dealkalized lignin and aluminum chloride are fully dissolved to obtain lignin nanowires.
Example 13:
a lignin nanowire, the method of making comprising the steps of:
adding dealkalized lignin into water, then adding cosolvent tetrahydrofuran, wherein the mass concentration of lignin in the system is 10%, the volume concentration of tetrahydrofuran is 50%, then adding aluminum chloride to enable the concentration of aluminum chloride to be 0.06mol/L, and dialyzing at 40 ℃ for 2 days after the dealkalized lignin and the aluminum chloride are fully dissolved, so as to obtain the lignin nanowire.
Example 14:
a lignin nanowire, the method of making comprising the steps of:
adding dealkalized lignin into water, then adding cosolvent tetrahydrofuran, wherein the mass concentration of lignin in the system is 20%, the volume concentration of tetrahydrofuran is 80%, then adding aluminum chloride to enable the concentration of aluminum chloride to be 0.1mol/L, and dialyzing at 60 ℃ for 1 day after the dealkalized lignin and the aluminum chloride are fully dissolved, so as to obtain the lignin nanowire.
Example 15:
a lignin nanowire, the method of making comprising the steps of:
adding dealkalized lignin into water, adding cosolvent N, N-dimethylformamide, wherein the mass concentration of lignin in the system is 1%, the volume concentration of N, N-dimethylformamide is 20%, adding aluminum chloride to enable the concentration of aluminum chloride to be 0.05mol/L, and dialyzing at 30 ℃ for 48 hours after the dealkalized lignin and the aluminum chloride are fully dissolved to obtain the lignin nanowire.
Example 16:
a lignin nanowire, the method of making comprising the steps of:
adding dealkalized lignin into water, adding cosolvent N, N-dimethylformamide, wherein the mass concentration of lignin in the system is 5%, the volume concentration of N, N-dimethylformamide is 40%, adding aluminum chloride to enable the concentration of aluminum chloride to be 0.01mol/L, and dialyzing at 20 ℃ for 4 days after the dealkalized lignin and the aluminum chloride are fully dissolved to obtain lignin nanowires.
Example 17:
a lignin nanowire, the method of making comprising the steps of:
adding dealkalized lignin into water, adding cosolvent N, N-dimethylformamide, wherein the mass concentration of lignin in the system is 10%, the volume concentration of N, N-dimethylformamide is 50%, adding aluminum chloride to enable the concentration of aluminum chloride to be 0.06mol/L, and dialyzing at 40 ℃ for 2 days after the dealkalized lignin and the aluminum chloride are fully dissolved to obtain lignin nanowires.
Example 18:
a lignin nanowire, the method of making comprising the steps of:
adding dealkalized lignin into water, adding cosolvent N, N-dimethylformamide, wherein the mass concentration of lignin in the system is 20%, the volume concentration of N, N-dimethylformamide is 80%, adding aluminum chloride to enable the concentration of 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 lignin nanowires.
In the preparation process, lignin is added into water, then cosolvent is added, finally electrolyte is added, and the lignin nanowire can be prepared by dissolving and dialyzing, or mixing water and cosolvent to form cosolvent aqueous solution, then adding lignin into cosolvent aqueous solution, then adding electrolyte, dissolving and dialyzing.
The lignin nanowires of examples 1-18 can be obtained well, and some examples of the results are shown, and examples 1 and 2 are taken as examples, and SEM morphology diagrams are specifically shown in fig. 1 and 2.
As can be seen from FIGS. 1 and 2, the obtained lignin nanowires have a diameter of less than 100nm and a length of more than 100 μm, the nanotubes have a diameter of 100-600nm and a length of more than 100nm.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.

Claims (6)

1. The preparation method of the lignin nanowire is characterized by comprising the following steps of:
adding lignin into water, then adding cosolvent, finally adding electrolyte with strong complexing ability, uniformly mixing, and dialyzing to obtain lignin nanowire; or (b)
Mixing water and a cosolvent to form a cosolvent aqueous solution, then adding lignin, adding an electrolyte with strong complexing ability, uniformly mixing, and dialyzing to obtain lignin nanowires;
wherein the electrolyte with strong complexing ability is any one of ferric chloride and aluminum chloride; when the electrolyte with strong complexing ability is ferric chloride, the concentration of the ferric chloride in the reaction system is 0.05-0.1mol/L; when the electrolyte with strong complexing ability is aluminum chloride, the concentration of the aluminum chloride in the reaction system is 0.01-0.1mol/L;
the cosolvent is methanol, ethanol, glycol, tetrahydrofuran, dioxane, N-dimethylformamide, choline chloride/citric acid, choline chloride/acetic acid, [ ami ] Cl, [ Bmim ] Cl or DMSO/TBAH.
2. The method for preparing lignin nanowires according to claim 1, wherein the mass concentration of lignin in the cosolvent aqueous solution is 1-20%.
3. The method for preparing lignin nanowires according to claim 1, wherein the cosolvent is added so that the cosolvent occupies 10-90% of the volume concentration in the reaction system.
4. 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.
5. A lignin nanowire produced by the production method according to any one of claims 1 to 4.
6. The lignin nanowire of claim 5 is used for preparing an adsorption material, a shape memory material, an energy storage material, a slow release material, an ultraviolet protection material, an antibacterial material and an antioxidant material.
CN202210637059.6A 2022-06-07 2022-06-07 Lignin nanowire and preparation method and application thereof Active CN114920952B (en)

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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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Publication number Priority date Publication date Assignee Title
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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"π-π作用和疏水效应对碱木质素聚集行为的影响".《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》.2013,(第01期),B016-307. *

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