CN110746557A - Lignin composite hydrogel with high elasticity and fatigue strength resistance and preparation method thereof - Google Patents
Lignin composite hydrogel with high elasticity and fatigue strength resistance and preparation method thereof Download PDFInfo
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Abstract
A lignin composite hydrogel with high elasticity and fatigue strength is prepared through ultrasonic treating lignin aqueous solution to obtain suspension, mixing lignin suspension with acrylamide to obtain precursor, adding cross-linking agent and trigger, and heating. The preparation process is simple, the prepared composite hydrogel has the characteristics of good elastic recovery, high compressive strength, excellent fatigue strength and the like, the hydrogel can still be completely recovered in 80% of compression cycle period and can dissipate low energy, and the hydrogel can be applied to elastic materials, flexible energy storage devices and other devices.
Description
Technical Field
The invention relates to a lignin-based hydrogel, in particular to a lignin composite hydrogel with high elasticity and fatigue strength and a preparation method thereof.
Background
Hydrogels are polymers with three-dimensional networks formed by chemical or physical crosslinking. Because of the super-strong performance of absorbing water, keeping water and intelligently responding, the development and utilization of the hydrogel relate to various aspects of desert control, daily chemical products, electronics, environmental protection and the like. According to the different hydrogel preparation methods, the hydrogel is divided into a chemical crosslinking type hydrogel and a physical crosslinking type hydrogel. The chemical crosslinking hydrogel is formed by chemical bonds among polymer macromolecular chains to construct a three-dimensional network structure, and the physical crosslinking hydrogel realizes crosslinking through interaction force (hydrophobic association, electrostatic interaction, hydrogen bond, complexation, van der waals force and the like) of non-chemical bonds. However, conventional chemically crosslinked hydrogels generally have irregular and non-uniform crosslinked network structures, resulting in that the internal network structures of the hydrogels cannot effectively dissipate energy when the hydrogels are subjected to external force; most of the physical crosslinked hydrogel has small crosslinking interaction force, can not bear enough external stress, so that the mechanical property and the mechanical stability of the hydrogel are poor, and the application of the hydrogel is greatly limited. Therefore, researchers have been devoted to the search and research of high-strength hydrogels, and the high-strength hydrogels reported at present include slip-ring hydrogels, double-network hydrogels, polymer microsphere composite hydrogels, nanocomposite hydrogels, and the like. The nano-composite hydrogel is subjected to free radical polymerization on the surface of a nano-particle adsorption raw material monomer to form a three-dimensional network structure taking nano-particles as cross-linking points, and further realizes the combination of rigidity and flexibility through physical interaction, so that the mechanical property of the hydrogel is enhanced, and therefore, the nano-composite hydrogel becomes a research hotspot in a series of novel enhanced hydrogels. At present, the nanoparticles in the nanocomposite hydrogel are mainly inorganic nanoparticles, such as graphene oxide, titanium dioxide and inorganic clay nanoparticles, however, the nanoparticles are limited by two main factors, namely hydrophilicity and size, the particles with poor hydrophilicity cannot be uniformly dispersed in a large amount in water, and the particles with larger size are easy to be coagulated in water. Therefore, it is very important to find a suitable nano-particle for preparing the nano-composite hydrogel.
Lignin is the only aromatic organic high molecular compound in nature, and the total amount of lignin is second only to cellulose, which is the second largest natural organic high molecular compound. The lignin is widely present in plant fiber raw materials, and forms a plant skeleton together with cellulose and hemicellulose. As one of main components of plants, the molecular structure and the aggregation structure of lignin are very complex, and lignin can be divided into softwood lignin, hardwood lignin, kraft lignin, lignosulfonate and the like according to the types of plant fiber raw materials and different separation methods, and the basic structural units of the lignin are syringyl phenylpropane, p-hydroxy phenylpropane and guaiacyl phenylpropane. Lignin has various functional groups (such as alcoholic hydroxyl, phenolic hydroxyl, carbonyl, carboxyl, methoxyl, double bond and the like) on the structure, and basic structural units are connected by carbon-carbon bonds, ether bonds and hydrogen bonds, so the lignin can carry out various chemical reactions such as sulfonation, oxidation, phenolization, polycondensation, graft copolymerization and the like, and the characteristics endow the lignin with higher reaction activity, but the lignin is not used with high value because of the defects of complex structure, large steric hindrance, poor water solubility and the like.
Disclosure of Invention
The technical problem to be solved is as follows: the invention provides the lignin composite hydrogel with high elasticity and fatigue resistance and the preparation method thereof aiming at the defects of inorganic nanoparticles in the nano composite hydrogel, and the prepared hydrogel has the characteristics of good elasticity recovery, excellent compression performance, fatigue resistance and the like, and is expected to be applied to elastic materials, flexible energy storage devices and other devices.
The technical scheme is as follows: a preparation method of lignin composite hydrogel with high elasticity and fatigue strength comprises the following steps: carrying out ultrasonic treatment on 1-60 wt.% lignin aqueous solution to obtain lignin suspension, mixing the lignin suspension and acrylamide to obtain a prepolymer, wherein the mass ratio of lignin to acrylamide is (1: 10) - (10: 1), adding a cross-linking agent and an initiator, the mass ratio of the cross-linking agent to an acrylamide monomer is 1 (100-2000), the mass ratio of the initiator to the acrylamide monomer is 1 (20-80), and obtaining the lignin composite hydrogel under the heating condition.
Preferably, the lignin is one of kraft lignin, lignosulfonate, ethanol lignin, formic acid lignin, acetic acid lignin, hydrolyzed lignin, ground wood lignin and enzymatic hydrolysis lignin.
Preferably, the average size of the particles in the lignin suspension is 80-500 nm.
Preferably, the concentration of the lignin suspension is 1wt.% to 20 wt.%.
Preferably, the mass ratio of the lignin to the acrylamide is (1: 10) - (5: 3).
Preferably, the crosslinking agent is N, N' -methylene bisacrylamide, and the mass ratio of the crosslinking agent to the acrylamide monomer is 1: (200-400).
Preferably, the initiator is a mixed solution of ascorbic acid and hydrogen peroxide, the concentration of ascorbic acid in the mixed solution is 6wt.%, the concentration of hydrogen peroxide is 30wt.%, and the mass ratio of the initiator to the acrylamide monomer is 1: (40-60).
The heating temperature of the gel is 60-90 ℃, and the gel time is 24 hours.
The lignin composite hydrogel prepared by the preparation method.
The water content of the gel is 50wt.% to 99 wt.%.
Has the advantages that: the invention provides the lignin composite hydrogel with high elasticity and fatigue strength and the preparation method thereof, the preparation process is simple, and the lignin composite hydrogel has the characteristics of good elastic recovery, higher compressive strength, excellent fatigue strength and the like, can still be completely recovered in 80% of compression cycle period, dissipates lower energy, and is expected to be applied to elastic materials, flexible energy storage devices and other devices.
Detailed Description
The following examples further illustrate the present invention but should not be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit and substance of the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. The raw materials and reagents used in the lignin composite hydrogel and the preparation method thereof are all commercially available.
Example 1: preparation of lignin composite hydrogel
In a 250mL stirred reactor, 3 g of lignin was mixed in 60mL of distilled water, and the aqueous lignin solution was subjected to ultrasonic treatment by an ultrasonic probe at a frequency of 25kHz and a power of 800W for 60min to prepare a lignin nanoparticle suspension. Then, 13 g of acrylamide monomer, 43.3 mg of N, N' -methylenebisacrylamide as a crosslinking agent, 700. mu.L of ascorbic acid (6 wt%) and 700. mu.L of an aqueous solution of hydrogen peroxide (30 wt%) as an initiator were added to the suspension, and stirred at room temperature for 1 hour to be uniformly mixed; and (3) carrying out ultrasonic treatment for 1-2 min, removing bubbles, pouring into a cylindrical die with the diameter of 13mm and the height of 150mm, and carrying out cross-linking polymerization in a constant temperature and humidity box at 80 ℃ for 24h to obtain the lignin composite hydrogel.
Example 2: preparation of lignin composite hydrogel
In a 250mL stirred reactor, 4 g of lignin was mixed in 60mL of distilled water, and the aqueous lignin solution was subjected to ultrasonic treatment by an ultrasonic probe at a frequency of 25kHz and a power of 800W for 60min to prepare a lignin nanoparticle suspension. Then 12 g of acrylamide monomer, 40 mg of N, N' -methylenebisacrylamide as a crosslinking agent, 660. mu.L of ascorbic acid (6 wt%) and 660. mu.L of hydrogen peroxide (30 wt%) as an initiator were added to the suspension, and stirred at room temperature for 1 hour to be uniformly mixed; the rest of the procedure was the same as in example 1. Obtaining the lignin composite hydrogel.
Example 3: preparation of lignin composite hydrogel
In a 250mL stirred reactor, 5 g of lignin was dissolved in 60mL of distilled water, and the aqueous lignin solution was subjected to ultrasonic treatment by an ultrasonic probe at a frequency of 25kHz and a power of 800W for 60min to prepare a lignin nanoparticle suspension. Then, 11 g of acrylamide monomer, 36.6 mg of N, N' -methylenebisacrylamide as a crosslinking agent, 610. mu.L of ascorbic acid (6 wt%) and 610. mu.L of an aqueous solution of hydrogen peroxide (30 wt%) as an initiator were added to the suspension, and stirred at room temperature for 1 hour to be mixed uniformly; the rest of the procedure was the same as in example 1. Obtaining the lignin composite hydrogel.
Example 4: preparation of lignin composite hydrogel
In a 250mL stirred reactor, 6 g of lignin was dissolved in 60mL of distilled water, and the aqueous lignin solution was subjected to ultrasonic treatment by an ultrasonic probe at a frequency of 25kHz and a power of 800W for 60min to prepare a lignin nanoparticle suspension. Then, 10 g of acrylamide monomer, 33.3 mg of N, N' -methylenebisacrylamide as a crosslinking agent, 555. mu.L of ascorbic acid (6 wt%) and 555. mu.L of aqueous hydrogen peroxide (30 wt%) as an initiator were added to the suspension, and stirred at room temperature for 1 hour to be uniformly mixed; the rest of the procedure was the same as in example 1. Obtaining the lignin composite hydrogel.
Example 5: preparation of lignin composite hydrogel
In a 250mL stirred reactor, 7 grams of lignin was dissolved in 60mL of distilled water, and the aqueous lignin solution was sonicated by an ultrasonic probe at a frequency of 25kHz and a power of 800W for 60min to prepare a lignin nanoparticle suspension. Then 9 g of acrylamide monomer, 30 mg of N, N' -methylenebisacrylamide as a crosslinking agent, 500. mu.L of ascorbic acid (6 wt%) and 500. mu.L of hydrogen peroxide (30 wt%) as an aqueous solution were added to the suspension, and stirred at room temperature for 1 hour to mix them uniformly; the rest of the procedure was the same as in example 1. Obtaining the lignin composite hydrogel.
Example 6: preparation of lignin composite hydrogel
In a 250mL stirred reactor, 8 g of lignin was dissolved in 60mL of distilled water, and the aqueous lignin solution was subjected to ultrasonic treatment by an ultrasonic probe at a frequency of 25kHz and a power of 800W for 60min to prepare a lignin nanoparticle suspension. Then 8 g of acrylamide monomer, 26.7 mg of N, N' -methylenebisacrylamide as a crosslinking agent, 444. mu.L of ascorbic acid (6 wt%) and 444. mu.L of hydrogen peroxide (30 wt%) as an initiator were added to the suspension, and stirred at room temperature for 1 hour to be mixed uniformly; the rest of the procedure was the same as in example 1. Obtaining the lignin composite hydrogel.
Example 7: preparation of lignin composite hydrogel
In a 250mL stirred reactor, 9 g of lignin was dissolved in 60mL of distilled water, and the aqueous lignin solution was subjected to ultrasonic treatment by an ultrasonic probe at a frequency of 25kHz and a power of 800W for 60min to prepare a lignin nanoparticle suspension. Then, 7 g of an acrylamide monomer, 23.3 mg of an N, N' -methylenebisacrylamide crosslinking agent, 388. mu.L of ascorbic acid (6 wt%) and 388. mu.L of an aqueous hydrogen peroxide solution (30 wt%) were added as an initiator to the dispersion, and stirred at room temperature for 1 hour to be mixed uniformly; the rest of the procedure was the same as in example 1. Obtaining the lignin composite hydrogel.
Example 8: preparation of lignin composite hydrogel
In a 250mL stirred reactor, 10 g of lignin was dissolved in 60mL of distilled water, and the aqueous lignin solution was subjected to ultrasonic treatment by an ultrasonic probe at a frequency of 25kHz and a power of 800W for 60min to prepare a lignin nanoparticle suspension. Then 6 g of acrylamide monomer, 20 mg of N, N' -methylenebisacrylamide as a crosslinking agent, 333. mu.L of ascorbic acid (6 wt%) and 333. mu.L of hydrogen peroxide (30 wt%) as an initiator were added to the suspension, and stirred at room temperature for 1 hour to be uniformly mixed; the rest of the procedure was the same as in example 1. Obtaining the lignin composite hydrogel.
Example 9: preparation of acrylamide hydrogel
Dissolving 13 g of acrylamide monomer in 60mL of distilled water in a 250mL stirring reactor, stirring and dissolving, adding 43.3 mg of N, N' -methylene bisacrylamide crosslinking agent, 700 μ L of ascorbic acid (6 wt%) and 700 μ L of hydrogen peroxide (30 wt%) aqueous solution as an initiator, and stirring at room temperature for 1h to mix uniformly; the rest of the procedure was the same as in example 1. An acrylamide hydrogel was obtained.
Example 10: elastic recovery and fatigue strength of lignin composite hydrogel
And testing the elastic recovery and the fatigue resistance of the lignin composite hydrogel by using an electronic universal testing machine. The hydrogels obtained in examples 1, 2, 3, 4, 5, 6, 7, 8 and 9 were cut into cylinders having a diameter of 13mm and a height of 5 to 10 mm. Then, a cylindrical sample is vertically loaded between two compression clamp planes, uniaxial compression and release with strain of 80% are applied along the vertical direction, the strain loading speed is 30mm/min, the number of continuous compression-release times is 100 times in total, the change relation between the cyclic stress and the strain of the lignin composite hydrogel under 80% strain is obtained, and the stress reduction rate, the plastic deformation rate and the energy loss coefficient are obtained through calculation, as shown in table 1. As can be seen from examples 1, 2, 3, 4, 5, 6, 7 and 8, the stress loss, plastic deformation and energy loss coefficient all tend to decrease and then increase as the lignin ratio increases. From examples 1 and 9, it is clear that the addition of lignin to the hydrogel reduced the stress loss, plastic deformation and energy loss coefficient.
The preparation method of the lignin composite hydrogel with high elasticity and fatigue strength provided by the invention takes a mixed solution of lignin and acrylamide as a prepolymer, and finally forms the polymer hydrogel by copolymerization crosslinking of a lignin suspension and an acrylamide monomer under the action of an initiator, a crosslinking agent and the like. The prepared lignin composite hydrogel has the characteristics of good elastic recovery, excellent compression performance, fatigue strength resistance and the like, and is expected to be applied to elastic materials, flexible energy storage devices and other devices.
Claims (10)
1. A preparation method of lignin composite hydrogel with high elasticity and fatigue strength is characterized by comprising the following steps: carrying out ultrasonic treatment on 1-60 wt.% lignin aqueous solution to obtain lignin suspension, mixing the lignin suspension and acrylamide to obtain a prepolymer, wherein the mass ratio of lignin to acrylamide is (1: 10) - (10: 1), adding a cross-linking agent and an initiator, the mass ratio of the cross-linking agent to an acrylamide monomer is 1 (100-2000), the mass ratio of the initiator to the acrylamide monomer is 1 (20-80), and obtaining the lignin composite hydrogel under the heating condition.
2. The method of claim 1, wherein the lignin is one of kraft lignin, lignosulfonate, ethanol lignin, formic acid lignin, acetic acid lignin, hydrolyzed lignin, ground wood lignin, and enzymatic lignin.
3. The method according to claim 1, wherein the average size of the particles in the lignin suspension is 80 to 500 nm.
4. The method according to claim 1, wherein the lignin suspension has a concentration of 1wt.% to 20 wt.%.
5. The preparation method according to claim 1, wherein the mass ratio of the lignin to the acrylamide is (1: 10) - (5: 3).
6. The method according to claim 1, wherein the crosslinking agent is N, N' -methylenebisacrylamide, and the mass ratio of the crosslinking agent to the acrylamide monomer is 1: (200-400).
7. The preparation method according to claim 1, wherein the initiator is a mixed solution of ascorbic acid and hydrogen peroxide, the concentration of ascorbic acid in the mixed solution is 6wt.%, the concentration of hydrogen peroxide is 30wt.%, and the mass ratio of the initiator to the acrylamide monomer is 1: (40-60).
8. The method according to claim 1, wherein the gel heating temperature is 60 to 90 ℃ and the gel time is 24 hours.
9. A lignin-containing composite hydrogel obtained by the method according to any one of claims 1 to 8.
10. The lignin composite hydrogel according to claim 9, wherein the gel water content is 50wt.% to 99 wt.%.
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Cited By (2)
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Cited By (2)
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CN115322510A (en) * | 2022-09-08 | 2022-11-11 | 中国林业科学研究院林产化学工业研究所 | Self-adhesive tough silver/lignin hydrogel and preparation method thereof |
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