CN114015075A - Preparation method of tough and transparent hydrogel based on cellulose self-assembly regulation - Google Patents
Preparation method of tough and transparent hydrogel based on cellulose self-assembly regulation Download PDFInfo
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- 238000002791 soaking Methods 0.000 claims abstract description 110
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- 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
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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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
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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- 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
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/24—Homopolymers or copolymers of amides or imides
- C08J2333/26—Homopolymers or copolymers of acrylamide or methacrylamide
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3442—Heterocyclic compounds having nitrogen in the ring having two nitrogen atoms in the ring
- C08K5/3445—Five-membered rings
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Abstract
The invention discloses a preparation method of tough and transparent hydrogel based on cellulose self-assembly regulation and control, and belongs to the technical field of hydrogel preparation. Dissolving cellulose in ionic liquid, and heating and dissolving to obtain a cellulose-ionic liquid solution; carrying out water-induced self-assembly on the cellulose solution to obtain cellulose gel; and soaking the cellulose gel in an acrylamide solution containing a photoinitiator for treatment, and then initiating polymerization by ultraviolet irradiation to obtain the tough and transparent hydrogel. According to the invention, the self-assembly action of the water-induced cellulose is adopted, so that the mechanical property of the hydrogel can be regulated, the problem that the strength, the stretching and the toughness cannot be considered in the traditional hydrogel reinforcing and toughening strategy is solved, and the hydrogel has good mechanical property and conductivity due to the existence of the ionic liquid in the system, and is expected to be used in the fields of flexible wearable equipment and the like.
Description
Technical Field
The invention belongs to the technical field of hydrogel preparation, and particularly relates to a preparation method of tough and transparent hydrogel based on cellulose self-assembly regulation and control.
Background
The hydrogel is a material containing water and having a three-dimensional cross-linked network, has the characteristics of softness and humidity, and has wide application prospects in various fields of biomedicine, water treatment, wearable electronic equipment and the like. However, the homogeneous structure of the hydrogels makes them deficient in crosslinking on the one hand and low solids content due to high water content on the other hand, which limits their range of application to a certain extent.
Currently, there are many methods for designing hydrogels to improve their strength and toughness, such as designing double networks, designing physical-chemical hybrid cross-linking, introducing sliding cross-linking agents, designing highly oriented hierarchical structures, and introducing strong/weak fibers to construct composite networks. However, the improvement of mechanical properties by the above method is limited. In addition, increasing the strength of the hydrogel tends to sacrifice its toughness and vice versa. Therefore, it is a challenge to compromise the strength, strain and toughness of hydrogels.
As the most abundant natural polysaccharide on the earth, cellulose is widely applied to the fields of preparation of biocompatible and biodegradable materials and the like. With the sequential development and application of a series of cellulose solvents including ionic liquids, alkali/urea water systems, and N-methylmorpholine-N-oxide, the construction of hydrogels based on cellulose is also a major research focus. The preparation of cellulose hydrogels with different structures and properties by first dissolving cellulose with a solvent and then regenerating it with ethanol or water is currently a widely used strategy. However, hydrogels prepared from regenerated cellulose tend to have poor light transmittance, which limits their applications in wearable devices and the like to some extent.
Disclosure of Invention
Aiming at the problems in the prior art, the technical problem to be solved by the invention is to provide a preparation method of tough and transparent hydrogel based on cellulose self-assembly regulation and control, the method can regulate and control the mechanical property of the hydrogel by inducing the self-assembly action of cellulose through water, not only solves the problem that the strength, the tensile property and the toughness cannot be considered at the same time in the traditional hydrogel reinforcing and toughening strategy, but also enables the hydrogel to have good mechanical property and conductivity due to the existence of ionic liquid in the system, and is expected to be used in the fields of flexible wearable equipment and the like.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a preparation method of tough and transparent hydrogel based on cellulose self-assembly regulation and control specifically comprises the following steps:
1) drying the cellulose in an air-blast drying oven to remove moisture to obtain dried cellulose for later use;
2) mixing the dried cellulose obtained in the step 1) with ionic liquid, and heating and dissolving to obtain a cellulose-ionic liquid mixed solution;
3) spreading the cellulose-ionic liquid mixed solution prepared in the step 2) in a culture dish, and performing moisture-induced cellulose self-assembly in an environment with certain humidity to obtain cellulose gel;
4) mixing a monomer, a cross-linking agent and a photoinitiator, and fully dissolving to obtain a soaking solution;
5) soaking the cellulose gel prepared in the step 3) in the soaking solution prepared in the step 4);
6) and after soaking, weighing the soaking solution, and polymerizing under ultraviolet initiation to obtain the tough and transparent hydrogel based on cellulose self-assembly regulation.
According to the preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation, the ionic liquid is any one of 1-butyl-3-methylimidazole chloride salt, 1-butyl-3-methylimidazole bromide salt, 1-ethyl-3-methylimidazole bromide salt, 1-allyl-3-methylimidazole chloride salt or 1-ethyl-3-methylimidazole acetate, and the ionic liquid is a salt consisting of anions and cations; the temperature for heating and dissolving is 60-150 ℃, and the dissolving time is 6-72 h; the mass fraction of the cellulose in the cellulose-ionic liquid mixed solution is 0.5 wt% -15 wt%.
According to the preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation, the ionic liquid is 1-butyl-3-methylimidazolium chloride or 1-ethyl-3-methylimidazolium acetate; the temperature for heating and dissolving the cellulose is 80-110 ℃, and the dissolving time is 24-60 h; the mass fraction of the cellulose in the cellulose-ionic liquid mixed solution is 2.5 wt% -10 wt%.
According to the preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation and control, the moisture-induced environment humidity is 5-95% RH, and the induced self-assembly time is 2-48 h.
According to the preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation, the moisture-induced environment humidity is 50-90% RH; the time for inducing cellulose self-assembly by water is 6-24 h.
According to the preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation, the monomer is any one of acrylic acid, acrylamide, methacrylic acid, methacrylamide, N-dimethylacrylamide, N-isopropylacrylamide, N-vinylcaprolactam, hydroxyethyl acrylate or hydroxyethyl methacrylate, and the monomers can form a polymer network; the cross-linking agent is N, N' -methylene bisacrylamide or polyethylene glycol diacrylate, and the cross-linking agent is a molecule capable of being cross-linked to form a network structure; the photoinitiator is any one of 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone, diphenyl (2,4, 6-trimethylbenzoyl) phosphine oxide or 1-hydroxycyclohexyl phenyl ketone, and the photoinitiator can release molecules of free radicals.
According to the preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation, the monomer is acrylamide, the cross-linking agent is N, N' -methylene bisacrylamide, and the photoinitiator is 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone.
According to the preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation, the concentration of the monomer is 2.8-11.2 mol/L, the addition amount of the cross-linking agent is 0.07-1.12 wt% of the mass of the monomer, and the addition amount of the photoinitiator is 0.15-2.7 wt% of the mass of the monomer.
According to the preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation, the concentration of the monomer is 5.6-8.4 mol/L, and the addition amounts of the cross-linking agent and the photoinitiator are 0.14 wt/% -0.84 wt/% and 0.45 wt/% -1.35 wt% of the monomer respectively.
According to the preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation, the mass ratio of the soaking solution to the cellulose gel is 0.5: 1-5: 1, and the soaking time is 6-48 h.
According to the preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation, the mass ratio of the soak solution to the cellulose gel is 1.5: 1-4.5: 1; the soaking time is 24-48 h.
According to the preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation, the mass ratio of the soaking solution to the soaking solution for soaking is 4.8: 100-47.7: 100.
According to the preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation, the mass ratio of the soaking solution to the soaking solution for soaking is 14.3: 100-42.9: 100.
According to the preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation and control, the ultraviolet light power is 6-48W, and the polymerization time initiated by ultraviolet light is 0.5-2 h.
According to the preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation, the ultraviolet light power is 36W; the polymerization time initiated by the ultraviolet light is 1-2 h.
Has the advantages that: compared with the prior art, the invention has the advantages that:
(1) according to the invention, the self-assembly action of the cellulose is induced by moisture to form a cellulose framework, so that the strength is provided for the hydrogel.
(2) The invention can regulate and control the mechanical property of the hydrogel by inducing the self-assembly behavior of the cellulose through moisture.
(3) According to the invention, acrylamide is used as an elastic matrix and forms strong hydrogen bond connection with a cellulose skeleton, so that flexibility is provided for hydrogel.
(4) The existence of the ionic liquid in the system can improve the mechanical property and the transparency of the hydrogel and also provide the conductivity for the hydrogel.
(5) Compared with the common hydrogel, the hydrogel disclosed by the invention has the advantages of high strength, high toughness and good stretchability.
(6) The hydrogel disclosed by the invention has good mechanical properties and transparency, and is expected to be used in the fields of wearable electronic equipment and the like.
Drawings
FIG. 1 is an XRD pattern of cellulose and cellulose gel of example 1;
FIG. 2 is an SEM photograph of the hydrogel obtained in example 1;
FIG. 3 is a stress response curve of the hydrogel obtained in example 1;
FIG. 4 is the electrical conductivity of the hydrogel obtained in example 1;
FIG. 5 is a light transmittance curve of the hydrogel obtained in example 1;
FIG. 6 is a stress-strain curve of 300 cycles of extension at 150% strain for the hydrogel obtained in example 1.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
Example 1
A preparation method of tough and transparent hydrogel based on cellulose self-assembly regulation and control specifically comprises the following steps:
1) drying the cellulose in an air-blast drying oven to remove moisture to obtain dried cellulose for later use;
2) mixing the cellulose dried in the step 1) with 1-butyl-3-methyl-imidazolium chloride ([ BMIm ] Cl) ionic liquid, heating to 110 ℃, and dissolving for 36 hours to obtain a cellulose-ionic liquid mixed solution with the cellulose mass fraction of 7.5 wt%;
3) spreading the cellulose-ionic liquid mixed solution prepared in the step 2) in a culture dish, then placing the culture dish in an environment of 90% RH for 12h, and obtaining cellulose gel by inducing cellulose self-assembly through water vapor;
4) mixing 8.4mol/L acrylamide, N' -methylene bisacrylamide with the mass fraction of the acrylamide being 0.28 wt% and 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone with the mass fraction of the acrylamide being 0.90 wt%, and stirring to fully dissolve the acrylamide and the 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone to obtain a soaking solution;
5) soaking the cellulose gel prepared in the step 3) in the soaking solution in the step 4) for 36 hours, wherein the mass ratio of the soaking solution to the cellulose gel is 1.5: 1;
6) and after soaking, weighing the mass ratio of the soaking solution to the soaking solution for soaking to be 14.3:100, and polymerizing for 1h under the initiation of ultraviolet light with the power of 36W to obtain the tough and transparent hydrogel based on cellulose self-assembly regulation and control.
Fig. 1 is an XRD chart of cellulose and cellulose gel, and it can be seen from fig. 1 that after cellulose is dissolved in ionic liquid, its crystal structure changes from cellulose type i to cellulose type ii. FIG. 2 is an SEM image of a hydrogel, and it can be seen from FIG. 1 that the hydrogel is dense in microstructure. Fig. 3 is a stress-strain curve of the hydrogel, and it can be seen from fig. 3 that the hydrogel has good mechanical properties, the tensile strain of the hydrogel can reach 1291%, and the tensile strength of the hydrogel can reach 2.3 MPa. FIG. 4 shows the electrical conductivity of the hydrogel, and it can be seen from FIG. 4 that the hydrogel has good electrical conductivity, and the electrical conductivity is 1.58S/m. FIG. 5 is a light transmittance curve of the hydrogel, and it can be seen from FIG. 5 that the hydrogel has good transparency and the light transmittance at 600nm is 86%. Fig. 6 is a stress-strain curve of 300 cycles of stretching of the hydrogel at 150% strain, and it can be seen from fig. 6 that the hydrogel has good cyclic stability, and the strain remains substantially stable after 300 cycles of stretching at 150% strain.
Example 2
A preparation method of tough and transparent hydrogel based on cellulose self-assembly regulation and control specifically comprises the following steps:
1) drying the cellulose in an air-blast drying oven to remove moisture to obtain dried cellulose for later use;
2) mixing the cellulose dried in the step 1) with 1-butyl-3-methyl-imidazolium chloride ([ BMIm ] Cl) ionic liquid, heating to 80 ℃ to dissolve for 24 hours to obtain a cellulose-ionic liquid mixed solution with the cellulose mass fraction of 2.5 wt%;
3) spreading the cellulose-ionic liquid mixed solution prepared in the step 2) in a culture dish, then placing the culture dish in an environment with 50% RH for 12h, and obtaining cellulose gel by inducing cellulose self-assembly through water vapor;
4) mixing 8.4mol/L acrylamide, N' -methylene bisacrylamide with the mass fraction of the acrylamide being 0.28 wt% and 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone with the mass fraction of the acrylamide being 0.90 wt%, and stirring to fully dissolve the acrylamide and the 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone to obtain a soaking solution;
5) soaking the cellulose gel prepared in the step 3) in the soaking solution in the step 4) for 36 hours, wherein the mass ratio of the soaking solution to the cellulose gel is 3: 1;
6) and after soaking, weighing the mass ratio of the soaking solution to the soaking solution for soaking to be 28.6:100, and polymerizing for 2 hours under the ultraviolet light initiation with the power of 6W to obtain the tough and transparent hydrogel based on cellulose self-assembly regulation and control.
The tensile stress of the hydrogel was 0.3MPa, and the tensile strain was 1100%.
Example 3
A preparation method of tough and transparent hydrogel based on cellulose self-assembly regulation and control specifically comprises the following steps:
1) drying the cellulose in an air-blast drying oven to remove moisture to obtain dried cellulose for later use;
2) mixing the cellulose dried in the step 1) with 1-ethyl-3-methylimidazole acetate ([ Emim ] [ OAc ]) ionic liquid, heating to 110 ℃, and dissolving for 24 hours to obtain a cellulose-ionic liquid mixed solution with the cellulose mass fraction of 2.5 wt%;
3) spreading the cellulose-ionic liquid mixed solution prepared in the step 2) in a culture dish, then placing the culture dish in an environment with 50% RH for reacting for 6h, and obtaining cellulose gel by inducing cellulose self-assembly through water vapor;
4) mixing 8.4mol/L acrylamide, N' -methylene bisacrylamide with the mass fraction of the acrylamide being 0.84 wt% and 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone with the mass fraction of 1.35 wt%, and stirring to fully dissolve the mixture to obtain a soaking solution;
5) soaking the cellulose gel prepared in the step 3) in the soaking solution in the step 4) for 36 hours, wherein the mass ratio of the soaking solution to the cellulose gel is 4.5: 1;
6) and after soaking, weighing the mass ratio of the soaking solution to the soaking solution for soaking to be 42.9:100, and polymerizing for 1h under the ultraviolet light initiation with the power of 24W to obtain the tough and transparent hydrogel based on cellulose self-assembly regulation and control.
The tensile stress of the hydrogel was 1.6MPa, and the tensile strain was 480%.
Example 4
A preparation method of tough and transparent hydrogel based on cellulose self-assembly regulation and control specifically comprises the following steps:
1) drying the cellulose in an air-blast drying oven to remove moisture to obtain dried cellulose for later use;
2) mixing the cellulose dried in the step 1) with 1-butyl-3-methyl-imidazolium chloride ([ BMIm ] Cl) ionic liquid, heating to 110 ℃, and dissolving for 24 hours to obtain a cellulose-ionic liquid mixed solution with the cellulose mass fraction of 2.5 wt%;
3) spreading the cellulose-ionic liquid mixed solution prepared in the step 2) in a culture dish, then placing the culture dish in an environment with 50% RH for 48h, and obtaining cellulose gel by inducing cellulose self-assembly through water vapor;
4) mixing 8.4mol/L acrylamide, N' -methylene bisacrylamide with the mass fraction of the acrylamide being 0.14 wt% and 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone with the mass fraction of the acrylamide being 0.45 wt%, and stirring to fully dissolve the acrylamide and the 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone to obtain a soaking solution;
5) soaking the cellulose gel prepared in the step 3) in the soaking solution in the step 4) for 36 hours, wherein the mass ratio of the soaking solution to the cellulose gel is 1.5: 1;
6) and after soaking, weighing the mass ratio of the soaking solution to the soaking solution for soaking to be 14.3:100, and polymerizing for 1h under the initiation of ultraviolet light with the power of 36W to obtain the tough and transparent hydrogel based on cellulose self-assembly regulation and control.
The tensile stress of the hydrogel was 1.5MPa, and the tensile strain was 980%.
Example 5
A preparation method of tough and transparent hydrogel based on cellulose self-assembly regulation and control specifically comprises the following steps:
1) drying the cellulose in an air-blast drying oven to remove moisture to obtain dried cellulose for later use;
2) mixing the cellulose dried in the step 1) with 1-ethyl-3-methylimidazole acetate ([ Emim ] [ OAc ]) ionic liquid, heating to 100 ℃ and dissolving for 48 hours to obtain a cellulose-ionic liquid mixed solution with the cellulose mass fraction of 10 wt%;
3) spreading the cellulose-ionic liquid mixed solution prepared in the step 2) in a culture dish, then placing the culture dish in an environment with 70% RH for 12h, and obtaining cellulose gel by inducing cellulose self-assembly through water vapor;
4) mixing 5.6mol/L acrylamide, N' -methylene bisacrylamide with the mass fraction of the acrylamide being 0.28 wt% and 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone with the mass fraction of the acrylamide being 0.90 wt%, and stirring to fully dissolve the acrylamide and the 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone to obtain a soaking solution;
5) soaking the cellulose gel prepared in the step 3) in the soaking solution in the step 4) for 48 hours, wherein the mass ratio of the soaking solution to the cellulose gel is 3: 1;
6) and after soaking, weighing the mass ratio of the soaking solution to the soaking solution for soaking to be 28.6:100, and polymerizing for 1h under the ultraviolet light initiation with the power of 48W to obtain the tough and transparent hydrogel based on cellulose self-assembly regulation and control.
The tensile stress of the hydrogel was 0.7MPa, and the tensile strain was 500%.
Example 6
A preparation method of tough and transparent hydrogel based on cellulose self-assembly regulation and control specifically comprises the following steps:
1) drying the cellulose in an air-blast drying oven to remove moisture to obtain dried cellulose for later use;
2) mixing the dried cellulose obtained in the step 1) with 1-butyl-3-methyl-imidazole chloride salt ([ BMIm ] Cl) ionic liquid, heating to 100 ℃, and dissolving for 60 hours to obtain a cellulose-ionic liquid mixed solution with the cellulose mass fraction of 7.5 wt%;
3) spreading the cellulose-ionic liquid mixed solution prepared in the step 2) in a culture dish, then placing the culture dish in an environment with 50% RH for 12h, and obtaining cellulose gel by inducing cellulose self-assembly through water vapor;
4) mixing 5.6mol/L acrylamide, N' -methylene bisacrylamide with the mass fraction of the acrylamide being 0.84 wt% and 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone with the mass fraction of 1.35 wt%, and stirring to fully dissolve the mixture to obtain a soaking solution;
5) soaking the cellulose gel prepared in the step 3) in the soaking solution in the step 4) for 24 hours, wherein the mass ratio of the soaking solution to the cellulose gel is 3: 1;
6) and after soaking, weighing the mass ratio of the soaking solution to the soaking solution for soaking to be 28.6:100, and polymerizing for 2 hours under the ultraviolet light initiation with the power of 6W to obtain the tough and transparent hydrogel based on cellulose self-assembly regulation and control.
The tensile stress of the hydrogel was 0.1MPa, and the tensile strain was 937%.
Example 7
A preparation method of tough and transparent hydrogel based on cellulose self-assembly regulation and control specifically comprises the following steps:
1) drying the cellulose in an air-blast drying oven to remove moisture to obtain dried cellulose for later use;
2) mixing the cellulose dried in the step 1) with 1-butyl-3-methyl-imidazolium chloride ([ BMIm ] Cl) ionic liquid, heating to 100 ℃, and dissolving for 36 hours to obtain a cellulose-ionic liquid mixed solution with the cellulose mass fraction of 5 wt%;
3) spreading the cellulose-ionic liquid mixed solution prepared in the step 2) in a culture dish, then placing the culture dish in an environment with 70% RH for 12h, and obtaining cellulose gel by inducing cellulose self-assembly through water vapor;
4) mixing 5.6mol/L acrylamide, N' -methylene bisacrylamide with the mass fraction of the acrylamide being 0.42 wt% and 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone with the mass fraction of 1.575 wt%, and stirring to fully dissolve the mixture to obtain a soaking solution;
5) soaking the cellulose gel prepared in the step 3) in the soaking solution in the step 4) for 24 hours, wherein the mass ratio of the soaking solution to the cellulose gel is 4.5: 1;
6) and after soaking, weighing the mass ratio of the soaking solution to the soaking solution for soaking to be 42.9:100, and polymerizing for 1.5h under the ultraviolet light initiation with the power of 24W to obtain the tough and transparent hydrogel based on cellulose self-assembly regulation and control.
The tensile stress of the hydrogel was 0.9MPa, and the tensile strain was 750%.
Example 8
A preparation method of tough and transparent hydrogel based on cellulose self-assembly regulation and control specifically comprises the following steps:
1) the cellulose was dried in an air-blast drying oven to remove moisture, and dried cellulose was obtained for use.
2) Mixing the dried cellulose obtained in the step 1) with 1-ethyl-3-methylimidazole acetate ([ Emim ] [ OAc ]) ionic liquid, heating to 90 ℃ and dissolving for 24 hours to obtain a cellulose-ionic liquid mixed solution with the cellulose mass fraction of 10 wt%;
3) spreading the cellulose-ionic liquid mixed solution prepared in the step 2) in a culture dish, then placing the culture dish in an environment with 70% RH for 6h, and obtaining cellulose gel by inducing cellulose self-assembly through water vapor;
4) mixing 8.4mol/L acrylamide, N' -methylene bisacrylamide with the mass fraction of the acrylamide being 0.14 wt% and 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone with the mass fraction of the acrylamide being 0.45 wt%, and stirring to fully dissolve the acrylamide and the 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone to obtain a soaking solution;
5) soaking the cellulose gel prepared in the step 3) in the soaking solution in the step 4) for 24 hours, wherein the mass ratio of the soaking solution to the cellulose gel is 1.5: 1;
6) and after soaking, weighing the mass ratio of the soaking solution to the soaking solution for soaking to be 14.3:100, and polymerizing for 1.5 hours under the initiation of ultraviolet light with the power of 36W to obtain the tough and transparent hydrogel based on cellulose self-assembly regulation and control.
The tensile stress of the hydrogel was 1.6MPa, and the tensile strain was 780%.
Example 9
A preparation method of tough and transparent hydrogel based on cellulose self-assembly regulation and control specifically comprises the following steps:
1) drying the cellulose in an air-blast drying oven to remove moisture to obtain dried cellulose for later use;
2) mixing the cellulose dried in the step 1) with 1-ethyl-3-methylimidazole acetate ([ Emim ] [ OAc ]) ionic liquid, heating to 90 ℃ and dissolving for 48 hours to obtain a cellulose-ionic liquid mixed solution with the cellulose mass fraction of 5 wt%;
3) spreading the cellulose-ionic liquid mixed solution prepared in the step 2) in a culture dish, then placing the culture dish in an environment of 90% RH for 24h, and obtaining cellulose gel by inducing cellulose self-assembly through water vapor;
4) mixing 5.6mol/L acrylamide, N' -methylene bisacrylamide with the mass fraction of the acrylamide being 0.42 wt% and 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone with the mass fraction of 1.35 wt%, and stirring to fully dissolve the mixture to obtain a soaking solution;
5) soaking the cellulose gel prepared in the step 3) in the soaking solution in the step 4) for 24 hours, wherein the mass ratio of the soaking solution to the cellulose gel is 3: 1;
6) and after soaking, weighing the mass ratio of the soaking solution to the soaking solution for soaking to be 28.6:100, and polymerizing for 1.5 hours under the ultraviolet light initiation with the power of 48W to obtain the tough and transparent hydrogel based on cellulose self-assembly regulation and control.
The tensile stress of the hydrogel was 1.2MPa, and the tensile strain was 800%.
Example 10
A preparation method of tough and transparent hydrogel based on cellulose self-assembly regulation and control specifically comprises the following steps:
1) drying the cellulose in an air-blast drying oven to remove moisture to obtain dried cellulose for later use;
2) mixing the cellulose dried in the step 1) with 1-ethyl-3-methylimidazole acetate ([ Emim ] [ OAc ]) ionic liquid, heating to 80 ℃ and dissolving for 36 hours to obtain a cellulose-ionic liquid mixed solution with the cellulose mass fraction of 2.5 wt%;
3) spreading the cellulose-ionic liquid mixed solution prepared in the step 2) in a culture dish, then placing the culture dish in an environment with 70% RH for 6h, and obtaining cellulose gel by inducing cellulose self-assembly through water vapor;
4) mixing 8.4mol/L acrylamide, N' -methylene bisacrylamide with the mass fraction of the acrylamide being 0.14 wt% and 1.575 wt% of 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone, and stirring to fully dissolve the mixture to obtain a soaking solution;
5) soaking the cellulose gel prepared in the step 3) in the soaking solution in the step 4) for 24 hours, wherein the mass ratio of the soaking solution to the cellulose gel is 4.5: 1;
6) and after soaking, weighing the mass ratio of the soaking solution to the soaking solution for soaking to be 42.9:100, and polymerizing for 2 hours under the ultraviolet light initiation with the power of 6W to obtain the tough and transparent hydrogel based on cellulose self-assembly regulation and control.
The tensile stress of the hydrogel was 1.4MPa, and the tensile strain was 980%.
Claims (15)
1. A preparation method of tough and transparent hydrogel based on cellulose self-assembly regulation is characterized by comprising the following steps:
1) drying the cellulose in an air-blast drying oven to remove moisture to obtain dried cellulose for later use;
2) mixing the dried cellulose obtained in the step 1) with ionic liquid, and heating and dissolving to obtain a cellulose-ionic liquid mixed solution;
3) spreading the cellulose-ionic liquid mixed solution prepared in the step 2) in a culture dish, and performing moisture-induced cellulose self-assembly in an environment with certain humidity to obtain cellulose gel;
4) mixing a monomer, a cross-linking agent and a photoinitiator, and fully dissolving to obtain a soaking solution;
5) soaking the cellulose gel prepared in the step 3) in the soaking solution prepared in the step 4);
6) and after soaking, weighing the soaking solution, and polymerizing under ultraviolet initiation to obtain the tough and transparent hydrogel based on cellulose self-assembly regulation.
2. The preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation and control of claim 1, wherein the ionic liquid is any one of 1-butyl-3-methylimidazole chloride salt, 1-butyl-3-methylimidazole bromide salt, 1-ethyl-3-methylimidazole bromide salt, 1-allyl-3-methylimidazole chloride salt or 1-ethyl-3-methylimidazole acetate; the temperature for heating and dissolving is 60-150 ℃, and the dissolving time is 6-72 h; the mass fraction of the cellulose in the cellulose-ionic liquid mixed solution is 0.5 wt% -15 wt%.
3. The preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation and control of claim 1 or 2, wherein the ionic liquid is 1-butyl-3-methylimidazolium chloride or 1-ethyl-3-methylimidazolium acetate; the temperature for heating and dissolving the cellulose is 80-110 ℃, and the dissolving time is 24-60 h; the mass fraction of the cellulose in the cellulose-ionic liquid mixed solution is 2.5 wt% -10 wt%.
4. The preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation and control as claimed in claim 1, wherein the moisture-induced environmental humidity is 5-95% RH, and the induced self-assembly time is 2-48 h.
5. The preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation and control of claim 1 or 4, wherein the moisture-induced environmental humidity is 50-90% RH; the time for inducing cellulose self-assembly by water is 6-24 h.
6. The preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation and control of claim 1, wherein the monomer is any one of acrylic acid, acrylamide, methacrylic acid, methacrylamide, N-dimethylacrylamide, N-isopropylacrylamide, N-vinylcaprolactam, hydroxyethyl acrylate or hydroxyethyl methacrylate; the cross-linking agent is N, N' -methylene bisacrylamide or polyethylene glycol diacrylate; the photoinitiator is any one of 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone, diphenyl (2,4, 6-trimethylbenzoyl) phosphine oxide or 1-hydroxycyclohexyl phenyl ketone.
7. The preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation and control as claimed in claim 1 or 6, wherein the monomer is acrylamide, the crosslinking agent is N, N' -methylenebisacrylamide, and the photoinitiator is 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone.
8. The preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation and control as claimed in claim 1, wherein the concentration of the monomer is 2.8-11.2 mol/L, the addition amount of the cross-linking agent is 0.07 wt% -1.12 wt% of the mass of the monomer, and the addition amount of the photoinitiator is 0.15 wt% -2.7 wt% of the mass of the monomer.
9. The preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation and control as claimed in claim 1 or 8, wherein the concentration of the monomer is 5.6-8.4 mol/L, and the addition amounts of the cross-linking agent and the photoinitiator are 0.14 wt/% -0.84 wt/% and 0.45 wt/% -1.35 wt% of the monomer, respectively.
10. The preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation and control as claimed in claim 1, wherein the mass ratio of the soaking solution to the cellulose gel is 0.5: 1-5: 1, and the soaking time is 6-48 h.
11. The preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation and control of claim 1 or 10, wherein the mass ratio of the soaking solution to the cellulose gel is 1.5: 1-4.5: 1; the soaking time is 24-48 h.
12. The preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation and control as claimed in claim 1, wherein the mass ratio of the weighed soaking solution to the soaking solution for soaking is 4.8: 100-47.7: 100.
13. The preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation and control as claimed in claim 1 or 12, wherein the mass ratio of the weight of the soaking solution to the weight of the soaking solution for soaking is 14.3: 100-42.9: 100.
14. The preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation and control as claimed in claim 1, wherein the ultraviolet light power is 6-48W, and the polymerization time initiated by ultraviolet light is 0.5-2 h.
15. The preparation method of the tough and transparent hydrogel based on cellulose self-assembly regulation and control of claim 1 or 14, wherein the ultraviolet power is 36W; the polymerization time initiated by the ultraviolet light is 1-2 h.
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CN115850781A (en) * | 2022-12-02 | 2023-03-28 | 沈阳化工大学 | Preparation method of solution-driven efficient light-regulated alcohol gel |
CN116606401A (en) * | 2023-07-06 | 2023-08-18 | 天津永续新材料有限公司 | Cellulose nanocrystalline ion gel temperature sensor and preparation method thereof |
CN116606401B (en) * | 2023-07-06 | 2023-09-22 | 天津永续新材料有限公司 | Cellulose nanocrystalline ion gel temperature sensor and preparation method thereof |
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