CN112300336B - Self-repairing conductive hydrogel material and preparation method thereof - Google Patents
Self-repairing conductive hydrogel material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a self-repairing conductive hydrogel material and a preparation method thereof, wherein the method comprises the following steps: 1) Adding pyrogallic acid into the dissolved borate solution, stirring, adding polypyrrole powder, and stirring until the mixture is uniformly dispersed to obtain a mixed solution; 2) Mixing the mixed solution with an acrylamide monomer, a cross-linking agent and tetramethyl ethylenediamine, fully stirring to fully dissolve the mixed solution to obtain a reaction system, adding glycerol and an initiator into the reaction system, and standing at normal temperature to form gel. The invention utilizes the self-repairing capability of the DOPA formed by oxidizing pyrogallic acid under the action of oxygen and water, and the carbon black modified polypyrrole can be uniformly dispersed in water and provide conductivity. The prepared hydrogel has good mechanical property, conductivity and self-repairing property.
Description
Technical Field
The invention belongs to the technical field of hydrogel materials, and particularly relates to a self-repairing conductive hydrogel material and a preparation method thereof.
Background
The hydrogel is used as a soft polymer material containing a three-dimensional network structure and is widely applied in a plurality of fields, wherein the conductive hydrogel combines the advantages of conductive polymers and the hydrogel, and has huge application prospects in the fields of biological materials, laboratory biosensors, biofuel cells, supercapacitors and the like. However, many hydrogels have poor strength and toughness, and cannot meet the application requirements. And once the common conductive hydrogel is mechanically damaged, the service performance of the common conductive hydrogel is greatly influenced, so that the development of the conductive hydrogel material with certain strength and self-repairing capability has great significance for the application and development of the hydrogel.
The construction of self-healing hydrogels is based mainly on the dynamic reversible effects present in the polymer system. For example, hydrogen bond and acylhydrazone bond, which are chemical bond that can be synthesized and decomposed dynamically under certain condition, are used for realizing self-repairing property.
Most of the self-repairing conductive hydrogels reported at home and abroad are composed of an insulating hydrogel matrix and a functional conductive filler. Such as: the hydrogel is compounded with inorganic matters or conductive polymers with good conductivity such as carbon nano tubes and metal nano particles, and the results obtained by the researches play an important role in promoting the development of the self-repairing conductive hydrogel.
However, these self-repairing conductive hydrogels have some problems that are difficult to ignore, such as insufficient mechanical strength, poor self-repairing properties, and insufficient preparation method. And because the traditional self-repairing hydrogel with hydrogen bonds and acylhydrazone bonds completes the self-repairing process by generating the hydrogen bonds and the acylhydrazone bonds, the acting force strength of the hydrogen bonds and the acylhydrazone bonds is lower than that of catechol substances. In addition, there is another point that the conductive filler is generally poorly soluble in water, and the uniformity of dispersion in the hydrogel is insufficient, which directly affects the conductivity and mechanical properties of the conductive hydrogel. Therefore, the self-repairing conductive hydrogel material with excellent mechanical strength and functionality is prepared by a simple and easy method, the relation between the internal structure and each property is explored, and the systematic research on the aspects is significant.
Disclosure of Invention
The invention provides a self-repairing conductive hydrogel material and a preparation method thereof, which are used for overcoming the defects in the prior art, and the hydrogel prepared by the method has good mechanical property, conductivity and structural characteristics of good self-repairing property.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a self-repairing conductive hydrogel material, which comprises the following steps:
1) Adding pyrogallic acid into the dissolved borate solution, stirring, adding polypyrrole powder, and stirring until the mixture is uniformly dispersed to obtain a mixed solution;
2) Mixing the mixed solution with an acrylamide monomer, a cross-linking agent and tetramethyl ethylenediamine, fully stirring to fully dissolve the mixed solution to obtain a reaction system, adding glycerol and an initiator into the reaction system, and standing at normal temperature to form gel.
According to the preparation method of the invention, in the step 1), the pyrogallic acid concentration is between 2.5mg/ml and 5 mg/ml.
According to the preparation method of the present invention, in the step 1), the ratio of the amounts of the borate to the pyrogallic acid is (3-4): 1, preferably 3:1. pyrogallic acid is slightly toxic, and the borate is preferably more than 3:1, and pyrogallic acid.
According to the preparation method of the invention, in the step 1), after adding pyrogallic acid into the dissolved borate solution, stirring for 10-30min to fully react the pyrogallic acid and the borate solution, preferably stirring for 15min; the pyrogallic acid is oxidized under the action of air and water, and the combination of borate and pyrogallic acid can reduce the oxidation of the pyrogallic acid. The invention protects the pyrogallic acid by borate, and the reaction is a reversible reaction, so that the oxidation speed of the pyrogallic acid can be reduced.
According to the preparation method of the invention, in the step 1), the polypyrrole powder is carbon black doped polypyrrole powder, preferably, the mixture ratio is 20% by mass of polypyrrole (PPy) and 80% by mass of carbon black, and at this time, PPy and carbon black can be uniformly dispersed in water. The stirring time after the addition of the polypyrrole powder is preferably from 20 to 40s, more preferably 30s, without stirring too long, since borates precipitate the dispersed carbon black polypyrrole. The borate is selected from one or more of tetraborates such as sodium tetraborate and potassium tetraborate.
According to the preparation method of the invention, in the step 2), the cross-linking agent is selected from one or more of N, N-methylene bisacrylamide, N-vinyl bisacrylamide, methylene bisacrylamide and ethylene glycol dimethacrylate; and/or the initiator is selected from one or more of persulfates such as ammonium persulfate, potassium persulfate and sodium persulfate.
According to the preparation method of the invention, acrylamide in step 2): the mass ratio of the cross-linking agent to the initiator is 500:2 to 5:50 to 200, in a specific embodiment, said step 2) reaction is carried out in an ice-water bath.
The normal temperature of the invention is the same as the ambient temperature, and is generally 15-30 ℃.
The invention also provides the self-repairing conductive hydrogel material prepared by the preparation method.
The technical scheme provided by the invention has the following beneficial effects:
(1) The compound for realizing self-repair is pyrogallic acid and has three hydroxyl groups. The dopa-like substance produced after oxidation provides more crosslinking points. Making the gel more tightly bonded after self-healing.
(2) The invention selects the protective agent borate to protect pyrogallic acid, and the protective agent borate can be changed into a cross-linking agent along with the progress of the reaction. Thereby greatly improving the self-repairing capability of the gel and enhancing the strength of the gel.
(3) The material used for enhancing the gel strength and improving the conductivity is modified carbon black doped polypyrrole powder. The modified carbon black doped polypyrrole powder can be well dispersed in water, and the prepared gel has uniform performance. And the carbon black and polypyrrole can further enhance the mechanical property of the gel. And the polypyrrole can be degraded by ammonium persulfate in the gel to obtain small-particle polypyrrole, and the small-particle polypyrrole powder formed by decomposition can effectively shield ultraviolet light.
(4) The gel prepared by the invention has good self-repairing performance and can be instantaneously self-adhered under natural conditions. And can reach an ideal self-repairing effect within 8 hours, the self-repairing effect is better and better along with the time. And because of the glycerol, the gel is not easy to lose water under natural conditions, and can keep stable performance for a long time.
In conclusion, the self-repairing capability is provided by oxidizing the pyrogallic acid under the action of oxygen and water to form the dopa-containing substance, and the carbon black modified polypyrrole can be uniformly dispersed in water and provide conductivity. The prepared hydrogel has good mechanical property, conductivity and self-repairing property.
Drawings
FIG. 1 is an ultraviolet spectrum of the conductive hydrogel prepared in examples 1 and 4 and comparative example 1.
Fig. 2 is a schematic diagram showing stress mechanical properties of the conductive hydrogels prepared in example 1 and comparative examples 1 to 3.
FIG. 3 is a graph showing the conductivity of the conductive hydrogels prepared in example 1 and comparative examples 1-3.
FIG. 4 is a graph showing the self-healing properties of the hydrogels prepared in example 1.
Detailed Description
In order to better understand the technical solutions described above, the following detailed description of the technical solutions of the present application is provided by specific embodiments, and it should be understood that specific features of the embodiments and embodiments of the present application are detailed descriptions of the technical solutions of the present application, and not limiting the technical solutions of the present application, and the technical features of the embodiments and embodiments of the present application may be combined with each other without conflict. It is to be understood that the term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the examples of the present invention are commercially available or may be prepared by existing methods. The preparation method is described in detail below.
The main idea of the embodiment of the invention is as follows: a preparation method of a self-repairing conductive hydrogel material comprises the following steps:
1) Adding pyrogallic acid into the dissolved borate solution, stirring, adding polypyrrole powder, and stirring until the mixture is uniformly dispersed to obtain a mixed solution;
2) Mixing the mixed solution with an acrylamide monomer, a cross-linking agent and tetramethyl ethylenediamine, fully stirring to fully dissolve the mixed solution to obtain a reaction system, adding glycerol and an initiator into the reaction system, and standing at normal temperature to form gel.
The compound for realizing self-repair is pyrogallic acid and has three hydroxyl groups. The dopa-like substance produced after oxidation provides more crosslinking points. Making the gel adhere more tightly after self-healing, the reaction of which is shown in the following formula:
in addition, the sodium tetraborate, a protective agent used for protecting pyrogallic acid, is selected in the embodiment of the invention, and becomes a crosslinking agent from the protective agent as the reaction proceeds. Thereby greatly improving the self-repairing capability of the gel and enhancing the strength of the gel. The reaction is shown as follows:
example 1
(1) Firstly, 0.192g of sodium tetraborate is dissolved in 16ml of distilled water, after the sodium tetraborate is completely dissolved, 0.040g of pyrogallic acid is added into the solution, and stirring is carried out for 15min to enable the pyrogallic acid to fully react with the sodium tetraborate, and the pyrogallic acid is protected by the sodium tetraborate. The reaction is a reversible reaction, and can reduce the oxidation rate of pyrogallic acid.
(2) 0.04g of carbon black doped polypyrrole powder (the mass ratio of carbon black to polypyrrole is 4:1) is added into the mixed solution of pyrogallic acid and sodium tetraborate, and the mixture is fully stirred for 30 seconds, so that the mixture is uniformly dispersed. The carbon black-doped polypyrrole powder of this example was purchased from Sigma ALDRICH (Sigma-ALDRICH) and was prepared from 20% by mass polypyrrole (PPy) and 80% by mass carbon black, CAS number: 30604-81-0).
(3) The mixed solution obtained in (2) was transferred to an ice-water bath, 4g of acrylamide monomer, 0.016g of N, N-methylenebisacrylamide, and 50. Mu.l of tetramethylethylenediamine were added to the mixed solution, and the mixed solution was stirred sufficiently to dissolve all of them, after which 0.5ml of glycerin and 0.42g of ammonium persulfate were added, and the mixed solution was transferred and left to gel at room temperature of 20 ℃. The ice-water bath was set to reduce the reaction rate in a short time after the addition of ammonium persulfate. The reaction is shown as follows:
example 2
(1) Firstly, 0.3g of sodium tetraborate is dissolved in 16ml of distilled water, after the sodium tetraborate is completely dissolved, 0.070g of pyrogallic acid is added into the solution, and stirring is carried out for 30min to enable the pyrogallic acid to fully react with the sodium tetraborate, and the pyrogallic acid is protected by the sodium tetraborate. The reaction is a reversible reaction, and can reduce the oxidation rate of pyrogallic acid.
(2) 0.08g of carbon black doped polypyrrole powder (the mass ratio of carbon black to polypyrrole is 4:1) is added into the mixed solution of pyrogallic acid and sodium tetraborate, and the mixture is fully stirred for 40 seconds, so that the mixture is uniformly dispersed.
(3) The mixed solution obtained in (2) was transferred to an ice-water bath, and 4g of an acrylamide monomer, 0.025g of N, N-methylenebisacrylamide, and 100. Mu.l of tetramethylethylenediamine were added to the mixed solution and stirred sufficiently to dissolve all of them. Then, 1.0ml of glycerin and 0.80g of ammonium persulfate were added, and the mixture was transferred out and allowed to stand at room temperature of 20℃for gelation.
Example 3
(1) Firstly, 0.127g of potassium tetraborate is dissolved in 16ml of distilled water, after the potassium tetraborate is completely dissolved, 0.040g of pyrogallic acid is added into the solution, and stirring is carried out for 10min, so that the pyrogallic acid and the potassium tetraborate fully react.
(2) 0.04g of carbon black doped polypyrrole powder (the mass ratio of carbon black to polypyrrole is 4:1) is added into the mixed solution of the pyrogallic acid and the potassium tetraborate, and the mixture is fully stirred for 20s, so that the mixture is uniformly dispersed.
(3) The mixed solution obtained in (2) was transferred to an ice-water bath, and 4g of an acrylamide monomer, 0.0154g of ethylene glycol dimethacrylate, and 50. Mu.l of tetramethyl ethylenediamine were added to the mixed solution and stirred sufficiently to dissolve all of them. Then, 0.5ml of glycerin and 0.5g of ammonium persulfate were added, and the mixture was transferred out and allowed to stand at room temperature of 15℃for gelation.
Example 4
Example 4 is similar to example 1 except that sodium tetraborate is added in a molar ratio to pyrogallic acid of 4:1, namely, 0.256g of sodium tetraborate is dissolved in 16ml of distilled water, and 0.040g of pyrogallic acid is added to the solution after the sodium tetraborate is completely dissolved.
Comparative example 1
Comparative example 1 is similar to example 1, except that: sodium tetraborate was not added.
FIG. 1 is an ultraviolet spectrum of the conductive hydrogel prepared in examples 1 and 4 and comparative example 1. It can be seen that the molar ratio of sodium tetraborate to pyrogallic acid is 3:1 or 4:1, the oxidation peak of pyrogallic acid is lower, the molar ratio is 3:1, sodium tetraborate binds to pyrogallic acid optimally.
Comparative example 2
Comparative example 2 is similar to example 1, except that: sodium tetraborate and pyrogallic acid were not added.
Comparative example 3
Comparative example 3 is similar to example 1, except that: the carbon black doped polypyrrole powder was not added.
The prepared hydrogel is put into a mould to be manufactured into rectangular sheet gel, the length, the width and the gauge length of the rectangular sheet gel are measured, and a plastic film option of an instrument CMT6503 universal testing machine is used for tensile testing. FIG. 2 is a graph showing the stress mechanical properties of hydrogels prepared in example 1, comparative example 2 and comparative example 3. Comparative example 3, comparative example 1, comparative example 2 and example 1 are shown in order from left to right. From FIG. 2, it can be seen that the mechanical properties of the hydrogel prepared in example 1 of the present invention are optimal. FIG. 3 is a schematic diagram showing the conductivity of the conductive hydrogels prepared in example 1 and comparative examples 1-3, and the ordinate represents conductivity data; from the left to right, the conductivity of example 1 and comparative example 1, comparative example 2 and comparative example 3 are shown in order, and it can be seen that the hydrogel of example 1 of the present invention also has better conductivity. Fig. 4 is a schematic diagram showing the self-repairing property of the hydrogel prepared in example 1, wherein line a represents the mold placed for 2 days, the constant temperature and humidity box is placed for 3 days, line b represents the mold placed for 2 days, the constant temperature and humidity box is self-repaired for 3 days, the control group 1#, and line c represents the mold placed for 2 days, and the constant temperature and humidity box is self-repaired for 3 days, the control group 2#. It is further demonstrated that the hydrogel prepared in example 1 of the present invention has self-healing properties.
It should be apparent that the foregoing examples of the present invention are merely illustrative of the present invention and not limiting of the embodiments of the present invention, and that other and different forms of changes and modifications may be made by those skilled in the art based on the foregoing description, and it is not intended to be exhaustive of all embodiments, and all obvious changes and modifications that come within the scope of the invention are still within the scope of the invention.
Claims (11)
1. A preparation method of a self-repairing conductive hydrogel material is characterized by comprising the following steps: the method comprises the following steps:
1) Adding pyrogallic acid into the dissolved borate solution, stirring, adding polypyrrole powder, and stirring until the mixture is uniformly dispersed to obtain a mixed solution;
2) Mixing the mixed solution with an acrylamide monomer, a cross-linking agent and tetramethyl ethylenediamine, fully stirring to fully dissolve the mixed solution to obtain a reaction system, adding glycerol and an initiator into the reaction system, and standing at normal temperature to form gel.
2. The method for preparing the self-repairing conductive hydrogel material according to claim 1, wherein the method comprises the following steps: in step 1), the pyrogallic acid concentration is between 2.5mg/ml and 5 mg/ml.
3. The method for preparing a self-healing conductive hydrogel material according to claim 1 or 2, wherein: in the step 1), the ratio of the borate to the pyrogallic acid is (3-4): 1.
4. the method for preparing a self-healing conductive hydrogel material according to claim 3, wherein: in the step 1), the ratio of the borate to the pyrogallic acid is 3:1.
5. the method for preparing the self-repairing conductive hydrogel material according to claim 1, wherein the method comprises the following steps: in the step 1), pyrogallic acid is added into the dissolved borate solution and stirred for 10-30min to fully react the pyrogallic acid and the pyrogallic acid.
6. The method for preparing the self-repairing conductive hydrogel material according to claim 1, wherein the method comprises the following steps: in the step 1), the polypyrrole powder is carbon black doped polypyrrole powder, and the mass ratio of carbon black to polypyrrole is 4:1, a step of; and/or stirring for 20-40s after adding polypyrrole powder.
7. The method for preparing the self-repairing conductive hydrogel material according to claim 1, wherein the method comprises the following steps: in the step 1), the borate is selected from one or more of sodium tetraborate and potassium tetraborate.
8. The method for preparing the self-repairing conductive hydrogel material according to claim 1, wherein the method comprises the following steps: in the step 2), the cross-linking agent is selected from one or more of N, N-methylene bisacrylamide, N-vinyl bisacrylamide, methylene bisacrylamide and ethylene glycol dimethacrylate; and/or the initiator is selected from one or more of ammonium persulfate, potassium persulfate and sodium persulfate.
9. The method for preparing the self-repairing conductive hydrogel material according to claim 1, wherein the method comprises the following steps: in step 2), the acrylamide: crosslinking agent: the mass ratio of the initiator is 500:2 to 5:50 to 200.
10. The method for preparing a self-healing conductive hydrogel material according to claim 1, wherein the reaction in the step 2) is performed in an ice-water bath, and the reaction temperature is 0 ° -15 °.
11. A self-healing conductive hydrogel material prepared by the method of any one of claims 1-10.
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