CN113150325A - Preparation method of PVA/PAM composite hydrogel - Google Patents
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- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 111
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 111
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 50
- 238000000034 method Methods 0.000 claims abstract description 19
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 18
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- 238000003756 stirring Methods 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 13
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 7
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- 238000006243 chemical reaction Methods 0.000 claims description 5
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- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
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- 239000003999 initiator Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
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- 238000009864 tensile test Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
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- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
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- 229920003176 water-insoluble polymer Polymers 0.000 description 1
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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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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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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
- C08J2329/00—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 at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- 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
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- C08J2333/26—Homopolymers or copolymers of acrylamide or methacrylamide
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Abstract
The invention mainly relates to a preparation method of PVA/PAM composite hydrogel, which belongs to the technical field of hydrogel materials and is characterized in that free radical polymerization reaction is carried out between Acrylamide (AM) by a physical-chemical double-crosslinking method and a freezing-unfreezing method to form a chemically crosslinked Polyacrylamide (PAM) network; polyvinyl alcohol (PVA) molecular chains form a physically cross-linked PVA network through the interaction of hydrogen bonds, winding and the like, and finally a physical-chemical double cross-linked network system is obtained. The method has the advantages of low preparation cost, simple conditions and environmental friendliness, and the obtained composite hydrogel has good mechanical properties and has wide application prospects in the technical fields of biomedicine, agriculture, electronic industry and the like.
Description
Technical Field
The invention relates to the technical field of hydrogel materials, in particular to a preparation method of PVA/PAM composite hydrogel.
Background
The polymer hydrogel is a soft and wet material and is a hydrophilic three-dimensional network structure. Meanwhile, the composite material has good mechanical properties, good biocompatibility and the like. Meanwhile, the hydrogel is a water-insoluble polymer, has strong water absorption, can swell after absorbing water, and can still keep the stable structure after swelling. In addition, it can sense the tiny stimuli of the external environment, such as light, electricity, temperature, pH, magnetic field, etc., and the swelling is the response to the external stimuli. By utilizing the characteristics, the hydrogel has wide application prospect in the aspects of manufacturing ion transmission membranes, sensors, controlled release switches, drug carriers, high water retention materials and the like.
Since the hydrogel can respond to weak external stimulation, the hydrogel has great application value in recent years. In medical treatment, the hydrogel can respond to the change of external temperature, and the temperature-sensitive hydrogel is used as a drug carrier to realize the intelligent release of drugs. In addition, the hydrogel can also be applied to the aspect of optical materials, and the photoresponse polymer gel is a new branch in the recent light-sensitive polymer materials, is formed by volume phase transition due to light stimulation, and is mainly applied to the preparation of novel polymer materials such as cell release, light-adjusting materials and intelligent drive. At present, the mechanical properties of the hydrogel are poor, and the mechanical properties are mainly determined by tensile, compression, tear and other properties. In order to improve the mechanical properties of the hydrogel, the double-network hydrogel is researched. The double-network hydrogel is a network structure formed by interpenetrating two asymmetric polymers. Polyvinyl alcohol (PVA) and Polyacrylamide (PAM) are used as raw materials to be polymerized to prepare the polyvinyl alcohol/polyacrylamide (PVA/PAM) double-network composite hydrogel, so that the hydrogel with a double-network cross-linked structure is formed, and the performances of the hydrogel in the aspects of water absorption speed, toughness, swelling and the like are enhanced.
Disclosure of Invention
The invention aims to provide a preparation method of PVA/PAM composite hydrogel; the method can effectively solve the technical problems in the preparation of the existing composite hydrogel.
The invention adopts the following technical scheme to realize the purpose and comprises the following steps:
1) taking a proper amount of polyvinyl alcohol (PVA) as a raw material, mixing the PVA with a proper amount of vinyltriethoxysilane to prepare an aqueous solution, and uniformly stirring.
2) And then placing the mixed solution in a water bath kettle at the temperature of 80-100 ℃, sealing, stirring and heating for 3-5 hours to dissolve polyvinyl alcohol (PVA), cooling and storing the mixed solution.
3) Taking a proper amount of methylene bisacrylamide to prepare an aqueous solution, and preparing a proper amount of potassium persulfate to prepare an aqueous solution.
4) And sequentially adding the methylene bisacrylamide aqueous solution and the potassium persulfate aqueous solution into a mixed solution of polyvinyl alcohol (PVA), uniformly stirring and cooling to room temperature.
5) Taking a proper amount of Acrylamide (AM), magnetically stirring for 1-2h, and putting the mixture into an ultrasonic cleaning machine for ultrasonic treatment for 30-60min to remove bubbles to form a uniform composite transparent aqueous solution of polyvinyl alcohol (PVA) and Polyacrylamide (PAM).
6) And transferring the prepared solution into a mold, completely sealing the surface of the mold by using an organic glass sheet, putting the mold into a sealed freshness protection package to prevent water loss, putting the mold into an oven at 80 ℃ for reaction for 1h, then putting the mold into a sealed environment at-20 ℃ for freezing for 12h, unfreezing the mold at room temperature for 2h, and repeating the freezing-unfreezing process for 5-10 times to prepare the polyvinyl alcohol/polyacrylamide (PVA/PAM) hybrid double-network composite hydrogel.
Further, the mass fraction of polyvinyl alcohol (PVA) in the step 1) is as follows: 1 to 10 percent of the total weight of the raw materials, and 0.5 to 2 percent of the mass fraction of the vinyl triethoxysilane.
Further, the mass ratio of polyvinyl alcohol (PVA) to vinyltriethoxysilane in step 1) is 0.5-5: 1.
further, the mass ratio of the potassium sulfate to the methylene bisacrylamide in the step 3) is 0.5-1: 1.
furthermore, the mass ratio of the Acrylamide (AM), the potassium persulfate and the methylene bisacrylamide in the mixed solution in the step 4) is 1: 0.5-1: 1.
further, the length of the mold is 100-150mm, the width is 100-150mm, and the height is 3.5-10 mm.
The invention has the following gain effects:
1) compared with single-network hydrogel, the PVA/PAM composite hydrogel has better mechanical strength, biocompatibility and water absorption.
2) The PVA/PAM composite hydrogel is more sensitive to the change of tiny force.
3) Compared with single-network hydrogel, the PVA/PAM composite hydrogel has the advantages that the swelling balance is achieved, and the composite hydrogel has higher swelling ratio, namely better water retention performance.
4) Compared with other methods, the method has the characteristics of simple process, low raw material cost, environmental friendliness and convenience in operation, and the preparation process is simple and the yield of the product is high.
5) The prepared composite gel can be widely applied to the fields of biomedicine, agriculture, industry and the like.
Detailed Description
Further analysis was performed in conjunction with specific examples, including the following examples.
Example one
1) Preparing 35g of deionized water solution from 1g of polyvinyl alcohol (PVA) and 1g of vinyltriethoxysilane, mixing and stirring uniformly, sealing, stirring and heating for 3 hours at 95 ℃ in a water bath kettle to dissolve the polyvinyl alcohol (PVA), and cooling to 50 ℃ to obtain the polyvinyl alcohol (PVA) aqueous solution.
2) And (3) taking 5g of methylene Bisacrylamide (BIS) aqueous solution and 5g of potassium persulfate (KPS) aqueous solution, sequentially adding the aqueous solution into the polyvinyl alcohol (PVA) aqueous solution, uniformly stirring, and cooling to room temperature to obtain a mixed polyvinyl alcohol (PVA) aqueous solution.
3) And adding 5g of Acrylamide (AM) into the mixed aqueous solution of polyvinyl alcohol (PVA), uniformly stirring for 1h, placing the mixture into an ultrasonic cleaning machine for ultrasonic treatment for 30min, and removing bubbles to obtain the uniform composite transparent aqueous solution of polyvinyl alcohol (PVA) and Polyacrylamide (PAM).
4) And transferring the prepared solution into a mold, sealing the surface of the mold by using an organic glass sheet, putting the mold into a sealed freshness protection bag to prevent water loss, putting the mold into an oven with the temperature of 80 ℃ for reaction for 1h, then putting the mold into a sealed environment with the temperature of-20 ℃ for freezing for 12h, unfreezing the mold at room temperature for 2h, and repeating the freezing-unfreezing process for 5 times to prepare the polyvinyl alcohol/polyacrylamide (PVA/PAM) hybrid double-network composite hydrogel.
5) In order to further study the mechanical properties of the composite hydrogel, the composite hydrogel was subjected to tensile testing, and the results are shown in FIGS. 1-2. Taking hydrogel mixed with PVA (2%, 6% and 10%) and PAM with different masses as an experimental object; FIGS. 1 and 2 show the tensile elastic modulus and tensile strength of 4 gels, respectively. When PVA is added, the double-network composite gel has better tensile property as shown in figures 1-2, and the tensile strength of the PVA/PAM double-network hydrogel can reach 434kPa to 8.7 times that of PAM single-network gel (50 kPa). The elastic modulus E of the PVA/PAM double-network hydrogel can reach up to 409kPa, which is 6.0 times of that of PAM single-network gel (68 kPa).
Example two
1) Preparing 35g of deionized water solution from 3g of polyvinyl alcohol (PVA) and 1g of vinyltriethoxysilane, mixing and stirring uniformly, sealing, stirring and heating for 3 hours at 95 ℃ in a water bath kettle to dissolve the polyvinyl alcohol (PVA), and cooling to 50 ℃ to obtain the polyvinyl alcohol (PVA) aqueous solution.
2) And (3) taking 5g of methylene Bisacrylamide (BIS) aqueous solution and 5g of potassium persulfate (KPS) aqueous solution, sequentially adding the aqueous solution into the polyvinyl alcohol (PVA) aqueous solution, uniformly stirring, and cooling to room temperature to obtain a mixed polyvinyl alcohol (PVA) aqueous solution.
3) And adding 5g of Acrylamide (AM) into the mixed aqueous solution of polyvinyl alcohol (PVA), uniformly stirring for 1h, placing the mixture into an ultrasonic cleaning machine for ultrasonic treatment for 30min, and removing bubbles to obtain the uniform composite transparent aqueous solution of polyvinyl alcohol (PVA) and Polyacrylamide (PAM).
4) And transferring the prepared solution into a mold, sealing the surface of the mold by using an organic glass sheet, putting the mold into a sealed freshness protection bag to prevent water loss, putting the mold into an oven with the temperature of 80 ℃ for reaction for 1h, then putting the mold into a sealed environment with the temperature of-20 ℃ for freezing for 12h, unfreezing the mold at room temperature for 2h, and repeating the freezing-unfreezing process for 5 times to prepare the polyvinyl alcohol/polyacrylamide (PVA/PAM) hybrid double-network composite hydrogel.
5) In order to further study the mechanical properties of the composite hydrogel, the composite hydrogel was subjected to tensile testing, and the results are shown in FIGS. 1-2. Taking hydrogel mixed with PVA (2%, 6% and 10%) and PAM with different masses as an experimental object; FIGS. 1 and 2 show the tensile elastic modulus and tensile strength of 4 gels, respectively. As can be seen from FIGS. 1-2, the mechanical properties of the gel are further improved due to the formation of crystallites between the PVA chains, which further strengthen the gel network as the density and size of the crystallites increases. With the increase of the content of PVA in the gel network, PVA can form microcrystals and can interact with PAM through hydrogen bonds to play a role of multiple physical cross-linking points.
EXAMPLE III
1) Preparing 35g of deionized water solution from 5g of polyvinyl alcohol (PVA) and 1g of vinyltriethoxysilane, mixing and stirring uniformly, sealing, stirring and heating for 3 hours at 95 ℃ in a water bath kettle to dissolve the polyvinyl alcohol (PVA), and cooling to 50 ℃ to obtain the polyvinyl alcohol (PVA) aqueous solution.
2) And (3) taking 5g of methylene Bisacrylamide (BIS) aqueous solution and 5g of potassium persulfate (KPS) aqueous solution, sequentially adding the aqueous solution into the polyvinyl alcohol (PVA) aqueous solution, uniformly stirring, and cooling to room temperature to obtain a mixed polyvinyl alcohol (PVA) aqueous solution.
3) And adding 5g of Acrylamide (AM) into the mixed aqueous solution of polyvinyl alcohol (PVA), uniformly stirring for 1h, placing the mixture into an ultrasonic cleaning machine for ultrasonic treatment for 30min, and removing bubbles to obtain the uniform composite transparent aqueous solution of polyvinyl alcohol (PVA) and Polyacrylamide (PAM).
4) And transferring the prepared solution into a mold, sealing the surface of the mold by using an organic glass sheet, putting the mold into a sealed freshness protection bag to prevent water loss, putting the mold into an oven with the temperature of 80 ℃ for reaction for 1h, then putting the mold into a sealed environment with the temperature of-20 ℃ for freezing for 12h, unfreezing the mold at room temperature for 2h, and repeating the freezing-unfreezing process for 5 times to prepare the polyvinyl alcohol/polyacrylamide (PVA/PAM) hybrid double-network composite hydrogel.
5) In order to further study the mechanical properties of the composite hydrogel, the composite hydrogel was subjected to tensile testing, and the results are shown in FIGS. 1-2. Taking hydrogel mixed with PVA (2%, 6% and 10%) and PAM with different masses as an experimental object; FIGS. 1 and 2 show the tensile elastic modulus and tensile strength of 4 gels, respectively. As shown in FIG. 2, as the amount of PVA added increases, the strength of the gel increases sharply first and then decreases slightly. At a concentration of 6% in the PVA solution, the gel strength reached a maximum (434 kPa). The result shows that a small amount of PVA is added to form microcrystalline crosslinking points in the PAM single network, so that the tensile modulus and the tensile strength are greatly improved, and the gel network is strengthened.
Claims (8)
1. A preparation method of PVA/PAM composite hydrogel is characterized in that the preparation method of the composite hydrogel comprises the following steps:
1) taking a proper amount of polyvinyl alcohol (PVA) and a proper amount of vinyltriethoxysilane, and uniformly mixing and stirring to prepare an aqueous solution. And then placing the mixed solution in a water bath kettle at the temperature of 80-100 ℃, sealing, stirring and heating for 3-5 hours to dissolve polyvinyl alcohol (PVA), cooling and storing the mixed solution.
2) Taking a proper amount of methylene bisacrylamide to prepare an aqueous solution, and preparing a proper amount of potassium persulfate to prepare an aqueous solution. Sequentially adding the prepared solution into the mixed solution in the step 1). And taking a proper amount of Acrylamide (AM), magnetically stirring for 1-2h, and placing the mixture into an ultrasonic cleaning machine to remove bubbles by ultrasonic treatment for 30-60min to form a uniform and transparent composite aqueous solution of polyvinyl alcohol (PVA) and Polyacrylamide (PAM).
3) And transferring the prepared solution into a mold, sealing the surface of the mold by using an organic glass sheet, putting the mold into a sealed freshness protection bag to prevent water loss, putting the mold into an oven at 80 ℃ for reaction for 1h, then putting the mold into a sealed environment at-20 ℃ for freezing for 12h, unfreezing the mold at room temperature for 2h, and repeating the freezing-unfreezing process for 5-10 times to prepare the polyvinyl alcohol/polyacrylamide (PVA/PAM) hybrid double-network composite hydrogel.
2. The method for preparing PVA/PAM composite hydrogel according to claim 1, wherein the raw materials are polyvinyl alcohol (PVA) and Acrylamide (AM).
3. The method for preparing PVA/PAM composite hydrogel according to claim 1, wherein the coupling agent is vinyltriethoxysilane.
4. The method for preparing PVA/PAM composite hydrogel according to claim 1, wherein the required cross-linking agent is methylene bisacrylamide.
5. The method for preparing PVA/PAM composite hydrogel according to claim 1, wherein the initiator is potassium persulfate (KPS).
6. The method for preparing the PVA/PAM composite hydrogel according to claim 1, wherein the mass fraction of the polyvinyl alcohol (PVA) in the step 1) is as follows: 1 to 10 percent of the total weight of the raw materials, and 0.5 to 2 percent of the mass fraction of the vinyl triethoxysilane.
7. The method for preparing PVA/PAM composite hydrogel according to claim 1, wherein the mass ratio of the polyvinyl alcohol (PVA) to the vinyltriethoxysilane in the step 1) is 0.5-5: 1.
8. the method for preparing PVA/PAM composite hydrogel according to claim 1, wherein the mass ratio of Acrylamide (AM), potassium persulfate and methylene bisacrylamide in the step 2) is 1: 0.5-1: 1.
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| CN113716909A (en) * | 2021-08-11 | 2021-11-30 | 绍兴职业技术学院 | Method for preparing high-elastic-modulus water-permeable mortar based on urban building waste |
| CN114031879A (en) * | 2021-11-24 | 2022-02-11 | 浙江省海洋水产研究所 | Hydrogel for marine antifouling and preparation method thereof |
| CN114478923A (en) * | 2022-03-22 | 2022-05-13 | 青岛科技大学 | High-toughness anti-freezing conductive hydrogel and preparation method thereof |
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| CN114031879A (en) * | 2021-11-24 | 2022-02-11 | 浙江省海洋水产研究所 | Hydrogel for marine antifouling and preparation method thereof |
| CN114031879B (en) * | 2021-11-24 | 2023-01-03 | 浙江省海洋水产研究所 | Hydrogel for marine antifouling and preparation method thereof |
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