CN112876603A - Preparation method of intelligent temperature-sensitive hydrogel - Google Patents
Preparation method of intelligent temperature-sensitive hydrogel Download PDFInfo
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- CN112876603A CN112876603A CN202110053657.4A CN202110053657A CN112876603A CN 112876603 A CN112876603 A CN 112876603A CN 202110053657 A CN202110053657 A CN 202110053657A CN 112876603 A CN112876603 A CN 112876603A
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Abstract
The invention provides a preparation method of intelligent temperature-sensitive hydrogel. The preparation steps are as follows: preparing hydrophobic modified sericite; drying, keeping the vacuum state, and cooling to room temperature; adding cyclohexanone and mixed solution carrying methyl methacrylate, and stirring and dispersing; vacuumizing and maintaining pressure; washing, centrifuging and drying to obtain a product A; preparing modified graphene oxide; dispersing the product A and the modified graphene oxide in cyclohexanone, adding dibenzoyl peroxide and stirring; pre-polymerizing after ultrasonic treatment, and polymerizing; replacing cyclohexanone with ethanol, and freeze-drying to obtain sericite loaded graphene oxide; adding deionized water, N-isopropyl acrylamide, N-N 'methylene bisacrylamide, potassium persulfate and N-N-N-N' tetramethyl ethylenediamine, carrying out ultrasonic treatment in an ice bath until the solution becomes uniform, and reacting to obtain the intelligent temperature-sensitive hydrogel. The intelligent temperature-sensitive hydrogel prepared by the invention has good water absorption rate and higher expansion ratio, and has the best effect at 20 ℃.
Description
Technical Field
The invention relates to the field of materials, in particular to a preparation method of intelligent temperature-sensitive hydrogel.
Background
Hydrogels are a class of crosslinked polymers that have a three-dimensional network structure in space, swell in water and retain a large amount of water without dissolving. Since water can exist in the polymer network in the form of bound water, free water, and the like, and loses its fluidity, the polymer hydrogel can always maintain a certain structural form in water. Hydrogels of poly-N-isopropylacrylamide are one of the most studied stimuli-responsive systems, belonging to the so-called smart materials. When the environmental temperature changes around the volume phase transition temperature, the properties of the poly-N-isopropylacrylamide hydrogel can be mutated, and based on the characteristics, the poly-N-isopropylacrylamide hydrogel has wide application prospects in the aspects of intelligent science and technology, new energy materials and the like.
Disclosure of Invention
The technical problem to be solved is as follows: the invention aims to provide a preparation method of intelligent temperature-sensitive hydrogel, and the prepared intelligent temperature-sensitive hydrogel has good water absorption rate, higher expansion ratio and optimal effect at 20 ℃.
The technical scheme is as follows: a preparation method of intelligent temperature-sensitive hydrogel comprises the following steps:
(1) dissolving 1-2g of sodium laurate in 50mL of water to obtain a sodium laurate aqueous solution, adding 0.5g of sericite, magnetically stirring for 48 hours at 20 ℃, centrifuging, and washing with deionized water to obtain hydrophobic modified sericite;
(2) drying at 100 deg.C in a single-neck bottle, and maintaining vacuum state until the temperature is reduced to room temperature;
(3) adding cyclohexanone and mixed solution carrying methyl methacrylate, and stirring and dispersing;
(4) vacuumizing for 20-30min, and maintaining the pressure for 30-40 min;
(5) transferring the mixture into a centrifuge tube, repeatedly washing the mixture by using acetone, centrifuging the mixture, and putting the mixture into an oven to dry the mixture to constant weight to obtain a product A;
(6) pouring 100mL of graphene oxide aqueous dispersion into a beaker, adding 20mL of absolute ethanol solution of KH560, stirring for 10min at room temperature, and carrying out ultrasonic treatment for 2 h;
(7) polymerizing in an oil bath at 50-80 ℃, cooling, and washing with deionized water to obtain modified graphene oxide;
(8) respectively dispersing the product A and the modified graphene oxide in 20-30mL of cyclohexanone, mixing the product A and the modified graphene oxide, adding 0.1g of dibenzoyl peroxide into the mixture, and stirring;
(9) ultrasonic processing for 2h, transferring into a four-neck flask, heating, introducing nitrogen, pre-polymerizing at 75 ℃ for 1.5-2h, and polymerizing under 50-100 ℃ oil bath for 1.5-2 h;
(10) replacing cyclohexanone with ethanol, and freeze-drying to obtain sericite loaded graphene oxide;
(11) adding deionized water to obtain a sericite loaded graphene oxide solution, adding 1.695g N-isopropyl acrylamide, 0.231g N-N 'methylene bisacrylamide, 0.027g potassium persulfate and 0.04mL N-N-N' tetramethyl ethylenediamine into an ice bath, carrying out ultrasonic treatment under the ice bath until the solution becomes uniform, and reacting for 20-24h to obtain the intelligent temperature-sensitive hydrogel.
Further, the mass ratio of the cyclohexanone to the methyl methacrylate in the step (3) is 1: 1.
Further, the concentration of the absolute ethyl alcohol solution of KH560 in the step (6) is 0.5 mg/mL.
Further, the concentration of the sericite-loaded graphene oxide solution in the step (11) is 5-10 mg/mL.
Description of the drawings:
FIG. 1 is a graph showing the results of water absorption rates (swelling ratios) in examples 1 to 5.
Has the advantages that:
1. sericite with methyl methacrylate loaded in the inner space is mixed with graphene oxide modified by KH560 to prepare sericite-graphene aerogel, and sericite uniformly exists among graphene oxide lamella to form a semi-hybrid three-dimensional network structure.
2. According to the invention, N-isopropyl acrylamide is used as a monomer, sericite loaded graphene oxide is used as an additive, and the prepared graphene composite hydrogel has good water absorption and expansion ratio.
3. The concentration of the sericite loaded graphene oxide has a certain influence on the water absorption rate. With the change of the concentration of the sericite loaded graphene oxide, the physical crosslinking among the sericite loaded graphene oxide nano sheets hinders the diffusion of water, so that the water absorption rate is reduced.
Detailed Description
Example 1
A preparation method of intelligent temperature-sensitive hydrogel comprises the following steps:
(1) dissolving 1g of sodium laurate in 50mL of water to obtain a sodium laurate aqueous solution, adding 0.5g of sericite, magnetically stirring for 48 hours at the temperature of 20 ℃, centrifuging, and washing with deionized water to obtain hydrophobic modified sericite;
(2) drying at 100 deg.C in a single-neck bottle, and maintaining vacuum state until the temperature is reduced to room temperature;
(3) adding a mixed solution of cyclohexanone and methyl methacrylate, and stirring and dispersing, wherein the mass ratio of cyclohexanone to methyl methacrylate is 1: 1;
(4) vacuumizing for 20min, and maintaining the pressure for 30 min;
(5) transferring the mixture into a centrifuge tube, repeatedly washing the mixture by using acetone, centrifuging the mixture, and putting the mixture into an oven to dry the mixture to constant weight to obtain a product A;
(6) pouring 100mL of graphene oxide aqueous dispersion into a beaker, adding 20mL of 0.5mg/mL KH560 absolute ethanol solution, stirring at room temperature for 10min, and performing ultrasonic treatment for 2 h;
(7) polymerizing in an oil bath at 50 ℃, cooling, and washing with deionized water to obtain modified graphene oxide;
(8) respectively dispersing the product A and the modified graphene oxide in 20mL of cyclohexanone, mixing the product A and the modified graphene oxide, adding 0.1g of dibenzoyl peroxide into the mixture, and stirring;
(9) ultrasonic treatment is carried out for 2h, then the mixture is transferred into a four-neck flask, heated and introduced with nitrogen, prepolymerized for 1.5h at 75 ℃, and then polymerized for 1.5h under 50 ℃ oil bath;
(10) replacing cyclohexanone with ethanol, and freeze-drying to obtain sericite loaded graphene oxide;
(11) adding deionized water to obtain a sericite loaded graphene oxide solution with the concentration of 5mg/mL, adding 1.695g N-isopropyl acrylamide, 0.231g N-N 'methylene bisacrylamide, 0.027g potassium persulfate and 0.04mL N-N-N-N' tetramethyl ethylenediamine into an ice bath, performing ultrasonic treatment under the ice bath until the solution becomes uniform, and reacting for 20 hours to obtain the intelligent temperature-sensitive hydrogel.
Example 2
A preparation method of intelligent temperature-sensitive hydrogel comprises the following steps:
(1) dissolving 1.2g of sodium laurate in 50mL of water to obtain a sodium laurate aqueous solution, adding 0.5g of sericite, magnetically stirring for 48 hours at the temperature of 20 ℃, centrifuging, and washing with deionized water to obtain hydrophobic modified sericite;
(2) drying at 100 deg.C in a single-neck bottle, and maintaining vacuum state until the temperature is reduced to room temperature;
(3) adding a mixed solution of cyclohexanone and methyl methacrylate, and stirring and dispersing, wherein the mass ratio of cyclohexanone to methyl methacrylate is 1: 1;
(4) vacuumizing for 23min, and maintaining the pressure for 33 min;
(5) transferring the mixture into a centrifuge tube, repeatedly washing the mixture by using acetone, centrifuging the mixture, and putting the mixture into an oven to dry the mixture to constant weight to obtain a product A;
(6) pouring 100mL of graphene oxide aqueous dispersion into a beaker, adding 20mL of 0.5mg/mL KH560 absolute ethanol solution, stirring at room temperature for 10min, and performing ultrasonic treatment for 2 h;
(7) polymerizing in an oil bath at 60 ℃, cooling, and washing with deionized water to obtain modified graphene oxide;
(8) respectively dispersing the product A and the modified graphene oxide in 25mL of cyclohexanone, mixing the product A and the modified graphene oxide, adding 0.1g of dibenzoyl peroxide into the mixture, and stirring;
(9) ultrasonic treatment is carried out for 2h, then the mixture is transferred into a four-neck flask, heated and introduced with nitrogen, prepolymerized for 1.5h at 75 ℃, and then polymerized for 1.5h under oil bath at 60 ℃;
(10) replacing cyclohexanone with ethanol, and freeze-drying to obtain sericite loaded graphene oxide;
(11) adding deionized water to obtain a sericite loaded graphene oxide solution with the concentration of 6mg/mL, adding 1.695g N-isopropyl acrylamide, 0.231g N-N 'methylene bisacrylamide, 0.027g potassium persulfate and 0.04mL N-N-N-N' tetramethyl ethylenediamine into an ice bath, performing ultrasonic treatment under the ice bath until the solution becomes uniform, and reacting for 21 hours to obtain the intelligent temperature-sensitive hydrogel.
Example 3
A preparation method of intelligent temperature-sensitive hydrogel comprises the following steps:
(1) dissolving 1.5g of sodium laurate in 50mL of water to obtain a sodium laurate aqueous solution, adding 0.5g of sericite, magnetically stirring for 48 hours at the temperature of 20 ℃, centrifuging, and washing with deionized water to obtain hydrophobic modified sericite;
(2) drying at 100 deg.C in a single-neck bottle, and maintaining vacuum state until the temperature is reduced to room temperature;
(3) adding a mixed solution of cyclohexanone and methyl methacrylate, and stirring and dispersing, wherein the mass ratio of cyclohexanone to methyl methacrylate is 1: 1;
(4) vacuumizing for 25min, and maintaining the pressure for 35 min;
(5) transferring the mixture into a centrifuge tube, repeatedly washing the mixture by using acetone, centrifuging the mixture, and putting the mixture into an oven to dry the mixture to constant weight to obtain a product A;
(6) pouring 100mL of graphene oxide aqueous dispersion into a beaker, adding 20mL of 0.5mg/mL KH560 absolute ethanol solution, stirring at room temperature for 10min, and performing ultrasonic treatment for 2 h;
(7) polymerizing in an oil bath at 65 ℃, cooling, and washing with deionized water to obtain modified graphene oxide;
(8) respectively dispersing the product A and the modified graphene oxide in 25mL of cyclohexanone, mixing the product A and the modified graphene oxide, adding 0.1g of dibenzoyl peroxide into the mixture, and stirring;
(9) ultrasonic treatment is carried out for 2h, then the mixture is transferred into a four-neck flask, heated and introduced with nitrogen, prepolymerized for 2h at 75 ℃, and then polymerized for 2h under the oil bath of 75 ℃;
(10) replacing cyclohexanone with ethanol, and freeze-drying to obtain sericite loaded graphene oxide;
(11) adding deionized water to obtain a sericite loaded graphene oxide solution with the concentration of 8mg/mL, adding 1.695g N-isopropyl acrylamide, 0.231g N-N 'methylene bisacrylamide, 0.027g potassium persulfate and 0.04mL N-N-N-N' tetramethyl ethylenediamine into an ice bath, performing ultrasonic treatment under the ice bath until the solution becomes uniform, and reacting for 22 hours to obtain the intelligent temperature-sensitive hydrogel.
Example 4
A preparation method of intelligent temperature-sensitive hydrogel comprises the following steps:
(1) dissolving 1.8g of sodium laurate in 50mL of water to obtain a sodium laurate aqueous solution, adding 0.5g of sericite, magnetically stirring for 48 hours at the temperature of 20 ℃, centrifuging, and washing with deionized water to obtain hydrophobic modified sericite;
(2) drying at 100 deg.C in a single-neck bottle, and maintaining vacuum state until the temperature is reduced to room temperature;
(3) adding a mixed solution of cyclohexanone and methyl methacrylate, and stirring and dispersing, wherein the mass ratio of cyclohexanone to methyl methacrylate is 1: 1;
(4) vacuumizing for 25min, and maintaining the pressure for 35 min;
(5) transferring the mixture into a centrifuge tube, repeatedly washing the mixture by using acetone, centrifuging the mixture, and putting the mixture into an oven to dry the mixture to constant weight to obtain a product A;
(6) pouring 100mL of graphene oxide aqueous dispersion into a beaker, adding 20mL of 0.5mg/mL KH560 absolute ethanol solution, stirring at room temperature for 10min, and performing ultrasonic treatment for 2 h;
(7) polymerizing in an oil bath at 70 ℃, cooling, and washing with deionized water to obtain modified graphene oxide;
(8) respectively dispersing the product A and the modified graphene oxide in 25mL of cyclohexanone, mixing the product A and the modified graphene oxide, adding 0.1g of dibenzoyl peroxide into the mixture, and stirring;
(9) ultrasonic treatment is carried out for 2h, then the mixture is transferred into a four-neck flask, heated and introduced with nitrogen, prepolymerized for 2h at 75 ℃, and then polymerized for 2h under 90 ℃ oil bath;
(10) replacing cyclohexanone with ethanol, and freeze-drying to obtain sericite loaded graphene oxide;
(11) adding deionized water to obtain a sericite loaded graphene oxide solution with the concentration of 9mg/mL, adding 1.695g N-isopropyl acrylamide, 0.231g N-N 'methylene bisacrylamide, 0.027g potassium persulfate and 0.04mL N-N-N-N' tetramethyl ethylenediamine into an ice bath, performing ultrasonic treatment under the ice bath until the solution becomes uniform, and reacting for 23h to obtain the intelligent temperature-sensitive hydrogel.
Example 5
A preparation method of intelligent temperature-sensitive hydrogel comprises the following steps:
(1) dissolving 2g of sodium laurate in 50mL of water to obtain a sodium laurate aqueous solution, adding 0.5g of sericite, magnetically stirring for 48 hours at the temperature of 20 ℃, centrifuging, and washing with deionized water to obtain hydrophobic modified sericite;
(2) drying at 100 deg.C in a single-neck bottle, and maintaining vacuum state until the temperature is reduced to room temperature;
(3) adding a mixed solution of cyclohexanone and methyl methacrylate, and stirring and dispersing, wherein the mass ratio of cyclohexanone to methyl methacrylate is 1: 1;
(4) vacuumizing for 30min, and maintaining the pressure for 40 min;
(5) transferring the mixture into a centrifuge tube, repeatedly washing the mixture by using acetone, centrifuging the mixture, and putting the mixture into an oven to dry the mixture to constant weight to obtain a product A;
(6) pouring 100mL of graphene oxide aqueous dispersion into a beaker, adding 20mL of 0.5mg/mL KH560 absolute ethanol solution, stirring at room temperature for 10min, and performing ultrasonic treatment for 2 h;
(7) polymerizing in an oil bath at 50-80 ℃, cooling, and washing with deionized water to obtain modified graphene oxide;
(8) respectively dispersing the product A and the modified graphene oxide in 30mL of cyclohexanone, mixing the product A and the modified graphene oxide, adding 0.1g of dibenzoyl peroxide into the mixture, and stirring;
(9) ultrasonic treatment is carried out for 2h, then the mixture is transferred into a four-neck flask, heated and introduced with nitrogen, prepolymerized for 2h at 75 ℃, and then polymerized for 2h under 100 ℃ oil bath;
(10) replacing cyclohexanone with ethanol, and freeze-drying to obtain sericite loaded graphene oxide;
(11) adding deionized water to obtain a sericite loaded graphene oxide solution with the concentration of 10mg/mL, adding 1.695g N-isopropyl acrylamide, 0.231g N-N 'methylene bisacrylamide, 0.027g potassium persulfate and 0.04mL N-N-N-N' tetramethyl ethylenediamine into an ice bath, performing ultrasonic treatment under the ice bath until the solution becomes uniform, and reacting for 24 hours to obtain the intelligent temperature-sensitive hydrogel.
The test method comprises the following steps:
determination of Water absorption Rate: weighing the xerogel and recording the mass W0Putting it into pure water at 20 ℃,the mass W was measured every 30min, and the surface water was first blotted with weighing paper and then weighed. The water absorption rate is expressed by the expansion ratio, and the formula is as follows:
testing of temperature sensitivity: taking dry gel and recording mass W0Then, the mixture is placed in pure water at 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃ and 45 ℃ respectively, and is taken out after water absorption balance, and the mass We is called. And recording the data. The expansion ratio is calculated as follows:
TABLE 1
Claims (4)
1. The preparation method of the intelligent temperature-sensitive hydrogel is characterized by comprising the following steps:
(1) dissolving 1-2g of sodium laurate in 50mL of water to obtain a sodium laurate aqueous solution, adding 0.5g of sericite, magnetically stirring for 48 hours at 20 ℃, centrifuging, and washing with deionized water to obtain hydrophobic modified sericite;
(2) drying at 100 deg.C in a single-neck bottle, and maintaining vacuum state until the temperature is reduced to room temperature;
(3) adding cyclohexanone and mixed solution carrying methyl methacrylate, and stirring and dispersing;
(4) vacuumizing for 20-30min, and maintaining the pressure for 30-40 min;
(5) transferring the mixture into a centrifuge tube, repeatedly washing the mixture by using acetone, centrifuging the mixture, and putting the mixture into an oven to dry the mixture to constant weight to obtain a product A;
(6) pouring 100mL of graphene oxide aqueous dispersion into a beaker, adding 20mL of absolute ethanol solution of KH560, stirring for 10min at room temperature, and carrying out ultrasonic treatment for 2 h;
(7) polymerizing in an oil bath at 50-80 ℃, cooling, and washing with deionized water to obtain modified graphene oxide;
(8) respectively dispersing the product A and the modified graphene oxide in 20-30mL of cyclohexanone, mixing the product A and the modified graphene oxide, adding 0.1g of dibenzoyl peroxide into the mixture, and stirring;
(9) ultrasonic processing for 2h, transferring into a four-neck flask, heating, introducing nitrogen, pre-polymerizing at 75 ℃ for 1.5-2h, and polymerizing under 50-100 ℃ oil bath for 1.5-2 h;
(10) replacing cyclohexanone with ethanol, and freeze-drying to obtain sericite loaded graphene oxide;
(11) adding deionized water to obtain a sericite loaded graphene oxide solution, adding 1.695g N-isopropyl acrylamide, 0.231g N-N 'methylene bisacrylamide, 0.027g potassium persulfate and 0.04mL N-N-N' tetramethyl ethylenediamine into an ice bath, carrying out ultrasonic treatment under the ice bath until the solution becomes uniform, and reacting for 20-24h to obtain the intelligent temperature-sensitive hydrogel.
2. The preparation method of the intelligent temperature-sensitive hydrogel according to claim 1, wherein the mass ratio of the cyclohexanone to the methyl methacrylate in the step (3) is 1: 1.
3. The preparation method of the intelligent temperature-sensitive hydrogel according to claim 1, wherein the preparation method comprises the following steps: the concentration of the absolute ethyl alcohol solution of KH560 in the step (6) is 0.5 mg/mL.
4. The preparation method of the intelligent temperature-sensitive hydrogel according to claim 1, wherein the concentration of the sericite-loaded graphene oxide solution in the step (11) is 5-10 mg/mL.
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