CN114874479A - Preparation method of spongy macroporous hydrogel and application of spongy macroporous hydrogel in antibiosis - Google Patents
Preparation method of spongy macroporous hydrogel and application of spongy macroporous hydrogel in antibiosis Download PDFInfo
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Abstract
The invention discloses a preparation method of spongy macroporous hydrogel and application of the spongy macroporous hydrogel in antibiosis, wherein the preparation method comprises the following steps: mixing acrylic acid, double-bonded dopamine and deionized water, adding an initiator and a cross-linking agent, uniformly stirring, and then adding Ti 3 C 2 MXene, and carrying out reaction to obtain the spongy macroporous hydrogel. The invention uses Ti 3 C 2 MXene induces gelation reactions of polyacrylic acid hydrogels, Ti 3 C 2 MXene oneThe gas generated by the action of the initiator promotes the generation of hydrogel sponge-like structures, and Ti 3 C 2 The strong interaction between MXene or the oxidation product thereof and the hydrogel molecular chain ensures that the spongy hydrogel has stable physical property and swelling resistance; in addition to that, Ti 3 C 2 TiO formed by MXene in-situ oxidation 2 @ C or TiO 2 @Ti 3 C 2 The hybrid structure has good photocatalytic sterilization effect, and the dopamine contained in the molecular chain can effectively remove active oxygen. Therefore, the spongy macroporous hydrogel has multiple treatment functions and can be well applied to the field of wound repair of patients with chronic diseases.
Description
Technical Field
The invention belongs to the field of composite material preparation, and particularly relates to a preparation method of spongy macroporous hydrogel and application of the spongy macroporous hydrogel in antibiosis.
Background
Delayed wound healing in diabetic patients due to microbial infection and oxidative stress remains a significant clinical challenge. At normal wound sites, immune cells (e.g., macrophages, neutrophils) secrete and maintain an amount of Reactive Oxygen Species (ROS) to scavenge exogenous contaminants (bacteria, fungi, foreign bodies), induce tissue differentiation and growth, and promote wound healing. However, due to persistent hyperglycemia, bacterial proliferation and impaired immune system can upset the balance of ROS levels in diabetic patients and present complications such as oxidative stress and vascular damage. Therefore, regulation of wound ROS levels, prevention of bacterial infection and oxidative stress are key parameters for promoting diabetic wound tissue repair.
Hydrogels are "soft and wet" materials, consisting of three-dimensional cross-linked polymer networks, which can retain large amounts of water. Hydrogels have a wide range of biomedical applications, from in vitro cell expansion, tissue repair, drug delivery, wound dressing, hemostasis, and antisepsis, due to the soft-wet nature of similar biological tissues. The properties of macroporous hydrogels that facilitate gas exchange, nutrient transport, and cell ingrowth make them more potential ideal materials for chronic wound therapy.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter.
To achieve these objects and other advantages in accordance with the present invention, there is provided a method for preparing a spongy macroporous hydrogel, comprising:
mixing acrylic acid, double-bonded dopamine and deionized water, adding an initiator and a cross-linking agent, uniformly stirring, and then adding Ti 3 C 2 MXene, mixing and degassing, and reacting at room temperature to obtain the spongy macroporous hydrogel.
Preferably, the preparation method of the double-bonded dopamine comprises the following steps: under the protection of nitrogen, adding dopamine hydrochloride into a mixed solution composed of sodium borate, sodium bicarbonate and water to obtain a dopamine mixed solution, dissolving methacrylic anhydride in tetrahydrofuran to obtain a methacrylic anhydride solution, dropwise adding the methacrylic anhydride solution into the dopamine mixed solution, and simultaneously adding 1mol/L of sodium hydroxide solution to keep the pH value of the reaction solution to be more than or equal to 8; after stirring and reacting overnight, reducing the pH of the reaction solution to below 2 by adding a hydrochloric acid solution to precipitate doubly-bonded dopamine; the doubly bonded dopamine was then extracted with ethyl acetate, recrystallized from hexane and freeze-dried.
Preferably, the mass ratio of the sodium borate to the sodium bicarbonate is 3-7: 1; the mass ratio of the sodium borate to the water is 1: 8-12; the mass ratio of the dopamine hydrochloride to the sodium borate is 1: 1.5 to 3; the volume ratio of the methacrylic anhydride to the tetrahydrofuran is 1: 4-6; the mass-volume ratio of the sodium borate to the methacrylic anhydride is 15-35 g: 8-12 mL.
Preferably, the mass ratio of the acrylic acid to the doubly-bonded dopamine is 100-200: 1; the mass ratio of the acrylic acid to the deionized water is 3: 8-12; the mass ratio of the acrylic acid to the initiator is 10-15: 1; the mass ratio of the acrylic acid to the cross-linking agent is 150-250: 1; the acrylic acid and Ti 3 C 2 The mass ratio of MXene is 1: 200-800.
Preferably, the initiator is ammonium persulfate and the crosslinking agent is N-N' -methylene-bisacrylamide.
Preferably, the reaction is carried out at room temperature for 30 to 480 seconds.
Preferably, the Ti is 3 C 2 MXene is treated before use in the following process: mixing Ti 3 C 2 Adding MXene into a supercritical reaction kettle, simultaneously adding ethylenediamine, treating for 5-10 min under the supercritical condition of the ethylenediamine, cooling to room temperature, filtering, and drying to obtain pretreated Ti 3 C 2 MXene。
Preferably, the Ti is 3 C 2 The mass volume ratio of MXene to ethylenediamine is 1-3 g: 100-300 mL; the temperature of the supercritical condition of the ethylenediamine is 320-350 ℃, and the pressure is 12-16 MPa.
Wherein, Ti 3 C 2 The preparation method of MXene comprises the following steps: LiF (1.0g) and Ti 3 AlC 2 (1.0g) in a Teflon bottle in 10mL of hydrochloric acid (9.0M); then, the mixture was continuously stirred (600rpm) at 35.0 ℃ for 48 hours to etch Ti 3 AlC 2 The Al layer of (1). After etching, the product was washed several times with distilled water and centrifugation (3500 rpm, 5 minutes) until the pH of the suspension was close to 6.0. The precipitate was redispersed in 50mL of distilled water and treated with water bath ultrasound (200w) for 10min to further exfoliate the MXene sheet.
The invention also discloses application of the spongy macroporous hydrogel prepared by the preparation method in antibiosis.
The invention at least comprises the following beneficial effects:
ti used in the invention 3 C 2 MXene induces acrylic acid and double-bonded dopamine to polymerize to form gel, and after the double-bonded dopamine is added, the double-bonded dopamine provides oxidation resistance for the hydrogel; ti 3 C 2 MXene and initiator act to induce generation of macroporous structure, and TiO formed by in-situ oxidation 2 The hybrid structure can also provide antibacterial performance for the hydrogel; therefore, the hydrogel can be used as a material with multiple functions of nutrient substance transmission, antibiosis, antioxidation and the like for repairing chronic wounds.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Description of the drawings:
FIG. 1 shows the bactericidal activity of different hydrogels on Escherichia coli in light;
FIG. 2 shows the bactericidal activity of different hydrogels on Escherichia coli in light;
FIG. 3 shows the bactericidal activity of different hydrogels on Staphylococcus epidermidis under light;
FIG. 4 shows the bactericidal activity of different hydrogels on Staphylococcus epidermidis under light;
FIG. 5 shows the bactericidal activity of different hydrogels on Escherichia coli under light and dark conditions;
FIG. 6 is a graph showing the bactericidal activity of various hydrogels on Staphylococcus epidermidis under light and dark conditions;
FIG. 7 is a UV-Vis spectrum of 1, 1-diphenylyl-2-piperidinylhydrazyl (DPPH) reacted with various hydrogels;
FIG. 8 shows the ROS (reactive oxygen species) scavenging efficiency of different hydrogels;
FIG. 9 shows cell proliferation on hydrogels after 1, 3 and 7 days of culture by CCK8 assay;
FIG. 10 is a graph of the relative activity of cells on various hydrogels;
FIG. 11 is a fluorescent photograph of cells cultured on various hydrogels for 3 days;
FIG. 12a is a photograph of actual wounds treated with each type of hydrogel for different days; fig. 12b is a quantitative analysis of wound area collected.
The specific implementation mode is as follows:
the present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Ti used in the present invention 3 C 2 The preparation method of MXene comprises the following steps: LiF (1.0g) and Ti 3 AlC 2 (1.0g) in a Teflon bottle in 10mL of hydrochloric acid (9.0M); then, the mixture was continuously stirred (600rpm) at 35.0 ℃ for 48 hours to etch Ti 3 AlC 2 The Al layer of (1). After etching, the product was washed several times with distilled water and centrifugation (3500 rpm, 5 minutes) until the pH of the suspension was close to 6.0. The precipitate was redispersed in 50mL of distilled water and treated with water bath ultrasound (200w) for 10min to further exfoliate the MXene sheet.
Examples 1 to 4:
a preparation method of spongy macroporous hydrogel comprises the following steps:
step one, under the protection of nitrogen, adding 10g of dopamine hydrochloride into a mixed solution composed of 20g of sodium borate, 8g of sodium bicarbonate and 200mL of water to obtain a dopamine mixed solution, dissolving 9.4mL of methacrylic anhydride in 50mL of tetrahydrofuran to obtain a methacrylic anhydride solution, dropwise adding the methacrylic anhydride solution into the dopamine mixed solution, and simultaneously adding 1mol/L of sodium hydroxide solution to keep the pH value of the reaction solution to be more than or equal to 8; after stirring and reacting overnight, reducing the pH of the reaction solution to below 2 by adding a hydrochloric acid solution to precipitate doubly-bonded dopamine; then, extracting doubly-bonded dopamine with ethyl acetate, recrystallizing with hexane, and freeze-drying;
mixing acrylic acid, doubly-bonded dopamine and deionized water, adding an initiator and a crosslinking agent, uniformly stirring, and then adding Ti 3 C 2 MXene, mixing and degassing, and reacting at room temperature to obtain spongy macroporous hydrogel;
in examples 1 to 4, acrylic acid, doubly-bonded dopamine, and deionized water H 2 O, initiator ammonium persulfate APS, cross-linking agent N-N' -methylene bisacrylamide BIS and Ti 3 C 2 The amount of MXene is shown in Table 1;
TABLE 1
Examples 5 to 6:
a preparation method of spongy macroporous hydrogel comprises the following steps:
step one, under the protection of nitrogen, adding 10g of dopamine hydrochloride into a mixed solution composed of 20g of sodium borate, 8g of sodium bicarbonate and 200mL of water to obtain a dopamine mixed solution, dissolving 9.4mL of methacrylic anhydride in 50mL of tetrahydrofuran to obtain a methacrylic anhydride solution, dropwise adding the methacrylic anhydride solution into the dopamine mixed solution, and simultaneously adding 1mol/L of sodium hydroxide solution to keep the pH value of the reaction solution to be more than or equal to 8; after stirring and reacting overnight, reducing the pH of the reaction solution to below 2 by adding a hydrochloric acid solution to precipitate doubly-bonded dopamine; then, extracting doubly-bonded dopamine with ethyl acetate, recrystallizing with hexane, and freeze-drying;
mixing acrylic acid, doubly-bonded dopamine and deionized water, adding an initiator and a crosslinking agent, uniformly stirring, and then adding pretreated Ti 3 C 2 MXene, mixing and degassing, and reacting at room temperature to obtain spongy macroporous hydrogel;
wherein, the Ti 3 C 2 MXene is treated before use in the following process: mixing Ti 3 C 2 Adding MXene into supercritical reaction kettle, adding ethylene diamine, treating under supercritical condition of ethylene diamine for 8min, cooling to room temperature, filtering, and drying to obtain pretreated Ti 3 C 2 MXene; the Ti 3 C 2 The mass-volume ratio of MXene to ethylenediamine is 1.5g:200 mL; the temperature of the supercritical condition of the ethylenediamine is 340 ℃, and the pressure is 15 MPa.
In examples 5 to 6, acrylic acid, doubly-bonded dopamine, and deionized water H 2 O, initiator ammonium persulfate APS, cross-linking agent N-N' -methylene bisacrylamide BIS and pretreatment Ti 3 C 2 The amount of MXene is shown in Table 2;
TABLE 2
Comparative example 1:
a preparation method of spongy macroporous hydrogel comprises the following steps:
mixing acrylic acid and deionized water, adding an initiator and a cross-linking agent, uniformly stirring, mixing and degassing, and carrying out ultraviolet irradiation reaction at room temperature to obtain hydrogel (PAA);
comparative example 2:
step two, mixing acrylic acid and deionized water, adding an initiator and a cross-linking agent, stirring uniformly, and then adding Ti 3 C 2 MXene, mixed and degassed, and then reacted at room temperature to obtain hydrogel (SMPAA);
comparative example 3:
a preparation method of spongy macroporous hydrogel comprises the following steps:
mixing acrylic acid, double-bonded dopamine and deionized water, adding an initiator and a cross-linking agent, uniformly stirring, mixing and degassing, and carrying out ultraviolet irradiation reaction at room temperature to obtain hydrogel (PAAM);
wherein in comparative examples 1-3, acrylic acid, doubly-bonded dopamine and deionized water H 2 O, initiator ammonium persulfate APS, cross-linking agent N-N' -methylene bisacrylamide BIS and Ti 3 C 2 The amount of MXene is shown in Table 3;
TABLE 3
Comparative example 4:
step two, mixing acrylic acid and deionized water, adding an initiator and a cross-linking agent, stirring uniformly, then adding nano titanium dioxide, mixing and degassing, and carrying out ultraviolet irradiation reaction at room temperature to obtain hydrogel (0.16% TiO) 2 -PAA)；
Comparative example 5:
a preparation method of spongy macroporous hydrogel comprises the following steps:
step one, under the protection of nitrogen, adding 10g of dopamine hydrochloride into a mixed solution composed of 20g of sodium borate, 8g of sodium bicarbonate and 200mL of water to obtain a dopamine mixed solution, dissolving 9.4mL of methacrylic anhydride in 50mL of tetrahydrofuran to obtain a methacrylic anhydride solution, dropwise adding the methacrylic anhydride solution into the dopamine mixed solution, and simultaneously adding 1mol/L of sodium hydroxide solution to keep the pH value of the reaction solution to be more than or equal to 8; after stirring and reacting overnight, reducing the pH of the reaction solution to below 2 by adding a hydrochloric acid solution to precipitate doubly-bonded dopamine; then, extracting doubly-bonded dopamine with ethyl acetate, recrystallizing with hexane, and freeze-drying;
mixing acrylic acid, doubly-bonded dopamine and deionized water, adding an initiator and a cross-linking agent, uniformly stirring, adding nano titanium dioxide, mixing and degassing, and performing ultraviolet irradiation reaction at room temperature to obtain hydrogel (0.16% TiO) 2 -PAAM)；
In comparative examples 4 to 5, acrylic acid, doubly-bonded dopamine, and deionized water H 2 The dosage of O, initiator ammonium persulfate APS, cross-linking agent N-N' -methylene bisacrylamide BIS and nano titanium dioxide is shown in Table 4;
TABLE 4
1. Hydrogel in vitro antimicrobial testing
Selecting PAA, PAAM, SMPAAM-0.16, SMPAAM-0.12, SMPAAM-0.08-1, SMPAAM-0.04-1, 0.16% TiO 2 -PAA、0.16％TiO 2 PAAM hydrogels as experimental group. Samples without hydrogel served as a control. Each set of four parallel samples was used for the antimicrobial test. All bacteria were cultured in agar protein medium. First, the samples were placed in a 24-well plate and 100 μ L of bacterial suspension (106 CFU/ml) was added to the surface of each sample. Next, the samples were incubated at 37 ℃ for 1 hour with or without 50W fluorescent lighting. Then, 900. mu.L of agar-protein medium was added to each well of the plateThe samples were further incubated at 37 ℃ for 24 hours. Finally, 200 μ L of bacterial suspension on each sample was collected and transferred to a 96-well plate. Bacterial growth was monitored by measuring the Optical Density (OD) at 600 nm. The bactericidal rate of the hydrogel was calculated according to the following formula:
wherein, FIG. 1 shows the bactericidal rate of Escherichia coli in different hydrogels under light; as can be seen from the figure, the hydrogel added with MXene has good antibacterial property;
FIG. 2 shows the bactericidal activity of different hydrogels on Escherichia coli in light; as can be seen from the figure, the MXene hydrogel after the addition of the pretreatment has better antibacterial property;
FIG. 3 shows the bactericidal activity of different hydrogels on Staphylococcus epidermidis under light; as can be seen from the figure, the hydrogel added with MXene has good antibacterial property;
FIG. 4 shows the bactericidal activity of different hydrogels on Staphylococcus epidermidis under light; as can be seen from the figure, the MXene hydrogel after the addition of the pretreatment has better antibacterial property;
FIG. 5 shows the bactericidal activity of different hydrogels on Escherichia coli under light and dark conditions; as can be seen from the figure, MXene-added gels were compared to TiO-added gels directly under light 2 The antibacterial property of the gel is better;
FIG. 6 shows the bactericidal activity of different hydrogels on Staphylococcus epidermidis under light and dark conditions; as can be seen from the figure, MXene-added gels were compared to TiO-added gels directly under light 2 The antibacterial property of the gel is better;
2. hydrogel in vitro active oxygen scavenging
The antioxidant activity of PAA, PAAM and SMPAAM was determined using DPPH clearance assay. First, PAA, PAAM and SMPAAM were added to ethanol (3 ml), respectively. Then, 1-diphenyl-2-picrylhydrazine (DPPH, 100 μm, 1 ml) solution and ethanol (1 ml) were added to the different samples, respectively. After various reaction times (10, 20, 40 and 60 minutes) in the dark, the uv absorption of the samples was measured using a uv-vis spectrophotometer (TU-1901, francisco, china). DPPH removal efficiency (E) was determined using the following equation:
wherein A is 0 Is the absorbance of a DPPH solution without sample, A S Is the absorbance of the DPPH solution with the sample;
wherein, FIG. 7 is a UV-Vis spectrum of 1, 1-diphenyl-2-piperidinylhydrazyl (DPPH) after reacting with various hydrogels;
FIG. 8 shows the ROS (reactive oxygen species) scavenging efficiency of different hydrogels; as can be seen from FIGS. 7 and 8, the hydrogel obtained good antioxidant properties after the double-bonded dopamine was added.
3. Hydrogel cell culture
The cellular compatibility of PAA, PAAM and SMPAAM hydrogels was studied. NIH-3T3 fibroblasts (ATCC cell bank) were cultured in Dulbecco's Minimum Essential Medium (DMEM) with 10% fetal bovine serum (HyClone) and 1% penicillin-streptomycin solution (HyClone) in a CO2 incubator at 37 ℃. Before seeding the cells, the hydrogel having a diameter of 7mm and a thickness of 2.5mm was first purified in Phosphate Buffered Saline (PBS), sterilized with 75% ethanol for 24 hours, and then placed in a 24-well plate with DMEM, and swelled to an equilibrium state at 37 ℃ for 2 days to prepare a leaching solution. Cells in the growth phase were treated with trypsin, harvested, and then suspended in culture medium to obtain a cell density of 1 × 105 cells/mL. Cells were seeded in the wells of tissue culture plates at a density of 5 × 104 cells for 3 hours to allow cell attachment, and then 1mL of the extract was added for co-culture. An additional 1mL of DMEM supplemented with 10% FBS was added to each well. Cells were allowed to adhere and grow for 3 and 5 days. After 3 days of culture, cells cultured with hydrogel extracts were stained with calcein AM and imaged by confocal laser scanning microscopy (CLSM, TCSSP5, laika). Cell viability was analyzed by the CCK8 assay. After 3 and 5 days of incubation, 200. mu.L of CCK8 solution was added to each well and the plates were incubated at 37 ℃ for 4 hours. After removing the medium, the resulting purple formazan was dissolved in 400. mu.L of Dimethyl (DMSO), and the absorbance at 450nm was measured with a microplate reader (TECAN, SPARK 10M).
FIG. 9 is cell proliferation on hydrogels cultured by CCK8 assay for 1, 3, and 7 days;
FIG. 10 is a graph of the relative activity of cells on various hydrogels;
FIG. 11 is a fluorescent photograph of cells cultured on various hydrogels for 3 days;
as can be seen from the above figures, the hydrogel of the present invention does not affect the proliferation and differentiation of cells.
4. Hydrogel wound therapy
(1) Diabetes model establishment
One week after dietary adaptation, mice were fasted overnight prior to the first infection, and then injected intravenously with STZ (75mg/kg, sigma) in the tail. Random blood glucose levels were measured every 5 days. After 5 days, polyphagia, polydipsia and polyuria were observed. After 2 weeks, mice with random glucose levels above 18mmol/L were designated as diabetic mice.
(2) Wound healing evaluation
The wound healing capacity of the hydrogel was evaluated using a full-thickness skin defect model. Briefly, diabetic mice were anesthetized and operated under sterile conditions. A circular full-thickness skin wound (8 mm diameter) was created on the back of each mouse, while normal skin (2mm) was peeled off around each wound to prevent the implanted hydrogel from falling off. The epidermis, dermis and cartilage membranes in each wound were completely removed. Mice were randomized into four groups and received control (untreated), PAA, PAAM and SMPAAM hydrogels. After recovery from anesthesia, the mice were returned to their cages. Wound healing was monitored on days 0, 3, 7, 10 and 14 post-surgery. The wound healing rate for each group was calculated as the ratio of the wound healing area to the original area of the wound.
16 male SD rats 2 months old, weighing 200-300g, were purchased from Kyodo Biotechnology Ltd. All surgical procedures were performed according to protocols approved by the local ethics committee and chinese experimental animal management regulations. All animal surgery procedures were approved by the Sichuan university Committee for animal use and Care (WCHSIRB-D-2021-.
Fig. 12a is a photograph of actual wound surface from different days of wound treatment with each type of hydrogel, which clearly shows that the hydrogel of the present invention treated the wound to heal better, and fig. 12b is a quantitative analysis of the area of the wound collected.
The invention uses Ti 3 C 2 MXene induces gelation reactions of polyacrylic acid hydrogels, Ti 3 C 2 MXene reacts with an initiator to generate gas to promote the generation of hydrogel sponge structure, and Ti 3 C 2 The strong interaction between MXene or the oxidation product thereof and the hydrogel molecular chain ensures that the spongy hydrogel has stable physical property and swelling resistance; in addition to that, Ti 3 C 2 TiO formed by MXene in-situ oxidation 2 @ C or TiO 2 @Ti 3 C 2 The hybrid structure has good photocatalytic sterilization effect, and the dopamine contained in the molecular chain can effectively remove active oxygen. Therefore, the spongy macroporous hydrogel has multiple treatment functions and can be well applied to the field of wound repair of patients with chronic diseases.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (9)
1. A preparation method of spongy macroporous hydrogel is characterized by comprising the following steps:
mixing acrylic acid, double-bonded dopamine and deionized water, adding an initiator and a cross-linking agent, uniformly stirring, and then adding Ti 3 C 2 MXene, mixing and degassing, and reacting at room temperature to obtain seaA cotton-like macroporous hydrogel.
2. The method for preparing the spongy macroporous hydrogel according to claim 1, wherein the method for preparing doubly-linked dopamine comprises: under the protection of nitrogen, adding dopamine hydrochloride into a mixed solution composed of sodium borate, sodium bicarbonate and water to obtain a dopamine mixed solution, dissolving methacrylic anhydride in tetrahydrofuran to obtain a methacrylic anhydride solution, dropwise adding the methacrylic anhydride solution into the dopamine mixed solution, and simultaneously adding 1mol/L of sodium hydroxide solution to keep the pH value of the reaction solution to be more than or equal to 8; after stirring and reacting overnight, reducing the pH of the reaction solution to below 2 by adding a hydrochloric acid solution to precipitate doubly-bonded dopamine; the doubly bonded dopamine was then extracted with ethyl acetate, recrystallized from hexane and freeze-dried.
3. The preparation method of the spongy macroporous hydrogel as claimed in claim 2, wherein the mass ratio of the sodium borate to the sodium bicarbonate is 3-7: 1; the mass ratio of the sodium borate to the water is 1: 8-12; the mass ratio of the dopamine hydrochloride to the sodium borate is 1: 1.5 to 3; the volume ratio of the methacrylic anhydride to the tetrahydrofuran is 1: 4-6; the mass-volume ratio of the sodium borate to the methacrylic anhydride is 15-35 g: 8-12 mL.
4. The preparation method of the spongy macroporous hydrogel as claimed in claim 1, wherein the mass ratio of acrylic acid to doubly-bonded dopamine is 100-200: 1; the mass ratio of the acrylic acid to the deionized water is 3: 8-12; the mass ratio of the acrylic acid to the initiator is 10-15: 1; the mass ratio of the acrylic acid to the cross-linking agent is 150-250: 1; the acrylic acid and Ti 3 C 2 The mass ratio of MXene is 1: 200-800.
5. The method for preparing the spongy macroporous hydrogel of claim 1, wherein the initiator is ammonium persulfate and the crosslinking agent is N-N' -methylenebisacrylamide.
6. The method for preparing the spongy macroporous hydrogel according to claim 1, wherein the reaction is carried out at room temperature for 30 to 480 seconds.
7. The method of making a spongy macroporous hydrogel of claim 1, wherein said Ti is 3 C 2 MXene is treated before use in the following process: mixing Ti 3 C 2 Adding MXene into a supercritical reaction kettle, simultaneously adding ethylenediamine, treating for 5-10 min under the supercritical condition of the ethylenediamine, cooling to room temperature, filtering, and drying to obtain pretreated Ti 3 C 2 MXene。
8. The method of preparing a spongy macroporous hydrogel of claim 1, wherein said Ti is 3 C 2 The mass volume ratio of MXene to ethylenediamine is 1-3 g: 100-300 mL; the temperature of the supercritical condition of the ethylenediamine is 320-350 ℃, and the pressure is 12-16 MPa.
9. Application of the spongy macroporous hydrogel prepared by the preparation method of any one of claims 1-8 in antibiosis.
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| US20150362437A1 (en) * | 2014-06-13 | 2015-12-17 | Industry-Academic Cooperation Foundation Yonsei University | HYDROGEL, PREPARATION METHOD THEREOF, AND pH SENSOR COMPRISING THE SAME |
| CN111171213A (en) * | 2020-01-16 | 2020-05-19 | 西南科技大学 | Preparation method of PAA hydrogel loaded with double-bonded dopamine |
| CN114023935A (en) * | 2021-10-28 | 2022-02-08 | 上海应用技术大学 | Three-dimensional TiO2Preparation method of nanowire/MXene composite material |
| CN114149599A (en) * | 2021-12-22 | 2022-03-08 | 华南师范大学 | Transparent conductive hydrogel with adhesiveness and preparation method and application thereof |
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| US20150362437A1 (en) * | 2014-06-13 | 2015-12-17 | Industry-Academic Cooperation Foundation Yonsei University | HYDROGEL, PREPARATION METHOD THEREOF, AND pH SENSOR COMPRISING THE SAME |
| CN111171213A (en) * | 2020-01-16 | 2020-05-19 | 西南科技大学 | Preparation method of PAA hydrogel loaded with double-bonded dopamine |
| CN114023935A (en) * | 2021-10-28 | 2022-02-08 | 上海应用技术大学 | Three-dimensional TiO2Preparation method of nanowire/MXene composite material |
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| CN116396529A (en) * | 2023-04-14 | 2023-07-07 | 成都大学 | Preparation of porous photo-thermal conversion hydrogel film and application of porous photo-thermal conversion hydrogel film in sewage purification |
| CN116396529B (en) * | 2023-04-14 | 2024-05-03 | 成都大学 | Preparation of porous photo-thermal conversion hydrogel film and application of porous photo-thermal conversion hydrogel film in sewage purification |
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