CN114405486A - Preparation method of porous cryogel with antifouling, antibacterial and anti-dye adsorption functions - Google Patents
Preparation method of porous cryogel with antifouling, antibacterial and anti-dye adsorption functions Download PDFInfo
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- CN114405486A CN114405486A CN202111361669.XA CN202111361669A CN114405486A CN 114405486 A CN114405486 A CN 114405486A CN 202111361669 A CN202111361669 A CN 202111361669A CN 114405486 A CN114405486 A CN 114405486A
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Abstract
The invention relates to the technical field of oil-water separation of underwater super-oleophobic membrane materials, in particular to a preparation method of an underwater super-oleophobic porous cryogel with antifouling, antibacterial and anti-dye adsorption functions; dispersing magnesium lithium silicate and Lap modified by antibacterial silver ions into a polyethylene glycol diacrylate prepolymer solution together to obtain a first solvent, adding a reactant into the first solvent, uniformly mixing to obtain a mixture, sucking the mixture into a mold in time, placing the mold in an environment with the temperature of-80 ℃ for freezing, transferring the mixture to an environment with the temperature of-20 ℃ for placing after the mixture is crystallized, thawing the mixture to obtain the porous cryogel with the antifouling, antibacterial and dye adsorption preventing functions, and the cryogel material prepared by the preparation method of the porous cryogel with the antifouling, antibacterial and dye adsorption preventing functions can realize antifouling, antibacterial, dye adsorption and oil-water separation.
Description
Technical Field
The invention relates to the technical field of oil-water separation of underwater super-oleophobic membrane materials, in particular to a preparation method of an underwater super-oleophobic porous cryogel with antifouling, antibacterial and anti-dye adsorption functions.
Background
The industrial development and the rapid population growth lead to the discharge of a large amount of oily sewage, cause serious resource waste and environmental ecological damage, and bring serious threat to the life health of human beings. The dye pollutants in the sewage have stable properties, complex chemical compositions and high toxicity, and most of the dye pollutants are difficult to biodegrade, thereby causing serious pollution to the ecological environment. In addition, bacteria are easy to attach to the surface of the material, so that the fouling is caused to the material, the permeability and the separation effect of the material are influenced, and great difficulty is added to the separation and purification technology. The traditional oil-water separation technology is limited, and complex pollution components of bacteria, dyes and oil contained in industrial wastewater and domestic sewage are difficult to completely treat by adopting a one-step membrane separation method.
The traditional oil-water separation is solved by using a membrane separation water treatment technology at present, but the currently prepared underwater super-oleophobic membrane material cannot realize the integration of oil-water separation and cannot realize one-step separation of bacteria, dye and oil complex sewage.
Disclosure of Invention
The invention aims to provide a preparation method of a porous cryogel with antifouling, antibacterial and anti-dye adsorption functions, and aims to solve the technical problems that the integration of oil-water separation and one-step separation of bacteria, dye and oil complex sewage cannot be realized in the prior art.
In order to achieve the purpose, the preparation method of the porous cryogel with the functions of antifouling, antibiosis and dye adsorption prevention, which is adopted by the invention, comprises the following steps:
dispersing Lap and antibacterial silver ion modified Lap in a polyethylene glycol diacrylate prepolymer solution to obtain a first solvent;
adding a reactant into the first solvent, and uniformly mixing to obtain a mixture;
sucking the mixture into a mold in time, and placing the mold in an environment with the temperature of minus 80 ℃ for freezing;
after the mixture is crystallized, transferring the mixture to an environment with the temperature of minus 20 ℃ for placing;
and unfreezing the mixture to prepare the porous cryogel with the functions of antifouling, antibiosis and dye adsorption prevention.
Wherein, in the step of dispersing Lap and the Lap modified by antibacterial silver ions in a polyethylene glycol diacrylate prepolymer solution together to obtain a first solvent:
the mass-volume ratio of the Lap modified by the antibacterial silver ions to the solution of the prepolymer of the polyethylene glycol diacrylate is 48 mg: 2 mg: 1 ml.
Wherein, in the step of adding a reactant into the first solvent and uniformly mixing to obtain a mixture:
the volume ratio of the reactants to the solution of the polyethylene glycol diacrylate prepolymer is 3.5: 75: 1000.
wherein, in the step of adding a reactant into the first solvent and uniformly mixing to obtain a mixture:
ammonium persulfate in the reactant is an ammonium persulfate solution with PBS buffer solution as a solvent and with the mass concentration of 10%.
In the step of dispersing the Lap modified by the antibacterial silver ions and the Lap in a polyethylene glycol diacrylate prepolymer solution to obtain a first solvent, the preparation method of the Lap modified by the antibacterial silver ions comprises the following steps:
0.68g of silver nitrate is weighed and added into 40ml of deionized water to obtain silver nitrate solution,
weighing 0.2g of Lap in a silver nitrate solution, stirring, and then putting into a refrigerator at the temperature of-80 ℃;
and (5) freeze-drying to obtain the antibacterial silver ion modified Lap.
The porous cryogel with the antifouling, antibacterial and anti-dye adsorption functions, which is prepared by the preparation method of the porous cryogel with the antifouling, antibacterial and anti-dye adsorption functions, can realize one-step separation of bacteria, dye and anti-adhesion pollution.
The invention has the beneficial effects that: firstly dispersing Lap modified by antibacterial silver ions and Lap in a polyethylene glycol diacrylate prepolymer solution to obtain a first solvent, then adding a reactant into the first solvent, uniformly mixing to obtain a mixture, then sucking the mixture into a mold in time, placing the mold in an environment with the temperature of minus 80 ℃ for freezing, then transferring the mixture to an environment with the temperature of minus 20 ℃ for placing after the mixture is crystallized, finally thawing the mixture to obtain the porous cryogel with the functions of preventing fouling, resisting bacteria and preventing dye adsorption, combining special infiltration property with functional green environment-friendly materials, taking polyethylene glycol as a raw material, combining the excellent ion exchange capacity of Lap, adopting a low-temperature controlled freeze polymerization mode, having simple and easy operation, mild reaction conditions and low cost and needing no large instruments and equipment, the product can be biodegraded, a foundation is laid for realizing the application of multifunctional complex wastewater treatment, and the cryogel material obtained by the preparation method of the porous cryogel with the antifouling, antibacterial and dye adsorption preventing functions can realize antifouling, antibacterial, dye adsorption and oil-water separation.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of the steps of example 1 of the present invention.
Fig. 2 is a flowchart of the steps of embodiment 2 of the present invention.
Fig. 3 is a flowchart of the steps of embodiment 3 of the present invention.
FIG. 4 is a separation diagram of five oils of soybean oil, engine oil, diesel oil, kerosene and n-hexane separated by porous cryogel with antifouling, antibacterial and anti-dye adsorption functions, which is prepared with a polyethylene glycol diacrylate solution of 200mg/ml, and separation efficiency thereof.
FIG. 5 is a photograph of an antifouling, antibacterial and stain adsorption-resistant porous cryogel antifouling self-cleaning prepared with a 200mg/ml polyethylene glycol diacrylate solution.
FIG. 6 is a graph showing the experimental results of adsorption of methine blue and rhodamine B by porous cryogel with antifouling, antibacterial and anti-dye adsorption functions prepared with a 200mg/ml polyethylene glycol diacrylate solution.
FIG. 7 is a graph showing the results of comparative tests on anti-bacterial and anti-dye adsorption porous cryogels prepared with a 200mg/ml polyethylene glycol diacrylate solution, anti-bacterial and anti-dye adsorption porous cryogels prepared with Lap modified without antibacterial silver ions, and anti-Escherichia coli and anti-Staphylococcus aureus porous cryogels prepared without Lap.
Detailed Description
Example 1, referring to fig. 1, the present invention provides a method for preparing a porous cryogel with antifouling, antibacterial and anti-dye adsorption functions, comprising the following steps:
s1: weighing 0.68g of silver nitrate, adding 40ml of deionized water to obtain a silver nitrate solution, weighing 0.2g of Lap in the silver nitrate solution, magnetically stirring for 24 hours, taking out, centrifuging at 5000rpm/min for 15 minutes, repeating for 3-4 times, then placing in a refrigerator at the temperature of-80 ℃, freeze-drying, and then obtaining the Lap modified by antibacterial silver ions through a 120-mesh filter screen;
s2: weighing 200mg of polyethylene glycol diacrylate, dissolving the polyethylene glycol diacrylate in 2ml of PBS, weighing 96mg of Lap and 4mg of the antibacterial silver ion modified Lap, uniformly mixing the Lap and the polyethylene glycol diacrylate, and heating the mixture in a 60 ℃ water bath kettle to obtain a mixture;
s3: weighing 0.1g of ammonium persulfate to be dissolved in 1ml of deionized water, and storing at low temperature;
s4: putting the mixture into an ice-water mixture for 2 minutes, and putting a cylindrical silica gel mold with the diameter of 8mm and the height of 5mm into an environment with the temperature of-80 ℃ for freezing;
s5: taking 0.15ml of the mixture and 0.007ml of tetramethylethylenediamine in the mixture of the mixture and ice water, sucking the mixture into a silica gel mold in time, and placing the silica gel mold in an environment with the temperature of-80 ℃ for freezing to wait for crystallization;
s6: and (3) after the obtained material is crystallized and solidified, transferring the material to an environment with the temperature of-20 ℃ for placing, taking out after reacting for 24 hours, and unfreezing by using deionized water to obtain the porous cryogel with the antifouling, antibacterial and anti-dye adsorption functions.
In the embodiment, 0.68g of silver nitrate is weighed and added with 40ml of deionized water to obtain a silver nitrate solution, 0.2g of Lap is weighed and added into the silver nitrate solution, the mixture is magnetically stirred for 24 hours, then the mixture is taken out and centrifuged at 5000rpm/min for 15 minutes, the centrifugation is repeated for 3 to 4 times, then the mixture is placed into a refrigerator with the temperature of-80 ℃, freeze-dried and filtered by a 120-mesh filter screen to obtain Lap modified by antibacterial silver ions, then 200mg of polyethylene glycol diacrylate is weighed and dissolved in 2ml of PBS, 96mg of Lap and 4mg of the Lap modified by the antibacterial silver ions are weighed and uniformly mixed in the polyethylene glycol diacrylate solution, the mixture is placed into a water bath kettle with the temperature of 60 ℃ for heating to obtain a mixture, then 0.1g of ammonium persulfate is weighed and dissolved in 1ml of deionized water for low-temperature storage, the mixture is placed into an ice water mixture for 2 minutes, and a cylindrical silica gel mold with the diameter of 8mm and the height of 5mm is placed into the environment with the temperature of-80 ℃ for freezing, then 0.15ml of the mixture and 0.007ml of tetramethylethylenediamine are taken from the mixture and ice water mixture, are sucked into a silica gel mold in time, are placed in an environment with the temperature of minus 80 ℃ for freezing, wait for crystallization, finally the obtained material is transferred to an environment with the temperature of minus 20 ℃ for placing after being crystallized and solidified, are taken out after reacting for 24 hours, are unfrozen by deionized water, and obtain the porous cryogel with the antifouling, antibacterial and anti-dye adsorption functions, the special infiltration property is combined with the functional green and environment-friendly material, polyethylene glycol is taken as the raw material, the excellent ion exchange capacity of Lap is combined, a low-temperature controlled freezing polymerization mode is adopted, the preparation method is simple and easy to operate, the reaction condition is mild, the cost is low, large instruments and equipment are not needed, the product can be biodegraded, and the foundation is laid for realizing the application of multifunctional complex wastewater treatment, the cryogel material prepared by the preparation method of the porous cryogel with antifouling, antibacterial and dye adsorption preventing functions can realize antifouling, antibacterial, dye adsorption and oil-water separation.
s1: weighing 0.68g of silver nitrate, adding 40ml of deionized water to obtain a silver nitrate solution, weighing 0.2g of Lap in the silver nitrate solution, magnetically stirring for 24 hours, taking out, centrifuging at 5000rpm/min for 15 minutes, repeating for 3-4 times, then placing in a refrigerator at the temperature of-80 ℃, freeze-drying, and then obtaining the Lap modified by antibacterial silver ions through a 120-mesh filter screen;
s2: weighing 600mg of polyethylene glycol diacrylate, dissolving the polyethylene glycol diacrylate in 2ml of PBS, weighing 96mg of Lap and 4mg of the antibacterial silver ion modified Lap, uniformly mixing the Lap and the polyethylene glycol diacrylate solution, and heating the Lap and the polyethylene glycol diacrylate solution in a 60 ℃ water bath kettle to obtain a mixture;
s3: weighing 0.1g of ammonium persulfate to be dissolved in 1ml of deionized water, and storing at low temperature;
s4: putting the mixture into an ice-water mixture for 2 minutes, and putting a cylindrical silica gel mold with the diameter of 8mm and the height of 5mm into an environment with the temperature of-80 ℃ for freezing;
s5: taking 0.15ml of the mixture and 0.007ml of tetramethylethylenediamine in the mixture of the mixture and ice water, sucking the mixture into a silica gel mold in time, and placing the silica gel mold in an environment with the temperature of-80 ℃ for freezing to wait for crystallization;
s6: and (3) after the obtained material is crystallized and solidified, transferring the material to an environment with the temperature of-20 ℃ for placing, taking out after reacting for 24 hours, and unfreezing by using deionized water to obtain the porous cryogel with the antifouling, antibacterial and anti-dye adsorption functions.
In the embodiment, 0.68g of silver nitrate is weighed and added with 40ml of deionized water to obtain a silver nitrate solution, 0.2g of Lap is weighed and added into the silver nitrate solution, the mixture is magnetically stirred for 24 hours, then the mixture is taken out and centrifuged at 5000rpm/min for 15 minutes, the centrifugation is repeated for 3-4 times, then the mixture is placed into a refrigerator with the temperature of-80 ℃, freeze-dried and filtered by a 120-mesh filter screen to obtain Lap modified by antibacterial silver ions, then 600mg of polyethylene glycol diacrylate is weighed and dissolved in 2ml of PBS, then 96mg of Lap and 4mg of the Lap modified by the antibacterial silver ions are weighed and uniformly mixed in the polyethylene glycol diacrylate solution, the mixture is placed into a water bath kettle with the temperature of 60 ℃ for heating to obtain a mixture, then 0.1g of ammonium persulfate is weighed and dissolved in 1ml of deionized water for low-temperature storage, then the mixture is placed into an ice water mixture for 2 minutes, and a cylindrical silica gel mold with the diameter of 8mm and the height of 5mm is placed into the environment with the temperature of-80 ℃ for freezing, then 0.15ml of the mixture and 0.007ml of tetramethylethylenediamine are taken from the mixture and the ice water mixture, are sucked into a silica gel mold in time, are placed in an environment with the temperature of minus 80 ℃ for freezing, wait for crystallization, finally the obtained material is transferred to an environment with the temperature of minus 20 ℃ for placing after being crystallized and solidified, are taken out after reacting for 24 hours, are unfrozen by deionized water, and obtain the porous cryogel with the antifouling, antibacterial and anti-dye adsorption functions, the special infiltration property is combined with the functional green and environment-friendly material, polyethylene glycol is taken as the raw material, the excellent ion exchange capacity of Lap is combined, a low-temperature controlled freezing polymerization mode is adopted, the preparation method is simple and easy to operate, the reaction condition is mild, the cost is low, large instruments and equipment are not needed, the product can be biodegraded, and the foundation is laid for realizing the application of multifunctional complex wastewater treatment, the cryogel material prepared by the preparation method of the porous cryogel with antifouling, antibacterial and dye adsorption preventing functions can realize antifouling, antibacterial, dye adsorption and oil-water separation.
s1: weighing 0.68g of silver nitrate, adding 40ml of deionized water to obtain a silver nitrate solution, weighing 0.2g of Lap in the silver nitrate solution, magnetically stirring for 24 hours, taking out, centrifuging at 5000rpm/min for 15 minutes, repeating for 3-4 times, then placing in a refrigerator at the temperature of-80 ℃, freeze-drying, and then obtaining the Lap modified by antibacterial silver ions through a 120-mesh filter screen;
s2: weighing 400mg of polyethylene glycol diacrylate, dissolving the polyethylene glycol diacrylate in 2ml of PBS, weighing 96mg of Lap and 4mg of the antibacterial silver ion modified Lap, uniformly mixing the Lap and the polyethylene glycol diacrylate, and heating the mixture in a 60 ℃ water bath kettle to obtain a mixture;
s3: weighing 0.1g of ammonium persulfate to be dissolved in 1ml of deionized water, and storing at low temperature;
s4: putting the mixture into an ice-water mixture for 2 minutes, and putting a cylindrical silica gel mold with the diameter of 8mm and the height of 5mm into an environment with the temperature of-80 ℃ for freezing;
s5: taking 0.15ml of the mixture and 0.007ml of tetramethylethylenediamine in the mixture of the mixture and ice water, sucking the mixture into a silica gel mold in time, and placing the silica gel mold in an environment with the temperature of-80 ℃ for freezing to wait for crystallization;
s6: and (3) after the obtained material is crystallized and solidified, transferring the material to an environment with the temperature of-20 ℃ for placing, taking out after reacting for 24 hours, and unfreezing by using deionized water to obtain the porous cryogel with the antifouling, antibacterial and anti-dye adsorption functions.
In the embodiment, 0.68g of silver nitrate is weighed and added with 40ml of deionized water to obtain a silver nitrate solution, 0.2g of Lap is weighed and added into the silver nitrate solution, the mixture is magnetically stirred for 24 hours, then the mixture is taken out and centrifuged at 5000rpm/min for 15 minutes, the centrifugation is repeated for 3 to 4 times, then the mixture is placed into a refrigerator with the temperature of-80 ℃, freeze-dried and filtered by a 120-mesh filter screen to obtain the Lap modified by antibacterial silver ions, then 400mg of polyethylene glycol diacrylate is weighed and dissolved in 2ml of PBS, 96mg of Lap and 4mg of the Lap modified by the antibacterial silver ions are weighed and uniformly mixed in the polyethylene glycol diacrylate solution, the mixture is placed into a water bath kettle with the temperature of 60 ℃ for heating to obtain a mixture, then 0.1g of ammonium persulfate is weighed and dissolved in 1ml of deionized water for low-temperature storage, then the mixture is placed into an ice water mixture for 2 minutes, and a cylindrical silica gel mold with the diameter of 8mm and the height of 5mm is placed into the environment with the temperature of-80 ℃ for freezing, then 0.15ml of the mixture and 0.007ml of tetramethylethylenediamine are taken from the mixture and the ice water mixture, are sucked into a silica gel mold in time, are placed in an environment with the temperature of minus 80 ℃ for freezing, wait for crystallization, finally the obtained material is transferred to an environment with the temperature of minus 20 ℃ for placing after being crystallized and solidified, are taken out after reacting for 24 hours, are unfrozen by deionized water, and obtain the porous cryogel with the antifouling, antibacterial and anti-dye adsorption functions, the special infiltration property is combined with the functional green and environment-friendly material, polyethylene glycol is taken as the raw material, the excellent ion exchange capacity of Lap is combined, a low-temperature controlled freezing polymerization mode is adopted, the preparation method is simple and easy to operate, the reaction condition is mild, the cost is low, large instruments and equipment are not needed, the product can be biodegraded, and the foundation is laid for realizing the application of multifunctional complex wastewater treatment, the cryogel material prepared by the preparation method of the porous cryogel with the antifouling, antibacterial and dye adsorption preventing functions can realize antifouling, antibacterial, dye adsorption and oil-water separation, the porous cryogel with the antifouling, antibacterial and dye adsorption preventing functions is subjected to separation tests on five kinds of oil, namely soybean oil, engine oil, diesel oil, kerosene and n-hexane respectively, the separation efficiency is calculated, a separation chart and the separation efficiency are obtained, and the porous cryogel with the antifouling, antibacterial and dye adsorption preventing functions has high separation efficiency on the five kinds of oil, and the separation efficiency exceeds 98%; further carrying out an anti-pollution adhesion test on the porous cryogel with the anti-pollution, antibacterial and anti-dye adsorption functions to obtain an anti-pollution self-cleaning picture, wherein the anti-pollution, antibacterial and anti-dye adsorption function is displayed to have the anti-pollution function, and oil drops are not easy to adhere to materials; further carrying out absorption test on the methine blue and rhodamine B dye on the porous cryogel with the antifouling, antibacterial and dye absorption prevention functions to obtain an experimental result graph for absorbing the methine blue and the rhodamine B, and displaying that the porous cryogel with the antifouling, antibacterial and dye absorption prevention functions has obvious absorption effect on the methine blue and the rhodamine B dye; further, the materials prepared in this example and example 4 were tested for escherichia coli resistance and staphylococcus aureus resistance to obtain a picture as shown in fig. 4, and fig. 4 shows that the cryogel material prepared in this example exhibits bacteriostatic and antibacterial effects on escherichia coli and staphylococcus aureus.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. A preparation method of the porous cryogel with antifouling, antibacterial and anti-dye adsorption functions is characterized by comprising the following steps:
dispersing Lap and antibacterial silver ion modified Lap in a polyethylene glycol diacrylate prepolymer solution to obtain a first solvent;
adding a reactant into the first solvent, and uniformly mixing to obtain a mixture;
sucking the mixture into a mold in time, and placing the mold in an environment with the temperature of minus 80 ℃ for freezing;
after the mixture is crystallized, transferring the mixture to an environment with the temperature of minus 20 ℃ for placing;
and unfreezing the mixture to prepare the porous cryogel with the functions of antifouling, antibiosis and dye adsorption prevention.
2. The method for preparing the anti-fouling, antibacterial and anti-dye adsorption porous cryogel according to claim 1, wherein the step of dispersing the Lap modified with antibacterial silver ions in a polyethylene glycol diacrylate prepolymer solution to obtain the first solvent comprises:
the mass-volume ratio of the Lap modified by the antibacterial silver ions to the solution of the prepolymer of the polyethylene glycol diacrylate is 48 mg: 2 mg: 1 ml.
3. The method for preparing the anti-fouling, anti-bacterial and anti-dye adsorption porous cryogel according to claim 1, wherein in the step of adding a reactant to the first solvent and mixing uniformly to obtain a mixture:
the volume ratio of the reactants to the solution of the polyethylene glycol diacrylate prepolymer is 3.5: 75: 1000.
4. the method for preparing the anti-fouling, anti-bacterial and anti-dye adsorption porous cryogel according to claim 1, wherein in the step of adding a reactant to the first solvent and mixing uniformly to obtain a mixture:
ammonium persulfate in the reactant is an ammonium persulfate solution with PBS buffer solution as a solvent and with the mass concentration of 10%.
5. The method for preparing the anti-fouling, antibacterial and anti-dye adsorption porous cryogel according to claim 1, wherein the step of dispersing the Lap modified with antibacterial silver ions in a polyethylene glycol diacrylate prepolymer solution to obtain the first solvent comprises:
0.68g of silver nitrate is weighed and added into 40ml of deionized water to obtain silver nitrate solution,
weighing 0.2g of Lap in a silver nitrate solution, stirring, and then putting into a refrigerator at the temperature of-80 ℃;
and (5) freeze-drying to obtain the antibacterial silver ion modified Lap.
6. The method for preparing the anti-fouling, anti-bacterial and anti-dye-adsorption porous cryogel according to claim 1,
the anti-fouling, antibacterial and anti-dye adsorption porous cryogel prepared by the preparation method of the anti-fouling, antibacterial and anti-dye adsorption porous cryogel can realize one-step separation of bacteria, dye and anti-adhesion pollution.
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