CN115569539A - Ultrafiltration membrane for treating acrylic resin wastewater - Google Patents
Ultrafiltration membrane for treating acrylic resin wastewater Download PDFInfo
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- CN115569539A CN115569539A CN202211267118.1A CN202211267118A CN115569539A CN 115569539 A CN115569539 A CN 115569539A CN 202211267118 A CN202211267118 A CN 202211267118A CN 115569539 A CN115569539 A CN 115569539A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
- B01D71/78—Graft polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/02—Hydrophilization
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/36—Introduction of specific chemical groups
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/38—Graft polymerization
- B01D2323/385—Graft polymerization involving radiation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/48—Antimicrobial properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
- C02F2103/38—Polymers
Abstract
The invention relates to an ultrafiltration membrane for treating acrylic resin wastewater, which belongs to the technical field of ultrafiltration membranes and is prepared by the following steps: firstly, preparing a hydrophilic modifier; secondly, adding a hydrophilic modifier into N, N-dimethylacetamide for ultrasonic dispersion, then adding a pore-foaming agent and polyether sulfone, setting the temperature to be 60 ℃, stirring for 2-3h, then carrying out air deaeration to obtain a membrane casting solution, pouring the membrane casting solution onto a glass plate, scraping the membrane by using a membrane scraping machine, naturally volatilizing, and carrying out coagulation bath deionized water phase conversion to obtain a basement membrane; and thirdly, surface treatment. The hydrophilic modifier is added in the preparation process, and is added in the preparation of the ultrafiltration membrane, so that the roughness of the ultrafiltration membrane can be increased, the undulation degree of the membrane surface is increased, the membrane surface is more hydrophilic, and compared with the modified nano-cellulose which is not subjected to amino-POSS treatment, the modified nano-cellulose has better hydrophilicity, the stain resistance of the ultrafiltration membrane is better improved, and the service life is further prolonged.
Description
Technical Field
The invention belongs to the technical field of ultrafiltration membranes, and particularly relates to an ultrafiltration membrane for treating acrylic resin wastewater.
Background
When the acrylic resin is produced, a large amount of acrylic resin wastewater is generated, and the wastewater is recycled after ultrafiltration, nanofiltration and reverse osmosis treatment according to needs; the ultrafiltration membrane is used for treating and recycling the wastewater in the acrylic resin production process, so that pollutants in the wastewater can be effectively intercepted, the environmental pollution is reduced, the components with utilization values in the industrial wastewater can be recycled, more resources are saved, the environmental protection and energy conservation can be effectively realized, and a better economic effect can be obtained while the water resources are recycled.
The efficient membrane separation technology should have high flux and rejection rate, and also should have good pollution resistance, prolong the service life of the membrane, and reduce the process operation cost. The Polyethersulfone (PES) material only contains ether bonds and a benzene ring skeleton in the structure and does not contain carbon chains and biphenyl structures, so that the PES material has good chemical stability and heat resistance, is one of the most common materials for preparing the membrane, but PES has hydrophobicity, and the PES membrane is not resistant to pollution in the application process, so that the service life of the membrane is shortened.
Disclosure of Invention
In order to solve the technical problems mentioned in the background art, the invention provides an ultrafiltration membrane for treating acrylic resin wastewater.
The purpose of the invention can be realized by the following technical scheme:
an ultrafiltration membrane for treating acrylic resin wastewater is prepared by the following steps:
firstly, mixing modified nano-cellulose and deionized water, performing ultrasonic dispersion, setting the temperature to be 80 ℃, adding amino-POSS, maintaining the temperature to be 70-80 ℃ after the amino-POSS is added, reacting for 3-4 hours, and performing freeze drying after the reaction is finished to obtain a hydrophilic modifier; POSS is short for polyhedral oligomeric silsesquioxane with a cage-shaped structure, the structure of the polyhedral oligomeric silsesquioxane is composed of an external organic substituent group and an internal silicon dioxide rigid core, the silicon dioxide rigid core endows the POSS with excellent heat resistance, modified nanocellulose and amino-POSS are used as raw materials, the POSS is introduced into the structure of the nanocellulose, on one hand, the POSS improves the heat resistance of the nanocellulose, on the other hand, a hydrophilic modifier prepared by using the modified nanocellulose and the amino-POSS as the raw materials is added into the preparation of the ultrafiltration membrane, the roughness of the ultrafiltration membrane can be increased, the undulation degree of the membrane surface is increased, the membrane surface is made to be more hydrophilic, the hydrophilicity is better compared with that of the modified nanocellulose which is not treated by the amino-POSS, the stain resistance of the ultrafiltration membrane is more favorably improved, and the service life is further prolonged.
Secondly, adding a hydrophilic modifier into N, N-dimethylacetamide, performing ultrasonic dispersion, then adding a pore-forming agent and polyether sulfone, setting the temperature at 60 ℃, stirring for 2-3h, then performing air defoaming for 35-45min to obtain a membrane casting solution, pouring the membrane casting solution onto a glass plate, scraping the membrane by using a membrane scraping machine, naturally volatilizing, and performing coagulation bath deionized water phase conversion to obtain a basement membrane;
and thirdly, soaking the base membrane in acetone for 5 seconds, taking out, adding the base membrane into a mixed solution a of methyl acrylate and deionized water, adding an initiator, irradiating for 5 minutes by using ultraviolet light, taking out, washing and drying, adding the base membrane into a mixed solution b of an antibacterial agent and N, N-dimethylformamide, heating to 70 ℃, carrying out oscillation reaction for 48 hours, washing with water, and drying in vacuum to obtain the ultrafiltration membrane for treating the acrylic resin wastewater.
Furthermore, the dosage ratio of the modified nano-cellulose, the amino-POSS and the deionized water in the first step is 0.05g:0.1-0.15g:80mL.
Further, the pore-forming agent is PEG2000, and the dosage ratio of the hydrophilic modifier, the pore-forming agent, the polyether sulfone and the N, N-dimethylacetamide in the second step is 0.1-0.2g:1.6g:20g:80mL.
Further, the dosage ratio of the methyl acrylate to the deionized water in the mixed solution a of the methyl acrylate and the deionized water in the third step is 1g;10mL; the dosage ratio of the initiator to the mixed liquid a is 50mmol:1L; the dosage ratio of the antibacterial agent to the N, N-dimethylformamide in the mixed solution b of the antibacterial agent and the N, N-dimethylformamide is 1g:3mL.
Further, the modified nanocellulose is prepared by the following steps:
mixing nano-cellulose and a sodium hydroxide aqueous solution, performing ultrasonic dispersion for 30min, heating to 60 ℃, stirring and dispersing for 30min, adding epoxy chloropropane, keeping the temperature unchanged, continuously stirring and reacting for 2h, and performing freeze drying after the reaction is finished to obtain the modified nano-cellulose. The modified nano-cellulose is obtained by taking nano-cellulose as a raw material and reacting with epoxy chloropropane under an alkaline condition, an epoxy group is introduced into the structure of the nano-cellulose, and the modified nano-cellulose can be used as the raw material to participate in the reaction.
Further, amino-POSS is prepared by the steps of:
under the protection of nitrogen, H-POSS and toluene are mixed, acrylamide and a Kanster catalyst with the mass fraction of 0.2% are added, the temperature is set to be 50 ℃, the reaction is carried out for 12 hours, after the reaction is finished, the reaction is cooled to the room temperature, the catalyst is adsorbed by active carbon, and then the solvent is removed through rotary evaporation, so that the amino-POSS is obtained. Carrying out hydrosilylation on H-POSS and acrylamide to obtain amino-POSS; wherein the dosage ratio of the H-POSS, the toluene, the acrylamide and the Karster catalyst is 3g:30mL of: 3g:0.02g.
Further, the antibacterial agent is prepared by the steps of:
adding 50% by mass of polyethyleneimine aqueous solution and N-methyl-N, N-diallyl-N-dodecyl ammonium chloride into a solvent, then adding sodium hydroxide aqueous solution to adjust the pH value to 12, setting the temperature to 80 ℃, stirring for 48h, dialyzing for 48h by using a dialysis bag with the molecular weight cutoff of 1000, and after the dialysis is finished, carrying out vacuum drying at 80 ℃ to obtain the antibacterial agent. Wherein the solvent is isopropanol and deionized water according to a volume ratio of 4:1, mixing; the dosage ratio of the polyethyleneimine water solution to the N-methyl-N, N-diallyl-N-dodecyl ammonium chloride to the solvent is 2g:0.2g:20mL; the antibacterial agent is prepared by the Michael addition reaction of polyethyleneimine and N-methyl-N, N-diallyl-N-dodecyl ammonium chloride.
The invention has the beneficial effects that:
in order to improve the stain resistance of the ultrafiltration membrane for treating acrylic resin wastewater, the hydrophilic modifier is added in the preparation process, and the hydrophilic modifier prepared by taking the modified nanocellulose and the amino-POSS as raw materials is added in the preparation of the ultrafiltration membrane, so that the roughness of the ultrafiltration membrane can be increased, the undulation degree of the membrane surface is increased, the membrane surface is more hydrophilic, the hydrophilicity is better compared with the hydrophilicity of the modified nanocellulose which is not treated by the amino-POSS, the stain resistance of the ultrafiltration membrane is more favorably improved, and the service life is further prolonged.
The surface of the ultrafiltration membrane for treating the acrylic resin wastewater is subjected to surface treatment, the surface of a prepared base membrane is subjected to graft polymerization initiated by ultraviolet light, and then the prepared base membrane and an antibacterial agent are subjected to amide condensation to obtain a final product, the hydrophilicity of the surface of the membrane cannot be damaged after the antibacterial agent is modified, and meanwhile, a large amount of amino groups are introduced after the antibacterial agent is modified, so that the ultrafiltration membrane has a better adsorption effect on substances such as acrylic acid and the like, is easy to desorb and regenerate, and has stable performance; the increase of the antibacterial effect is more beneficial to improving the pollution resistance and the service life of the ultrafiltration membrane.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparing modified nano-cellulose:
mixing the nano-cellulose and a sodium hydroxide aqueous solution, performing ultrasonic dispersion for 30min, then heating to 60 ℃, stirring and dispersing for 30min, adding epoxy chloropropane, keeping the temperature unchanged, continuously stirring for reaction for 2h, and performing freeze drying after the reaction is finished to obtain the modified nano-cellulose.
Preparation of amino-POSS:
mixing H-POSS and toluene under the protection of nitrogen, adding acrylamide and 0.2 mass percent of Kaster catalyst, setting the temperature to 50 ℃, reacting for 12 hours, cooling to room temperature after the reaction is finished, adsorbing the catalyst by using activated carbon, and removing the solvent by rotary evaporation to obtain the amino-POSS. Wherein the dosage ratio of the H-POSS, the toluene, the acrylamide and the Karster catalyst is 3g:30mL of: 3g:0.02g.
Preparing an antibacterial agent:
adding 50% by mass of polyethyleneimine aqueous solution and N-methyl-N, N-diallyl-N-dodecyl ammonium chloride into a solvent, then adding sodium hydroxide aqueous solution to adjust the pH value to 12, setting the temperature to 80 ℃, stirring for 48h, dialyzing for 48h by using a dialysis bag with the molecular weight cutoff of 1000, and after the dialysis is finished, carrying out vacuum drying at 80 ℃ to obtain the antibacterial agent. Wherein the solvent is isopropanol and deionized water according to a volume ratio of 4:1, mixing; the dosage ratio of the polyethyleneimine water solution, the N-methyl-N, N-diallyl-N-dodecyl ammonium chloride and the solvent is 2g:0.2g:20mL.
Example 2
An ultrafiltration membrane for treating acrylic resin wastewater is prepared by the following steps:
step one, mixing the modified nanocellulose prepared in example 1 with deionized water, performing ultrasonic dispersion, setting the temperature to be 80 ℃, adding the amino-POSS prepared in example 1, maintaining the temperature to be 70 ℃ after the addition, reacting for 4 hours, and performing freeze drying after the reaction is finished to obtain a hydrophilic modifier; the dosage ratio of the modified nano-cellulose to the amino-POSS to the deionized water is 0.05g:0.1g:80mL;
secondly, adding a hydrophilic modifier into N, N-dimethylacetamide for ultrasonic dispersion, then adding PEG2000 and polyether sulfone, setting the temperature at 60 ℃, stirring for 2 hours, then performing vacuum defoaming for 35 minutes to obtain a membrane casting solution, pouring the membrane casting solution onto a glass plate, scraping the membrane by using a membrane scraping machine, naturally volatilizing, and performing phase conversion by coagulating bath and deionized water to obtain a basement membrane; the dosage ratio of the hydrophilic modifier to the PEG2000 to the polyether sulfone to the N, N-dimethylacetamide is 0.1g:1.6g:20g:80mL.
And thirdly, soaking the base membrane in acetone for 5 seconds, taking out the base membrane, adding the base membrane into a mixed solution a of methyl acrylate and deionized water, adding an initiator, irradiating the mixture for 5 minutes by using ultraviolet light, taking out the base membrane, washing and drying the base membrane, adding the base membrane into a mixed solution b of the antibacterial agent and N, N-dimethylformamide prepared in the embodiment 1, heating the mixture to 70 ℃, carrying out oscillation reaction for 48 hours, washing the mixture with water, and drying the mixture in vacuum to obtain the ultrafiltration membrane for treating the acrylic resin wastewater. The dosage ratio of the methyl acrylate to the deionized water in the mixed solution a of the methyl acrylate and the deionized water is 1g;10mL; the dosage ratio of the initiator to the mixed liquid a is 50mmol:1L; the dosage ratio of the antibacterial agent to the N, N-dimethylformamide in the mixed solution b of the antibacterial agent and the N, N-dimethylformamide is 1g:3mL.
Example 3
An ultrafiltration membrane for treating acrylic resin wastewater is prepared by the following steps:
firstly, mixing the modified nano-cellulose prepared in the example 1 with deionized water, performing ultrasonic dispersion, setting the temperature to be 80 ℃, adding the amino-POSS prepared in the example 1, maintaining the temperature to be 70 ℃ after the addition, reacting for 3 hours, and after the reaction is finished, performing freeze drying to obtain a hydrophilic modifier; the dosage ratio of the modified nano-cellulose to the amino-POSS to the deionized water is 0.05g:0.15g:80mL;
secondly, adding a hydrophilic modifier into N, N-dimethylacetamide, performing ultrasonic dispersion, then adding PEG2000 and polyether sulfone, setting the temperature at 60 ℃, stirring for 3 hours, then performing vacuum deaeration for 45 minutes to obtain a casting solution, pouring the casting solution onto a glass plate, scraping the film by using a film scraping machine, naturally volatilizing, and performing phase conversion by using coagulation bath deionized water to obtain a basement membrane; the dosage ratio of the hydrophilic modifier to the PEG2000 to the polyether sulfone to the N, N-dimethylacetamide is 0.1g:1.6g:20g:80mL.
And thirdly, soaking the base membrane in acetone for 5 seconds, taking out the base membrane, adding the base membrane into a mixed solution a of methyl acrylate and deionized water, adding an initiator, irradiating the mixture for 5 minutes by using ultraviolet light, taking out the base membrane, washing and drying the base membrane, adding the base membrane into a mixed solution b of the antibacterial agent and N, N-dimethylformamide prepared in the embodiment 1, heating the mixture to 70 ℃, carrying out oscillation reaction for 48 hours, washing the mixture with water, and drying the mixture in vacuum to obtain the ultrafiltration membrane for treating the acrylic resin wastewater. The dosage ratio of the methyl acrylate to the deionized water in the mixed liquid a of the methyl acrylate and the deionized water is 1g;10mL; the dosage ratio of the initiator to the mixed liquid a is 50mmol:1L; and (3) mixing the antibacterial agent and the N, N-dimethylformamide in a mixed solution b of the antibacterial agent and the N, N-dimethylformamide in a dosage ratio of 1g:3mL.
Example 4
An ultrafiltration membrane for treating acrylic resin wastewater is prepared by the following steps:
step one, mixing the modified nanocellulose prepared in example 1 with deionized water, performing ultrasonic dispersion, setting the temperature to be 80 ℃, adding the amino-POSS prepared in example 1, maintaining the temperature to be 80 ℃ after the addition, reacting for 4 hours, and performing freeze drying after the reaction is finished to obtain a hydrophilic modifier; the dosage ratio of the modified nano-cellulose to the amino-POSS to the deionized water is 0.05g:0.15g:80mL;
secondly, adding a hydrophilic modifier into N, N-dimethylacetamide for ultrasonic dispersion, then adding PEG2000 and polyether sulfone, setting the temperature at 60 ℃, stirring for 3 hours, then performing vacuum defoaming for 45min to obtain a membrane casting solution, pouring the membrane casting solution onto a glass plate, scraping the membrane by using a membrane scraping machine, naturally volatilizing, and performing phase conversion by coagulating bath and deionized water to obtain a basement membrane; the dosage ratio of the hydrophilic modifier to the PEG2000 to the polyether sulfone to the N, N-dimethylacetamide is 0.2g:1.6g:20g:80mL.
And thirdly, soaking the base membrane in acetone for 5 seconds, taking out the base membrane, adding the base membrane into a mixed solution a of methyl acrylate and deionized water, adding an initiator, irradiating the mixture for 5 minutes by using ultraviolet light, taking out the base membrane, washing and drying the base membrane, adding the base membrane into a mixed solution b of the antibacterial agent and N, N-dimethylformamide prepared in the embodiment 1, heating the mixture to 70 ℃, carrying out oscillation reaction for 48 hours, washing the mixture with water, and drying the mixture in vacuum to obtain the ultrafiltration membrane for treating the acrylic resin wastewater. The dosage ratio of the methyl acrylate to the deionized water in the mixed solution a of the methyl acrylate and the deionized water is 1g;10mL; the dosage ratio of the initiator to the mixed liquid a is 50mmol:1L; and (3) mixing the antibacterial agent and the N, N-dimethylformamide in a mixed solution b of the antibacterial agent and the N, N-dimethylformamide in a dosage ratio of 1g:3mL.
Comparative example 1
Firstly, adding nanocellulose into N, N-dimethylacetamide for ultrasonic dispersion, then adding PEG2000 and polyether sulfone, setting the temperature at 60 ℃, stirring for 3 hours, then performing vacuum defoaming for 45 minutes to obtain a membrane casting solution, pouring the membrane casting solution onto a glass plate, scraping the membrane by using a membrane scraping machine, naturally volatilizing, and performing coagulation bath and deionized water phase conversion to obtain a basement membrane; the dosage ratio of the nano-cellulose to the PEG2000 to the polyether sulfone to the N, N-dimethylacetamide is 0.2g:1.6g:20g:80mL.
And secondly, soaking the base membrane in acetone for 5 seconds, taking out the base membrane, then adding the base membrane into a mixed solution a of methyl acrylate and deionized water, adding an initiator, irradiating for 5 minutes by using ultraviolet light, taking out the base membrane, washing and drying the base membrane, then adding the base membrane into a mixed solution b of the antibacterial agent and N, N-dimethylformamide prepared in the embodiment 1, heating the mixture to 70 ℃, carrying out oscillation reaction for 48 hours, washing the mixture with water, and drying the mixture in vacuum to obtain the ultrafiltration membrane for treating the acrylic resin wastewater. The dosage ratio of the methyl acrylate to the deionized water in the mixed liquid a of the methyl acrylate and the deionized water is 1g;10mL; the dosage ratio of the initiator to the mixed liquid a is 50mmol:1L; the dosage ratio of the antibacterial agent to the N, N-dimethylformamide in the mixed solution b of the antibacterial agent and the N, N-dimethylformamide is 1g:3mL.
Comparative example 2
In comparison with example 4, the third step was not carried out, and the remaining starting materials and preparation were kept the same as in example 4.
The samples prepared in example 2 to example 4 and comparative example 1 to comparative example 2 were subjected to the test;
in the experiment, the measuring instrument fixes the diaphragm on the glass slide flatly, the diaphragm is stably placed on an observation platform of the contact angle measuring instrument, water drops are slowly dripped on the diaphragm to observe the contact angle of the diaphragm, and the average value of 3 times of measurement is taken as the result.
And (3) pure water flux test: the water flux of the composite membrane was measured using a cup ultrafilter. The composite membrane is pre-pressed for 15min under the pressure of 0.1MPa before the test. The water flux was calculated as formula J = V/(S × t). Wherein, the water flux of the membrane under the pressure of J-0.1 MPa; v-volume of permeate within time t; s-effective measurement area of the membrane; t-measurement time.
The membrane sample is immersed in a suspension containing E.coli bacteria (10) 7 CFU/mL) for 24h, and testing the antibacterial rate.
The test results are shown in table 1 below:
TABLE 1
| Item | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 |
| Contact Angle/° | 48.8 | 48.2 | 48.1 | 58.4 | 51.4 |
| Pure water flux/(L.m) -2 ·h -1 ) | 192 | 195 | 195 | 177 | 182 |
| Antibacterial ratio/%) | 95 | 95 | 95 | 95 | - |
According to test data, the ultrafiltration membrane for treating the acrylic resin wastewater, which is prepared by the invention, has good hydrophilicity, permeability and antibacterial property; is more beneficial to prolonging the service life.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (7)
1. An ultrafiltration membrane for treating acrylic resin wastewater is characterized by being prepared by the following steps:
firstly, mixing modified nano-cellulose and deionized water, carrying out ultrasonic dispersion, setting the temperature to be 80 ℃, adding amino-POSS, maintaining the temperature to be 70-80 ℃ after the amino-POSS is added, reacting for 3-4h, and carrying out freeze drying after the reaction is finished to obtain a hydrophilic modifier;
secondly, adding a hydrophilic modifier into N, N-dimethylacetamide, performing ultrasonic dispersion, then adding a pore-forming agent and polyether sulfone, setting the temperature at 60 ℃, stirring for 2-3h, then performing air defoaming for 35-45min to obtain a membrane casting solution, pouring the membrane casting solution onto a glass plate, scraping the membrane by using a membrane scraping machine, naturally volatilizing, and performing coagulation bath deionized water phase conversion to obtain a basement membrane;
and thirdly, soaking the base membrane in acetone for 5 seconds, taking out the base membrane, adding the base membrane into a mixed solution a of methyl acrylate and deionized water, adding an initiator, irradiating for 5 minutes by using ultraviolet light, taking out the base membrane, washing and drying the base membrane, adding the base membrane into a mixed solution b of an antibacterial agent and N, N-dimethylformamide, heating the mixture to 70 ℃, carrying out oscillation reaction for 48 hours, washing and drying in vacuum to obtain the ultrafiltration membrane for treating the acrylic resin wastewater.
2. The ultrafiltration membrane for acrylic resin wastewater treatment as claimed in claim 1, wherein the amount ratio of the modified nanocellulose, the amino-POSS and the deionized water in the first step is 0.05g:0.1-0.15g:80mL.
3. The ultrafiltration membrane for acrylic resin wastewater treatment as claimed in claim 1, wherein the pore-forming agent is PEG2000, and the amount ratio of the hydrophilic modifier, the pore-forming agent, the polyethersulfone and the N, N-dimethylacetamide in the second step is 0.1-0.2g:1.6g:20g:80mL.
4. The ultrafiltration membrane for acrylic resin wastewater treatment as claimed in claim 1, wherein the amount ratio of the methyl acrylate to the deionized water in the mixed solution a of the methyl acrylate and the deionized water in the third step is 1g;10mL; the dosage ratio of the initiator to the mixed liquid a is 50mmol:1L; the dosage ratio of the antibacterial agent to the N, N-dimethylformamide in the mixed solution b of the antibacterial agent and the N, N-dimethylformamide is 1g:3mL.
5. The ultrafiltration membrane for acrylic resin wastewater treatment as claimed in claim 1, wherein the modified nanocellulose is prepared by the following steps:
mixing the nano-cellulose and a sodium hydroxide aqueous solution, performing ultrasonic dispersion for 30min, then heating to 60 ℃, stirring and dispersing for 30min, adding epoxy chloropropane, keeping the temperature unchanged, continuously stirring for reaction for 2h, and performing freeze drying after the reaction is finished to obtain the modified nano-cellulose.
6. The ultrafiltration membrane for acrylic resin wastewater treatment as claimed in claim 1, wherein the amino-POSS is prepared by the following steps:
under the protection of nitrogen, H-POSS and toluene are mixed, acrylamide and a Kanster catalyst with the mass fraction of 0.2% are added, the temperature is set to be 50 ℃, the reaction is carried out for 12 hours, after the reaction is finished, the reaction is cooled to the room temperature, the catalyst is adsorbed by active carbon, and then the solvent is removed through rotary evaporation, so that the amino-POSS is obtained.
7. The ultrafiltration membrane for acrylic resin wastewater treatment as claimed in claim 1, wherein the antibacterial agent is prepared by the following steps:
adding 50% by mass of polyethyleneimine aqueous solution and N-methyl-N, N-diallyl-N-dodecyl ammonium chloride into a solvent, adjusting the pH value to 12, setting the temperature to 80 ℃, stirring for 48h, dialyzing for 48h by using a dialysis bag with the molecular weight cutoff of 1000, and after the dialysis is finished, carrying out vacuum drying at 80 ℃ to obtain the antibacterial agent.
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| CN202211267118.1A CN115569539A (en) | 2022-10-17 | 2022-10-17 | Ultrafiltration membrane for treating acrylic resin wastewater |
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| CN202211267118.1A CN115569539A (en) | 2022-10-17 | 2022-10-17 | Ultrafiltration membrane for treating acrylic resin wastewater |
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| CN202211267118.1A Pending CN115569539A (en) | 2022-10-17 | 2022-10-17 | Ultrafiltration membrane for treating acrylic resin wastewater |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115920658A (en) * | 2023-01-15 | 2023-04-07 | 安徽科博瑞环境科技有限公司 | Low-surface-energy anti-pollution hollow fiber membrane and preparation method thereof |
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2022
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115920658A (en) * | 2023-01-15 | 2023-04-07 | 安徽科博瑞环境科技有限公司 | Low-surface-energy anti-pollution hollow fiber membrane and preparation method thereof |
| CN115920658B (en) * | 2023-01-15 | 2023-10-20 | 安徽科博瑞环境科技有限公司 | Low-surface-energy anti-pollution hollow fiber membrane and preparation method thereof |
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