CN113209828B - Antibacterial ultrafiltration membrane and preparation method thereof - Google Patents
Antibacterial ultrafiltration membrane and preparation method thereof Download PDFInfo
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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
- B01D69/12—Composite membranes; Ultra-thin membranes
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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
- B01D71/80—Block polymers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/08—Copolymers of ethene
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- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/06—Polyamides derived from polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses an antibacterial ultrafiltration membrane, which comprises the following raw materials: ethylene-vinyl acetate copolymer, polyacrylate, polytetramethylene adipamide, alkyl amide phthalate, triisooctyl phosphite, propylene glycol monolaurate, 2-hydroxy-4-methoxybenzophenone, 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 4-amino-2, 1, 3-benzothiadiazole, polytetrafluoroethylene, decanoyl acetaldehyde, 4-isopropyl-2-hydroxy-cycloheptyl-2, 4, 6-trien-1-one, nanosilver ions, silane coupling agent, antibacterial agent, organic solvent, leveling agent, and pore-forming agent. The invention also discloses a preparation method of the antibacterial ultrafiltration membrane. The antibacterial effect of the ultrafiltration membrane is ensured by the matching use of the nano silver ions and the antibacterial agent; through the combined action of various raw materials, the overall strength of the ultrafiltration membrane is improved, the thickness of a single-layer ultrafiltration membrane is thinner, and the filtering antibacterial effect is better after the multi-layer ultrafiltration membrane is compounded.
Description
Technical Field
The invention relates to the technical field of ultrafiltration membranes, in particular to an antibacterial ultrafiltration membrane and a preparation method thereof.
Background
With the rapid development of economy in China, water resources become more and more the restricting factor of the economic development, so that the reduction of sewage discharge and the recycling of waste water become a necessary trend. At present, a plurality of methods for treating wastewater exist, the methods have the defects of low effluent quality, poor stability, large occupied area and the like, the method for recycling the wastewater by using a membrane separation technology is a commonly used method at present, and the membrane separation technology is widely applied to the fields of water resource utilization, biological medicine preparation, food production and environmental purification due to the advantages of low energy consumption, low cost, simple separation device, easy operation, simple manufacture, easy combination with other separation technologies and the like.
Ultrafiltration membranes are widely used for separation of macromolecular compositions and low molecular mass substances, and are very common in the field of water treatment. The ultrafiltration membrane inevitably encounters the problem of membrane pollution along with the prolonging of the service time in the use process. The ultrafiltration membrane can adsorb microorganisms in the use process, and the microorganisms propagate on the surface of the ultrafiltration membrane in a large quantity, so that the membrane flux and the separation performance are greatly reduced, the service life of the ultrafiltration membrane is greatly reduced, and the filtration and purification effects on water quality are also influenced. Therefore, development of an ultrafiltration membrane having antibacterial properties is urgently required.
Disclosure of Invention
The invention aims to provide an antibacterial ultrafiltration membrane to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
an antibacterial ultrafiltration membrane comprises the following raw materials in parts by weight: 80-120 parts of ethylene-vinyl acetate copolymer, 5-10 parts of polyacrylate, 2-5 parts of polytetramethylene adipamide, 3-7 parts of phthalic acid alkylamide, 2-5 parts of triisooctyl phosphite, 3-6 parts of propylene glycol monolaurate, 1-2 parts of 2-hydroxy-4-methoxybenzophenone, 1-2 parts of 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 1-2 parts of 4-amino-2, 1, 3-benzothiadiazole, 8-14 parts of polytetrafluoroethylene, 3-5 parts of decanoyl acetaldehyde, 2-3 parts of 4-isopropyl-2-hydroxy-cycloheptyl-2, 4,6 trien-1-one, 0.2-0.5 part of nano silver ion, and the like, 0.4-0.8 part of silane coupling agent, 0.3-0.5 part of antibacterial agent, 6-10 parts of organic solvent, 2-4 parts of flatting agent and 0.5-1 part of pore-forming agent.
As a further scheme of the invention: the feed comprises the following raw materials in parts by weight: 90-110 parts of ethylene-vinyl acetate copolymer, 6-8 parts of polyacrylate, 3-4 parts of polytetramethylene adipamide, 4-6 parts of alkyl amide phthalate, 3-4 parts of triisooctyl phosphite, 3-5 parts of propylene glycol monolaurate, 1.2-1.8 parts of 2-hydroxy-4-methoxybenzophenone, 1.2-1.7 parts of 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 1.4-1.6 parts of 4-amino-2, 1, 3-benzothiadiazole, 9-12 parts of polytetrafluoroethylene, 3.5-4.5 parts of decanoyl acetaldehyde, 2.2-2.7 parts of 4-isopropyl-2-hydroxy-cycloheptyl-2, 4,6 trien-1-one and 0.3-0.4 part of nano silver ions, 0.5-0.7 part of silane coupling agent, 0.4-0.5 part of antibacterial agent, 7-9 parts of organic solvent, 2.5-3.5 parts of flatting agent and 0.6-0.8 part of pore-forming agent.
As a still further scheme of the invention: 100 parts of ethylene-vinyl acetate copolymer, 7 parts of polyacrylate, 4 parts of polytetramethylene adipamide, 5 parts of phthalic acid alkylamide, 3 parts of triisooctyl phosphite, 4 parts of propylene glycol monolaurate, 1.5 parts of 2-hydroxy-4-methoxybenzophenone, 1.6 parts of 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 1.6 parts of 4-amino-2, 1, 3-benzothiadiazole, 11 parts of polytetrafluoroethylene, 4 parts of decanoyl acetaldehyde, 2.5 parts of 4-isopropyl-2-hydroxy-cycloheptyl-2, 4, 6-triene-1-one, 0.3 part of nano silver ions, 0.6 part of silane coupling agent, 0.4 part of antibacterial agent, 8 parts of organic solvent, 3 parts of leveling agent and 0.7 part of pore-making agent.
As a still further scheme of the invention: the organic solvent is at least one of N, N-dimethylformamide and N-methylpyrrolidone.
As a still further scheme of the invention: the antibacterial agent is at least one of o-hydroxycyclopentendione and tetrachloro-p-quinone.
The preparation method of the antibacterial ultrafiltration membrane comprises the following steps:
1) dissolving 2-hydroxy-4-methoxybenzophenone, 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 4-amino-2, 1, 3-benzothiadiazole and 4-isopropyl-2-hydroxy-cycloheptyl-2, 4, 6-triene-1-one in an organic solvent, adding the solution into a reaction kettle, heating to 80-90 ℃, reacting for 3-5h, heating to 260-280 ℃, reducing the pressure to 100-200Pa, reacting for 8-10h, cooling to room temperature, and recovering the normal pressure state to obtain a reaction solution;
2) uniformly mixing ethylene-vinyl acetate copolymer, polyacrylate, polytetramethylene adipamide, alkyl amide phthalate, triisooctyl phosphite, propylene glycol monolaurate, polytetrafluoroethylene, decanoyl acetaldehyde and a silane coupling agent, adding the mixture into an open mill, mixing for 6-10min at the mixing temperature of 100-120 ℃, mixing for 10-15min, and cooling to obtain a mixed product;
3) crushing the mixing product obtained in the step 2), sieving the crushed mixing product with a 300-mesh and 400-mesh sieve, adding the reaction liquid obtained in the step 1), adding nano silver ions, an antibacterial agent, a leveling agent and a pore-forming agent, stirring the mixture for 10 to 15min at the rotating speed of 600-mesh and 800r/min, heating the mixture to 80 to 100 ℃, performing ultrasonic dispersion for 15 to 25min, and performing vacuum defoaming to obtain a membrane casting solution;
4) uniformly scraping the casting solution obtained in the step 3) on the surface of a macroporous organic membrane to form a coating with the thickness of 15-25 mu m; standing and evaporating in air at room temperature for 1-2min, and soaking in pure water coagulation bath at 25-35 deg.C for 20-30min to precipitate coating on the surface of macroporous organic membrane to form ultrafiltration membrane.
Compared with the prior art, the invention has the beneficial effects that:
1. the antibacterial effect of the ultrafiltration membrane is ensured by the matching use of the nano silver ions and the antibacterial agent;
2. by preparing the reaction liquid in advance and then mixing the reaction liquid with the mixed material, the polymerization effect between the ultrafiltration membrane and the nano silver ions is improved, the nano silver ions are not easy to fall off, the effect is good, the duration is long, and the multiplication of microorganisms can be effectively inhibited;
3. through the combined cooperation of various raw materials, the overall strength of the ultrafiltration membrane is improved, the thickness of a single-layer ultrafiltration membrane is thinner, and the filtering and antibacterial effects are better after the multi-layer ultrafiltration membrane is compounded.
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
An antibacterial ultrafiltration membrane comprises the following raw materials in parts by weight: 80 parts of ethylene-vinyl acetate copolymer, 5 parts of polyacrylate, 2 parts of polytetramethylene adipamide, 3 parts of alkyl amide phthalate, 2 parts of triisooctyl phosphite, 3 parts of propylene glycol monolaurate, 1 part of 2-hydroxy-4-methoxybenzophenone, 1 part of 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 1 part of 4-amino-2, 1, 3-benzothiadiazole, 8 parts of polytetrafluoroethylene, 3 parts of decanoyl acetaldehyde, 2 parts of 4-isopropyl-2-hydroxy-cycloheptyl-2, 4, 6-triene-1-one, 0.2 part of nano silver ions, 0.4 part of silane coupling agent, 0.3 part of antibacterial agent, 6 parts of organic solvent, 2 parts of leveling agent and 0.5 part of pore-making agent.
Wherein the organic solvent is N, N-dimethylformamide.
Wherein the antibacterial agent is o-hydroxycyclopentendione.
In this embodiment, the preparation method of the antibacterial ultrafiltration membrane comprises the following steps:
1) dissolving 2-hydroxy-4-methoxybenzophenone, 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 4-amino-2, 1, 3-benzothiadiazole and 4-isopropyl-2-hydroxy-cycloheptyl-2, 4,6 trien-1-one in an organic solvent, adding the solution into a reaction kettle, heating to 80 ℃, reacting for 3 hours, heating to 260 ℃, reducing the pressure to 100Pa, reacting for 8 hours, cooling to room temperature, and recovering to normal pressure to obtain a reaction solution;
2) uniformly mixing ethylene-vinyl acetate copolymer, polyacrylate, polytetramethylene adipamide, alkyl amide phthalate, triisooctyl phosphite, propylene glycol monolaurate, polytetrafluoroethylene, decanoyl acetaldehyde and a silane coupling agent, adding the mixture into an open mill, mixing for 6min at the mixing temperature of 100 ℃, mixing for 10min, and cooling to obtain a mixed product;
3) crushing the mixing product obtained in the step 2), sieving the crushed mixing product with a 300-mesh sieve, adding the reaction liquid obtained in the step 1), adding nano silver ions, an antibacterial agent, a leveling agent and a pore-forming agent, stirring for 10min at a rotating speed of 600r/min, heating to 80 ℃, performing ultrasonic dispersion for 15min, and performing vacuum defoaming to obtain a casting solution;
4) uniformly scraping the casting solution obtained in the step 3) on the surface of a macroporous organic membrane to form a coating with the thickness of 15 mu m; standing and evaporating in air at room temperature for 1min, and immersing in pure water coagulation bath at 25 deg.C for 20min to precipitate the coating on the surface of macroporous organic membrane to form ultrafiltration membrane.
Example 2
An antibacterial ultrafiltration membrane comprises the following raw materials in parts by weight:
90 parts of ethylene-vinyl acetate copolymer, 6 parts of polyacrylate, 3 parts of polytetramethylene adipamide, 4 parts of phthalic acid alkylamide, 3 parts of triisooctyl phosphite, 3 parts of propylene glycol monolaurate, 1.2 parts of 2-hydroxy-4-methoxybenzophenone, 1.2 parts of 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 1.6 parts of 4-amino-2, 1, 3-benzothiadiazole, 12 parts of polytetrafluoroethylene, 4.5 parts of decanoyl acetaldehyde, 2.7 parts of 4-isopropyl-2-hydroxy-cycloheptyl-2, 4, 6-triene-1-one, 0.4 part of nano silver ions, 0.7 part of silane coupling agent, 0.5 part of antibacterial agent, 9 parts of organic solvent, 3.5 parts of flatting agent and 0.8 part of pore-making agent.
Wherein the organic solvent is a mixture of N, N-dimethylformamide and N-methylpyrrolidone.
Wherein the antibacterial agent is a mixture of o-hydroxycyclopentendione and tetrachloro-p-quinone.
In this embodiment, the preparation method of the antibacterial ultrafiltration membrane comprises the following steps:
1) dissolving 2-hydroxy-4-methoxybenzophenone, 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 4-amino-2, 1, 3-benzothiadiazole and 4-isopropyl-2-hydroxy-cycloheptyl-2, 4,6 trien-1-one in an organic solvent, adding the solution into a reaction kettle, heating to 85 ℃, reacting for 4 hours, heating to 270 ℃, reducing the pressure to 150Pa, reacting for 9 hours, cooling to room temperature, and recovering to normal pressure to obtain a reaction solution;
2) uniformly mixing ethylene-vinyl acetate copolymer, polyacrylate, polytetramethylene adipamide, alkyl amide phthalate, triisooctyl phosphite, propylene glycol monolaurate, polytetrafluoroethylene, decanoyl acetaldehyde and a silane coupling agent, adding the mixture into an open mill, mixing for 8min at the mixing temperature of 110 ℃ for 12min, and cooling to obtain a mixed product;
3) crushing the mixing product obtained in the step 2), sieving the crushed mixing product with a 350-mesh sieve, adding the reaction liquid obtained in the step 1), adding nano silver ions, an antibacterial agent, a leveling agent and a pore-forming agent, stirring for 12min at the rotating speed of 700r/min, heating to 90 ℃, performing ultrasonic dispersion for 20min, and performing vacuum defoaming to obtain a casting solution;
4) uniformly scraping the casting solution obtained in the step 3) on the surface of a macroporous organic membrane to form a coating with the thickness of 20 mu m; standing and evaporating in air at room temperature for 1.5min, and then immersing in pure water coagulating bath at 30 deg.C for 25min to separate out the coating on the surface of the macroporous organic membrane to obtain the ultrafiltration membrane.
Example 3
An antibacterial ultrafiltration membrane comprises the following raw materials in parts by weight:
100 parts of ethylene-vinyl acetate copolymer, 7 parts of polyacrylate, 4 parts of poly-tetramethylene adipamide, 5 parts of alkyl amide phthalate, 3 parts of triisooctyl phosphite, 4 parts of propylene glycol monolaurate, 1.5 parts of 2-hydroxy-4-methoxybenzophenone, 1.6 parts of 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 1.6 parts of 4-amino-2, 1, 3-benzothiadiazole, 11 parts of polytetrafluoroethylene, 4 parts of decanoyl acetaldehyde, 2.5 parts of 4-isopropyl-2-hydroxy-cycloheptyl-2, 4, 6-triene-1-one, 0.3 part of nano silver ion, 0.6 part of silane coupling agent, 0.4 part of antibacterial agent, 8 parts of organic solvent, 3 parts of leveling agent and 0.7 part of pore-making agent.
Wherein the organic solvent is a mixture of N, N-dimethylformamide and N-methylpyrrolidone.
Wherein the antibacterial agent is a mixture of o-hydroxycyclopentendione and tetrachloro-p-quinone.
In this embodiment, the preparation method of the antibacterial ultrafiltration membrane comprises the following steps:
1) dissolving 2-hydroxy-4-methoxybenzophenone, 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 4-amino-2, 1, 3-benzothiadiazole and 4-isopropyl-2-hydroxy-cycloheptyl-2, 4,6 trien-1-one in an organic solvent, adding the solution into a reaction kettle, heating to 85 ℃, reacting for 4 hours, heating to 270 ℃, reducing the pressure to 150Pa, reacting for 9 hours, cooling to room temperature, and recovering to normal pressure to obtain a reaction solution;
2) uniformly mixing ethylene-vinyl acetate copolymer, polyacrylate, polytetramethylene adipamide, alkyl amide phthalate, triisooctyl phosphite, propylene glycol monolaurate, polytetrafluoroethylene, decanoyl acetaldehyde and a silane coupling agent, adding the mixture into an open mill, mixing for 8min at the mixing temperature of 110 ℃ for 12min, and cooling to obtain a mixed product;
3) crushing the mixing product obtained in the step 2), sieving the crushed mixing product with a 350-mesh sieve, adding the reaction liquid obtained in the step 1), adding nano silver ions, an antibacterial agent, a leveling agent and a pore-forming agent, stirring for 12min at the rotating speed of 700r/min, heating to 90 ℃, performing ultrasonic dispersion for 20min, and performing vacuum defoaming to obtain a casting solution;
4) uniformly scraping the casting solution obtained in the step 3) on the surface of a macroporous organic membrane to form a coating with the thickness of 20 mu m; standing and evaporating in air at room temperature for 1.5min, and immersing in pure water coagulation bath at 30 deg.C for 25min to precipitate the coating on the surface of the macroporous organic membrane to form a membrane, thereby obtaining the ultrafiltration membrane.
Example 4
An antibacterial ultrafiltration membrane comprises the following raw materials in parts by weight:
110 parts of ethylene-vinyl acetate copolymer, 8 parts of polyacrylate, 4 parts of polytetramethylene adipamide, 6 parts of phthalic acid alkylamide, 4 parts of triisooctyl phosphite, 5 parts of propylene glycol monolaurate, 1.8 parts of 2-hydroxy-4-methoxybenzophenone, 1.7 parts of 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 1.6 parts of 4-amino-2, 1, 3-benzothiadiazole, 9 parts of polytetrafluoroethylene, 3.5 parts of decanoyl acetaldehyde, 2.2 parts of 4-isopropyl-2-hydroxy-cycloheptyl-2, 4, 6-triene-1-one, 0.3 part of nano silver ions, 0.5 part of silane coupling agent, 0.4 part of antibacterial agent, 7 parts of organic solvent, 2.5 parts of flatting agent and 0.6 part of pore-making agent.
Wherein the organic solvent is a mixture of N, N-dimethylformamide and N-methylpyrrolidone.
Wherein the antibacterial agent is a mixture of o-hydroxycyclopentendione and tetrachloro-p-quinone.
In this embodiment, the preparation method of the antibacterial ultrafiltration membrane comprises the following steps:
1) dissolving 2-hydroxy-4-methoxybenzophenone, 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 4-amino-2, 1, 3-benzothiadiazole and 4-isopropyl-2-hydroxy-cycloheptyl-2, 4,6 trien-1-one in an organic solvent, adding the solution into a reaction kettle, heating to 85 ℃, reacting for 4 hours, heating to 270 ℃, reducing the pressure to 150Pa, reacting for 9 hours, cooling to room temperature, and recovering to normal pressure to obtain a reaction solution;
2) uniformly mixing ethylene-vinyl acetate copolymer, polyacrylate, polytetramethylene adipamide, alkyl amide phthalate, triisooctyl phosphite, propylene glycol monolaurate, polytetrafluoroethylene, decanoyl acetaldehyde and a silane coupling agent, adding the mixture into an open mill, mixing for 8min at the mixing temperature of 110 ℃ for 12min, and cooling to obtain a mixed product;
3) crushing the mixing product obtained in the step 2), sieving the crushed mixing product with a 350-mesh sieve, adding the reaction liquid obtained in the step 1), adding nano silver ions, an antibacterial agent, a leveling agent and a pore-forming agent, stirring for 12min at the rotating speed of 700r/min, heating to 90 ℃, performing ultrasonic dispersion for 20min, and performing vacuum defoaming to obtain a casting solution;
4) uniformly scraping the casting solution obtained in the step 3) on the surface of a macroporous organic membrane to form a coating with the thickness of 20 mu m; standing and evaporating in air at room temperature for 1.5min, and immersing in pure water coagulation bath at 30 deg.C for 25min to precipitate the coating on the surface of the macroporous organic membrane to form a membrane, thereby obtaining the ultrafiltration membrane.
Example 5
An antibacterial ultrafiltration membrane comprises the following raw materials in parts by weight:
120 parts of ethylene-vinyl acetate copolymer, 10 parts of polyacrylate, 5 parts of poly-tetramethylene adipamide, 7 parts of alkyl amide phthalate, 5 parts of triisooctyl phosphite, 6 parts of propylene glycol monolaurate, 2 parts of 2-hydroxy-4-methoxybenzophenone, 2 parts of 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 2 parts of 4-amino-2, 1, 3-benzothiadiazole, 14 parts of polytetrafluoroethylene, 5 parts of decanoyl acetaldehyde, 3 parts of 4-isopropyl-2-hydroxy-cycloheptyl-2, 4, 6-triene-1-one, 0.5 part of nano silver ion, 0.8 part of silane coupling agent, 0.5 part of antibacterial agent, 10 parts of organic solvent, 4 parts of flatting agent and 1 part of pore-making agent.
Wherein the organic solvent is N-methyl pyrrolidone.
Wherein the antibacterial agent is tetrachloro-p-quinone.
In this embodiment, the preparation method of the antibacterial ultrafiltration membrane comprises the following steps:
1) dissolving 2-hydroxy-4-methoxybenzophenone, 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 4-amino-2, 1, 3-benzothiadiazole and 4-isopropyl-2-hydroxy-cycloheptyl-2, 4,6 trien-1-one in an organic solvent, adding the solution into a reaction kettle, heating to the temperature, reacting for 5 hours, heating to 280 ℃, reducing the pressure to 200Pa, reacting for 10 hours, cooling to room temperature, and recovering to the normal pressure state to obtain a reaction solution;
2) uniformly mixing ethylene-vinyl acetate copolymer, polyacrylate, polytetramethylene adipamide, alkyl amide phthalate, triisooctyl phosphite, propylene glycol monolaurate, polytetrafluoroethylene, decanoyl acetaldehyde and a silane coupling agent, adding the mixture into an open mill, mixing for 10min at the mixing temperature of 120 ℃ for 15min, and cooling to obtain a mixed product;
3) crushing the mixing product obtained in the step 2), sieving with a 400-mesh sieve, adding the reaction liquid obtained in the step 1), adding nano silver ions, an antibacterial agent, a leveling agent and a pore-forming agent, stirring at the rotating speed of 800r/min for 15min, heating to 100 ℃, performing ultrasonic dispersion for 25min, and performing vacuum defoaming to obtain a casting solution;
4) uniformly scraping the casting solution obtained in the step 3) on the surface of a macroporous organic membrane to form a coating with the thickness of 25 mu m; standing and evaporating in air at room temperature for 2min, and immersing in pure water coagulation bath at 35 deg.C for 30min to precipitate the coating on the surface of the macroporous organic membrane to form a membrane, thereby obtaining the ultrafiltration membrane.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (6)
1. The antibacterial ultrafiltration membrane is characterized by comprising the following raw materials in parts by weight: 80-120 parts of ethylene-vinyl acetate copolymer, 5-10 parts of polyacrylate, 2-5 parts of polytetramethylene adipamide, 3-7 parts of phthalic acid alkylamide, 2-5 parts of triisooctyl phosphite, 3-6 parts of propylene glycol monolaurate, 1-2 parts of 2-hydroxy-4-methoxybenzophenone, 1-2 parts of 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 1-2 parts of 4-amino-2, 1, 3-benzothiadiazole, 8-14 parts of polytetrafluoroethylene, 3-5 parts of decanoyl acetaldehyde, 2-3 parts of 4-isopropyl-2-hydroxy-cycloheptyl-2, 4,6 trien-1-one, 0.2-0.5 part of nano silver ion, and the like, 0.4-0.8 part of silane coupling agent, 0.3-0.5 part of antibacterial agent, 6-10 parts of organic solvent, 2-4 parts of flatting agent and 0.5-1 part of pore-forming agent.
2. The antibacterial ultrafiltration membrane of claim 1, which is characterized by comprising the following raw materials in parts by weight: 90-110 parts of ethylene-vinyl acetate copolymer, 6-8 parts of polyacrylate, 3-4 parts of polytetramethylene adipamide, 4-6 parts of alkyl amide phthalate, 3-4 parts of triisooctyl phosphite, 3-5 parts of propylene glycol monolaurate, 1.2-1.8 parts of 2-hydroxy-4-methoxybenzophenone, 1.2-1.7 parts of 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 1.4-1.6 parts of 4-amino-2, 1, 3-benzothiadiazole, 9-12 parts of polytetrafluoroethylene, 3.5-4.5 parts of decanoyl acetaldehyde, 2.2-2.7 parts of 4-isopropyl-2-hydroxy-cycloheptyl-2, 4,6 trien-1-one and 0.3-0.4 part of nano silver ions, 0.5-0.7 part of silane coupling agent, 0.4-0.5 part of antibacterial agent, 7-9 parts of organic solvent, 2.5-3.5 parts of flatting agent and 0.6-0.8 part of pore-forming agent.
3. The antibacterial ultrafiltration membrane of claim 2, which is characterized by comprising the following raw materials in parts by weight: 100 parts of ethylene-vinyl acetate copolymer, 7 parts of polyacrylate, 4 parts of polytetramethylene adipamide, 5 parts of phthalic acid alkylamide, 3 parts of triisooctyl phosphite, 4 parts of propylene glycol monolaurate, 1.5 parts of 2-hydroxy-4-methoxybenzophenone, 1.6 parts of 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 1.6 parts of 4-amino-2, 1, 3-benzothiadiazole, 11 parts of polytetrafluoroethylene, 4 parts of decanoyl acetaldehyde, 2.5 parts of 4-isopropyl-2-hydroxy-cycloheptyl-2, 4, 6-triene-1-one, 0.3 part of nano silver ions, 0.6 part of silane coupling agent, 0.4 part of antibacterial agent, 8 parts of organic solvent, 3 parts of leveling agent and 0.7 part of pore-making agent.
4. The antimicrobial ultrafiltration membrane of claim 1, wherein the organic solvent is at least one of N, N-dimethylformamide and N-methylpyrrolidinone.
5. The antimicrobial ultrafiltration membrane of claim 4, wherein the antimicrobial agent is at least one of o-hydroxycyclopentendione and tetrachloro-p-quinone.
6. A method of preparing an antimicrobial ultrafiltration membrane according to any of claims 1 to 5 comprising the steps of:
1) dissolving 2-hydroxy-4-methoxybenzophenone, 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole, 4-amino-2, 1, 3-benzothiadiazole and 4-isopropyl-2-hydroxy-cycloheptyl-2, 4, 6-triene-1-one in an organic solvent, adding the solution into a reaction kettle, heating to 80-90 ℃, reacting for 3-5h, heating to 260-280 ℃, reducing the pressure to 100-200Pa, reacting for 8-10h, cooling to room temperature, and recovering the normal pressure state to obtain a reaction solution;
2) uniformly mixing ethylene-vinyl acetate copolymer, polyacrylate, polytetramethylene adipamide, alkyl amide phthalate, triisooctyl phosphite, propylene glycol monolaurate, polytetrafluoroethylene, decanoyl acetaldehyde and a silane coupling agent, adding the mixture into an open mill, mixing for 6-10min at the mixing temperature of 100-120 ℃, mixing for 10-15min, and cooling to obtain a mixed product;
3) crushing the mixing product obtained in the step 2), sieving the crushed mixing product with a 300-mesh and 400-mesh sieve, adding the reaction liquid obtained in the step 1), adding nano silver ions, an antibacterial agent, a leveling agent and a pore-forming agent, stirring the mixture for 10 to 15min at the rotating speed of 600-mesh and 800r/min, heating the mixture to 80 to 100 ℃, performing ultrasonic dispersion for 15 to 25min, and performing vacuum defoaming to obtain a membrane casting solution;
4) uniformly scraping the casting solution obtained in the step 3) on the surface of a macroporous organic membrane to form a coating with the thickness of 15-25 mu m; standing and evaporating in air at room temperature for 1-2min, and soaking in pure water coagulation bath at 25-35 deg.C for 20-30min to precipitate coating on the surface of macroporous organic membrane to form ultrafiltration membrane.
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| CN102553466A (en) * | 2011-12-26 | 2012-07-11 | 东北林业大学 | Antimicrobial polysulphone flat ultrafiltration membrane and preparation method thereof |
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