CN104437140B - Nano aramid fiber reinforced polysulfone membrane and preparation method and application thereof - Google Patents
Nano aramid fiber reinforced polysulfone membrane and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a nano aramid fiber reinforced polysulfone membrane and a preparation method and application thereof. The method comprises adding aramid fiber, alkali and auxiliary into organic solvent, and performing heating and uniform stirring to obtain nano aramid fiber solution; then blending the nano aramid fiber with polysulfone, producing the nano aramid fiber reinforced polysulfone membrane by polysorbate-20 or polyethylene glycol as the additive and through the phase inversion method. In the prepared polysulfone membrane, the nano aramid fiber serves as support materials to form a grid structure, so that the mechanical property and the fatigue durability of the polysulfone membrane can be greatly enhanced; meanwhile, the nano aramid fiber has little influence on the water flux and the rejection performance of the polysulfone membrane. By enhancing the mechanical property and the fatigue durability of the polysulfone membrane, the application range of the polysulfone membrane can be widened to a great extent.
Description
Technical field
The invention belongs to field of compound material, the enhanced polysulfone membrane of more particularly, to a kind of aramid nano-fiber and its preparation side
Method and application.
Background technology
With social development, substantial amounts of natural water is polluted by sanitary wastewater and industrial wastewater, particularly weeding
Agent, insecticide, bacteria remover, heat exchange catalyst, the extensive application of insulator, cause and contain a large amount of high-concentration hardly-degradables in waste water
Organic substance, this certainly will cause water pollution, the environment that impact people depend on for existence.In addition, with the increase of population, scientific and technological sends out
Exhibition, people are increasing to the demand of fresh water, and the freshwater resources that the earth is provided that are more and more rare, therefore the depth to waste water
Degree processes and recycles, and improves the utilization rate of water resource, solves the problems, such as that current hydropenia difficulty is national governments' all very concerns.And
Advanced treating industrial and agricultural wastewater is that the waste water treatment process such as traditional coagulation, precipitation, filtration and sterilization are implacable.
Membrane ultrafiltration technology has the advantages that separation efficiency is high, equipment is simple and convenient to operate because of it, no phase transformation and energy-conservation, because
This is paid attention to by relevant scientific research personnel, and shows great application potential in field of Environment Protection, will necessarily become waste water from now on
The important method processing.Various membrane materials have been widely used in the wastewater treatment in food and medicine industry at present, and normal
Ultrafiltration membrane material mainly has polysulfones, polrvinyl chloride, Kynoar, polyacrylonitrile etc..Polysulfones is even more wide at present
The ultrafiltration membrane material of general application, it has cheap and easy to get, good chemical stability, electrical insulating property, resistance to water, thermostability, chi
Very little stable and preferable film property and mechanical strength.But ultrafilter membrane is with pressure as motive force, therefore it is required that membrane material will have
There are excellent mechanical property, fatigue performance, although polysulfone membrane has preferable mechanical strength, but its tensile strength
Only 5MPa about, and the anti-fatigue performance of polysulfone membrane is bad.Therefore wanting preparation no backing material polysulfone membrane needs into one
Step improves mechanical property and the fatigue resistance of polysulfone membrane.
And it is a kind of new high-tech synthetic fibers that aramid fiber has, there are superhigh intensity, high-moduluss and high temperature resistant, acidproof resistance to
The premium properties such as alkali, lightweight, insulation, aging resistance, life cycle length, be widely used in composite, ballistic-resistant article, building materials,
The fields such as special type protection clothing, electronic equipment.Research US 20130288050 A1 before once reported dissolving aramid fiber system
For obtaining aramid nano-fiber, then there is excellent mechanical property using the aramid fiber film that LBL self assembly has prepared.Cause
This, aramid nano-fiber can be used for mechanical strength, the anti-fatigue performance strengthening polysulfone membrane, thus preparing high-performance polysulfones
Film, extensively improves range of application in ultrafiltration and reverse osmosiss for the polysulfone membrane.
Content of the invention
In order to overcome shortcoming and the deficiency on existing polysulfones film dynamic performance and fatigue performance, it is an object of the invention to
A kind of preparation method of the enhanced polysulfone membrane of aramid nano-fiber is provided.The method is blended into polysulfones using aramid nano-fiber
Film, thus obtain a kind of high intensity polysulfone membrane.
Another object of the present invention is to providing the enhanced polysulfones of aramid nano-fiber obtaining by above-mentioned preparation method
Film.This polysulfone membrane has more preferable thermostability, high chemical stability.
It is still another object of the present invention to provide the application of the enhanced polysulfone membrane of above-mentioned aramid nano-fiber.
The purpose of the present invention is achieved through the following technical solutions：A kind of preparation side of the enhanced polysulfone membrane of aramid nano-fiber
Method, comprises the following steps：
(1) aramid fiber, alkali and auxiliary agent are added in organic solvent, heated and stirred uniformly, obtains aramid nano-fiber molten
Liquid；
(2) polysulfones and additive are added in the aramid nano-fiber solution obtaining to step (1), heating for dissolving stirring is all
Even, then standing and defoaming, obtain casting solution；
(3) casting solution obtaining step (2) is uniformly poured on base material, then scratches film forming, then puts into base material
In constant temperature ultrafiltration water, standing, obtain the enhanced polysulfone membrane of aramid nano-fiber.
In the present invention, described aramid fiber is preferably aramid fiber Kevlar49；
In the present invention, described organic solvent is intensive polar solvent；
Preferably, described organic solvent is preferably DMF (DMF), dimethyl sulfoxide (DMSO), N-
At least one in methyl pyrrolidone (NMP) and DMAC N,N' dimethyl acetamide (DMAC).
In the present invention, described alkali is organic or inorganic highly basic；
Preferably, described alkali is preferably potassium tert-butoxide, sodium hydride, hydrofining, sodium hydroxide, potassium hydroxide and Sodium ethylate
In at least one；
The consumption of described alkali is preferably 60%～300% of amido link mole in aramid fiber.
In the present invention, described auxiliary agent refers to small molecule proton translocation agent；
Preferably, described auxiliary agent is preferably at least one in water, ethanol, methanol and propanol；
The consumption of described auxiliary agent is preferably 100%～600% of amido link mole in aramid fiber；
The condition of the heated and stirred described in step (1) is preferably and stirs 1～4 day at 30～50 DEG C.
In aramid nano-fiber solution described in step (1), the concentration of aramid fiber is preferably 2～5wt/v%；
In the present invention, described polysulfones is preferably polyether sulfone；
Described aramid fiber is preferably (0.1～0.3) with the mass ratio of polysulfones：1.
In the present invention, described additive is water-soluble polymer；
Preferably, described additive is preferably at least one in tween 20 and Polyethylene Glycol；
The temperature of the heating described in step (2) is preferably 40～80 DEG C；
The condition of the standing described in step (2) is preferably room temperature and stands 1 day；
In casting solution described in step (2), the concentration of polysulfones is preferably 15～20wt/v%；
In casting solution described in step (2), the concentration of additive is 5～15wt/v%.
In the present invention, the base material described in step (3) is preferably glass plate base material；
The thickness of described blade coating film forming is preferably 300 μm；
The condition of the standing described in step (3) is preferably 30 DEG C of standing 10～60min；
Application in ultrafiltration for the enhanced polysulfone membrane of described aramid nano-fiber.
The mechanism of the present invention is：
The present invention obtains aramid nano-fiber by dissolving aramid fiber, and the aramid nano-fiber then dissolving is with polysulfones altogether
Mixed, form casting solution, polysulfone membrane is obtained by the method for phase transfer, aramid nano-fiber plays reinforcing bar in the polysulfone membrane of preparation
Skeleton function, thus obtain high intensity polysulfone membrane.
The present invention, with respect to prior art, has such advantages as and effect：
(1) present invention introduces aramid nano-fiber in polysulfone membrane, using the excellent mechanical performance of aramid fiber, makes polysulfones is obtained
The mechanical property of film is greatly improved.
(2) in the present invention, aramid nano-fiber constitutes network structure in polysulfone membrane, simultaneously aramid nano-fiber and polysulfones
Preferably, aramid nano-fiber is wrapped up by bulk material, is not susceptible to come off, the use of the polysulfone membrane greatly increasing for the compatibility of film
Life-span.
(3) due in the present invention aramid fiber have superhigh intensity, high-moduluss and high temperature resistant, acid-fast alkali-proof, lightweight, insulation,
The premium properties such as aging resistance, life cycle length, therefore being added in of the fiber of aramid fiber nanometer greatly enhance polysulfone membrane
Performance.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention not limited to this.
Wt/v in embodiment refers to g/mL.
Embodiment 1：The preparation of polysulfone membrane
(1) polyether sulfone (the S3010 type polysulfones of BASF Aktiengesellschaft, shearing point are added in dimethyl sulfoxide (DMSO)
Son is measured as 50000Da) and Polyethylene Glycol, 50 DEG C are uniformly mixing to obtain casting solution, and the wherein concentration of polyether sulfone is 20wt/v%, gathers
The concentration of ethylene glycol is 10wt/v%.
(2) casting solution is uniformly poured on glass plate, then utilizes scraper to scratch film forming, film thickness is 300 μm, then
Glass plate is put in constant temperature ultrafiltration water, temperature is 30 DEG C, stand 30min, obtain polysulfone membrane.
The tensile strength testing this film is 5～8MPa.Preferably, fenestra is evenly distributed obtained polysulfone membrane pore-creating character, 1g/L
In bovine serum albumin buffer retention experiments, flux can maintain 215L/ (m2H), rejection is 99%.
Embodiment 2：A kind of preparation of the enhanced polysulfone membrane of aramid nano-fiber
(1) potassium tert-butoxide, methanol are added in dimethyl sulfoxide (DMSO), (Dupont is public to be subsequently adding Kevlar fiber
Department buys), stir 1 day at 30 DEG C, compound concentration is the aramid nano-fiber solution of 2wt/v%, the addition of potassium tert-butoxide is
The 60% of polyfiber amide key mole, the addition of methanol is the 100% of polyfiber amide key mole.
(2) add the polyether sulfone (S3010 of BASF Aktiengesellschaft in the aramid nano-fiber solution obtaining to step (1)
Type polysulfones, shearing molecular weight is 50000Da) and Polyethylene Glycol, 80 DEG C stir, and then room temperature stands deaeration in 1 day, is cast
Film liquid, in casting solution, the concentration of polyether sulfone is 20wt/v%, and the concentration of Polyethylene Glycol is 10wt/v%.
(3) casting solution obtaining step (2) is uniformly poured on glass plate, then utilizes scraper to scratch film forming, thickness
Spend for 300 μm, then glass plate is put in constant temperature ultrafiltration water, temperature is 30 DEG C, stand 10min, obtain aramid nano-fiber
Enhanced polysulfone membrane.
The tensile strength of this film is 30～35MPa.Obtained polysulfone membrane becomes sky preferably, and fenestra is evenly distributed, 1g/L cattle
In serum albumin buffer retention experiments, flux can maintain 215L/ (m2H), rejection is 99%.
Embodiment 3：A kind of preparation of the enhanced polysulfone membrane of aramid nano-fiber
(1) potassium tert-butoxide, ethanol are added in dimethyl sulfoxide (DMSO), (Dupont is public to be subsequently adding Kevlar fiber
Department buys), stir 2 days at 40 DEG C, compound concentration is the aramid nano-fiber solution of 3wt/v%, the addition of potassium tert-butoxide is
The 150% of polyfiber amide key mole, the addition of ethanol is the 400% of polyfiber amide key mole.
(2) add the polyether sulfone (S3010 of BASF Aktiengesellschaft in the aramid nano-fiber solution obtaining to step (1)
Type polysulfones, shearing molecular weight is 50000Da) and Polyethylene Glycol, 40 DEG C stir, and then room temperature stands deaeration in 1 day, is cast
Film liquid, in casting solution, the concentration of polyether sulfone is 18wt/v%, and the concentration of Polyethylene Glycol is 15wt/v%.
(3) casting solution obtaining step (2) is uniformly poured on glass plate, then utilizes scraper to scratch film forming, thickness
Spend for 300 μm, then glass plate is put in constant temperature ultrafiltration water, temperature is 30 DEG C, stand 30min, obtain aramid nano-fiber
Enhanced polysulfone membrane.
The tensile strength of this film is 40～45MPa.Obtained polysulfone membrane becomes sky preferably, and fenestra is evenly distributed, 1g/L cattle
In serum albumin buffer retention experiments, flux can maintain 267L/ (m2H), rejection is 98%.
Embodiment 4：A kind of preparation of the enhanced polysulfone membrane of aramid nano-fiber
(1) add sodium hydride, propanol in DMF (DMF), be subsequently adding Kevlar fiber (Dupont
Company buys), stir 2 days at 30 DEG C, compound concentration is the aramid nano-fiber solution of 4wt/v%, the addition of sodium hydride is
The 100% of polyfiber amide key mole, the addition of propanol is the 400% of polyfiber amide key mole.
(2) add the polyether sulfone (S3010 of BASF Aktiengesellschaft in the aramid nano-fiber solution obtaining to step (1)
Type polysulfones, shearing molecular weight is 50000Da) and Polyethylene Glycol, 70 DEG C stir, and then room temperature stands deaeration in 1 day, is cast
Film liquid, in casting solution, the concentration of polyether sulfone is 20wt/v%, and the concentration of Polyethylene Glycol is 5wt/v%.
(3) casting solution obtaining step (2) is uniformly poured on glass plate, then utilizes scraper to scratch film forming, thickness
Spend for 300 μm, then glass plate is put in constant temperature ultrafiltration water, temperature is 30 DEG C, stand 30min, obtain aramid nano-fiber
Enhanced polysulfone membrane.
The tensile strength of this film is 40～45MPa.Obtained polysulfone membrane becomes sky preferably, and fenestra is evenly distributed, 1g/L cattle
In serum albumin buffer retention experiments, flux can maintain 168L/ (m2H), rejection is 99%.
Embodiment 5：A kind of preparation of the enhanced polysulfone membrane of aramid nano-fiber
(1) sodium hydride, methanol are added in N-Methyl pyrrolidone (NMP), (Dupont is public to be subsequently adding Kevlar fiber
Department buys), stir 4 days at 50 DEG C, compound concentration is the aramid nano-fiber solution of 5wt/v%, the addition of sodium hydride is virtue
The 300% of synthetic fibre amido link mole, the addition of methanol is the 600% of polyfiber amide key mole.
(2) add the polyether sulfone (S3010 of BASF Aktiengesellschaft in the aramid nano-fiber solution obtaining to step (1)
Type polysulfones, shearing molecular weight is 50000Da) and tween 20,80 DEG C stir, and then room temperature stands deaeration in 1 day, is cast
Film liquid, in casting solution, the concentration of polyether sulfone is 20wt/v%, and tween 20 is 10wt/v%.
(3) casting solution obtaining step (2) is uniformly poured on glass plate, then utilizes scraper to scratch film forming, thickness
Spend for 300 μm, then glass plate is put in constant temperature ultrafiltration water, temperature is 30 DEG C, stand 60min, obtain aramid nano-fiber
Enhanced polysulfone membrane.
The tensile strength of this film is 30～35MPa.Obtained polysulfone membrane becomes sky preferably, and fenestra is evenly distributed, 1g/L cattle
In serum albumin buffer retention experiments, flux can maintain 215L/ (m2H), rejection is 99%.
Embodiment 6：A kind of preparation of the enhanced polysulfone membrane of aramid nano-fiber
(1) hydrofining, methanol are added in N-Methyl pyrrolidone (NMP), (Dupont is public to be subsequently adding Kevlar fiber
Department buys), stir 1 day at 30 DEG C, compound concentration is the aramid nano-fiber solution of 2wt/v%, the addition of hydrofining is virtue
The 200% of synthetic fibre amido link mole, the addition of methanol is the 200% of polyfiber amide key mole.
(2) add the polyether sulfone (S3010 of BASF Aktiengesellschaft in the aramid nano-fiber solution obtaining to step (1)
Type polysulfones, shearing molecular weight is 50000Da) and Polyethylene Glycol, 60 DEG C stir, and then room temperature stands deaeration in 1 day, is cast
Film liquid, in casting solution, the concentration of polyether sulfone is 16wt/v%, and the concentration of Polyethylene Glycol is 10wt/v%.
(3) casting solution obtaining step (2) is uniformly poured on glass plate, then utilizes scraper to scratch film forming, thickness
Spend for 300 μm, then glass plate is put in constant temperature ultrafiltration water, temperature is 30 DEG C, stand 20min, obtain aramid nano-fiber
Enhanced polysulfone membrane.
The tensile strength of this film is 32～35MPa.Obtained polysulfone membrane becomes sky preferably, and fenestra is evenly distributed, 1g/L cattle
In serum albumin buffer retention experiments, flux can maintain 198L/ (m2H), rejection is 99%.
Embodiment 7：A kind of preparation of the enhanced polysulfone membrane of aramid nano-fiber
(1) add potassium hydroxide, water in dimethyl sulfoxide, be subsequently adding Kevlar fiber (purchase of Dupont company),
Stir 1 day at 30 DEG C, compound concentration is the aramid nano-fiber solution of 3wt/v%, the addition of potassium hydroxide is polyfiber amide
The 200% of key mole, the addition of water is the 500% of polyfiber amide key mole.
(2) add the polyether sulfone (S3010 of BASF Aktiengesellschaft in the aramid nano-fiber solution obtaining to step (1)
Type polysulfones, shearing molecular weight is 50000Da) and tween 20,50 DEG C stir, and then room temperature stands deaeration in 1 day, is cast
Film liquid, in casting solution, the concentration of polyether sulfone is 15wt/v%, and the concentration of tween 20 is 15wt/v%.
(3) casting solution obtaining step (2) is uniformly poured on glass plate, then utilizes scraper to scratch film forming, thickness
Spend for 300 μm, then glass plate is put in constant temperature ultrafiltration water, temperature is 30 DEG C, stand 60min, obtain aramid nano-fiber
Enhanced polysulfone membrane.
The tensile strength of this film is 32～38MPa.Obtained polysulfone membrane becomes sky preferably, and fenestra is evenly distributed, 1g/L cattle
In serum albumin buffer retention experiments, flux can maintain 279L/ (m2H), rejection is 99%.
Embodiment 8：A kind of preparation of the enhanced polysulfone membrane of aramid nano-fiber
(1) add sodium hydroxide, water in N,N-dimethylacetamide (DMAC), be subsequently adding Kevlar fiber
(purchase of Dupont company), stirs 3 days at 40 DEG C, and compound concentration is the aramid nano-fiber solution of 4wt/v%, sodium hydroxide
Addition is the 300% of polyfiber amide key mole, and the addition of water is the 400% of polyfiber amide key mole.
(2) add the polyether sulfone (S3010 of BASF Aktiengesellschaft in the aramid nano-fiber solution obtaining to step (1)
Type polysulfones, shearing molecular weight is 50000Da) and tween 20,50 DEG C stir, and then room temperature stands deaeration in 1 day, is cast
Film liquid, in casting solution, the concentration of polyether sulfone is 15wt/v%, and the concentration of tween 20 is 10wt/v%.
(3) casting solution obtaining step (2) is uniformly poured on glass plate, then utilizes scraper to scratch film forming, thickness
Spend for 300 μm, then glass plate is put in constant temperature ultrafiltration water, temperature is 30 DEG C, stand 30min, obtain aramid nano-fiber
Enhanced polysulfone membrane.
The tensile strength of this film is 40～46MPa.Obtained polysulfone membrane becomes sky preferably, and fenestra is evenly distributed, 1g/L cattle
In serum albumin buffer retention experiments, flux can maintain 205L/ (m2H), rejection is 99%.
Embodiment 9：A kind of preparation of the enhanced polysulfone membrane of aramid nano-fiber
(1) add Sodium ethylate, ethanol in N,N-dimethylacetamide (DMAC), be subsequently adding Kevlar fiber
(purchase of Dupont company), 50 DEG C stir 4 days, compound concentration be 4wt/v% aramid nano-fiber solution, Sodium ethylate plus
Enter amount for the 200% of polyfiber amide key mole, the addition of ethanol is the 400% of polyfiber amide key mole.
(2) add the polyether sulfone (S3010 of BASF Aktiengesellschaft in the aramid nano-fiber solution obtaining to step (1)
Type polysulfones, shearing molecular weight is 50000Da) and Polyethylene Glycol, 80 DEG C stir, and then room temperature stands deaeration in 1 day, is cast
Film liquid, in casting solution, the concentration of polyether sulfone is 20wt/v%, and the concentration of Polyethylene Glycol is 10wt/v%.
(3) casting solution obtaining step (2) is uniformly poured on glass plate, then utilizes scraper to scratch film forming, thickness
Spend for 300 μm, then glass plate is put in constant temperature ultrafiltration water, temperature is 30 DEG C, stand 60min, obtain aramid nano-fiber
Enhanced polysulfone membrane.
The tensile strength of this film is 33～38MPa.Obtained polysulfone membrane becomes sky preferably, and fenestra is evenly distributed, 1g/L cattle
In serum albumin buffer retention experiments, flux can maintain 221L/ (m2H), rejection is 99%.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not subject to above-described embodiment
Limit, other any spirit without departing from the present invention and the change made under principle, modification, replacement, combine, simplify,
All should be equivalent substitute mode, be included within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of the enhanced polysulfone membrane of aramid nano-fiber is it is characterised in that comprise the following steps：
(1) aramid fiber, alkali and auxiliary agent are added in organic solvent, heated and stirred uniformly, obtains aramid nano-fiber solution；
(2) polysulfones and additive are added in the aramid nano-fiber solution obtaining to step (1), heating for dissolving stirs, so
Standing and defoaming afterwards, obtains casting solution；
(3) casting solution obtaining step (2) is uniformly poured on base material, then scratches film forming, then base material is put into constant temperature
In ultrafiltration water, standing, obtain the enhanced polysulfone membrane of aramid nano-fiber；
The consumption of described alkali is 60%～300% of amido link mole in aramid fiber；
The consumption of described auxiliary agent is 100%～600% of amido link mole in aramid fiber；
Described aramid fiber is Kevlar fiber；
Described auxiliary agent is at least one in water, ethanol, methanol and propanol；
In aramid nano-fiber solution described in step (1), the concentration of aramid fiber is 2～5wt/v%；
In casting solution described in step (2), the concentration of polysulfones is 15～20wt/v%；
In casting solution described in step (2), the concentration of additive is 5～15wt/v%；
Wt/v refers to g/mL.
2. preparation method according to claim 1 it is characterised in that：Described organic solvent is N, N- dimethyl formyl
At least one in amine, dimethyl sulfoxide, N-Methyl pyrrolidone and DMAC N,N' dimethyl acetamide.
3. preparation method according to claim 1 it is characterised in that：
Described alkali is at least one in potassium tert-butoxide, sodium hydride, hydrofining, sodium hydroxide, potassium hydroxide and Sodium ethylate.
4. preparation method according to claim 1 it is characterised in that：Described additive is tween 20 and Polyethylene Glycol
In at least one.
5. preparation method according to claim 1 it is characterised in that：The condition of the heated and stirred described in step (1) is
Stir 1～4 day at 30～50 DEG C；
The temperature of the heating described in step (2) is 40～80 DEG C；
The condition of the standing described in step (3) is 30 DEG C of standing 10～60min.
6. a kind of enhanced polysulfone membrane of aramid nano-fiber is it is characterised in that by the preparation described in any one of Claims 1 to 5
Method prepares.
7. application in ultrafiltration for the enhanced polysulfone membrane of the aramid nano-fiber described in claim 6.
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