CN108837716A - A kind of big flux modified polysulfone film and preparation method thereof - Google Patents
A kind of big flux modified polysulfone film and preparation method thereof Download PDFInfo
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- CN108837716A CN108837716A CN201810745457.3A CN201810745457A CN108837716A CN 108837716 A CN108837716 A CN 108837716A CN 201810745457 A CN201810745457 A CN 201810745457A CN 108837716 A CN108837716 A CN 108837716A
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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
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0013—Casting processes
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Abstract
The invention discloses a kind of big flux modified polysulfone films and preparation method thereof.The preparation method of big flux modified polysulfone film includes the following steps, nano graphene oxide, pore-foaming agent and dressing agent are placed in organic solvent and dispersed, and forms dispersion liquid；Polysulfones is added in dispersion liquid, heating water bath simultaneously stirs, until polysulfones dissolves, forms casting solution；After casting solution standing and defoaming, on a glass, liquid film is scraped；Liquid film is stopped into the predetermined time in air, with volatile fraction organic solvent, is put into togerther in coagulating bath together with glass plate later；Solidify to liquid film and be independently detached from glass plate and formed after diaphragm, cleans diaphragm to remove the organic solvent and pore-foaming agent in diaphragm, big flux modified polysulfone film is made.
Description
Technical field
The present invention relates to ultrafiltration membrane technique fields more particularly to a kind of big flux modified polysulfone film and preparation method thereof.
Background technique
UF membrane is the process of the sieve pore separation carried out using film pressure at both sides difference as driving force, and it is light to be widely used in seawater
The fields such as change, medical science and drinking water treatment.Between dozens to a few hundred nanometers, operating pressure difference is generally in ultrafiltration aperture
0.1MPa to 1MPa can be realized classification, the purifying of the macromoleculars such as protein, remove the virus in water, pyrogen body and naturally have
The poisonous and harmful substances such as machine object.Ultrafiltration membrane product is mostly using high molecular polymer as raw material currently on the market, and wherein PS membrane makes
With relatively wide, but because polysulfones surface hydrophilicity is poor, obtained film permeation flux is small, and rejection is low, intensity is high, practical performance not
It is good.Ultrafiltration membrane flux is generally in 20-200L/ (hm2), if wanting to further increase the water flux of ultrafiltration membrane, it will reduce film
Separating effect.
In order to break the balance limitation of ultrafiltration membrane flux and rejection, need to be modified ultrafiltration membrane.Polysulfones at present
The method of modifying of film has that modification by copolymerization, membrane material sheet is modifies, surface is modified and interfacial polymerization is modified.Modification by copolymerization, this structural reform
The step of property more, complex process.Surface is modified to need radiation or low temperature plasma irradiation film surface to generate hydroxyl radical free radical
To achieve the purpose that grafting, equipment used is expensive, higher cost.Blending and modifying makes two or more material uniform
The method to enhance product performance or assign product new capability of mixing, have it is at low cost, it is easy to operate, it is excellent more than optional material
Point can prepare high water flux to the maximum extent, the seperation film of high rejection is suitble to apply on a large scale in industry.There are commonly
Iron oxide, zirconium oxide, zinc oxide, aluminum magnesium hydroxide.In recent years, research finds inorganic nano material energy is blended with polysulfone material
The water flux and rejection of film are improved simultaneously.But inorganic nano-particle blending content just can effectively improve ultrafiltration membrane when larger
Can, and agglomeration easily occurs for nanoparticle, adversely affects to the structure and performance of film.
Patent CN105664739A discloses a kind of preparation method of high-hydrophilic polysulfone ultrafiltration membrane, and graphene oxide is used
After ultrasonic wave dispersion forms dispersion liquid in organic solvent, then polysulfones and pore-foaming agent are added in dispersion liquid, pass through immersion precipitation
Forming film with phase transformation method.The PS membrane rejection of this method process preparation and the balance of water flux need to be further increased.
Summary of the invention
The purpose of the present invention is to provide a kind of big flux modified polysulfone films and preparation method thereof, to solve problem above.
For this purpose, the present invention uses following technical scheme：
A kind of preparation method of big flux modified polysulfone film, includes the following steps：
(1) nano graphene oxide, pore-foaming agent and dressing agent are placed in organic solvent and are dispersed, form dispersion liquid；
(2) polysulfones is added in step (1) resulting dispersion liquid, heating water bath simultaneously stirs, until polysulfones dissolves, forms casting
Film liquid；
(3) by after the resulting casting solution standing and defoaming of step (2), on a glass, liquid film is scraped；
(4) step (3) resulting liquid film is stopped into the predetermined time in air, with volatile fraction organic solvent, Zhi Houlian
It is put into togerther in coagulating bath with glass plate；
(5) liquid film in bath to be solidified solidifies and is independently detached from glass plate and formed after diaphragm, cleans diaphragm to remove striping
Big flux modified polysulfone film is made in organic solvent and pore-foaming agent in piece.
Optionally, the dressing agent is earth alkali inorganic salt, cationic surfactant or aluminium oxide, the dressing agent
Mass concentration be 0.5%~5%；The organic solvent is highly polar organic solvent.
Optionally, the earth alkali inorganic salt is zinc chloride or lithium chloride, and the cationic surfactant is 16
Alkyl trimethyl ammonium bromide or dodecyl dimethyl benzyl ammonium bromide, the aluminium oxide are nanoscale；It is described highly polar organic
Solvent is dimethyl acetamide or N-Methyl pyrrolidone.
Optionally, the step (1) is specially：Nano graphene oxide, pore-foaming agent and dressing agent are placed in simultaneously organic
In solvent, ultrasonic disperse forms dispersion liquid until nano graphene oxide is evenly dispersed in the solution.
Optionally, the pore-foaming agent is polyvinylpyrrolidone, and the mass concentration of the pore-foaming agent is 1%~5%, described
The K value of polyvinylpyrrolidone is 30；The coagulating bath is deionized water, and the temperature of the coagulating bath is 25 DEG C.
Optionally, the ultrasonic disperse process of the step (1), reaction temperature control is at 85 DEG C hereinafter, supersonic frequency is
40kHz, ultrasonic time 90min.
Optionally, during the heating water bath process of the step (2) and the standing and defoaming of the step (3), casting solution
It is in a sealed state；In the step (2), the condition of heating water bath and stirring is 70 DEG C of waters bath with thermostatic control and magnetic agitation 7h.
Optionally, in the step (3), the concrete operations for scraping liquid film are to scrape liquid film using 200 μm of single side preparing devices；
In the step (4), the predetermined time that liquid film stops in air is 20s；
In the step (5), the method for cleaning diaphragm is that diaphragm is put into pure water to impregnate, and soaking time is for 24 hours, to impregnate
It changes in the process water 2 times.
A kind of big flux modified polysulfone film is made according to the preparation method of above-described big flux modified polysulfone film.
Compared with prior art, the invention has the advantages that：
The present invention is by evenly dispersed by nano graphene oxide, pore-foaming agent and dressing agent, realization immersion precipitation inversion of phases,
It is successfully prepared big flux modified polysulfone film.The dispersibility of nano graphene oxide is more preferable, and the addition of dressing agent effectively improves
The water flux of PS membrane.
Specific embodiment
In order to make the invention's purpose, features and advantages of the invention more obvious and easy to understand, below in conjunction with specific reality
Example is applied, technical solution of the present invention is clearly and completely described, it is clear that the embodiments described below are only this hair
Bright a part of the embodiment, and not all embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art are not having
All other embodiment obtained under the premise of creative work is made, shall fall within the protection scope of the present invention.
The present invention provides a kind of big flux modified polysulfone film and preparation method thereof, the preparation sides of big flux modified polysulfone film
Method includes the following steps：
(1) nano graphene oxide, pore-foaming agent and dressing agent are placed in organic solvent simultaneously, ultrasonic disperse, until receiving
Rice graphene oxide is evenly dispersed in the solution, forms uniform dispersion liquid；
(2) polysulfones being added in step (1) resulting dispersion liquid, heating water bath simultaneously stirs, until polysulfones is completely dissolved, shape
At stabilization, uniform casting solution；
(3) it by after the resulting casting solution standing and defoaming of step (2), is poured on the glass plate of dry cleansing, it is equal to scrape thickness
Even liquid film；
(4) step (3) resulting liquid film is stopped into the predetermined time in air, with volatile fraction organic solvent, Zhi Houlian
It is put into coagulating bath with glass plate together rapid level；
(5) in coagulating bath, liquid film, which solidifies and is independently detached from glass plate, forms diaphragm, and resulting diaphragm is put into pure water
It impregnates, removes the organic solvent and pore-foaming agent in diaphragm, big flux modified polysulfone film is made.
It further include a pre-treatment step before step (1)：Freeze-day with constant temperature processing is carried out to polysulfones, to remove the water in resin
Point.The specific method of freeze-day with constant temperature processing is that polysulfones is placed in constant temperature blast drying oven to dry for 24 hours.
Wherein, the organic solvent in step (1) is highly polar organic solvent, specially dimethyl acetamide (DMAC) or N-
Methyl pyrrolidone.
Nano graphene oxide dispersibility is more preferable in step (1), may not need preparatory ultrasonic disperse, directly with pore-foaming agent,
Organic solvent blending is added in dressing agent together, shortens the time is blended in this way, and it is more preferable to be blended effect, dispersibility, hydrophily and steady
It is qualitative to be improved largely.
Pore-foaming agent in step (1) is polyvinylpyrrolidone (PVP), and mass concentration is 1%~5%, preferably PVP-
K30。
The mass concentration of dressing agent in step (1) is 0.5%~5%.Dressing agent select earth alkali inorganic salt, sun from
One of sub- surfactant (and aluminium oxide,.Specifically, earth alkali inorganic salt is zinc chloride or lithium chloride, cation
Surfactant is cetyl trimethylammonium bromide or dodecyl dimethyl benzyl ammonium bromide, and aluminium oxide is nanoscale.
The ultrasonic disperse process of step (1) and the heating water bath process of step (2), reaction temperature control 85 DEG C with
Under, avoid the oxygen-containing group of nano graphene oxide from decomposing at high temperature.
Ultrasonic disperse condition in step (1) is preferably supersonic frequency 40kHz, ultrasonic time 90min.
During the heating water bath process of step (2) and the standing and defoaming of step (3), casting solution is in a sealed state,
Organic solvent volatilization, oxidation and steam is avoided to enter.
The condition of heating water bath and stirring in step (2) is preferably 70 DEG C of waters bath with thermostatic control and magnetic agitation 7h.
In step (3), liquid film in homogeneous thickness is specifically scraped using 200 μm of single side preparing devices.
In step (4), the predetermined time that liquid film stops in air is preferably 20s.
In step (4), coagulating bath is preferably deionized water.Coagulating bath can also be water-soluble for dehydrated alcohol or dimethyl acetamide
Liquid.The preferable temperature of coagulating bath is 25 DEG C.
In step (5), diaphragm is put into the preferred soaking conditions impregnated in pure water and changes water 2 for 24 hours, in soaking process to impregnate
It is secondary, to eliminate organic solvent and pore-foaming agent in big flux modified polysulfone film.
The present invention provides the big flux modified polysulfone films obtained by above step, and adopt to big flux modified polysulfone film
It is tested with cross-flow filtration device.Water flux is surveyed under 0.1MPa pressure.Ask albumen (BSA) as raw material using the ox blood of 1g/L
Liquid surveys rejection under 0.1MPa pressure.The present invention compares test result and pure PS membrane.
Embodiment one
Weigh the nano graphene oxide of mass concentration 0.75%~1.0% and the pore-foaming agent of mass concentration 2%~3%
PVP-K30, while being added in DMAC and being blended, ultrasonic disperse.Ultrasonic disperse condition is frequency 40kHz, ultrasonic 90min.Later plus
The polysulfones for entering 20%~22% dissolves polysulfones, forms uniform and stable casting film in 70 DEG C of waters bath with thermostatic control and magnetic agitation 7h
Liquid.For 24 hours by casting solution standing and defoaming.Casting solution is poured on clean clean glass plate at room temperature, uses 200 μm of thickness
Single side preparing device scrapes to obtain liquid film, and liquid film volatilizees 20s in air, is connected to glass plate rapidly and is put into 25 DEG C of pure water coagulating baths, to
After the entirely autonomous disengaging glass plate of diaphragm, diaphragm is impregnated for 24 hours in pure water, is changed in soaking process water 2 times, to eliminate in diaphragm
Organic solvent and pore-foaming agent, obtain big flux modified polysulfone film.
The rejection of big flux modified polysulfone film provided in this embodiment and pure PS membrane are very close, and the big flux is modified
The water flux of PS membrane improves 212% compared to the water flux of pure PS membrane.
Embodiment two
Weigh the nano graphene oxide of mass concentration 0.3%~0.5%, the pore-foaming agent PVP- of mass concentration 2%~3%
The dressing agent lithium chloride of K30 and mass concentration 1%~1.5%, while being added in DMAC and being blended, ultrasonic disperse.Ultrasonic disperse item
Part is that frequency is 40kHz, ultrasonic 90min.20%~22% polysulfones is added later, in 70 DEG C of waters bath with thermostatic control and magnetic agitation
7h dissolves polysulfones, forms uniform and stable casting solution, for 24 hours by casting solution standing and defoaming.Casting solution is poured at room temperature
On clean clean glass plate, liquid film is scraped to obtain using 200 μm of single side preparing devices of thickness, and liquid film volatilizees 20s in air, connects rapidly
It is put into 25 DEG C of pure water coagulating baths with glass plate, after the entirely autonomous disengaging glass plate of diaphragm, diaphragm is impregnated in pure water
For 24 hours, it is changed in soaking process water 2 times, to eliminate the organic solvent and pore-foaming agent in diaphragm, obtains big flux modified polysulfone film.
The rejection of big flux modified polysulfone film provided in this embodiment and pure PS membrane are very close, and the big flux is modified
The water flux of PS membrane improves 317% compared to the water flux of pure PS membrane, i.e., is modified in the big flux that embodiment one provides poly-
105% water flux is further improved on the basis of sulfone film.
Embodiment three
Weigh the nano graphene oxide of mass concentration 0.3%~0.5%, the pore-foaming agent PVP- of mass concentration 2%~3%
The dressing agent cetyl trimethylammonium bromide of K30 and mass concentration 0.5%~0.75%, while being added in DMAC and being blended, surpass
Sound dispersion.Ultrasonic disperse condition is that frequency is 40kHz, ultrasonic 90min.20% polysulfones is added later, in 70 DEG C of waters bath with thermostatic control
And magnetic agitation 7h, polysulfones is dissolved, uniform and stable casting solution is formed, for 24 hours by casting solution standing and defoaming.At room temperature casting
Film liquid is poured on clean clean glass plate, scrapes to obtain liquid film using 200 μm of single side preparing devices of thickness, liquid film volatilizees in air
20s, liquid film volatilize 20s in air, are put into 25 DEG C of pure water coagulating baths together with glass plate rapidly, entirely autonomous de- to diaphragm
After glass plate, diaphragm is impregnated for 24 hours in pure water, changed in soaking process water 2 times, to eliminate organic solvent and the cause in diaphragm
Hole agent obtains big flux modified polysulfone film.
The rejection of big flux modified polysulfone film provided in this embodiment and pure PS membrane are very close, and the big flux is modified
The water flux of PS membrane and the water flux for the big flux modified polysulfone film that embodiment two provides are almost the same, compared to pure PS membrane
Water flux improves 317%.
Example IV
Weigh the nano graphene oxide of mass concentration 0.3%~0.5%, the pore-foaming agent PVP- of mass concentration 2%~3%
The dressing agent alumina in Nano level of K30 and mass concentration 0.5%~0.75%, while being added in DMAC and being blended, ultrasonic disperse.It is super
Sound dispersion condition is that frequency is 40kHz, ultrasonic 90min.20% polysulfones is added later, in 70 DEG C of waters bath with thermostatic control and magnetic agitation
7h dissolves polysulfones, forms uniform and stable casting solution, for 24 hours by casting solution standing and defoaming.Casting solution is poured at room temperature
On clean clean glass plate, liquid film is scraped to obtain using 200 μm of single side preparing devices of thickness, and liquid film volatilizees 20s in air, liquid film
Volatilize 20s in air, is put into 25 DEG C of pure water coagulating baths together with glass plate rapidly, to the entirely autonomous disengaging glass plate of diaphragm
Afterwards, diaphragm is impregnated for 24 hours in pure water, changes in soaking process water 2 times, to eliminate the organic solvent and pore-foaming agent in diaphragm, obtains
Obtain big flux modified polysulfone film.
The rejection of big flux modified polysulfone film provided in this embodiment and pure PS membrane are very close, and the big flux is modified
The water flux of PS membrane improves 361% compared to the water flux of pure PS membrane, i.e., is modified in the big flux that embodiment one provides poly-
149% water flux is further improved on the basis of sulfone film.
The experimental results showed that the increase rate for not adding the pure water flux of the Modified Membrane of dressing agent reaches 200% or more, add
The increase rate of the pure water flux of the Modified Membrane of dressing agent is added to reach 300% or more.
Through the foregoing embodiment one to example IV test result it is found that the big flux modified polysulfone film that the present invention obtains
Compared to pure PS membrane, water flux is significantly improved, and is not had an impact substantially to rejection, has been broken ultrafiltration membrane flux and has been cut
The balance of rate is stayed to limit.The experimental results showed that not adding the raising width of the pure water flux of the big flux modified polysulfone film of dressing agent
Degree reach 200% or more, add the pure water flux of the big flux modified polysulfone film of dressing agent increase rate reach 300% with
On, illustrate that the addition of dressing agent can be effectively improved the performance of PS membrane.
Present invention utilizes the characteristics of nano graphene oxide, and organic solvent is added with pore-foaming agent, dressing agent in it simultaneously
Ultrasonic disperse is blended, and not only shortens the blending reaction time, but also blending effect such as dispersibility, hydrophily and stability have
Significantly promoted.The present invention selects suitable dressing agent to be added, and effectively improves the water flux of PS membrane, successfully makes
For big flux modified polysulfone film.
The above, the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although referring to before
Stating embodiment, invention is explained in detail, those skilled in the art should understand that：It still can be to preceding
Technical solution documented by each embodiment is stated to modify or equivalent replacement of some of the technical features；And these
It modifies or replaces, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (9)
1. a kind of preparation method of big flux modified polysulfone film, which is characterized in that include the following steps：
(1) nano graphene oxide, pore-foaming agent and dressing agent are placed in organic solvent and are dispersed, form dispersion liquid；
(2) polysulfones is added in step (1) resulting dispersion liquid, heating water bath simultaneously stirs, until polysulfones dissolves, forms casting film
Liquid；
(3) by after the resulting casting solution standing and defoaming of step (2), on a glass, liquid film is scraped；
(4) step (3) resulting liquid film is stopped into the predetermined time in air, with volatile fraction organic solvent, later together with glass
Glass plate is put into togerther in coagulating bath；
(5) liquid film in bath to be solidified solidifies and is independently detached from glass plate and formed after diaphragm, cleans diaphragm to remove in diaphragm
Organic solvent and pore-foaming agent, big flux modified polysulfone film is made.
2. the preparation method of big flux modified polysulfone film according to claim 1, which is characterized in that the dressing agent is alkali
Earth metal inorganic salts, cationic surfactant or aluminium oxide, the mass concentration of the dressing agent are 0.5%~5%；It is described to have
Solvent is highly polar organic solvent.
3. the preparation method of big flux modified polysulfone film according to claim 2, which is characterized in that the alkaline-earth metal without
Machine salt is zinc chloride or lithium chloride, and the cationic surfactant is cetyl trimethylammonium bromide or dimethyl
Base Benzylphosphonium Bromide ammonium, the aluminium oxide are nanoscale；The highly polar organic solvent is dimethyl acetamide or N- methylpyrrole
Alkanone.
4. the preparation method of big flux modified polysulfone film according to claim 1, which is characterized in that step (1) tool
Body is：Nano graphene oxide, pore-foaming agent and dressing agent are placed in organic solvent simultaneously, ultrasonic disperse, until nano oxidized
Graphene uniform disperses in the solution, to form dispersion liquid.
5. the preparation method of big flux modified polysulfone film according to claim 1, which is characterized in that the pore-foaming agent is poly-
Vinylpyrrolidone, the mass concentration of the pore-foaming agent are 1%~5%, and the K value of the polyvinylpyrrolidone is 30；It is described
Coagulating bath is deionized water, and the temperature of the coagulating bath is 25 DEG C.
6. the preparation method of big flux modified polysulfone film according to claim 4, which is characterized in that the step (1)
Ultrasonic disperse process, reaction temperature control is at 85 DEG C hereinafter, supersonic frequency is 40kHz, ultrasonic time 90min.
7. the preparation method of big flux modified polysulfone film according to claim 1, which is characterized in that the step (2)
During the standing and defoaming of heating water bath process and the step (3), casting solution is in a sealed state；In the step (2),
Heating water bath and the condition stirred are 70 DEG C of waters bath with thermostatic control and magnetic agitation 7h.
8. the preparation method of big flux modified polysulfone film according to claim 1, which is characterized in that in the step (3),
The concrete operations for scraping liquid film are to scrape liquid film using 200 μm of single side preparing devices；
In the step (4), the predetermined time that liquid film stops in air is 20s；
In the step (5), the method for cleaning diaphragm is that diaphragm is put into pure water to impregnate, and soaking time is soaking process for 24 hours
In change water 2 times.
9. a kind of big flux modified polysulfone film, which is characterized in that according to claim 1 to big logical described in 8 any claims
The preparation method of amount modified polysulfone film is made.
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