CN107174950A - The positive osmosis composite membrane of high-performance and preparation method that a kind of graphene oxide is modified - Google Patents
The positive osmosis composite membrane of high-performance and preparation method that a kind of graphene oxide is modified Download PDFInfo
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- CN107174950A CN107174950A CN201710506514.8A CN201710506514A CN107174950A CN 107174950 A CN107174950 A CN 107174950A CN 201710506514 A CN201710506514 A CN 201710506514A CN 107174950 A CN107174950 A CN 107174950A
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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
- B01D61/002—Forward osmosis or direct osmosis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/10—Testing of membranes or membrane apparatus; Detecting or repairing leaks
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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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- 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
- B01D67/0016—Coagulation
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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
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
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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
- 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
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
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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
- B01D2325/02—Details relating to pores or porosity of the 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
- B01D2325/36—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
Abstract
The positive osmosis composite membrane of high-performance and preparation method being modified the invention discloses a kind of graphene oxide, belong to water-treatment technology field.Comprise the following steps：First by blending method, polysulfones, graphene oxide, Macrogol 600, Tween 80 and solvent are added in flask, casting solution is prepared, using phase inversion, graphene oxide/polysulfone supporting layer is made.Then the positive osmosis composite membrane of graphene oxide/polyamide is obtained in support layer surface composite polyamide active layer using interfacial polymerization mode.The positive osmosis composite membrane of graphene oxide/polyamide prepared by the present invention has the advantages that flux is high, reverse flux salt is small, resistance tocrocking is strong, its water flux is up to 9 12LMH, reverse flux salt is 2 4gMH, in antifouling property test, the flux fall caused by pollution is only 30% the 50% of unmodified membrane.
Description
Technical field
The positive osmosis composite membrane of high-performance and preparation method being modified the present invention relates to a kind of graphene oxide, more particularly, to
A kind of preparation method of the positive osmosis composite membrane of high-performance.
Background technology
China is a water resource country that there is a serious shortage in the supply, and occupancy volume per person is only a quarter of world average level.
The growing and industrial of population develops rapidly so that shortage of water resources problem is increasingly serious.Water technology is developed into
People solve the problems, such as that shortage of water resources provides direction.Membrane separation technique is used as a kind of efficient, environmental protection, the new separation skill of energy-conservation
Art occupies critical role in water technology.It mainly includes micro-filtration, ultrafiltration, nanofiltration, counter-infiltration, positive infiltration etc..Wherein, instead
The more other several technology development of infiltration are more ripe, but because its operating pressure height, high energy consumption, fouling membrane are serious, actually should
There is certain limitation in.NF membrane can retain small organic molecule and salt, and operating pressure is low, but pollution problem also compared with
To be serious.Compared with the membrane separation technique such as counter-infiltration and nanofiltration, positive infiltration technology has low energy consumption, equipment with high desalinization, antipollution energy
The advantages of power is strong, attracts wide attention in recent years.
At present, the research of positive infiltration technology is concentrated mainly on two aspects：The preparation of high performance membrane material and high efficiency are drawn
Take the selection of liquid.Film is the core of whole positive permeability and separation process, therefore prepares high performance membrane material for improving system
Overall performance is most important.Polysulfones, cellulose acetate etc. are all the most frequently used material of preparing.Wherein, polysulfones is with its good change
Learn stability, heat endurance, film forming mechanicalness and be widely used.But in actual applications, conventional polysulfones membrane aperture is larger,
Porosity, film surface are rougher, cause that water flux is small, desalting effect is poor, the problems such as easily polluting.Therefore, exploitation prepares high
The forward osmosis membrane of performance is significant.
Polyamide composite film has the special construction of asymmetry, by amino-contained functional group and the oil of aqueous phase (m-phenylene diamine (MPD))
Phase (trimesoyl chloride) is formed containing acid chloride groups in porous support layer surface aggregate.Polyamide composite bed can make film surface thick
Rugosity is reduced, and hydrophily is improved, so as to increase the water flux and antifouling property of film.In addition, polyamide composite film can be real
Now to the bidirectional optimistic of porous support layer and ultra-thin active layer, realize that film properties are integrally improved by using respective optimal conditions.
It is another important channel for improving forward osmosis membrane performance, conventional method of modifying that porous support layer, which is modified,
Have：Blending and modifying, surface graft modification, coating modification, plasma modification.Wherein, blending and modifying refers to add solid matter
Enter and form three phase spaces into casting solution to prepare forward osmosis membrane, method is simple to operate, effect substantially, can directly change film
Basal body structure, such as pore size, Hole Wall Roughness etc., the performance of film is improved with this.
In recent years, nano material is ground with its higher specific surface area and excellent physicochemical characteristics as technical field of membrane
The focus studied carefully.Wherein, graphene oxide is as a kind of nano material for the laminated structure being made up of carbon atom, with a large amount of carboxylics
The hydrophilic functional groups such as base, hydroxyl, epoxy radicals.Simultaneous oxidation graphene can destroy cell membrane or induced oxidation and stress kill
Bacterium, the hydroxyl radical free radical included can also aggravate the lipid peroxidation of biological cell, and the formation for film surface biological film has
There is obvious inhibitory action.Therefore, special construction based on polyamide composite film and the hydrophily of graphene oxide and antibacterial
Property, graphene oxide and membrane material blending are prepared into positive infiltration supporting layer, then carry by interfacial polymerization aramid layer, and then effectively
The infiltration of high forward osmosis membrane and desalting performance, and film resistance tocrocking, be membrane technology should be provided with extensively in water process
Technical support.
The content of the invention
The purpose of the present invention be for existing forward osmosis membrane exist flux it is low, desalting effect is poor, antifouling property is low
Problem, prepares a kind of high performance positive osmosis composite membrane and provides its preparation method.
The positive osmosis composite membrane of high-performance and preparation method that a kind of graphene oxide is modified, concrete operation step are completed such as
Under：
1. the preparation of graphene oxide/polysulfone supporting layer
The composition of high performance flat formula graphene oxide/polysulfones blending forward osmosis membrane formula of casting is：Membrane material is poly-
Sulfone, 8.0%~25.0wt%；Additive is Macrogol 600,0~20.0wt%；Modifying agent is graphene oxide, 0~
1.5wt%；Solvent is DMF, 65.0%~80.0wt%；Solubilizer is Tween 80,0.5%~2wt%.
N,N-dimethylformamide, Macrogol 600, Tween 80 are added to three-necked flask according to certain ratio first
In, then a certain amount of graphene oxide is added in solution, 10~60min of ultrasound makes graphene oxide equal in the solution
It is even scattered；After ultrasound terminates, solution is moved on magnetic stirring apparatus, 3~10min is stirred, polysulfone material is added, at 50~70 DEG C
At a temperature of 6~10h of stirring and dissolving, obtain uniform graphene oxide/polysulfones casting solution；Then, by casting solution in reaction temperature
Under static 4~8h, removing casting solution in bubble；Finally, it is 80~120 a certain amount of casting solution to be poured on and be equipped with mesh number
On the glass plate of polyester screen, with the scraper striking film forming that thickness is 50~200 μm, freezing film in ultra-pure water is immersed, film is treated
After the automatic disengaging from glass plate, 24~72h is soaked in ultra-pure water, a water was changed every 6 hours, that is, obtains flat oxidation stone
Black alkene/polysulfone supporting layer.
2. the preparation of graphene oxide/polyamide composite film
By interfacial polymerization on supporting layer synthesizing polyamides layer.Basement membrane is dipped in 2~4wt% m-phenylene diamine (MPD) first
(MPD) 3~5min in aqueous phase, after basement membrane is taken out from aqueous phase, supporting layer back side solution is washed out with ultra-pure water, then inhaled with filter paper
Dry film both sides it is water stain；Then film is soaked in oil phase, i.e., concentration is 0.15~0.25wt% trimesoyl chloride (TMC)
Taken out after hexane solution, 1~3min, and remove unnecessary oil phase.Obtain the just infiltration of graphene oxide/polyamide compound
Film.To make polyamide be combined the more firm of layers of polymer, composite membrane is heat-treated 5~10min in drying box with 40-80 DEG C,
Take out, preserve standby in deionized water.
In the preparation process for the positive osmosis composite membrane of high-performance that graphene oxide is modified, by controlling to gather in casting solution
The indexs such as sulfone, Macrogol 600, the mixed proportion of graphene oxide and casting solution stirring and dissolving temperature, enter to preparation condition
Row optimization, and then control the structure and performance of prepared blending forward osmosis membrane.The positive osmosis composite membrane prepared is placed in mistake
Tested in stream filtration system, investigate the water flux of positive osmosis composite membrane of graphene oxide modification, reverse flux salt and
Antifouling property.
Beneficial effect：
The advantage of graphene oxide/polyamide composite film is in the present invention：The polysulfones support being blended by graphene oxide
Layer has the features such as Stability Analysis of Structures, porosity are high, fenestra is small, hydrophily is high, can ensure that composite membrane is logical with higher film simultaneously
Amount and relatively low reverse flux salt.In addition, according to studies have reported that graphene oxide there is bactericidal action, and to film parent
Aqueous raising, can make graphene oxide/polyamide composite film of preparation has very strong stable against biological contamination performance.
Embodiment
Below in conjunction with the specific embodiment of the invention, technical scheme is verified, the embodiment verified
Only section Example of the invention.Based on the embodiment in the present invention, this area researcher is not making any creation
Property work under the premise of the other embodiment that is obtained, belong to the scope of protection of the invention.
Embodiment 1
First by N,N-dimethylformamide, Macrogol 600, Tween 80 respectively according to 70wt%, 13.3wt%,
1wt% ratio is added in three-necked flask, and then the ultrapure graphene oxide of 0.2wt% individual layer is added in solution, is surpassed
Sound 30min, makes graphene oxide full and uniform dispersion in the solution, after ultrasound terminates, solution is moved on magnetic stirring apparatus, stirred
Mix and polysulfone material is added after 5min, the stirring and dissolving 8h at a temperature of 70 DEG C obtains uniform graphene oxide/polysulfones casting solution；
Then, the bubble in casting solution static 5h at the reaction temperatures, removing casting solution；Finally, a certain amount of casting solution is poured on and put
On the glass plate for having the polyester screen that mesh number is 100, with the scraper striking film forming that thickness is 50 μm, immerse in ultra-pure water and solidify
Film forming, after after the automatic disengaging from glass plate of film, 72h is soaked in ultra-pure water, a water was changed every 6 hours, that is, is obtained flat
Graphene oxide/polysulfone supporting layer.
The supporting layer prepared is dipped in 5min in 3.5wt% m-phenylene diamine (MPD) (MPD) aqueous phase first, by basement membrane from water
After being taken out in phase, the solution at the supporting layer back side is washed out with deionized water, then blots with filter paper the water stain of film both sides；Then film is soaked
Steep in oil phase, i.e., concentration is taking-up after the hexane solution of 0.15wt% trimesoyl chloride (TMC), 2min, and is removed many
Remaining oil phase, obtains the positive osmosis composite membrane of graphene oxide/polyamide (GO/TFC films).Driving is used as by the use of 2M NaCl solutions
Liquid, deionized water is as material liquid, in 1h testing time, and the average water flux of prepared film reaches 11.29LMH, reversely
Flux salt is 2.1gMH.
For test the positive osmosis composite membrane of graphene oxide antifouling property, the present embodiment by the use of pseudomonas aeruginosa as
Contaminating microorganisms, use synthetic wastewater simulate secondary effluent (with water constituent for：1.2mM sodium citrates, 0.8mM NH4Cl、
0.5mM NaHCO3、0.2mM K2HPO4、8.0mM NaCl、0.2mM CaCl2·H2O、0.15mM MgSO4·7H2O, microorganism
Concentration is 5 × 107CFU/L), antipollution experimental study is carried out to film.Driving liquid, synthetic wastewater conduct are used as by the use of 2M NaCl
Material liquid.After continuous operation pollution experiment in two days, by calculating, the water flux fall as caused by biological pollution is 11%.
Embodiment 2
It based on the method for modifying in embodiment 1, the difference is that only during preparing supporting layer, do not add oxidation
Graphene, obtains the positive osmosis composite membrane of polysulfones polyamide (TFC films).Likewise, prepared forward osmosis membrane is tested,
In 1h testing time, the average water flux of film is 5.9LMH, and reverse flux salt is 8gMH；In biological pollution experiment, pass through
The pollution experiment of continuous operation two days, the water flux fall as caused by biological pollution is 25%.
Embodiment 1-2 graphene oxides be modified positive osmosis composite membrane and be not added with graphene oxide positive infiltration be combined
Film items test data detailed comparisons such as table 1.
Table 1
| The classification of film | Water flux/LMH | Reverse flux salt/gMH | Contact angle/° | Porosity | Flux fall after pollution |
| GO/TFC films | 11.29 | 2 | 60.6 | 33% | 11% |
| TFC films | 5.9 | 8 | 47.32 | 53% | 25% |
As can be seen that by the modified positive osmosis composite membrane of graphene oxide, water flux is greatly improved, reverse salt leads in table
Amount reduces；And contact angle is reduced, illustrate that the modified film hydrophilies of GO are improved；Porosity increase, illustrates the aperture structure to film
Substantially improve；Tested by antipollution, the antifouling property of GO/TFC films is better than traditional TFC films.
Claims (9)
1. the positive osmosis composite membrane of high-performance and preparation method that a kind of graphene oxide is modified, it is characterised in that including following step
Suddenly：
(1) preparation of graphene oxide/polysulfone supporting layer
DMF, Macrogol 600, Tween 80 are added in three-necked flask according to certain ratio, then
A certain amount of graphene oxide is added in solution, ultrasound adds polysulfone material, stirred at a certain temperature to being completely dispersed
Mix, obtain uniform graphene oxide/polysulfones casting solution；Then, by casting solution static to complete deaeration at the reaction temperatures；Most
Afterwards, a certain amount of casting solution is poured on the glass plate for being equipped with polyester screen, with certain thickness scraper knifing, immerses ultra-pure water
Middle freezing film, after film is automatic depart from from glass plate after, in ultra-pure water be dipped to solvent separates out completely, that is, obtains flat
Graphene oxide/polysulfone supporting layer；
(2) preparation of graphene oxide/polyamide composite film
Using interfacial polymerization on supporting layer synthesizing polyamides layer.Basement membrane is dipped in certain density m-phenylene diamine (MPD) (MPD) first
Aqueous phase in, after basement membrane is taken out from aqueous phase, the solution at the supporting layer back side is washed out with ultra-pure water, then blot with filter paper film both sides
It is water stain；Then film is soaked in oil phase, i.e., the hexane solution of certain density trimesoyl chloride (TMC), taken out, and go
Except unnecessary oil phase, the positive osmosis composite membrane of graphene oxide/polyamide is obtained.To make polyamide be combined the more firm of layers of polymer
Gu, composite membrane is heat-treated in drying box, taken out, is preserved standby in deionized water；
To investigate the performance of film, the positive osmosis composite membrane prepared is placed in cross-flow filtration system and tested, investigate oxidation
Water flux, reverse flux salt and the antifouling property for the positive osmosis composite membrane that graphene is modified.
2. the positive osmosis composite membrane of high-performance and preparation method that a kind of graphene oxide according to claim 1 is modified, its
It is characterised by step (1), preparing the material of graphene oxide/polysulfone supporting layer has：Membrane material is polysulfones, 8.0%~
25.0wt%；Modifying agent is graphene oxide, 0~1.5wt%；Solvent is DMF, 65.0%~
80.0wt%；Additive is Macrogol 600,0~20.0wt%；Solubilizer is Tween 80,0.5%~2wt%.
3. method of modifying according to claim 1, it is characterised in that, it is necessary to first before polysulfone material addition in step (1)
By graphene oxide, ultrasonic disperse is uniform in the solution, and ultrasonic time is 10~60min, then moves to and 3 are stirred on magnetic stirring apparatus
~10min.
4. method of modifying according to claim 1, it is characterised in that after the addition of step (1) polysulfone material, stirring condition
For：6~10h of stirring and dissolving at a temperature of 50~70 DEG C.
5. method of modifying according to claim 1, it is characterised in that in step (1) cast film process, the mesh number of polyester screen
For 80~120, blade thickness is 50~200 μm.
6. the positive osmosis composite membrane of high-performance and preparation method that a kind of graphene oxide according to claim 1 is modified, its
It is characterised by two kinds of the trimesoyl chloride of the m-phenylene diamine (MPD) for being synthesized by aqueous phase of polyamide active layer and oil phase in step (2)
Solution occurs interface polymerization reaction on film surface and obtained, and the concentration of two kinds of solution is respectively 2~4wt%, 0.15~0.25wt%.
7. method of modifying according to claim 1, it is characterised in that after basement membrane is taken out from aqueous phase in step (2), be
The problem of supporting layer both sides after dipping have m-phenylene diamine (MPD) and cause double-sided polymerization is prevented, supporting layer need to be washed out with ultra-pure water
The solution at the back side, then blots the water stain of film both sides with filter paper, then film is soaked in oil phase, completes further polymerization.
8. method of modifying according to claim 1, it is characterised in that be to make polyamide be combined layers of polymer more in step (2)
Plus firmly, composite membrane is heat-treated 5~10min for 40-80 DEG C in drying box.
9. method of modifying according to claim 1, it is characterised in that be the performance of test film, the positive infiltration prepared is answered
Close film to be placed in cross-flow filtration system and is tested, investigate the water flux, reverse for the positive osmosis composite membrane that graphene oxide is modified
Flux salt and antifouling property, as a result draw：Water flux is up to 9-12LMH, and reverse flux salt is 2-4gMH, is surveyed in antipollution
In examination, water flux fall caused by pollution is the 30%-50% of unmodified membrane.
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Cited By (6)
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|---|---|---|---|---|
| CN107789994A (en) * | 2017-11-16 | 2018-03-13 | 清华大学 | Positive permeability and separation film and preparation method thereof |
| CN109647223A (en) * | 2018-11-14 | 2019-04-19 | 天津大学 | A kind of preparation method of the compound forward osmosis membrane in high activity site |
| CN110508164A (en) * | 2019-08-07 | 2019-11-29 | 大连理工大学 | A kind of preparation method of the graphene oxide composite membrane of stable structure |
| CN111318178A (en) * | 2020-02-27 | 2020-06-23 | 江苏大学 | Graphene oxide/attapulgite composite membrane and preparation method and application thereof |
| CN114437339A (en) * | 2020-11-03 | 2022-05-06 | 天津工业大学 | Preparation method and application of high-absorbance honeycomb polyamide membrane |
| CN115888430A (en) * | 2022-11-09 | 2023-04-04 | 江苏德环环保集团有限公司 | Graphene oxide/aminated attapulgite intercalation compound surface modified forward osmosis membrane and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107789994A (en) * | 2017-11-16 | 2018-03-13 | 清华大学 | Positive permeability and separation film and preparation method thereof |
| CN109647223A (en) * | 2018-11-14 | 2019-04-19 | 天津大学 | A kind of preparation method of the compound forward osmosis membrane in high activity site |
| CN110508164A (en) * | 2019-08-07 | 2019-11-29 | 大连理工大学 | A kind of preparation method of the graphene oxide composite membrane of stable structure |
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| CN111318178B (en) * | 2020-02-27 | 2022-04-26 | 江苏大学 | Graphene oxide/attapulgite composite membrane and preparation method and application thereof |
| CN114437339A (en) * | 2020-11-03 | 2022-05-06 | 天津工业大学 | Preparation method and application of high-absorbance honeycomb polyamide membrane |
| CN114437339B (en) * | 2020-11-03 | 2023-07-21 | 天津工业大学 | Preparation method and application of high-absorbance honeycomb polyamide membrane |
| CN115888430A (en) * | 2022-11-09 | 2023-04-04 | 江苏德环环保集团有限公司 | Graphene oxide/aminated attapulgite intercalation compound surface modified forward osmosis membrane and preparation method thereof |
| CN115888430B (en) * | 2022-11-09 | 2023-11-14 | 江苏德环环保集团有限公司 | Graphene oxide/amination attapulgite intercalation compound surface modified forward osmosis membrane and preparation method thereof |
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