CN104607069A - Compound desalination membrane as well as preparation method and application thereof - Google Patents
Compound desalination membrane as well as preparation method and application thereof Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
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- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
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Abstract
The invention discloses a compound desalination membrane as well as a preparation method and an application thereof. The compound desalination membrane comprises a microporous filter membrane substrate layer and a functional layer, wherein the functional layer comprises reduced graphene oxide sheets and titanium oxide nanosheets, which are uniformly mixed and mutually stacked to form a laminar membrane. The preparation method comprises the following steps: uniformly mixing a water solution containing the graphene oxide sheets with a water solution containing the titanium oxide nanosheets; taking a microporous filter membrane as a substrate, preparing the laminar graphene oxide and titanium oxide compound membrane on the microporous filter membrane substrate by adopting a vacuum suction filtration method, and drying; uniformly converting graphene oxide into reduced graphene oxide through ultraviolet radiation to finally obtain the compound desalination membrane. The method realizes composition and structural design of the compound desalination membrane formed on the microporous filter membrane substrate based on reduced graphene oxide and the titanium oxide nanosheets; the prepared compound desalination membrane is soft, uniform, controllable in area and thickness, high in mechanical strength and high in desalination performance, and is used in the field of water desalination.
Description
Technical field
The present invention relates to the application of nano environment material, particularly a kind of compound desalination membrane with high desalination performance and high Water permeability and its preparation method and application.
Background technology
Along with critical shortage and the pollution of freshwater resources are cleaned in the whole world, water desalination technology seems especially important.Now widely used water desalination technology mainly contains hot multistage flash evaporation, hot multi-effect distilling, electrodialysis and film reverse osmosis technology, and wherein film reverse osmosis technology is subject to extensive concern because energy consumption is low, and obtains wider application by future.At present, widely used in film reverse osmosis technology is organic polyamine film, because it has flexibility, cheap and prepare the advantages such as simple.Meanwhile, the chemical resistance of organic polyamine film is poor, the life-span is short and Film Contamination serious etc. be also the serious problems of restriction film reverse osmosis technology development.Therefore, the exploitation of novel trans permeable membrane is most important in the application in water desalination field for reverse osmosis technology.
Graphene (Graphene) [bibliography 1:K.S.Novoselov, A.K.Geim, S.V.Morozov, D.Jiang, Y.Zhang, S.V.Dubonos, I.V.Grigorieva, A.A.Firsov.Electric field effectin atomically thin carbon films.Science, 2004,306:666-669], be by sp
2the two dimensional crystal material that the carbon atom arrangement of hydridization forms in honeycomb lattice structure, cause because having excellent performance and study interest widely, researcher is exploring the potential application of Graphene in water desalination field.For perfect Graphene monocrystal, gas and liquid all cannot carry out transmembrane infiltration, thus result of study shows, Graphene is the thinnest, capable barrier film materials [the bibliography 2:J.S.Bunch being separated different two-phase found up to now, S.S.Verbridge, J.S.Alden, A.M.Zande, J.M.Parpia, H.G.Craighead, P.L.McEuen.Impermeable atomic membranes from graphene sheets.Nano Lett., 2008,8:2458-2462.].On the other hand, by mutually stacking for the graphene platelet (graphene oxide) of the micron dimension size of selective oxidation, by sp in the macroscopical laminar film formed
2the sp that fragrance cluster is interconnected to constitute
2nanotube capillaries network shows ultrafast transmission characteristic [bibliography 3:N.N.Nair to hydrone, H.A.Wu, P.N.Jayaram, I.V.Grigorieva, A.K.Geim.Unimpeded permeation of water throughhelium-leak – tight graphene-based membranes.Science 2012, 335:442 – 444.], and excellent selected area update strategy characteristic [bibliography 4:R.K.Joshi is shown to solute different in water body, P.Carbone, F.C.Wang, V.G.Kravets, Y.Su, I.V.Grigorieva, H.A.Wu, A.K.Geim, R.R.Nair.Precise and ultrafast molecular sieving through graphene oxide membranes.Science2014, 343:752 – 754.], layered graphite oxide alkene film is made to possess wide application prospect in filtration & separation field.But the solute that hydration radius is less than 0.45nm has ultrafast infiltration rate [bibliography 4], and this makes to be restricted in the application in water desalination field by the laminar laminar film of micro-meter scale graphene oxide.In addition, result of study shows, it is made to be less than 0.7nm by the interlamellar spacing also originally regulating and controlling graphene oxide film, sodium ion can be removed from the aqueous solution, and then realize water desalination [bibliography 5:B.Mi.Graphene oxide membranes for ionic and molecular sieving.Science 2014,343:740 – 742.], but the Water permeability of oxidation graphene film also has variation [bibliography 3] simultaneously.When the graphene oxide thin slice in film is reduced sufficiently and closely stacking, sp in the laminar film formed
2nanotube capillaries network is closed, to hydrone and any salt ion all completely not saturating, oxidation graphene film is made to lose desalting performance [bibliography 6:Y.Su, V.G.Kravets, S.L.Wong, J.Waters, A.K.Geim, R.R.Nair.Impermeable barrier films and protective coatings based on reducedgraphene oxide.Nat.Comm.2014,5:4843.].Therefore, by regulating and controlling the interlamellar spacing of graphene oxide film and interlayer physical chemical characteristic, and then realize the efficient desalination of graphene oxide film and most important in the application in water desalination field.
On the other hand, TiOx nano sheet (Titania nanosheets, Ti
0.87o
2), the outstanding two-dimension nano materials of another kind [the bibliography 7:T.Sasaki prepared by the method for soft chemical stripping titanate, M.Watanabe, H.Hashizume, H.Yamada, H.Nakazawa, Macromolecule-like aspects for a colloidalsuspension of an exfoliated titanate.Pairwise association of nanosheets and dynamicreassembling process initiated from it.J.Am.Chem.Soc.1996, 118:8329 – 8335.], there is excellent photocatalysis characteristic [bibliography 8:P.Sun, M.Zhu, R.Ma, K.Wang, J.Wei, D.Wu, T.Sasaki, H.Zhu, Graphene oxide/titania hybrid films with dual-UV-responsivesurfaces of tunable wettability.RSC Adv.2012, 2:10829 – 10835.] and photic hydrophilic conversion characteristic [bibliography 9:N.Sakai, K.Fukuda, T.Shibata, Y.Ebina, K.Takada, T.Sasaki, Photoinduced hydrophilic conversion properties of titania nanosheets.J.Phys.Chem.B, 2006, 110:6198 – 6203.].So far, existing pertinent literature [bibliography 8] reports preparation and the correlation properties research of the laminated film that graphene oxide and TiOx nano sheet form, but only rest on basic character conceptual phase, all do not relate to redox graphene and the practical application in industry of titanium oxide composite film in water desalination field.
Summary of the invention
For realizing based on the lifting of the laminar laminar film desalting performance of graphene oxide and the application in water desalination field, the object of the present invention is to provide a kind of redox graphene thin slice and TiOx nano sheet compound desalination membrane and preparation method thereof, and realize the application of compound desalination membrane in water desalination field.
For achieving the above object, technical scheme of the present invention is achieved in that
A preparation method for compound desalination membrane, is characterized in that comprising the following steps:
1) by the aqueous solution Homogeneous phase mixing of the aqueous solution and TiOx nano sheet that comprise graphene oxide thin slice; Graphene oxide water solution volume mass concentration adopts 0.5 ~ 40mg/L, TiOx nano sheet aqueous solution volume mass concentration adopts 0.4 ~ 32mg/L, in the mixed solution of graphene oxide and TiOx nano sheet, graphene oxide and TiOx nano tablet quality are than being 1:0.25 ~ 4;
2) take miillpore filter as substrate, adopt vacuum filtration method that the mixed solution of graphene oxide and TiOx nano sheet is dewatered under negative pressure, and then mutual stacking self assembly is laminar film in miillpore filter substrate, dry 4 ~ 24h under 40 ~ 80 DEG C of conditions;
3) by UV-irradiation 1 ~ 5 day, utilize the photocatalysis characteristic of TiOx nano sheet to make graphene oxide uniform change for redox graphene, finally obtain compound desalination membrane.
Miillpore filter basalis used in the present invention adopts cellulose mixture miillpore filter, polyethersulfone millipore filter, polytetrafluoroethylene (PTFE) miillpore filter or anodised aluminium miillpore filter, and its pore diameter range is 100 ~ 450nm.
The application of compound desalination membrane of the present invention in water desalination.
The present invention compared with prior art, has the following advantages and the technique effect of high-lighting:
The compound desalination membrane prepared by above technical scheme is made up of miillpore filter basalis and functional layer, and wherein miillpore filter basalis has higher force intensity, ensures that functional layer Stability Analysis of Structures in water desalination process of compound desalination membrane is not damaged; Functional layer is laminar film by redox graphene and the mutual stacking self assembly of TiOx nano sheet Homogeneous phase mixing.Based on the efficient photocatalysis characteristic of TiOx nano sheet, under UV-irradiation, graphene oxide can be redox graphene by uniform change, and local is closely stacking, sp
2nanotube capillaries network shrinks, and effectively prevents the transmembrane of salt ion to permeate, and thus laminar film has excellent desalting performance, and its salt rejection rate is up to more than 90%; Based on the photic hydrophilic conversion characteristic of TiOx nano sheet excellence, under UV-irradiation, the surface of TiOx nano sheet by hydrophobic change into super hydrophilic, thus the hydrophily of laminar film has been regulated and controled, more juicy is made to suck in laminar film, and then through laminar film, improve the Water permeability of laminar film, its Water permeability can remain to original graphene oxide and TiOx nano sheet laminated film under non-reducing condition more than 50%, thus the compound desalination membrane provided in the present invention has excellent water desalination performance, for water desalination field.In addition, the area of laminated film regulates and controls by the area of miillpore filter substrate, can reach 1cm
2~ 1m
2thickness regulates and controls by the gross mass of solute in graphene oxide in vacuum filtration process and TiOx nano sheet mixed solution, can be controlled in 10nm ~ 10 μm, prepared compound desalination membrane have flexibility, evenly, area and thickness is controlled, form and the advantage such as structure is adjustable, high strength and high desalination performance, can be used for water desalination field.
Accompanying drawing explanation
Fig. 1 is structure and the desalination principle schematic of compound desalination membrane provided by the invention.
In Fig. 1: 1-redox graphene; 2-TiOx nano sheet; The substrate of 3-miillpore filter; 4-salt ion; 5-hydrone.
Fig. 2 is the light microscopic microscopic sdIBM-2+2q.p.approach photo of the compound desalination membrane of redox graphene and the mutual stacking formation of TiOx nano sheet Homogeneous phase mixing in miillpore filter substrate.
Fig. 3 a is that the salt ion Penetration Signature of compound desalination membrane of the present invention after ultraviolet light irradiates 0 day and 3 days respectively compares.
Fig. 3 b records the hydrone Penetration Signature of compound desalination membrane after ultraviolet light irradiates 0 day and 3 days respectively by isotope-labelling method to compare.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention will be further described.
A kind of compound desalination membrane provided by the invention, this compound desalination membrane is made up of miillpore filter basalis 3 and functional layer, and described functional layer is by redox graphene 1 and the laminar film of TiOx nano sheet 2 by the mutual stacking self assembly of Homogeneous phase mixing.The mutual stacking formation compound desalination membrane of redox graphene thin slice and TiOx nano sheet Homogeneous phase mixing in miillpore filter substrate, the existing efficient desalting performance of compound desalination membrane of gained, Water permeability excellent in original graphene oxide and TiOx nano sheet laminated film can be kept again, can be used for water desalination field.
Fig. 2 is the light microscopic microscopic sdIBM-2+2q.p.approach photo of the compound desalination membrane of redox graphene and the mutual stacking formation of TiOx nano sheet Homogeneous phase mixing in miillpore filter substrate.The area of this laminated film regulates and controls by the area of miillpore filter substrate, can reach 1cm
2~ 1m
2, thickness regulates and controls by the gross mass of solute in graphene oxide in vacuum filtration process and TiOx nano sheet mixed solution, can be controlled in 10nm ~ 10 μm; Prepared compound desalination membrane have flexibility, evenly, area and thickness controlled.
The preparation method of a kind of compound desalination membrane provided by the invention, it specifically comprises the following steps:
1) by the aqueous solution Homogeneous phase mixing of the aqueous solution and TiOx nano sheet that comprise graphene oxide thin slice; Graphene oxide water solution volume mass concentration adopts 0.5 ~ 40mg/L, TiOx nano sheet aqueous solution volume mass concentration adopts 0.4 ~ 32mg/L, in the mixed solution of graphene oxide and TiOx nano sheet, graphene oxide and TiOx nano tablet quality are than being 1:0.25 ~ 4;
2) take miillpore filter as substrate, adopt vacuum filtration method that the mixed solution of graphene oxide and TiOx nano sheet is dewatered under negative pressure, and then mutual stacking self assembly is laminar film in miillpore filter substrate 3, dry 4 ~ 24h under 40 ~ 80 DEG C of conditions;
3) by UV-irradiation 1 ~ 5 day, utilize the photocatalysis characteristic of TiOx nano sheet to make graphene oxide uniform change for redox graphene, finally obtain compound desalination membrane.
Described miillpore filter basalis generally adopts cellulose mixture miillpore filter, polyethersulfone millipore filter, polytetrafluoroethylene (PTFE) miillpore filter or anodised aluminium miillpore filter, and its pore diameter range is 100 ~ 450nm.
Fig. 3 a is graphene oxide is that the salt ion Penetration Signature of compound desalination membrane after ultraviolet light irradiates 0 day and 3 days respectively that the cellulose mixture miillpore filter substrate of 220nm forms compares with TiOx nano sheet in aperture.
Fig. 3 b is the graphene oxide that recorded by isotope-labelling method is that the hydrone Penetration Signature of compound desalination membrane after ultraviolet light irradiates 0 day and 3 days respectively that the cellulose mixture miillpore filter substrate of 220nm forms compares with TiOx nano sheet in aperture.So-called isotope-labelling method is with a certain amount of heavy water molecule D
2o goes to mark the aqueous solvent in salting liquid, by research D
2the transmembrane Penetration Signature of O molecule and then the Penetration Signature of extrapolated hydrone.
Be described below by several specific embodiment.
Embodiment one
The present embodiment comprises the following steps:
1) by the aqueous solution Homogeneous phase mixing of the aqueous solution and TiOx nano sheet that comprise graphene oxide thin slice; Graphene oxide water solution volume mass concentration is 40mg/L, and TiOx nano sheet aqueous solution volume mass concentration is 32mg/L, and in the mixed solution of graphene oxide and TiOx nano sheet, graphene oxide and TiOx nano tablet quality are than being 1:0.8;
2) take aperture as the cellulose mixture miillpore filter of 220nm be substrate, adopt vacuum filtration method that the mixed solution of graphene oxide and TiOx nano sheet is dewatered under negative pressure, and then mutual stacking self assembly is laminar film in miillpore filter substrate, dry 24h under 55 DEG C of conditions;
3) by UV-irradiation 3 days, utilize the photocatalysis characteristic of TiOx nano sheet to make graphene oxide uniform change for redox graphene, finally obtain compound desalination membrane.
The miillpore filter diameter adopted in the present embodiment is about 5cm, and the area of prepared compound desalination membrane is about 15cm
2the functional layer thickness of redox graphene and the mutual stacking self assembly of TiOx nano sheet is about 8 μm, prepared compound desalination membrane have flexibility, evenly, area and thickness is controlled, form and the advantage such as structure is adjustable, high strength and high desalination performance, can be used for water desalination field.
Fig. 2 is the light microscopic microscopic sdIBM-2+2q.p.approach photo of compound desalination membrane prepared by the present embodiment, and wherein redox graphene and TiOx nano sheet are that in the cellulose mixture miillpore filter substrate of 220nm, the mutual stacking surface that formed has the layered composite film of a lot of microcosmic fold in aperture.Graphene oxide and TiOx nano sheet in aperture be compound desalination membrane that the cellulose mixture miillpore filter substrate of 220nm the forms salt ion permeance property after ultraviolet light irradiates 0 day and 3 days respectively more as shown in Figure 3 a, hydrone permeance property is more as shown in Figure 3 b.Result shows, compared to the UV-irradiation compound desalination membrane of 0 day, the compound desalination membrane of UV-irradiation after 3 days has excellent desalting performance, salt rejection rate is up to more than 95%, simultaneously its Water permeability can remain to more than 60% before UV-irradiation, and show thus, the compound desalination membrane prepared by the present invention has excellent desalting performance, high Water permeability can be kept simultaneously, can be applicable to water desalination field.
Embodiment two
The present embodiment comprises the following steps:
1) by the aqueous solution Homogeneous phase mixing of the aqueous solution and TiOx nano sheet that comprise graphene oxide thin slice; Graphene oxide water solution volume mass concentration is 40mg/L, and TiOx nano sheet aqueous solution volume mass concentration is 10mg/L, and in the mixed solution of graphene oxide and TiOx nano sheet, graphene oxide and TiOx nano tablet quality are than being 1:0.25;
2) take aperture as the anodised aluminium miillpore filter of 100nm be substrate, adopt vacuum filtration method that the mixed solution of graphene oxide and TiOx nano sheet is dewatered under negative pressure, and then mutual stacking self assembly is laminar film in miillpore filter substrate, dry 24h under 40 DEG C of conditions;
3) by UV-irradiation 1 day, utilize the photocatalysis characteristic of TiOx nano sheet to make graphene oxide uniform change for redox graphene, finally obtain compound desalination membrane.
The miillpore filter diameter adopted in the present embodiment is about 2.5cm, and the area of prepared compound desalination membrane is about 4cm
2the functional layer thickness of redox graphene and the mutual stacking self assembly of TiOx nano sheet is about 1 μm, prepared compound desalination membrane have flexibility, evenly, area and thickness is controlled, form and the advantage such as structure is adjustable, high strength and high desalination performance, can be used for water desalination field.
Embodiment three
The present embodiment comprises the following steps:
1) by the aqueous solution Homogeneous phase mixing of the aqueous solution and TiOx nano sheet that comprise graphene oxide thin slice; Graphene oxide water solution volume mass concentration is 0.5mg/L, and TiOx nano sheet aqueous solution volume mass concentration is 2mg/L, and in the mixed solution of graphene oxide and TiOx nano sheet, graphene oxide and TiOx nano tablet quality are than being 1:4;
2) take aperture as the polyethersulfone millipore filter of 450nm be substrate, adopt vacuum filtration method that the mixed solution of graphene oxide and TiOx nano sheet is dewatered under negative pressure, and then mutual stacking self assembly is laminar film in miillpore filter substrate, dry 4h under 80 DEG C of conditions;
3) by UV-irradiation 5 days, utilize the photocatalysis characteristic of TiOx nano sheet to make graphene oxide uniform change for redox graphene, finally obtain compound desalination membrane.
The miillpore filter diameter adopted in the present embodiment is about 1.5cm, and the area of prepared compound desalination membrane is about 1cm
2the functional layer thickness of redox graphene and the mutual stacking self assembly of TiOx nano sheet is about 20nm, prepared compound desalination membrane have flexibility, evenly, area and thickness is controlled, form and the advantage such as structure is adjustable, high strength and high desalination performance, can be used for water desalination field.
Embodiment four
The present embodiment comprises the following steps:
1) by the aqueous solution Homogeneous phase mixing of the aqueous solution and TiOx nano sheet that comprise graphene oxide thin slice; Graphene oxide water solution volume mass concentration is 0.5mg/L, and TiOx nano sheet aqueous solution volume mass concentration is 0.4mg/L, and in the mixed solution of graphene oxide and TiOx nano sheet, graphene oxide and TiOx nano tablet quality are than being 1:0.8;
2) take aperture as the polytetrafluoroethylene (PTFE) miillpore filter of 220nm be substrate, adopt vacuum filtration method that the mixed solution of graphene oxide and TiOx nano sheet is dewatered under negative pressure, and then mutual stacking self assembly is laminar film in miillpore filter substrate, dry 12h under 50 DEG C of conditions;
3) by UV-irradiation 3 days, utilize the photocatalysis characteristic of TiOx nano sheet to make graphene oxide uniform change for redox graphene, finally obtain compound desalination membrane.
The miillpore filter diameter adopted in the present embodiment is about 1.2m, and the area of prepared compound desalination membrane is about 1m
2the functional layer thickness of redox graphene and the mutual stacking self assembly of TiOx nano sheet is about 10nm, prepared compound desalination membrane have flexibility, evenly, area and thickness is controlled, form and the advantage such as structure is adjustable, high strength and high desalination performance, can be used for water desalination field.
The compound desalination membrane that redox graphene in above-described embodiment and TiOx nano sheet form in miillpore filter substrate all has excellent desalting performance, can keep excellent Water permeability simultaneously.Laminated film area can reach 1cm
2~ 1m
2, thickness can be controlled in 10nm ~ 10 μm, have flexibility, evenly, area and thickness is controlled, form and the advantage such as structure is adjustable, high strength and high desalination performance, can be used for water desalination field.
Claims (5)
1. a compound desalination membrane, it is characterized in that, this compound desalination membrane is made up of miillpore filter basalis (3) and functional layer, and described functional layer is by redox graphene (1) and the laminar film of TiOx nano sheet (2) by the mutual stacking self assembly of Homogeneous phase mixing.
2. a kind of compound desalination membrane as claimed in claim 1, is characterized in that: the area of laminated film is 1cm
2~ 1m
2, thickness is in 10nm ~ 10 μm.
3. the preparation method of a kind of compound desalination membrane as claimed in claim 1, is characterized in that described method comprises the steps:
1) by the aqueous solution Homogeneous phase mixing of the aqueous solution and TiOx nano sheet that comprise graphene oxide thin slice; Graphene oxide water solution volume mass concentration adopts 0.5 ~ 40mg/L, TiOx nano sheet aqueous solution volume mass concentration adopts 0.4 ~ 32mg/L, in the mixed solution of graphene oxide and TiOx nano sheet, graphene oxide and TiOx nano tablet quality are than being 1:0.25 ~ 4;
2) take miillpore filter as substrate, adopt vacuum filtration method that the mixed solution of graphene oxide and TiOx nano sheet is dewatered under negative pressure, and then mutual stacking self assembly is laminar film in miillpore filter substrate, dry 4 ~ 24h under 40 ~ 80 DEG C of conditions;
3) by UV-irradiation 1 ~ 5 day, utilize the photocatalysis characteristic of TiOx nano sheet to make graphene oxide uniform change for redox graphene, finally obtain compound desalination membrane.
4. the preparation method of a kind of compound desalination membrane as claimed in claim 3, it is characterized in that, described miillpore filter basalis adopts cellulose mixture miillpore filter, polyethersulfone millipore filter, polytetrafluoroethylene (PTFE) miillpore filter or anodised aluminium miillpore filter, and its pore diameter range is 100 ~ 450nm.
5. the application of compound desalination membrane in water desalination as claimed in claim 1.
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