CN104258738A - Forward osmosis organic-inorganic composite membrane and preparation method thereof - Google Patents
Forward osmosis organic-inorganic composite membrane and preparation method thereof Download PDFInfo
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- CN104258738A CN104258738A CN201410508096.2A CN201410508096A CN104258738A CN 104258738 A CN104258738 A CN 104258738A CN 201410508096 A CN201410508096 A CN 201410508096A CN 104258738 A CN104258738 A CN 104258738A
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Abstract
The invention discloses a forward osmosis organic-inorganic composite membrane. The forward osmosis organic-inorganic composite membrane comprises at least one basement membrane layer, wherein the basement membrane layer comprises a polymer and nano-particles dispersed in the basement membrane layer; the water flux of the forward osmosis organic-inorganic composite membrane is more than 12L.m<-2>.h<-1>. The invention further discloses a preparation method of the forward osmosis organic-inorganic composite membrane. The contact area between the forward osmosis organic-inorganic composite membrane provided by the invention and water is large, the forward osmosis organic-inorganic composite membrane has high hydrophily, and the water flux of the forward osmosis organic-inorganic composite membrane is improved to a great extent. In addition, the antibacterial performance of the forward osmosis membrane is obviously improved, the defect that a conventional forward osmosis organic-inorganic composite membrane is easily polluted by microorganisms in a water treatment environment is overcome, the service life of the forward osmosis membrane is prolonged, and the forward osmosis organic-inorganic composite membrane is a novel forward osmosis organic-inorganic composite membrane with a wide application potential.
Description
Technical field
The present invention relates to technical field of membrane separation, be specially and just permeate Organic inorganic film and preparation method thereof.
Background technology
Membrane separating process is a kind of energy-efficient water treatment procedure, and membrane for water treatment is the core of water treatment by membrane process, and can the quality of its performance decides water treatment by membrane process large-scale application.Forward osmosis membrane separation process is a kind of new membrane isolation technics grown up in the last few years, and compared with traditional pressure-driven membrane process, positive process of osmosis does not need impressed pressure, energy consumption is less, the pollution level of process to film is lower, and the rate of recovery of process is higher, and environmental effect is friendly.Forward osmosis membrane is the core of positive process of osmosis, and can the quality of its performance decide positive process of osmosis and obtain large-scale application.In current diffusion barrier market, reverse osmosis membrane accounts for 85% of film market, the preparation process development of reverse osmosis membrane is comparatively ripe, commodity reverse osmosis membrane can reach very high flux, and it is less to the research for the forward osmosis membrane in positive process of osmosis at present, in Patents WO2006110497A2, the material selection cellulose acetate class of forward osmosis membrane, make the restriction being subject to Treatment Solution pH condition in its application process, and its membrane flux is lower.
The principal element restricting membrane flux in positive process of osmosis is the interior concentration polarization phenomenon occurred in process in porous support layer, its existence makes forward osmosis membrane flux far below theoretical membrane flux, and the flux that therefore will improve forward osmosis membrane will interior concentration polarization phenomenon in reduction process as far as possible.A lot of research institution just carries out research and probe in the preparation of involutory forward osmosis membrane in the world at present, but generally, is just permeating and having the raising of the flux of film not to be very large.Therefore develop high flux, high performance forward osmosis membrane aligns process of osmosis and has great importance.
Because membrane for water treatment is applied in water body environment, the microorganism in water body of long duration is easily attached to the surface of film, damages, thus change the original performance of film to fenestra.Therefore, prepare the membrane for water treatment with high anti-microbial property the application of film in water treatment procedure is also had great importance.Especially for the forward osmosis membrane all at multiple fields with extensive use potentiality that new development is got up, it is compared to traditional pressure-driven film, in application process, the both sides of film all contact with solution, thus add the tendency of film by microbial contamination, therefore antibacterial film is also very important for positive process of osmosis.
Summary of the invention
Technical problem solved by the invention is to provide one just to permeate Organic inorganic film and preparation method thereof, this is just permeating the permeation flux that Organic inorganic film not only can significantly improve film, remain high rejection, and anti-microbial property also can significantly be increased, in order to solve the problem proposed in above-mentioned background technology.
For achieving the above object, the invention provides following technical scheme:
Just permeate Organic inorganic film, comprise at least one bottom membrane, described bottom membrane comprises polymer and is scattered in the nano particle in described bottom membrane; The described water flux just permeating Organic inorganic film is greater than 12Lm
-2h
-1.
In described bottom membrane, the content of nano particle is the 0.05-5wt% of the gross weight of bottom membrane, and preferred version is 0.1-2wt%.
Described nano particle is TiO
2one or more in nano particle, metal nanoparticle, the zeolite molecular sieve being loaded with metal ion, NaA type zeolite molecular sieve, the particle diameter of nano particle is 0.1-4 μm, preferably, is 0.5-2 μm.
Polymer in described bottom membrane comprises (a) and organizes the polymer that polymer or (b) organize, wherein (a) organizes polymer is one or more in polysulfones, polyether sulfone, SPSF, polysulfonamides, poly (aryl ether sulfone ketone), poly (arylene ether nitrile) ketone, copolyether sulfone, Kynoar, polyacrylonitrile, and the polymer that (b) organizes is cellulose acetate base polymer.
The mass ratio of described polymer and nano particle is 10-22: 0.04-20, and preferred version is 10-18: 0.1-2.
The described Organic inorganic film that just permeates also comprises supporting layer for support base rete and/or the active layer that is positioned on bottom membrane.
Described active layer is by interface polymerization reaction and bottom membrane compound.
Described supporting layer is non-woven fabrics, polyester screen, brown paper or its combination.
Described metal nanoparticle is Nano silver grain, copper nano-particle, zinc nano particle, Fe nanometer particles or its combination.
Described nano particle is porous material.
Just permeating the preparation method of Organic inorganic film, comprising the following steps:
(1) provide a casting solution, described casting solution contains polymer, nano particle and solvent;
(2) described casting solution is coated on base material, then leave standstill in atmosphere, until solvent volatilization wherein forms dense layer surface, the film of the dense layer surface of formation is placed on gel in coagulation bath, required bottom membrane is obtained after inversion of phases, by the bottom membrane washed with de-ionized water obtained, thus the organic solvent that removing is remaining;
(3) gained bottom membrane is both for just to permeate Organic inorganic film; Or when described base material is used as supporting layer, obtain the just infiltration Organic inorganic film containing supporting layer and polymer film.
In described casting solution, the content of polymer is the 10-22wt% of casting solution gross weight, and in described casting solution, the content of nano particle is the 0.04-20wt% of casting solution gross weight.
The thickness of described bottom membrane is 80-200 μm, is preferably 80-180 μm, is more preferably 100-150 μm.
Casting solution described in step (1) is by following placement preparation:
(1) polymer is dissolved in solvent (preferably dissolve adding under thermal agitation, stir 6-9 hour under 60 DEG C of conditions), forms polymer solution;
(2) nano particle is added in described polymer solution, form casting solution.
The coagulation bath used in described phase inversion comprises the mixed solution of deionized water or deionized water and solvent for use.
Described solvent is dioxane, 1-METHYLPYRROLIDONE, DMA, triethyl phosphate or its combination.
The method of just permeating, comprises the following steps: use the just infiltration Organic inorganic film described in claim 1 just to permeate.
The present invention, compared with conventional art, has the following advantages:
Provided by the inventionly just permeate Organic inorganic film and water has larger contact area, and there is good hydrophily, improve the water flux just permeating Organic inorganic film largely.In addition, the anti-microbial property of forward osmosis membrane significantly improves, and solves tradition and is just permeating the defect that Organic inorganic film is subject to microbial contamination in water treatment environment, extending the service life of forward osmosis membrane, is a kind ofly have the novel of extensive use potentiality and just permeate Organic inorganic film.
Detailed description of the invention
Below in conjunction with the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
Just permeate Organic inorganic film and preparation method thereof:
Adopt cellulose acetate as polymer, 12g cellulose acetate and 0.4gAg nano particle (particle diameter is 1.5 μm) are added 87.6g 1, in 4-dioxane solvent, stirring and dissolving forms the casting solution that content is the Ag nano particle of 0.4wt%, gel-forming film in coagulation bath, by prepared film washed with de-ionized water, the organic solvent that removing is remaining, obtain and just permeate Organic inorganic film, preserve for subsequent use in deionized water.
After tested, the flux just permeating Organic inorganic film that prepared by the present embodiment is 20Lm
-2h
-1, rejection is more than 99%.
The prepared Organic inorganic film that just permeates carries out microbial contamination experiment at identical conditions with the film of not plus nano particle.E. coli microorganisms is added on film surface, the microbial adhesion situation on microscopic examination film surface is adopted after 24h, find a large amount of microorganism of the film surface attachment that the film adding nano particle does not add without microbial adhesion, indicate the film adding nano particle and there is obvious antibiotic property.Antibiotic rate is greater than 90%.
Embodiment 2
Just permeate Organic inorganic film and preparation method thereof:
Take 16g polysulfone polymer, be dissolved in the mixed solvent that 84g is made up of DMA and PEG400 (the two ratio is 76: 8), be made into the polysulfones solution that polymer concentration is 18%.The NaA type zeolite molecular sieve nano particle (particle diameter is 1.5 μm) carrying silver that 2g has hexahedral shape is added in the polysulfones solution prepared, the casting solution carrying the NaA type zeolite molecular sieve nano particle of silver containing 2wt% is made at ultrasonic middle dispersion 30min, casting solution is coated on low-density nonwoven fabric supporting layer, certain thickness scraper is adopted to carry out knifing, put into coagulation bath gel film forming, m-phenylene diamine (MPD) and pyromellitic trimethylsilyl chloride is adopted to carry out interface polymerization reaction (reacting 3min at 110 DEG C) on the film formed, thus obtained just permeate Organic inorganic film.
After tested, the water flux just permeating Organic inorganic film that prepared by the present embodiment is 18Lm
-2h
-1, rejection is more than 99%.
Microbial contamination experiment is carried out to prepared film, adds e. coli microorganisms on film surface, after 24h, adopt the microbial adhesion situation on microscopic examination film surface, find that its surface is without microbial adhesion, shows that this film has obvious anti-microbial property.Antibiotic rate is greater than 90%.
Embodiment 3
Just permeate Organic inorganic film and preparation method thereof:
Take 18g polysulfone polymer, the TiO2 nano particle (particle diameter is 2 μm) that 0.6g is spherical, be dissolved in 82g by N, in the mixed solvent of N-dimethylacetylamide and PEG400 composition (the two ratio is 72: 10), to be made into polysulfones concentration be 18wt%, TiO2 nanoparticle concentration is the casting solution of 0.6wt%.Casting solution is coated on low-density nonwoven fabric supporting layer, adopts certain thickness scraper to carry out knifing, put into coagulation bath gel film forming, obtain and just permeate Organic inorganic film, preserve for subsequent use in deionized water.
After tested, the water flux just permeating Organic inorganic film that prepared by the present embodiment is 22Lm
-2h
-1, rejection is more than 99%.
Microbial contamination experiment is carried out to prepared film, adds e. coli microorganisms on film surface, after 24h, adopt the microbial adhesion situation on microscopic examination film surface, find that its surface is without microbial adhesion, shows that this film has obvious anti-microbial property.Antibiotic rate is greater than 90%.
Embodiment 4
Just permeate Organic inorganic film and preparation method thereof:
Take 8g Triafol T polymer, be dissolved in the mixed solvent that 84g is made up of triethyl phosphate and PEG400 (the two ratio is 72: 8), be made into the triacetate fiber cellulose solution that concentration is 8wt%.In the solution prepared, add the zeolite molecular sieve nano particle (particle diameter is 1.5 μm) carrying iron ion that 1g has tetrahedron shape, obtain at ultrasonic middle dispersion 30min the casting solution that nanoparticle concentration is 1%.Casting solution is coated on low-density nonwoven fabric supporting layer, adopts certain thickness scraper to carry out knifing, put into coagulation bath gel film forming, obtain and just permeate Organic inorganic film, preserve for subsequent use in deionized water.
After tested, the water flux just permeating Organic inorganic film that prepared by the present embodiment is 25Lm
-2h
-1, rejection is more than 99%.
Microbial contamination experiment is carried out to prepared film, adds e. coli microorganisms on film surface, after 24h, adopt the microbial adhesion situation on microscopic examination film surface, find that its surface is without microbial adhesion, shows that this film has obvious anti-microbial property.Antibiotic rate is greater than 90%.
Embodiment 5
Just permeate Organic inorganic film and preparation method thereof:
Adopt cellulose acetate as polymer, 10g cellulose acetate is added in 90g dioxane, dissolve add thermal agitation 6-9 hour at 60 DEG C after, form the cellulose acetate solution of 10wt%, in this solution, add 0.1g Ag nano particle (particle diameter is 1.5 μm), after ultrasonic disperse, be made into the casting solution of the Ag nano particle containing 0.1wt%, through inversion of phases film forming, by prepared film washed with de-ionized water, the organic solvent that removing is remaining, thus obtained forward osmosis membrane.
After tested, the water flux of forward osmosis membrane that prepared by the present embodiment is 12Lm
-2h
-1.
Microbial contamination experiment is carried out to prepared film, adds e. coli microorganisms on film surface, after 24h, adopt the microbial adhesion situation on microscopic examination film surface, find its surperficial less microbial adhesion, show that this film has certain anti-microbial property.Antibiotic rate is greater than 90%.
Comparative example 1
Tradition is just permeating the preparation of Organic inorganic film:
Adopt cellulose acetate as polymer, 10g cellulose acetate is added in 90g dioxane, dissolve add thermal agitation 6-9 hour at 60 DEG C after, form the cellulose acetate casting solution of 10wt%, through inversion of phases film forming, by prepared film washed with de-ionized water, the organic solvent that removing is remaining, thus obtainedly just permeate Organic inorganic film.
After tested, the water flux just permeating Organic inorganic film that prepared by the present embodiment is 8Lm
-2h
-1.
Microbial contamination experiment is carried out to prepared film, e. coli microorganisms is added on film surface, after 24h, adopt the microbial adhesion situation on microscopic examination film surface, find that its surperficial Escherichia coli number increases, show the easy microbial contamination of film that non-plus nano is particle modified.
Comparative example 2
Tradition is just permeating the preparation of Organic inorganic film:
Adopt cellulose acetate as polymer, 10g cellulose acetate is added in 90g dioxane, dissolve add thermal agitation 6-9 hour at 60 DEG C after, form the cellulose acetate solution of 10wt%, 0.01g Ag nano particle (particle diameter is 1.5 μm) is added in this solution, the casting solution of the Ag nano particle containing 0.01wt% is made into after ultrasonic disperse, through inversion of phases film forming, by prepared film washed with de-ionized water, the organic solvent that removing is remaining, thus obtainedly just permeate Organic inorganic film.
After tested, the water flux just permeating Organic inorganic film that prepared by the present embodiment is 7.5Lm
-2h
-1.
Microbial contamination experiment is carried out to prepared film, adds e. coli microorganisms on film surface, after 24h, adopt the microbial adhesion situation on microscopic examination film surface, find that its surperficial Escherichia coli number has certain increase.
The various performance parameters of just permeating Organic inorganic film of embodiment 1-5 and comparative example 1-2 is in table 1.
Table 1
As shown in table 1, the anti-microbial property just permeating Organic inorganic film of the present invention significantly improves, and antibiotic rate is all greater than 90%, and the penetrating amount of positive osmosis composite membrane is also significantly improved, up to 25Lm simultaneously
-2h
-1, and positive osmosis composite membrane has the high rejection of 99-99.99%, and the penetrating amount of just permeating Organic inorganic film not adding nano particle is only 7-8Lm
-2h
-1, anti-microbial property is poor, and rejection does not reach requirement yet.When nanoparticle content is too low, the obtained penetrating amount of just permeating Organic inorganic film is also only 7-8Lm
-2h
-1, anti-microbial property and rejection effect can not get improving, and show that nanoparticle content is very few and not only do not reach the effect of increase water flux but also effectively can not improve the anti-microbial property of film.As can be seen here, the Organic inorganic film that just permeating of the present invention significantly improves water flux and has high rejection, solve the defect that traditional forward osmosis membrane is subject to microbial contamination in water treatment environment, be a kind of novel forward osmosis membrane with extensive use potentiality simultaneously.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
In addition, be to be understood that, although this description is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of description is only for clarity sake, those skilled in the art should by description integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (10)
1. just permeate Organic inorganic film, it is characterized in that, comprise at least one bottom membrane, described bottom membrane comprises polymer and is scattered in the nano particle in described bottom membrane.
2. according to claim 1ly just permeate Organic inorganic film, it is characterized in that, in described bottom membrane, the content of nano particle is the 0.05-5wt% of the gross weight of bottom membrane.
3. according to claim 1ly just permeate Organic inorganic film, it is characterized in that, described nano particle is TiO
2one or more in nano particle, metal nanoparticle, the zeolite molecular sieve being loaded with metal ion, NaA type zeolite molecular sieve, the particle diameter of nano particle is 0.1-4 μm.
4. according to claim 1ly just permeate Organic inorganic film, it is characterized in that, polymer in described bottom membrane comprises (a) and organizes the polymer that polymer or (b) organize, wherein (a) organizes polymer is one or more in polysulfones, polyether sulfone, SPSF, polysulfonamides, poly (aryl ether sulfone ketone), poly (arylene ether nitrile) ketone, copolyether sulfone, Kynoar, polyacrylonitrile, and the polymer that (b) organizes is cellulose acetate base polymer.
5. according to claim 1ly just permeate Organic inorganic film, it is characterized in that, the mass ratio of described polymer and nano particle is 10-22: 0.04-20.
6. according to claim 1ly just permeate Organic inorganic film, it is characterized in that, also comprise the supporting layer for support base rete and/or the active layer that is positioned on bottom membrane.
7. just permeating the preparation method of Organic inorganic film, it is characterized in that, comprise the following steps:
(1) provide a casting solution, described casting solution contains polymer, nano particle and solvent;
(2) described casting solution is coated on base material, then leave standstill in atmosphere, until solvent volatilization wherein forms dense layer surface, the film of the dense layer surface of formation is placed on gel in coagulation bath, required bottom membrane is obtained after inversion of phases, by the bottom membrane washed with de-ionized water obtained, thus the organic solvent that removing is remaining;
(3) gained bottom membrane is both for just to permeate Organic inorganic film; Or when described base material is used as supporting layer, obtain the just infiltration Organic inorganic film containing supporting layer and polymer film.
8. the described preparation method just permeating Organic inorganic film according to claim 7, it is characterized in that, in casting solution, the content of polymer is the 10-22wt% of casting solution gross weight, and in described casting solution, the content of nano particle is the 0.04-20wt% of casting solution gross weight.
9. the described preparation method just permeating Organic inorganic film according to claim 7, is characterized in that, casting solution described in step (1) is by following placement preparation:
(1) polymer is dissolved in solvent, forms polymer solution;
(2) nano particle is added in described polymer solution, form casting solution.
10. the method for just permeating, is characterized in that, comprises the following steps: use the just infiltration Organic inorganic film described in claim 1 just to permeate.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105771704A (en) * | 2016-04-22 | 2016-07-20 | 浙江工业大学 | Preparation method of novel anti-pollution high-selectivity sulfonated polysulfone nanofiltration membrane |
| CN106166451A (en) * | 2016-06-28 | 2016-11-30 | 安徽松泰包装材料有限公司 | A kind of preparation method of forward osmosis membrane |
| CN106492637A (en) * | 2016-12-14 | 2017-03-15 | 东华大学 | Positive osmosis composite membrane of a kind of TiO2/PSF nanofibers and preparation method thereof |
| CN108314891A (en) * | 2018-03-21 | 2018-07-24 | 安徽江淮汽车集团股份有限公司 | A kind of PEO composite material and preparation methods |
| CN109289808A (en) * | 2018-10-31 | 2019-02-01 | 陕西科技大学 | A kind of aromatic polysulfonamide adsorbing material of graphene oxide doped and its preparation method and application |
| CN112221363A (en) * | 2020-09-10 | 2021-01-15 | 闽南师范大学 | Forward osmosis composite membrane and preparation method and application thereof |
| CN113491961A (en) * | 2021-09-09 | 2021-10-12 | 北京宝盛通国际电气工程技术有限公司 | Forward osmosis membrane and preparation method thereof |
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2014
- 2014-09-28 CN CN201410508096.2A patent/CN104258738A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105771704A (en) * | 2016-04-22 | 2016-07-20 | 浙江工业大学 | Preparation method of novel anti-pollution high-selectivity sulfonated polysulfone nanofiltration membrane |
| CN106166451A (en) * | 2016-06-28 | 2016-11-30 | 安徽松泰包装材料有限公司 | A kind of preparation method of forward osmosis membrane |
| CN106492637A (en) * | 2016-12-14 | 2017-03-15 | 东华大学 | Positive osmosis composite membrane of a kind of TiO2/PSF nanofibers and preparation method thereof |
| CN108314891A (en) * | 2018-03-21 | 2018-07-24 | 安徽江淮汽车集团股份有限公司 | A kind of PEO composite material and preparation methods |
| CN109289808A (en) * | 2018-10-31 | 2019-02-01 | 陕西科技大学 | A kind of aromatic polysulfonamide adsorbing material of graphene oxide doped and its preparation method and application |
| CN112221363A (en) * | 2020-09-10 | 2021-01-15 | 闽南师范大学 | Forward osmosis composite membrane and preparation method and application thereof |
| CN113491961A (en) * | 2021-09-09 | 2021-10-12 | 北京宝盛通国际电气工程技术有限公司 | Forward osmosis membrane and preparation method thereof |
| CN113491961B (en) * | 2021-09-09 | 2022-02-01 | 北京宝盛通国际电气工程技术有限公司 | Forward osmosis membrane and preparation method thereof |
| WO2023035555A1 (en) * | 2021-09-09 | 2023-03-16 | 北京宝盛通国际电气工程技术有限公司 | Forward osmosis membrane and preparation method therefor |
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