CN109876681A - A kind of high throughput mixed-matrix nanofiltration membrane and preparation method thereof - Google Patents
A kind of high throughput mixed-matrix nanofiltration membrane and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of high-throughput mixed-matrix nanofiltration membranes and preparation method thereof, will dry after polysulfone ultrafiltration membrane support membrane and time of infusion in zinc nitrate hexahydrate aqueous solution；It will be dried after time of infusion in obtained film and aqueous phase monomers, form water phase liquid layer；Wherein aqueous phase monomers are piperazine；It is dried in an oven after obtained film is contacted a period of time with the organic phase solution containing activated monomer；Wherein organic phase activated monomer is pyromellitic trimethylsilyl chloride；Film is immersed in the methanol solution containing 2-methylimidazole ligand and washes off extra ligand after a period of time with methanol solvate.ZIF-8 nano particle in the present invention can be dispersed in nanofiltration film layer bottom by situ synthesis, and intermediate and surface can increase the surface area of separating layer, to improve water flux in this way.
Description
Technical field
The present invention relates to Nanofiltration-membrane technique fields, and in particular to it is a kind of high throughput mixed-matrix nanofiltration membrane and its preparation side
Method.
Background technique
Addition nanoparticle, which is modified it, in nanofiltration functional layer has many advantages, addition nanoparticle has behaviour
Make simple feature, as the nanotechnology in molecular scale function system have it is more longlasting, more clean, safer product,
Have become a kind of very important means in modified nanofiltration membrane now.Composite membrane is modified with particle-filled method and has been attracted more
Carry out the concern of more researchers, and inorganic nano-particle is also developed into from initial general particle method and hurts to compound film properties
The lesser nanoparticle of evil, such as: nano-TiO2, Nano-meter SiO_22, NaX, nanometer Al2O3, nanometer Ag, the nanoparticles such as ZIF-8.MOF
The common feature of organic polymer and inorganic compound is had both, Yaghi team researches and develops at the beginning of 21 century and ZIF-8 material is prepared
Material, they are dissolved separately in n,N-Dimethylformamide China by zinc nitrate hexahydrate and 2- methyl azoles, are closed with solvent-thermal method
At preparation ZIF-8 zeolite imidazole frame material.There is low-density, high-specific surface area, structure function can design for it, pore size can
The features such as tune, in multiple fields such as UF membrane, gas absorption, catalysis and drug releases.However traditional particle-filled method meeting
There are inorganic problems compatible with the interface of organic material, make Zn using in situ synthesis2+ can be complexed with aqueous phase monomers, from
And overcome inorganic problem compatible with the interface of organic material；The surface area of the mixed substrate membrane containing nano-grade molecular sieve is increased simultaneously, is solved existing
There is the problem that nanometer filtering film water flux is not high in technology, improves nanofiltration membrane sewage treatment capacity.
Summary of the invention
Present invention solves the technical problem that be that interfacial polymerization mode forms a film in the presence of uneven, this defective disadvantage of surface,
It, in this way can be with so that ZIF-8 nano particle can be dispersed in nanofiltration film layer bottom, centre and surface by situ synthesis
Increase the surface area of separating layer；Simultaneously because Zn2+It can be complexed with aqueous phase monomers, to overcome inorganic and organic material boundary
The compatible problem in face.
For this purpose, The technical solution adopted by the invention is as follows:
A kind of preparation method of high throughput mixed-matrix nanofiltration membrane, includes the following steps:
(1) it will be dried after polysulfone ultrafiltration membrane support membrane and time of infusion in zinc nitrate hexahydrate aqueous solution；
(2) it will be dried after time of infusion in film and aqueous phase monomers that step (1) obtains, form water phase liquid layer；Wherein
Aqueous phase monomers are piperazine；
(3) film for obtaining step (2) with containing activated monomer organic phase solution contact a period of time after in an oven
Drying；Wherein organic phase activated monomer is pyromellitic trimethylsilyl chloride；
(4) film that step (3) obtains was immersed in the methanol solution containing 2-methylimidazole ligand after a period of time and is used
Methanol solvate washes off extra ligand.
Preferably, the mass fraction of the zinc nitrate hexahydrate aqueous solution in step (1) is 0.01-10wt%；Dip time
For 1-15min.
Preferably, the mass fraction of the aqueous phase monomers in step (2) is 0.001-0.5wt%；Dip time is 1-
10min。
Preferably, the mass fraction of the organic phase activated monomer in step (3) is 0.001-0.5wt%；Dipping
Time is 1-5min.
Preferably, the oven temperature in step (3) is 30-80 DEG C, drying time 5-30min.
Preferably, the mass fraction of the 2-methylimidazole ligand in step (4) is 0.1-2wt%, soaking time 1h-
24h。
The above method obtains a kind of mixed-matrix nanofiltration membrane of high throughput.
Effect of the invention is that:
(1) ZIF-8 nano particle can be dispersed in nanofiltration film layer bottom, centre and surface by situ synthesis, in this way
The surface area of separating layer can be increased, to improve water flux.
(2) simultaneously because Zn2+It can be complexed with aqueous phase monomers, to overcome inorganic compatible with the interface of organic material ask
Topic.
(3) the nanometer particle-modified water flux for effectively increasing polyamide composite film of ZIF-8, and rejection does not drop
It is low.
Detailed description of the invention
Fig. 1 is the exterior view of 1 mixed-matrix nanofiltration membrane of embodiment.
Fig. 2 is the cross-section diagram of 2 mixed-matrix nanofiltration membrane of embodiment.
Fig. 3 is the exterior view of nanofiltration membrane in comparative example.
In figure, probe receives secondary electron signal in SU8010 expression machine models, SE (UL) expression.
Specific embodiment
It to facilitate the understanding of the present invention, below will be to invention is more fully described.But the present invention can be to be permitted
Mostly different form is realized, however it is not limited to embodiment described herein.On the contrary, purpose of providing these embodiments is makes
It is more thorough and comprehensive to the understanding of the disclosure.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more phases
Any and all combinations of the listed item of pass.
Embodiments of the present invention is further illustrated below:
Embodiment 1:
Do film condition: 25 DEG C, relative humidity 40% ± 2.
(1) it weighs 1.2306g zinc nitrate hexahydrate and is dissolved in 100ml deionized water, by polysulfone ultrafiltration membrane support membrane and six
It is dried after impregnating 4min in nitric hydrate zinc aqueous solution.
(2) 0.2502g piperazine dissolved is weighed in 100ml deionized water, in the film and aqueous phase monomers that step (1) is obtained
It is dried after 4min, forms water phase liquid layer.
(3) 0.1003g pyromellitic trimethylsilyl chloride is weighed to be dissolved in 100ml n-hexane, by film that step (2) obtains with contain
15min is dried in 60 DEG C of baking oven after the organic phase solution 1min of activated monomer.
(4) it weighs 2.7111g 2-methylimidazole to be dissolved in 300ml methanol, the film that step (3) obtains is immersed in and is contained
Have in the methanol solution of 2-methylimidazole ligand steeped after 12h it is to be tested in methanol solvate.
1 gained mixed-matrix nanofiltration membrane of embodiment is analyzed:
Membrane structure is observed under Electronic Speculum, as a result as shown in Figure 1:
Mixed-matrix nanofiltration membrane prepared by this example is fitted into film properties evaluating apparatus, experiment condition: 0.6M Pa, in advance
Press 1h, sodium sulfate concentration 1000ppm；Experimental result: water flux: 99.87L/m2H retention: 90.51%.
Embodiment 2:
Do film condition: 25 DEG C, relative humidity 40% ± 2.
(1) it weighs 1.8406g zinc nitrate hexahydrate and is dissolved in 100ml deionized water, by polysulfone ultrafiltration membrane support membrane and six
It is dried after impregnating 4min in nitric hydrate zinc aqueous solution.
(2) 0.2502g piperazine dissolved is weighed in 100ml deionized water, in the film and aqueous phase monomers that step (1) is obtained
It is dried after 4min, forms water phase liquid layer.
(3) 0.1003g pyromellitic trimethylsilyl chloride is weighed to be dissolved in 100ml n-hexane, by film that step (2) obtains with contain
15min is dried in 60 DEG C of baking oven after the organic phase solution 1min of activated monomer.
(4) it weighs 2.7111g 2-methylimidazole to be dissolved in 300ml methanol, the film that step (3) obtains is immersed in and is contained
Have in the methanol solution of 2-methylimidazole ligand steeped after 12h it is to be tested in methanol solvate.
2 gained mixed-matrix nanofiltration membrane of embodiment is analyzed:
Mixed-matrix nanofiltration membrane prepared by this example is fitted into film properties evaluating apparatus, experiment condition: 0.6M Pa, in advance
Press 1h, sodium sulfate concentration 1000ppm；Experimental result: water flux: 89.68L/m2H retention: 90.99%.
Embodiment 3:
Do film condition: 25 DEG C, relative humidity 40% ± 2.
(1) it weighs 2.1501g zinc nitrate hexahydrate and is dissolved in 100ml deionized water, by polysulfone ultrafiltration membrane support membrane and six
It is dried after impregnating 4min in nitric hydrate zinc aqueous solution.
(2) 0.2502g piperazine dissolved is weighed in 100ml deionized water, in the film and aqueous phase monomers that step (1) is obtained
It is dried after 4min, forms water phase liquid layer.
(3) 0.1003g pyromellitic trimethylsilyl chloride is weighed to be dissolved in 100ml n-hexane, by film that step (2) obtains with contain
15min is dried in 60 DEG C of baking oven after the organic phase solution 1min of activated monomer.
(4) it weighs 2.7111g 2-methylimidazole to be dissolved in 300ml methanol, the film that step (3) obtains is immersed in and is contained
Have in the methanol solution of 2-methylimidazole ligand steeped after 12h it is to be tested in methanol.
3 gained mixed-matrix nanofiltration membrane of embodiment is analyzed:
Mixed-matrix nanofiltration membrane prepared by this example is fitted into film properties evaluating apparatus, experiment condition: 0.6M Pa, in advance
Press 1h, sodium sulfate concentration 1000ppm；Experimental result: water flux: 87.664L/m2H retention: 90.14%.
Comparative example:
Do film condition: 25 DEG C, relative humidity 40% ± 2.
(1) 0.2502g piperazine dissolved is weighed in 100ml deionized water, it will be by polysulfone ultrafiltration membrane support membrane and water phase list
It is dried after 4min in body, forms water phase liquid layer.
(2) 0.1003g pyromellitic trimethylsilyl chloride is weighed to be dissolved in 100ml n-hexane, by film that step (1) obtains with contain
15min is dried in 60 DEG C of baking oven after the organic phase solution 1min of activated monomer.It impregnates to be tested in deionized water.
1 gained nanofiltration membrane of comparative example is analyzed:
Mixed-matrix nanofiltration membrane prepared by this example is fitted into film properties evaluating apparatus, experiment condition: 0.6M Pa, in advance
Press 1h, sodium sulfate concentration 1000ppm；Experimental result: water flux: 12.29L/m2H retention: 90.86%.
Claims (7)
1. a kind of preparation method of high throughput mixed-matrix nanofiltration membrane, characterized by the following steps:
(1) it will be dried after polysulfone ultrafiltration membrane support membrane and time of infusion in zinc nitrate hexahydrate aqueous solution；
(2) it will be dried after time of infusion in film and aqueous phase monomers that step (1) obtains, form water phase liquid layer；Wherein water phase
Monomer is piperazine；
(3) it is dried in an oven after the film that step (2) obtains being contacted a period of time with the organic phase solution containing activated monomer；
Wherein organic phase activated monomer is pyromellitic trimethylsilyl chloride；
(4) film that step (3) obtains was immersed in the methanol solution containing 2-methylimidazole ligand after a period of time and uses methanol
Solvent washes off extra ligand.
2. a kind of preparation method of high-throughput mixed-matrix nanofiltration membrane as described in claim 1, it is characterised in that: step (1)
In zinc nitrate hexahydrate aqueous solution mass fraction be 0.01-10wt%；Dip time is 1-15min.
3. a kind of preparation method of high-throughput mixed-matrix nanofiltration membrane as described in claim 1, it is characterised in that: step (2)
In aqueous phase monomers mass fraction be 0.001-0.5wt%；Dip time is 1-10min.
4. a kind of preparation method of high-throughput mixed-matrix nanofiltration membrane as described in claim 1, it is characterised in that: step (3)
In organic phase activated monomer mass fraction be 0.001-0.5wt%；Dip time is 1-5min.
5. a kind of preparation method of high-throughput mixed-matrix nanofiltration membrane as described in claim 1, it is characterised in that: step (3)
In oven temperature be 30-80 DEG C, drying time 5-30min.
6. a kind of preparation method of high-throughput mixed-matrix nanofiltration membrane as described in claim 1, it is characterised in that: step (4)
In 2-methylimidazole ligand mass fraction be 0.1-2wt%, soaking time 1h-24h.
7. a kind of high-throughput mixed-matrix nanofiltration membrane of any one of claim 1~6 the method preparation.
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Cited By (11)
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| CN110559889A (en) * | 2019-08-29 | 2019-12-13 | 浙江工业大学 | Hollow nano-particle composite nanofiltration membrane and preparation method and application thereof |
| CN111135733A (en) * | 2020-01-13 | 2020-05-12 | 北京赛诺膜技术有限公司 | MOFs polymer hollow fiber composite membrane and preparation method thereof |
| CN111282451A (en) * | 2020-02-24 | 2020-06-16 | 浙江工业大学 | High-flux polyamide nanofiltration membrane prepared from divalent metal ions and preparation method thereof |
| CN111939774A (en) * | 2020-08-11 | 2020-11-17 | 哈尔滨工业大学 | Method for preparing composite nanofiltration membrane by growing nano particles after etching |
| CN113318605A (en) * | 2021-07-01 | 2021-08-31 | 浙江工业大学 | MOF-based mixed matrix membrane and preparation method thereof |
| CN113694741A (en) * | 2021-09-13 | 2021-11-26 | 浙江工业大学 | Preparation method of full heat exchange membrane based on interfacial polymerization and reverse diffusion growth ZIF |
| CN113786731A (en) * | 2021-09-13 | 2021-12-14 | 浙江工业大学 | Preparation method of composite forward osmosis membrane based on ZIFs nano material modified supporting layer |
| CN114028946A (en) * | 2021-10-25 | 2022-02-11 | 浙江工业大学 | Nano composite cellulose acetate forward osmosis membrane and preparation method thereof |
| CN114849473A (en) * | 2022-04-25 | 2022-08-05 | 浙江工业大学 | Secondary polymerization synchronous self-sealing ZIF-8 modified reverse osmosis membrane and preparation method thereof |
| CN115487693A (en) * | 2022-09-30 | 2022-12-20 | 浙江工业大学 | Polyamide/polyolefin mixed matrix nanofiltration membrane and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110559889A (en) * | 2019-08-29 | 2019-12-13 | 浙江工业大学 | Hollow nano-particle composite nanofiltration membrane and preparation method and application thereof |
| CN111135733A (en) * | 2020-01-13 | 2020-05-12 | 北京赛诺膜技术有限公司 | MOFs polymer hollow fiber composite membrane and preparation method thereof |
| CN111282451A (en) * | 2020-02-24 | 2020-06-16 | 浙江工业大学 | High-flux polyamide nanofiltration membrane prepared from divalent metal ions and preparation method thereof |
| CN111939774A (en) * | 2020-08-11 | 2020-11-17 | 哈尔滨工业大学 | Method for preparing composite nanofiltration membrane by growing nano particles after etching |
| CN113318605A (en) * | 2021-07-01 | 2021-08-31 | 浙江工业大学 | MOF-based mixed matrix membrane and preparation method thereof |
| CN113786731A (en) * | 2021-09-13 | 2021-12-14 | 浙江工业大学 | Preparation method of composite forward osmosis membrane based on ZIFs nano material modified supporting layer |
| CN113694741A (en) * | 2021-09-13 | 2021-11-26 | 浙江工业大学 | Preparation method of full heat exchange membrane based on interfacial polymerization and reverse diffusion growth ZIF |
| CN114028946A (en) * | 2021-10-25 | 2022-02-11 | 浙江工业大学 | Nano composite cellulose acetate forward osmosis membrane and preparation method thereof |
| CN114849473A (en) * | 2022-04-25 | 2022-08-05 | 浙江工业大学 | Secondary polymerization synchronous self-sealing ZIF-8 modified reverse osmosis membrane and preparation method thereof |
| CN114849473B (en) * | 2022-04-25 | 2023-09-05 | 浙江工业大学 | Secondary polymerization synchronous self-sealing ZIF-8 modified reverse osmosis membrane and preparation method thereof |
| CN115487693A (en) * | 2022-09-30 | 2022-12-20 | 浙江工业大学 | Polyamide/polyolefin mixed matrix nanofiltration membrane and preparation method thereof |
| CN117547974A (en) * | 2024-01-12 | 2024-02-13 | 河南师范大学 | Polyaiperazine amide nanofiltration membrane with high acid-base stability and preparation method thereof |
| CN117547974B (en) * | 2024-01-12 | 2024-04-12 | 河南师范大学 | Polyaiperazine amide nanofiltration membrane with high acid-base stability and preparation method thereof |
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