CN105013333B - A kind of high flux and high retention ratio positive charge composite nanometer filtering film and preparation method thereof - Google Patents
A kind of high flux and high retention ratio positive charge composite nanometer filtering film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of high flux and high retention ratio positive charge composite nanometer filtering film and preparation method thereof, preparation method is：(1) PEI is dissolved in organic solvent, polyetherimide solution is made into, is stirred, standing and defoaming, casting solution is made, casting solution is scraped on the shiny surface of non-woven fabrics, is placed in atmosphere, is put into ethylenediamine solution, immersion, the one side for scraping casting solution of non-woven fabrics is claimed A faces by taking-up deionized water rinsing, the basement membrane after being crosslinked after drying；(2) m-phenylene diamine (MPD) and positive charge material are put into water and are made into the aqueous solution；(3) the A faces of the basement membrane after crosslinking are immersed in the aqueous solution of step (2) preparation, taking-up is dried, then A faces are immersed in the hexane solution of pyromellitic trimethylsilyl chloride, take out, dry, obtain high flux and high retention ratio positive charge composite nanometer filtering film.A kind of high flux and high retention ratio positive charge composite nanometer filtering film of the present invention has high flux, higher rejection.Production time is short, and technique is simple.
Description
Technical field
The present invention relates to a kind of high flux and high retention ratio positive charge composite nanometer filtering film and preparation method thereof.
Background technology
Nanofiltration is a kind of new membrane separation technique, and the precision that it is separated is considered as between ultrafiltration and counter-infiltration
Loose counter-infiltration and low pressure reverse osmosis.The molecular cut off of nanofiltration is between 200-1000, and aperture is 0.5-2nm, main mass transfer
Mechanism basic theories model has nonequilibrium thermodynamics model, pore Flow Model, solubility-diffusion model and Dao Nan effects.NF membrane
Application be even more to be related to modern industry-by-industry and every field, such as in petrochemical industry, food pharmaceutical, sewage disposal, seawater
Desalination, electronic bio, or even military field, membrane technology all play more and more important effect.
Preparing the method for NF membrane has following several：Phase inversion method, blending method, charged method and composite algorithm.Wherein using most
Extensively also most efficient method is composite algorithm.Composite algorithm, which can be related to, prepares basement membrane and two, ultra-thin top layer of NF membrane step.Nanofiltration
The preparation method of film basement membrane is mainly phase inversion, and the preparation method on film top layer is most commonly used that interfacial polymerization.
NF membrane with positive charge has the advantages that acid and alkali-resistance, the pollution of resistance to microorganism, in separation Mg2+、Ca2+It is contour
Valence state metal ion, purifying possess very in terms of being less than the amino acid of isoelectric point and the dye of positive ion compared with conventional nanofiltration membrane
Big advantage.At present, the polyamide nanofiltration membrane reported is in mainly electroneutral or elecrtonegativity, and positively charged NF membrane mainly has
Epichlorohydrin series positive charge NF membrane, the serial positive charge NF membrane of polyamide.
Huang Ruihua etc., which is grafted pi-allyl trimethyl ammonium chloride on the chitosan of epichlorohydrin cross-linked and obtains a kind of positive charge, to be received
Filter membrane, under 1.2MPa, to 1000mg/L MgCl2, MgSO4Flux with NaCl solution is respectively 6.8,6.12 and 5.51L/
(m2H), rejection is respectively 97.6%, 89.7% and 40.7% [Separation and Purification
Technology,2008,61,424-429].Huang Ruihua etc. using epichlorohydrin cross-linked n-trimethyl chitosan chloride and polyacrylonitrile
Composite nanometer filtering film, to 1000mg/L MgCl2Flux and rejection be respectively 7.04L/ (m2H) with 96.7%.These research tables
Bright Chitosan-phospholipid complex can as Modified Membrane surface charge material, but there is the problem of flux is too low, have impact on this just
The popularization [Journal of Membrane Science, 2006,286,237-244] of electric charge film.Yong Zhou etc. are in polyamides
In amine commodity NF membrane, the electric charge on film surface is changed for the electrostatic precipitation of 750000 polyethyleneimine by molecular weight, sunk
The product time is 2-20 hours, and resulting film is improved to MgCl2 rejection to 91.2%, but flux is less than 15.0Lm-2h-1
It is obvious that and be deposited as electrostatic interaction, active force is small, and the polyethyleneimine on surface is easily lost in, dense with polyethyleneimine
Degree reduction, the film of gained is to MgCl2Rejection be down to 70% [Separation and Purification by 90%
Technology,2009,66,287-294]。
For current positive charge NF membrane generally existing rejection it is low, flux is low, charged material is easy to run off the problems such as, compel
The high-performance composite nanometer filtering film not easily runed off with high flux and high rejection and charged material will be developed by being essential.
The content of the invention
The purpose of the present invention is to overcome the deficiencies in the prior art there is provided a kind of high flux and high retention ratio positive charge composite nanometer filter
Film.
Second object of the present invention is to provide a kind of preparation method of high flux and high retention ratio positive charge composite nanometer filtering film.
Technical scheme is summarized as follows：
A kind of high flux and high retention ratio positive charge composite nanometer filtering film and preparation method thereof, comprises the following steps：
(1) PEI is dissolved in organic solvent, is made into the PEI that mass concentration is 15%-30% molten
Liquid, at 40-80 DEG C, is stirred 3-8 hours, casting solution is made, in proportion in 600cm in standing and defoaming 3-24 hours2The light of non-woven fabrics
12-20g casting solution is scraped on sliding surface, is placed in atmosphere, standing time is 0-60 seconds, it is 3%-12%'s to be put into mass concentration
In ethylenediamine solution, soak time is 5-60min, and taking-up deionized water rinsing, the basement membrane after being crosslinked after drying is incited somebody to action
The one side for scraping casting solution of non-woven fabrics claims A faces；
(2) m-phenylene diamine (MPD) and positive charge material are put into water and are made into the aqueous solution, the mass concentration for making m-phenylene diamine (MPD) is
1%-2%, the mass concentration for making positive charge material is 0.5%-2%；
(3) the A faces of the basement membrane after crosslinking are immersed in the aqueous solution of step (2) preparation 30-120 seconds, taking-up is dried, then
In the hexane solution that the A faces are immersed in the pyromellitic trimethylsilyl chloride that mass concentration is 0.05%-0.1%, after 30-120 seconds
Take out, dry, obtain high flux and high retention ratio positive charge composite nanometer filtering film.
The preferred DMA of organic solvent, volume are 1-2：1 DMF and Isosorbide-5-Nitrae-dioxy
The mixed liquor or volume of six rings are 1-2：1 1-METHYLPYRROLIDONE and the mixed liquor of tetrahydrofuran.
The mass concentration preferably 20% of step (1) described polyetherimide solution.
The material of non-woven fabrics is preferably polypropylene, polyester or polyacrylonitrile.
Preferably 3-60 seconds step (1) standing time.
The polypropylene that polyethyleneimine that positive charge material preferably molecular weight is 600-10000, molecular weight are 70000
The polymethylacrylic acid dimethylamine that PDDA that imines, molecular weight are 20000, molecular weight are 15700
Ethyl ester, molecular weight are the HACC or molecule that 16000 n-trimethyl chitosan chlorides, molecular weight are 70000
Measure the 2- hydroxyl -3- trimethylammonio-propyl chitosans for 30000.
A kind of high flux and high retention ratio positive charge composite nanometer filtering film prepared by the above method.
The advantage of the invention is that：
1. the method for the present invention selects water as solvent in the cross-linking step of basement membrane, it is to avoid usually made using methanol this area
The deficiency of solvent, it is to avoid pollution of the methanol to environment.
2. a kind of high flux and high retention ratio positive charge composite nanometer filtering film prepared by the method for the present invention has high flux (16L
h-1m-2-20Lh-1m-2Between) there is higher rejection (more than 91%) to some inorganic salts (such as magnesium chloride).
3. the positive charge material that the method for the present invention is used is cationic polymer, hydrophily is strong, you can change film surface
Electric charge, can also improve water flux, positive charge material is added step (2) (interfacial polymerization) step by method of the invention, it is to avoid
The loss of positive charge material.
4. the production time is short, technique is simple.
Brief description of the drawings
Fig. 1 is the structure in the cross section of the basement membrane after crosslinking；
Fig. 2 is the structure on the surface of the basement membrane after crosslinking；
Fig. 3 is the cross-sectional configuration of high flux and high retention ratio positive charge composite nanometer filtering film；
Fig. 4 is the surface texture of high flux and high retention ratio positive charge composite nanometer filtering film.
Embodiment
The present invention has abandoned traditional charged material adding method such as electrostatic precipitation, and charged material is added into participation interface
In the membrane material of polymerization, make being present in the cortex obtained by interfacial polymerization for positive charge material settling out, solve film surface charge
The problem of material is easy to run off.
With reference to specific embodiment, the present invention is further illustrated, and embodiments of the invention are in order that this area
Technical staff better understood when the present invention, but the present invention is not imposed any restrictions.
From the PEI that molecular weight is 4500.
Material used is MgCl in membrane separating property experiment2, the test condition of experiment is：25 DEG C, inorganic salt concentration is equal
For 2000ppm.
Embodiment 1
A kind of preparation method of high flux and high retention ratio positive charge composite nanometer filtering film, comprises the following steps：
(1) PEI is dissolved in DMA, is made into the PEI that mass concentration is 15%
Solution, at 80 DEG C, is stirred 3 hours, casting solution is made, in proportion in 600cm in standing and defoaming 24 hours2Material is polyacrylic
15g casting solution is scraped on the shiny surface of non-woven fabrics, is put into the ethylenediamine solution that mass concentration is 3%, soak time is
5min, taking-up deionized water rinsing, basement membrane (see Fig. 1,2) after being crosslinked after drying, by the casting solution of scraping of non-woven fabrics
Simultaneously claim A faces；
(2) m-phenylene diamine (MPD) and positive charge material are put into water and are made into the aqueous solution, the mass concentration for making m-phenylene diamine (MPD) is
2%, the mass concentration for making positive charge material is 0.5%；Positive charge material is the polyethyleneimine that molecular weight is 600；
(3) the A faces of the basement membrane after crosslinking are immersed in the aqueous solution of step (2) preparation 30 seconds, taking-up is dried, then by institute
State A faces to be immersed in the hexane solution for the pyromellitic trimethylsilyl chloride that mass concentration is 0.05%, taken out after 30 seconds, dry, obtain
High flux and high retention ratio positive charge composite nanometer filtering film (see Fig. 3,4).
The flux of gained film is 18.7Lh-1m-2, filted chroma is 2000ppm MgCl2Solution, rejection is 93.8%,
Operating pressure is 0.8MPa.
Embodiment 2
A kind of preparation method of high flux and high retention ratio positive charge composite nanometer filtering film, comprises the following steps：
(1) PEI is dissolved in organic solvent, the polyetherimide solution that mass concentration is 20% is made into, 40
DEG C, stir 8 hours, casting solution is made, in proportion in 600cm in standing and defoaming 3 hours2Material is the non-woven fabrics of polyacrylonitrile
20g casting solution is scraped on shiny surface, is placed in atmosphere, standing time is 60 seconds, the ethylenediamine that mass concentration is 12% is put into
In the aqueous solution, soak time is 60min, taking-up deionized water rinsing, the basement membrane after being crosslinked after drying, by non-woven fabrics
The one side for scraping casting solution claims A faces；
Organic solvent is that volume ratio is 1：1 DMF and Isosorbide-5-Nitrae-dioxane；
(2) m-phenylene diamine (MPD) and positive charge material are put into water and are made into the aqueous solution, the mass concentration for making m-phenylene diamine (MPD) is
2%, the mass concentration for making positive charge material is 2%；Positive charge material is the PPI that molecular weight is 70000；
(3) the A faces of the basement membrane after crosslinking are immersed in the aqueous solution of step (2) preparation 120 seconds, taking-up is dried, then will
The A faces are immersed in the hexane solution for the pyromellitic trimethylsilyl chloride that mass concentration is 0.1%, are taken out after 120 seconds, are dried, obtain
To high flux and high retention ratio positive charge composite nanometer filtering film.
The flux of gained film is 17.1Lh-1m-2, filted chroma is 2000ppm MgCl2Solution, rejection is 98.6%,
Operating pressure is 0.8MPa.
Embodiment 3
A kind of preparation method of high flux and high retention ratio positive charge composite nanometer filtering film, comprises the following steps：
(1) PEI is dissolved in DMA, is made into the PEI that mass concentration is 30%
Solution, at 60 DEG C, is stirred 6 hours, casting solution is made, in proportion in 600cm in standing and defoaming 12 hours2Material is the nothing of polyester
16g casting solution is scraped on the shiny surface for spinning cloth, is placed in atmosphere, standing time is 3 seconds, the second that mass concentration is 5% is put into
In two amine aqueous solutions, soak time is 30min, taking-up deionized water rinsing, the basement membrane after being crosslinked after drying, by nonwoven
The one side for scraping casting solution of cloth claims A faces；
(2) m-phenylene diamine (MPD) and positive charge material are put into water and are made into the aqueous solution, the mass concentration for making m-phenylene diamine (MPD) is
2%, the mass concentration for making positive charge material is 1%；Positive charge material is the poly dimethyl allyl chlorine that molecular weight is 20000
Change ammonium；
(3) the A faces of the basement membrane after crosslinking are immersed in the aqueous solution of step (2) preparation 120 seconds, taking-up is dried, then will
The A faces are immersed in the hexane solution for the pyromellitic trimethylsilyl chloride that mass concentration is 0.1%, are taken out after 60 seconds, are dried, obtain
High flux and high retention ratio positive charge composite nanometer filtering film.
The flux of gained film is 20.8Lh-1m-2, filted chroma is 2000ppm MgCl2Solution, rejection is 91.4%,
Operating pressure is 0.8MPa.
Embodiment 4
A kind of preparation method of high flux and high retention ratio positive charge composite nanometer filtering film, comprises the following steps：
(1) PEI is dissolved in DMA, is made into the PEI that mass concentration is 15%
Solution, at 80 DEG C, is stirred 3 hours, casting solution is made, in proportion in 600cm in standing and defoaming 12 hours2Material is polyacrylic
12g casting solution is scraped on the shiny surface of non-woven fabrics, is put into the ethylenediamine solution that mass concentration is 6%, soak time is
The one side for scraping casting solution of non-woven fabrics is claimed A by 60min, taking-up deionized water rinsing, the basement membrane after being crosslinked after drying
Face；
Organic solvent is that volume ratio is 2：1 1-METHYLPYRROLIDONE and tetrahydrofuran；
(2) m-phenylene diamine (MPD) and positive charge material are put into water and are made into the aqueous solution, the mass concentration for making m-phenylene diamine (MPD) is
2%, the mass concentration for making positive charge material is 0.5%；Positive charge material is that molecular weight is 10000 polyethyleneimines；
(3) the A faces of the basement membrane after crosslinking are immersed in the aqueous solution of step (2) preparation 120 seconds, taking-up is dried, then will
The A faces are immersed in the hexane solution for the pyromellitic trimethylsilyl chloride that mass concentration is 0.1%, are taken out after 60 seconds, are dried, obtain
High flux and high retention ratio positive charge composite nanometer filtering film.
The flux of gained film is 16.7Lh-1m-2, filted chroma is 2000ppm MgCl2Solution, rejection is 93.6%,
Operating pressure is 0.8MPa.
Embodiment 5
A kind of preparation method of high flux and high retention ratio positive charge composite nanometer filtering film, comprises the following steps：
(1) 2 are used：1 DMF and the step of mixed liquor alternate embodiment 4 (1) of Isosorbide-5-Nitrae-dioxane
DMA, the other the same as in Example 4 step (1)；
(2) m-phenylene diamine (MPD) and positive charge material are put into water and are made into the aqueous solution, the mass concentration for making m-phenylene diamine (MPD) is
2%, the mass concentration for making positive charge material is 0.5%；Positive charge material is the polymethylacrylic acid diformazan that molecular weight is 15700
Amine ethyl ester；
(3) the A faces of the basement membrane after crosslinking are immersed in the aqueous solution of step (2) preparation 60 seconds, taking-up is dried, then by institute
State A faces to be immersed in the hexane solution for the pyromellitic trimethylsilyl chloride that mass concentration is 0.1%, taken out after 60 seconds, dry, obtain height
The high rejection positive charge composite nanometer filtering film of flux.
The flux of gained film is 18.3Lh-1m-2, filted chroma is 2000ppm MgCl2Solution, rejection is 92.1%,
Operating pressure is 0.8MPa.
Embodiment 6
A kind of preparation method of high flux and high retention ratio positive charge composite nanometer filtering film, comprises the following steps：
(1) 1 is used：The N, N- bis- of 1 1-METHYLPYRROLIDONE and the step of mixed liquor alternate embodiment 4 (1) of tetrahydrofuran
Methylacetamide, the other the same as in Example 4 step (1)；
(2) m-phenylene diamine (MPD) and positive charge material are put into water and are made into the aqueous solution, the mass concentration for making m-phenylene diamine (MPD) is
2%, the mass concentration for making positive charge material is 1%；Positive charge material is the n-trimethyl chitosan chloride that molecular weight is 16000；
(3) the A faces of the basement membrane after crosslinking are immersed in the aqueous solution of step (2) preparation 120 seconds, taking-up is dried, then will
The A faces are immersed in the hexane solution for the pyromellitic trimethylsilyl chloride that mass concentration is 0.1%, are taken out after 60 seconds, are dried, obtain
High flux and high retention ratio positive charge composite nanometer filtering film.
The flux of gained film is 19.3L h-1m-2, filted chroma is 2000ppm MgCl2Solution, rejection is 92.4%,
Operating pressure is 0.8MPa.
Embodiment 7
A kind of preparation method of high flux and high retention ratio positive charge composite nanometer filtering film, comprises the following steps：
(1) step of be the same as Example 4 (1)；
(2) m-phenylene diamine (MPD) and positive charge material are put into water and are made into the aqueous solution, the mass concentration for making m-phenylene diamine (MPD) is
2%, the mass concentration for making positive charge material is 1.5%；Positive charge material is the Hydroxyproyl Trimethyl chlorination that molecular weight is 70000
Ammonium chitosan；
(3) the A faces of the basement membrane after crosslinking are immersed in the aqueous solution of step (2) preparation 30 seconds, taking-up is dried, then by institute
State A faces to be immersed in the hexane solution for the pyromellitic trimethylsilyl chloride that mass concentration is 0.1%, taken out after 60 seconds, dry, obtain height
The high rejection positive charge composite nanometer filtering film of flux.
The flux of gained film is 17.8L h-1m-2, filted chroma is 2000ppm MgCl2Solution, rejection is 94.6%,
Operating pressure is 0.8MPa.
Embodiment 8
A kind of preparation method of high flux and high retention ratio positive charge composite nanometer filtering film, comprises the following steps：
(1) step of be the same as Example 4 (1)；
(2) m-phenylene diamine (MPD) and positive charge material are put into water and are made into the aqueous solution, the mass concentration for making m-phenylene diamine (MPD) is
2%, the mass concentration for making positive charge material is 2%；Positive charge material be molecular weight be 30000 2- hydroxyl -3- front threes ammonium -
Propyl group chitosan；
(3) the A faces of the basement membrane after crosslinking are immersed in the aqueous solution of step (2) preparation 90 seconds, taking-up is dried, then by institute
State A faces to be immersed in the hexane solution for the pyromellitic trimethylsilyl chloride that mass concentration is 0.1%, taken out after 60 seconds, dry, obtain height
The high rejection positive charge composite nanometer filtering film of flux.
The flux of gained film is 18.6L h-1m-2, filted chroma is 2000ppm MgCl2Solution, rejection is 92.3%,
Operating pressure is 0.8MPa.
Claims (7)
1. a kind of preparation method of high flux and high retention ratio positive charge composite nanometer filtering film, it is characterized in that comprising the following steps：
(1) PEI is dissolved in organic solvent, is made into the polyetherimide solution that mass concentration is 15%-30%,
40-80 DEG C, stir 3-8 hours, casting solution is made, in proportion in 600cm in standing and defoaming 3-24 hours2The shiny surface of non-woven fabrics
On scrape 12-20g casting solution, place in atmosphere, standing time is 0-60 second, be put into second two of the mass concentration for 3%-12%
In amine aqueous solution, soak time is 5-60min, taking-up deionized water rinsing, the basement membrane after being crosslinked after drying, by nonwoven
The one side for scraping casting solution of cloth claims A faces；
(2) m-phenylene diamine (MPD) and positive charge material are put into water and are made into the aqueous solution, the mass concentration for making m-phenylene diamine (MPD) is 1%-
2%, the mass concentration for making positive charge material is 0.5%-2%；
(3) the A faces of the basement membrane after crosslinking are immersed in the aqueous solution of step (2) preparation 30-120 seconds, taking-up is dried, then by institute
State A faces to be immersed in the hexane solution for the pyromellitic trimethylsilyl chloride that mass concentration is 0.05%-0.1%, taken out after 30-120 seconds,
Dry, obtain high flux and high retention ratio positive charge composite nanometer filtering film.
2. a kind of preparation method of high flux and high retention ratio positive charge composite nanometer filtering film according to claim 1, its feature
It is that the organic solvent is that DMA, volume are 1-2：1 DMF and Isosorbide-5-Nitrae-dioxane
Mixed liquor or volume be 1-2：1 1-METHYLPYRROLIDONE and the mixed liquor of tetrahydrofuran.
3. a kind of preparation method of high flux and high retention ratio positive charge composite nanometer filtering film according to claim 1, its feature
The mass concentration for being step (1) described polyetherimide solution is 20%.
4. a kind of preparation method of high flux and high retention ratio positive charge composite nanometer filtering film according to claim 1, its feature
The material for being the non-woven fabrics is polypropylene, polyester or polyacrylonitrile.
5. a kind of preparation method of high flux and high retention ratio positive charge composite nanometer filtering film according to claim 1, its feature
It is 3-60 seconds step (1) standing time to be.
6. a kind of preparation method of high flux and high retention ratio positive charge composite nanometer filtering film according to claim 1, its feature
Be the positive charge material be molecular weight be 600-10000 polyethyleneimine, molecular weight be 70000 PPI, point
It is sub to measure the PDDA for being 20000, the polymethylacrylic acid dimethylamine ethyl ester that molecular weight is 15700, divide
Son amount is that the HACC or molecular weight that 16000 n-trimethyl chitosan chlorides, molecular weight are 70000 are
30000 2- hydroxyl -3- trimethylammonio-propyl chitosans.
7. a kind of high flux and high retention ratio positive charge composite nanometer filtering film prepared by the method described in one of claim 1-6.
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| 聚醚砜-聚酰胺复合荷电纳滤膜的制备技术研究;杨艳红;《中国优秀博硕士学位论文全文数据库(硕士) 工程科技I辑》;20051215;第15,16页 * |
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