CN106582304A - Preparation method of charged mosaic membrane - Google Patents
Preparation method of charged mosaic membrane Download PDFInfo
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- CN106582304A CN106582304A CN201611255013.9A CN201611255013A CN106582304A CN 106582304 A CN106582304 A CN 106582304A CN 201611255013 A CN201611255013 A CN 201611255013A CN 106582304 A CN106582304 A CN 106582304A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0006—Organic membrane manufacture by chemical reactions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/28—Polymers of vinyl aromatic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/52—Polyethers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/18—Membrane materials having mixed charged functional groups
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention discloses a preparation method of a charged mosaic membrane. The preparation method comprises the steps that a brominated polyphenyl ether solution with the mass concentration being 15-30% is stewed for 24 h at the room temperature and subjected to membrane scraping on a glass plate, then a membrane and the glass plate are rapidly put into deionized water together to be stewed into a membrane, the membrane is taken out and dried to obtain a porous brominated polyphenyl ether membrane; the porous brominated polyphenyl ether membrane is soaked in a diamine compound aqueous solution at the room temperature, crosslinked, taken out and dried to obtain a crosslinked porous membrane; and the crosslinked porous membrane is placed into an anionic charged polymer solution, subjected to ultrasonic defoaming, taken out and dried to obtain the charged mosaic membrane. The charged mosaic membrane has a large salt permeation flux and a high rejection rate on nonionic matter such as sucrose, can effectively separate an electrolyte from a non-electrolyte or conduct electrolyte dilution, desalting and the like, can further be used for pressure dialysis, diffusion dialysis and the like, and is remarkably improved in mechanical performance compared with a porous BPPO membrane.
Description
(1) technical field
The present invention relates to a kind of preparation of charge embedded film, the material is simultaneously containing separate anionic polymer group
Divide and cationic polymer component, realize the preparation of charge embedded film truly.
(2) background technology
In a broad sense, the double property ionic polymer membranes containing anions and canons cation exchange groups (unordered) can be referred to as simultaneously
For embedded film.And embedded film truly refers to what is be made up of countless longitudinally staggered parallel anions and canons polymer
Ion exchange membrane.As which contains two kinds of charged groups simultaneously, therefore electrolyte can be selectively allowed by film, and prevent non-
The transmission of electrolyte.In view of which only prevents the property of non-electrolyte, water demineralizing, biochemical material and food are typically can apply to
The purification of thing additive etc..
The preparation method of embedded film is numerous, such as zwitterion resin completion method, polymer blend method, layer upon layer method, embedding
Section polymer self assembles method etc..Japan Patent (the clear 59-203613 of JP) is reported using poly- containing anion and cation respectively
The block polymer self-assembly method of compound prepares embedded film, although can prepare embedded film, but for inlaying polymer itself
Building-up process is excessively loaded down with trivial details, and design and preparation cost are more high, so the strategy is not appropriate for commercial applications.
Chinese patent (102548646 A of CN) proposes the method using two kinds of block polymer blendings, in order to realize two kinds
The effective combination of material realize simultaneously phase separation, and it is embedding that prepared two kinds of polymer all contains identical vinyl alcohol system polymer
Section, and another block is then respectively anionic polymer block and cationic polymer block.Then by self assembly reality is blended
Effective preparation of existing embedded film.But block polymer problem with high costs still cannot be solved, meanwhile, two kinds of charged groups
Interaction of hydrogen bond during blending between opposite charges will necessarily consume substantial amounts of ion transmission site, be unfavorable for the efficient biography of ion
It is defeated.
It is charged that Chinese patent (102770197 A of CN) proposes prepared by the method for utilizing ionomer solution to coat layer by layer
Embedded film, although prepare the charge embedded film close to perfect condition, but preparation process is excessively loaded down with trivial details, width are only several centimetres
Film need to carry out several times even thousands of layers film liquid coating, the process greatly reduces production efficiency, with the coating number of plies
Increase its defect also will necessarily increase therewith, while needing to carry out former film the ultra-thin cutting in longitudinal direction, the work to obtain embedded film
The realization of skill also certainly exists a numerous difficult problems.
Preparation technology of the Chinese patent (101530748 A of CN) based on composite nanofiltration membrane, with ultrafilter membrane as supporter,
In the difference cation exchange group and anion exchange groups of interfacial polymerization thing, one layer of ultra-thin pair of property ionomer is prepared
Film layer (tens to hundreds of nanometer).Supporter provides mechanical strength, and amphiphilic superthin layer provides Selective Separation performance, Jin Ershi
The performance of existing embedded film.But the embedded film prepared by the technology is due to causing which to univalent state ion the problems such as boundary layer is excessively thin
Retention efficiency it is undesirable.Meanwhile, the chemical stability of the boundary layer waits to investigate.
(3) content of the invention
It is an object of the present invention to provide a kind of preparation method of new charge embedded film, its objective is to prepare selection performance excellent
Different, flux salt is big, while the high charge embedded film of film-strength.Above-mentioned technical problem is by the BPPO bases with finger-like pore structure
Fill SPPO to realize the relatively independent presence of anion charged polymer in charge embedded film in the hole of material, while passing through
The follow-up season ammoniated treatment to BPPO matrixes realizes being individually present for cation charged polymer.
The technical solution used in the present invention is：
The present invention provides a kind of preparation method of charge embedded film, and methods described is：The preparation of open support：By common
BPPO is configured to corresponding polymer solution knifing, then the film forming in coagulation bath by out-phase membrane formation process, prepares BPPO ultrafiltration
Film；The crosslinking Treatment of supporting layer：BPPO is immersed in into Diamines (NH2-(CH2)n-NH2) in aqueous solution, carry out crosslinking Treatment；It is cloudy
The implantation of Ion Charged polymer solution：By prepared film immersion anion charged polymer solution, then at vacuum outgass
Reason a period of time, the gas inside film is discharged, so that polymer solution enters the inside of film；The drying and processing of film：
Fall solution, the solution on striping surface scraped with scraper, then film is put into vacuum drying oven drying film forming or is put on hot plate and dried,
Film is put into in hot press under uniform temperature further heat whether finally according to the different choice of the species of anion charged membrane
Pressure process.
Specifically, the preparation method of charge embedded film of the present invention is carried out as follows：(1) brominated polyphenylether (BPPO) is used
1-Methyl-2-Pyrrolidone (NMP) is made into the brominated polyphenylene ethereal solution of mass concentration 15-30% (preferably 15%), is stored at room temperature
Then film is put in deionized water together with glass plate rapidly and soaks film forming by 24h knifing on the glass plate, takes out film
(sloughing glass plate) dries, and obtains brominated polyphenylether perforated membrane；
(2) step (1) brominated polyphenylether perforated membrane is immersed in diamine compounds aqueous solution, room temperature (preferably 25 DEG C)
Immersion (preferred 5-10h) is crosslinked, and is taken out, and is dried (preferably 60 DEG C), the perforated membrane after being crosslinked；
(3) perforated membrane after step (2) crosslinking is placed in anion charged polymer solution, after ultrasonic deaeration (preferably
300W ultrasound 2h), perforated membrane is taken out, is dried (preferably 60 DEG C), obtain charge embedded film；The anion charged polymer solution
It is that anion charged polymer dimethylformamide is dissolved the solution for being configured to mass concentration 5-30%, the anion lotus
Electric polymer is the one kind in sulfonated poly (phenylene oxide), sulfonated polystyrene or sulfonated polyether sulfone, more preferably 15% sulfonated polystyrene
Solution.
Further, step (1) the brominated polyphenylether bromination degree is between 25% and 70%.
Further, step (1) is described scrapes film thickness for 200-600 μm.
Further, step (1) membrance casting condition is：Water was changed once every 2 hours, film, 60 DEG C of bakings are taken out after 12 hours
It is dry.
Further, step (2) diamine compounds be ethylenediamine, propane diamine, butanediamine, pentanediamine or hexamethylene diamine,
It is preferred that ethylenediamine.
Further, step (2) the diamine compounds concentration of aqueous solution be 1-3mol/L, preferred 1mol/L, more preferably
1mol/L ethylenediamine solutions.
Further, step (2) crosslinking is crosslinked in soaking at room temperature 6h.
Further, step (3) the anion charged polymer concentration of polymer solution 15%.
Further, step (3) drying meanss are sandwiched in perforated membrane in the middle of 2 blocks of glass to take out perforated membrane, and glass
Non-woven fabrics are placed and film between, 60 DEG C of vacuum dryings are removed film, obtain charge embedded film.
Further, step (3) is carried out as follows：It is put in buchner funnel by filter membrane of the perforated membrane after crosslinking, bottom
One metafiltration paper of portion's pad, pours anion charged polymer solution into, and the solution of film excess surface is scraped off, so by water pump decompression sucking filtration
60 DEG C of drying of vacuum drying oven, obtain charge embedded film afterwards.
Brominated polyphenylether (BPPO) structural formula of the present invention is as follows, and the scope of wherein bromination degree a is：70%≤a≤
25%；
Sulfonated poly (phenylene oxide) (SPPO, n are 500-5000) of the present invention, sulfonated polystyrene (SPS, n be 300～600),
Sulfonated polyether sulfone (SPES, n are 5000-6000) structural formula is as follows：
Compared with prior art, beneficial effect of the present invention is mainly reflected in：The charge embedded film of the present invention is connect from structure
Preferable embedded film is bordering on, the interspersed complementary interference of the alternating in anion structure domain and cationic domain is realized, and from film
One side to the continuous charged structure of another side.Prepared embedded film have the permeation flux of salt it is big, it is non-to sucrose etc. from
The characteristics of subclass material rejection is high.Therefore, it can efficiently separate electrolyte and non-electrolyte or carry out the dilution of electrolyte
And desalination etc., pressure dialysis and diffusion dialysis etc. are can be also used for, wherein carrying out to Sodium Chloride sodium sulfate mixed solution detached
Substantially, charge embedded film is all significantly improved effect compared with BPPO perforated membrane mechanical performances, is measured by instron
Percentage elongation when tensile strength and fracture, wherein tensile strength (Ts) are respectively increased 193%, 126.7%, 137.3%, extension at break
Rate (Eb) is respectively increased 64.3%, 125.7%, 185.7%.
(4) illustrate
The plane and tangent plane design sketch of Fig. 1 charge embedded films of the present invention.
Fig. 2 electrodialysis dialysis apparatuss schematic diagrams.
Charge embedded film prepared by Fig. 3 embodiment of the present invention 2 is to monovalence (Cl-) and bivalence (SO4 2-) anion selectivity point
From design sketch.
2 charge embedded film Electronic Speculum phenogram of Fig. 4 embodiments, A are profile, and B is upper surface figure.
3 charge embedded film of Fig. 5 embodiments immersion variety classes amine test Anion separation efficiency chart.
Fig. 6 is tensile strength (Ts) and elongation at break (Eb) test chart.
(5) specific embodiment
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This：
Sulfonated polystyrene used by the embodiment of the present invention (SPS) n is 500, and sulfonated poly (phenylene oxide) (SPPO) n is 450, and sulfonation gathers
Ether sulfone (SPES), n is 5400.
Room temperature described in the embodiment of the present invention is 25 DEG C.
Embodiment 1
The BPPO2g that bromination degree is 57.2% is taken, quality 15% is made into as solvent with 1-Methyl-2-Pyrrolidone (NMP)
BPPO solution, after standing 24h deaerations, knifing on glass plate, scrapes film thickness for 200 μm, then rapidly by film together with glass plate
Film forming in deionized water being put into, water being changed once every 2 hours, film is taken out after 12 hours, 60 degree of drying obtain BPPO perforated membranes.
Take out after BPPO perforated membranes are put into the immersion 6 hours of (25 DEG C) of room temperature in the ethylenediamine solution of 1mol/L, again dry for standby.
With DMF as sulfonated polystyrene (SPS) solution of solvent configuration quality concentration 15%, the ultrasound 6h under power 300W
It is stand-by after deaeration.The BPPO perforated membranes of preparation are put in SPS solution, BPPO perforated membranes are discharged in ultrasonic (300W) deaeration 2 hours
Interior gas, while the inside of SPS solution access aperture.BPPO perforated membranes are taken out, folder upper glass in film both sides is put between glass and film
Put non-woven fabrics, 60 DEG C of vacuum dryings subsequently remove non-woven fabrics with pocket knife auxiliary, charge embedded film sample preparation success, plane and
Tangent plane design sketch as shown in Figure 1, electron microscope as shown in Figure 4, by vacuum draw SPS to BPPO films in, generate in film big
The hole of amount, among SPS has entered into the space of film by pressure, has obtained charge embedded structure in theory.
Embodiment 2
With in embodiment 1, BPPO perforated membranes are put in buchner funnel as filter membrane, one metafiltration paper of bottom pad；Enforcement is poured on top into
SPS solution in example 1, water pump decompression (vacuum -0.1MPa) sucking filtration, removes together with filter paper after 20 minutes, by film excess surface
SPS solution scraped off with knife, then 60 degrees Celsius of vacuum drying oven drying obtains charge embedded film.
The charge embedded film is applied to into monovalention Selective Separation electrodialysis, electrodialysis plant schematic diagram is shown in Fig. 2
It is shown.Two pole room solution are 0.5mol/L aqueous sodium persulfate solutions, and light room and dense room solution are 0.5mol/L aqueous sodium persulfate solutions
With 0.5mol/L sodium-chloride water solutions, DC current density：5.1mA/m2, light room solution is sampled every 15min, use chromatography of ions
Instrument detects chloride ion and sulfate ion concentration, a dianion concentration-time profile show as shown in Figure 3, as a result with when
Between elapse, univalent anion is separated in the presence of dc-battery from mixed solution.
Embodiment 3
By the ethylenediamine in embodiment 1, propane diamine, butanediamine, pentanediamine, hexamethylene diamine are changed to respectively, then according to implementing
Step in example 1 prepares charge embedded film, tests Anion separation efficiency using 2 method of embodiment, as a result as shown in Figure 5.
The separation efficiency highest of ethylenediamine is found wherein, hexamethylene diamine is minimum, and with the increase of amido carbochain, separation efficiency is gradually lowered.
Embodiment 4
SPS in embodiment 1 is changed to into sulfonated poly (phenylene oxide) (SPPO), sulfonated polyether sulfone (SPES), then according to embodiment 1
Step prepares charge embedded film, and as shown in Figure 6, the BPPO perforated membranes mechanical performance that charge embedded film is prepared compared with embodiment 1 is all
It is significantly improved, percentage elongation when measuring tensile strength and fracture by instron, wherein tensile strength (Ts) point
It is indescribably high by 193%, 126.7%, 137.3%, elongation at break (Eb) is respectively increased 64.3%, 125.7%, 185.7%.
Claims (10)
1. a kind of preparation method of charge embedded film, it is characterised in that methods described is：(1) by brominated polyphenylether 1- methyl-
2-Pyrrolidone is made into the brominated polyphenylene ethereal solution of mass concentration 15-30%, is stored at room temperature 24h knifing on the glass plate, so
Rapidly film is put in deionized water together with glass plate afterwards and stands film forming, taken out film drying, obtain brominated polyphenylether porous
Film；
(2) step (1) brominated polyphenylether perforated membrane is immersed in diamine compounds aqueous solution, soaking at room temperature is crosslinked,
Take out, drying, the perforated membrane after being crosslinked；
(3) perforated membrane after step (2) crosslinking is placed in anion charged polymer solution, after ultrasonic deaeration, takes out porous
Film, is dried, and obtains charge embedded film；The anion charged polymer solution is by anion charged polymer dimethyl methyl
Amide dissolving is configured to the solution of mass concentration 5-30%, and the anion charged polymer is sulfonated poly (phenylene oxide), sulfonated polyphenyl
One kind in ethylene or sulfonated polyether sulfone.
2. the preparation method of charge embedded film as claimed in claim 1, it is characterised in that step (1) the brominated polyphenylether bromination
Degree is between 25% and 70%.
3. the preparation method of charge embedded film as claimed in claim 1, it is characterised in that step (1) is described to scrape film thickness for 200-
600μm。
4. the preparation method of charge embedded film as claimed in claim 1, it is characterised in that step (1) membrance casting condition is：Often
Water was changed once every 2 hours, take out film after 12 hours.
5. the preparation method of charge embedded film as claimed in claim 1, it is characterised in that step (2) diamine compounds are
Ethylenediamine, propane diamine, butanediamine, pentanediamine or hexamethylene diamine.
6. the preparation method of charge embedded film as claimed in claim 1, it is characterised in that step (2) the diamine compounds water
Solution concentration is 1-3mol/L.
7. the preparation method of charge embedded film as claimed in claim 1, it is characterised in that step (2) crosslinking is soaked in room temperature
Bubble 6h is crosslinked.
8. the preparation method of charge embedded film as claimed in claim 1, it is characterised in that the charged polymerization of step (3) anion
Thing concentration of polymer solution 15%.
9. the preparation method of charge embedded film as claimed in claim 1, it is characterised in that step (3) drying meanss are：Take
Go out perforated membrane, perforated membrane is sandwiched in the middle of 2 blocks of glass, and between glass and film, place non-woven fabrics, vacuum drying is removed film, obtained
Obtain charge embedded film.
10. the preparation method of charge embedded film as claimed in claim 1, it is characterised in that step (3) is carried out as follows：With
Perforated membrane after crosslinking is put in buchner funnel for filter membrane, one metafiltration paper of bottom pad, pours anion charged polymer solution, water into
Pump decompression sucking filtration, the solution of film excess surface is scraped off, and then 60 DEG C of drying of vacuum drying oven, obtain charge embedded film.
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| CN201611255013.9A CN106582304B (en) | 2016-12-30 | 2016-12-30 | A kind of preparation method of charge embedded film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109745868A (en) * | 2019-01-25 | 2019-05-14 | 广东省医疗器械研究所 | It is a kind of for treating the preparation method of uremic antibacterial hollow-fibre membrane |
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|---|---|---|---|---|
| JPH0584430A (en) * | 1991-09-27 | 1993-04-06 | Dainichiseika Color & Chem Mfg Co Ltd | Mosaic charge membrane |
| CN101530748A (en) * | 2009-03-17 | 2009-09-16 | 郑州大学 | Method for preparing composite charged mosaic membrane via interfacial polymerization |
| WO2010117036A1 (en) * | 2009-04-09 | 2010-10-14 | 国立大学法人山口大学 | Charge-mosaic membrane |
| CN102770197A (en) * | 2009-12-28 | 2012-11-07 | 可乐丽股份有限公司 | Multilayered charge-mosaic membrane and manufacturing method therefor |
| CN106110900A (en) * | 2016-07-15 | 2016-11-16 | 浙江工业大学 | A kind of anion selectivity separation film and application thereof |
-
2016
- 2016-12-30 CN CN201611255013.9A patent/CN106582304B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0584430A (en) * | 1991-09-27 | 1993-04-06 | Dainichiseika Color & Chem Mfg Co Ltd | Mosaic charge membrane |
| CN101530748A (en) * | 2009-03-17 | 2009-09-16 | 郑州大学 | Method for preparing composite charged mosaic membrane via interfacial polymerization |
| WO2010117036A1 (en) * | 2009-04-09 | 2010-10-14 | 国立大学法人山口大学 | Charge-mosaic membrane |
| CN102770197A (en) * | 2009-12-28 | 2012-11-07 | 可乐丽股份有限公司 | Multilayered charge-mosaic membrane and manufacturing method therefor |
| CN106110900A (en) * | 2016-07-15 | 2016-11-16 | 浙江工业大学 | A kind of anion selectivity separation film and application thereof |
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| Title |
|---|
| 吴翠明等: "BPPO中空纤维荷电镶嵌膜制备及其蛋白质吸附性能", 《膜科学与技术》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109745868A (en) * | 2019-01-25 | 2019-05-14 | 广东省医疗器械研究所 | It is a kind of for treating the preparation method of uremic antibacterial hollow-fibre membrane |
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