CN106110910A - A kind of infiltration vaporization separation film and preparation method thereof - Google Patents

A kind of infiltration vaporization separation film and preparation method thereof Download PDF

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Publication number
CN106110910A
CN106110910A CN201610461441.0A CN201610461441A CN106110910A CN 106110910 A CN106110910 A CN 106110910A CN 201610461441 A CN201610461441 A CN 201610461441A CN 106110910 A CN106110910 A CN 106110910A
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basement membrane
solution
preparation
dopamine
poly
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吴青龙
史宏
谢吉民
刘玲
范俭青
朱桂生
周祖涛
唐丽
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Jiangsu Thorpe Engineering Technology Co Ltd
JIANGSU SOPO (GROUP) CO Ltd
Jiangsu University
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Jiangsu Thorpe Engineering Technology Co Ltd
JIANGSU SOPO (GROUP) CO Ltd
Jiangsu University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D71/00Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06Organic material
    • B01D71/76Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D67/00Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002Organic membrane manufacture
    • B01D67/0006Organic membrane manufacture by chemical reactions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D67/00Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0081After-treatment of organic or inorganic membranes
    • B01D67/0093Chemical modification
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D69/00Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/02Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D69/00Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12Composite membranes; Ultra-thin membranes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D71/00Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06Organic material
    • B01D71/58Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
    • B01D71/60Polyamines
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2323/00Details relating to membrane preparation
    • B01D2323/02Hydrophilization
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2323/00Details relating to membrane preparation
    • B01D2323/06Specific viscosities of materials involved
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2325/00Details relating to properties of membranes
    • B01D2325/30Chemical resistance
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2325/00Details relating to properties of membranes
    • B01D2325/36Hydrophilic membranes

Abstract

The invention discloses a kind of infiltration vaporization separation film and preparation method thereof, be DOPA or dopamine to be stablized autohemagglutination together in membrane surface, then carry out being grafted and cross-linking and prepare gained.The present invention is based on bioadhesive principle, obtain a kind of can be with the poly-DOPA of basement membrane strong bonded or poly-dopamine composite bed, this composite bed directly crosslinks reaction with the hydroxyl in long-chain molecule, thus prepares good hydrophilic property, permeation flux height, separating property is good and membrane stability is good infiltration vaporization separation film.Preparation process of the present invention is easy, and raw material is easy to get, mild condition, and prepared infiltrating and vaporizing membrane, for the separation of ethyl acetate/water, has higher permeation flux and membrane stability.

Description

A kind of infiltration vaporization separation film and preparation method thereof
Technical field
The present invention relates to the preparation method of a kind of composite membrane, be specifically related to a kind of infiltration vaporization separation film and preparation side thereof Method, belongs to separation film composite material field.
Background technology
Infiltration evaporation is a kind of novel membrane separation technique, and it utilizes different component dissolving in film and diffusion Different and realize separating, have that energy consumption is low, environmental friendliness, do not limited by vapor liquid equilibrium, that process is simple and convenient to operate etc. is excellent Point.Infiltration evaporation can also transform traditional handicraft with the PROCESS COUPLING such as rectification, absorption simultaneously, and is derived from huge energy-conservation effect Really.Infiltrating and vaporizing membrane can be divided into homogeneous membrane and composite membrane by structure.Homogeneous membrane is thicker, and component is big through the resistance of film, and infiltration is logical Measure little.Composite membrane is the membrane material different by two kinds, is respectively prepared to have the cortex (stratum disjunctum) of separation function and play support and makees Porous layer (basement membrane) and the film that forms, preparation it is critical that interface interaction intensity between stratum disjunctum and supporting layer, Stronger interaction is not only advantageous to improve the stability of film and service life, and the most ultra-thin, zero defect stratum disjunctum Coating, improve permeation flux, particularly difference in material properties bigger organic-inorganic hybridized osmotic vaporization film.Owing to dividing Viscosity weak between absciss layer and supporting layer or active force, conventional composite membrane preparation method such as dip-coating, Lay-by-Lay or Cast coating method is the most invalid, so that supporting layer or coating material carry out graft modification, and these methods are the most very Complicated tediously long.Therefore, find a kind of simply, effectively can improve the method for interfacial interaction intensity to the preparation of composite membrane extremely Close important.
In recent years, the common concern of researchers is received based on the poly-dopamine coating that mussel is bionical.Normal as one " biological glue " seen, dopamine can spontaneous polymerization in the basic conditions, it is strong, hydrophilic that the poly-dopamine of formation has adhesiveness Property is strong, applied widely and is prone to the advantages such as Post functionalization and is widely used in surface modification.Such as patent " a kind of nanometer The preparation method of silver/poly-dopamine composite membrane " in use phase inversion prepare polyether sulfone (PES) ultrafiltration membranes;Again film is soaked In dopamine solution, by poly-depositing dopamine in PES membrane surface, form ultra-thin active layer.The method is directly by basement membrane PES It is immersed in dopamine, is unfavorable for the cohesive between dopamine and basement membrane PES.Patent " a kind of poly-dopamine modified lithium polyamide The preparation method of compound forward osmosis membrane " in, prepare polyamide stratum disjunctum on the surface of dopamine modification supporting layer, obtain poly-DOPA Amine modified polyamide is combined forward osmosis membrane, and the method does not carries out pretreatment to basement membrane, does not takes into account basement membrane and polyamide stratum disjunctum Interface interaction.Patent " Dopamine-polyethersucomposite composite membrane and preparation method thereof " first prepared polyether sulfone basement membrane, then by film successively Being immersed in aqueous phase monomers dopamine and organic facies monomer pyromellitic trimethylsilyl chloride, the dopamine made through interfacial polymerization is combined Film, does not takes into account the above yet.In patent " PDMS/PVDF osmosis vaporizing compound membrane, preparation method and applications ", disclose A kind of PDMS/PVDF osmosis vaporizing compound membrane, by preparing the PVDF supporting layer of different pore size, then coats poly-two at supporting layer Methylsiloxane composite bed, obtains osmosis vaporizing compound membrane, but does not takes into account the interface work of basement membrane and infiltrating and vaporizing membrane stratum disjunctum Use intensity.In patent " a kind of fluoro-acrylate copolymer osmosis vaporizing compound membrane and preparation method thereof ", disclose one and contain Fluorinated monomer copolymer infiltration vaporization composite membrane, including supporting layer and activity stratum disjunctum, activity stratum disjunctum is uniformly distributed in props up On support layer, supporting layer is politef micropore support membrane, and activity stratum disjunctum is fluoro-acrylate copolymer, does not also take into account Basement membrane mentioned above and the interaction of infiltration evaporation composite bed.
Summary of the invention
Solve the technical problem that: the present invention is based on some shortcomings of the prior art, it is provided that a kind of infiltration evaporation separates Film and preparation method thereof, i.e. based on DOPA or dopamine auto polymerization composite bed infiltration vaporization separation film and preparation method thereof, On the basis of keeping excellent release energy, strengthen the combined strength bination between coating and basement membrane, extend the service life separating film, preparation Technique is simple, it is easy to operates and promotes, has a good application prospect.
Technical scheme: a kind of infiltration vaporization separation film that the present invention provides, is to be in aperture by DOPA or dopamine autohemagglutination 0.01~1 μm, thickness are the membrane surface of 10~500 μm, form surface compact, thickness is the 1~200 poly-DOPA of μm or poly-DOPA The separation film of amine composite bed.
The preparation method of a kind of infiltration vaporization separation film that the present invention provides, its preparation process is as follows:
(1) basement membrane being carried out pretreatment, by basement membrane static immersing 2~5h in the solution of 0.1~2mol/L, temperature is 20 ~60 DEG C, then with ethanol and deionized water alternately shake cleaning (wash number 2~10 times, each scavenging period 5~30min, Concussion rotating speed is 100~200r/min), and the most fully infiltrate;
(2) it is 0.1~5mg/L with DOPA or dopamine as solute that step (1) pretreated basement membrane is placed in concentration Mixed solution is carried out concussion reaction, then with ethanol and deionized water alternately shake cleaning (wash number 2~10 times, every time Scavenging period 5~30min, concussion rotating speed are 100~200r/min), obtain surface with poly-DOPA or poly-dopamine composite bed Basement membrane;The described concussion response time is 2~48h, temperature is 20~40 DEG C, concussion rotating speed is 100~200r/min;
(3) surface step (2) obtained is soaked in graft copolymer solution with the basement membrane of poly-DOPA or poly-dopamine composite bed Bubble processes, the basement membrane after being grafted;The concentration of described graft copolymer solution is 0.1~5wt%, and soak time is 2~48h, temperature It it is 20~60 DEG C;
(4) immersion treatment during the basement membrane after grafting step (3) obtained immerses cross-linking agent aqueous solution, obtains infiltration evaporation Separate film;The concentration of described cross-linking agent aqueous solution is 0.1~2wt%, and soak time is 2~48h, and temperature is 20~80 DEG C.
Step (1) described solution is sodium hydroxide solution, sulfuric acid solution, hydrochloric acid solution, liquor natrii hypochloritis or hydrogen peroxide Solution.
Step (1) described basement membrane is organic basement membrane or inorganic basement membrane;Described organic basement membrane is polyacrylonitrile, polyether sulfone, gathers Vinylidene, polysulfones, polypropylene or politef;Described inorganic basement membrane is aluminium oxide, titanium oxide, zirconium oxide or silicon oxide.
Step (2) described with DOPA or dopamine the solvent of the mixed solution as solute as sea water, deionized water, pH be for 6 ~the Tris-hydrochloric acid buffer solution of 10 or ethanol water that ethanol mass fraction is 5~40%.
Step (3) described graft copolymer solution is aqueous solution or the ethanol solution of the long-chain molecule of hydroxyl, amino or sulfydryl;Institute The long-chain molecule stating hydroxyl, amino or sulfydryl is tetraethyl orthosilicate, polymine, polyvinyl alcohol, sulfhydrylation or amino The Polyethylene Glycol changed or amidized chitosan.
Step (4) described cross-linking agent is glutaraldehyde, glycerin triglycidyl ether or epoxychloropropane.
The present invention, based on bioadhesive principle, obtains a kind of to be combined with the poly-DOPA of basement membrane strong bonded or poly-dopamine Layer.This composite bed directly reacts with the hydroxyl in long-chain molecule, amino or sulfydryl, it is possible to carry out further with cross-linking agent Process, thus prepare that series of hydrophilic is good, permeation flux is high, the good infiltration evaporation good with membrane stability of separating property separates Film.
Beneficial effect: the advantage of infiltration vaporization separation film of the present invention and preparation method thereof is: (1) does not destroy basement membrane originally Body, and basement membrane profile and size are not limited;(2) the poly-DOPA prepared by or poly-DOPA amine layer, have special attachments (viscous Close) property, the combined strength bination being greatly reinforced between stratum disjunctum and basement membrane, substantially prolongs stability and the service life of film;(3) Prepared poly-DOPA or poly-dopamine composite bed hydrophilic are strong, can improve the water permeability of film;(4) selected by material and connect Branch and cross-linking procedure, poly-DOPA prepared by imparting or poly-dopamine composite bed with infiltrating and vaporizing membrane feature, be suitable for organic molten The high-performance infiltrating and vaporizing membrane of agent particularly ethyl acetate, ethanol equal solvent dehydration, has a good application prospect.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of embodiment 1 polyacrylonitrile porous membrane surface;
Fig. 2 is the stereoscan photograph on the infiltration vaporization separation film surface prepared by embodiment 1;
Fig. 3 is the stereoscan photograph in the infiltration vaporization separation film cross section prepared by embodiment 1;
Fig. 4 is the stereoscan photograph in the polyvinyl alcohol prepared by reference examples 1/polyacrylonitrile infiltrating and vaporizing membrane cross section.
Detailed description of the invention
Further illustrate the present invention below by the mode of embodiment, but the most therefore protection scope of the present invention is confined to Following embodiment, but limited by description and claims of this specification.
Embodiment 1
By polyacrylonitrile basement membrane (as shown in Figure 1) in 0.5%NaOH aqueous solution after static immersing 3h, then with ethanol with go Ionized water alternately shakes cleaning, and the most fully infiltrates;Being dissolved in deionized water by dopamine, configuration concentration is 2.0mg/ The dopamine solution of L;Basement membrane is soaked in dopamine solution, rotating speed be 100r/min, temperature be 25 DEG C concussion cultivate Case shakes 24h, then alternately shakes cleaning with ethanol and deionized water, by the basement membrane with poly-dopamine composite bed in temperature It is immersion 4h in the 0.5wt% polyvinyl alcohol water solution of 40 DEG C, cleans with deionized water concussion;Then the film obtained is immersed 60 DEG C 0.5% glutaraldehyde water solution in cross-link 5h;Clean with deionized water concussion, prepare infiltrating and vaporizing membrane, be illustrated in figure 2 it The stereoscan photograph on surface, Fig. 3 is the stereoscan photograph in its cross section.
Measuring this film dewatering to ethyl acetate, result is as follows.For the ethyl acetate solution of water content 3%, Under conditions of operation temperature is 50 DEG C, initial flux about 427g m-2·h-1, water content can be down to about 0.2%.Film is continuous Run 48h, swelling, deformation and the phenomenon separated with basement membrane do not occur, presents preferable combined strength bination.
Embodiment 2
By polyacrylonitrile basement membrane in 0.5%NaOH aqueous solution after static immersing 3h, then with ethanol and deionized water alternately Concussion is cleaned, and the most fully infiltrates;Dopamine is dissolved in the Tris-HCl buffer solution that pH is 8.0, configuration concentration Dopamine solution for 1.0mg/L;Basement membrane is soaked in dopamine solution, rotating speed be 100r/min, temperature be 25 DEG C Concussion incubator shakes 24h, then alternately shakes cleaning with ethanol and deionized water, by the base with poly-dopamine composite bed Film soaks 4h in the 0.5wt% polyvinyl alcohol water solution that temperature is 40 DEG C, cleans with deionized water concussion;Then will obtain 0.5% glutaraldehyde water solution of film immersion 60 DEG C cross-links 5h;Clean with deionized water concussion, prepare infiltrating and vaporizing membrane.
Measuring this film dewatering to ethyl acetate, result is as follows.For the ethyl acetate solution of water content 3%, Under conditions of operation temperature is 50 DEG C, initial flux about 500g m-2·h-1, water content can be down to about 0.2%.Film is continuous Run 48h, swelling, deformation and the phenomenon separated with basement membrane do not occur, presents preferable combined strength bination.
Embodiment 3
By polyacrylonitrile basement membrane in 0.5%NaOH aqueous solution after static immersing 3h, then with ethanol and deionized water alternately Concussion is cleaned, and the most fully infiltrates;Dopamine is dissolved in the Tris-HCl buffer solution that pH is 8.0, configuration concentration Dopamine solution for 2.0mg/L;Basement membrane is soaked in dopamine solution, rotating speed be 100r/min, temperature be 25 DEG C Concussion incubator shakes 24h, then alternately shakes cleaning with ethanol and deionized water, by the base with poly-dopamine composite bed Film soaks 4h in the 0.5wt% polyvinyl alcohol water solution that temperature is 40 DEG C, cleans with deionized water concussion;Then will obtain 0.5% glutaraldehyde water solution of film immersion 60 DEG C cross-links 5h;Clean with deionized water concussion, prepare infiltrating and vaporizing membrane.
Measuring this film dewatering to ethyl acetate, result is as follows.For the ethyl acetate solution of water content 3%, Under conditions of operation temperature is 50 DEG C, initial flux about 450g m-2·h-1, water content can be down to about 0.2%.Film is continuous Run 48h, swelling, deformation and the phenomenon separated with basement membrane do not occur, presents preferable combined strength bination.
Embodiment 4
By polyacrylonitrile basement membrane in 0.5%NaOH aqueous solution after static immersing 3h, then with ethanol and deionized water alternately Concussion is cleaned, and the most fully infiltrates;Dopamine is dissolved in the Tris-HCl buffer solution that pH is 8.0, configuration concentration Dopamine solution for 1.0mg/L;Basement membrane is soaked in dopamine solution, rotating speed be 100r/min, temperature be 25 DEG C Concussion incubator shakes 24h, then alternately shakes cleaning with ethanol and deionized water, by the base with poly-dopamine composite bed Film soaks 4h in the amidized Aqueous Solutions of Polyethylene Glycol of the 0.5wt% that temperature is 40 DEG C, cleans with deionized water concussion;Then The film obtained is immersed in 0.5% glutaraldehyde water solution of 60 DEG C and cross-link 5h;Clean with deionized water concussion, prepare infiltration evaporation Film.
Measuring this film dewatering to ethyl acetate, result is as follows.For the ethyl acetate solution of water content 3%, Under conditions of operation temperature is 50 DEG C, initial flux about 480g m-2·h-1, water content can be down to about 0.2%.Film is continuous Run 48h, swelling, deformation and the phenomenon separated with basement membrane do not occur, presents preferable combined strength bination.
Embodiment 5
By polyacrylonitrile basement membrane in 0.5%NaOH aqueous solution after static immersing 3h, then with ethanol and deionized water alternately Concussion is cleaned, and the most fully infiltrates;Dopamine is dissolved in the Tris-HCl buffer solution that pH is 8.0, configuration concentration Dopamine solution for 1.0mg/L;Basement membrane is soaked in dopamine solution, rotating speed be 100r/min, temperature be 25 DEG C Concussion incubator shakes 24h, then alternately shakes cleaning with ethanol and deionized water, by the base with poly-dopamine composite bed Film soaks 4h in the amidized Aqueous Solutions of Polyethylene Glycol of the 0.5wt% that temperature is 40 DEG C, cleans with deionized water concussion;Then The film obtained is immersed in the 0.5% epoxychloropropane aqueous solution of 60 DEG C and cross-link 5h;Clean with deionized water concussion, prepare infiltration Vaporization film.
Measuring this film dewatering to ethyl acetate, result is as follows.For the ethyl acetate solution of water content 3%, Under conditions of operation temperature is 50 DEG C, initial flux about 430g m-2·h-1, water content can be down to about 0.2%.Film is continuous Run 48h, swelling, deformation and the phenomenon separated with basement membrane do not occur, presents preferable combined strength bination.
Embodiment 6
By polyacrylonitrile basement membrane in 0.5%NaOH aqueous solution after static immersing 3h, then with ethanol and deionized water alternately Concussion is cleaned, and the most fully infiltrates;Dopamine is dissolved in the Tris-HCl buffer solution that pH is 8.0, configuration concentration Dopamine solution for 1.0mg/L;Basement membrane is soaked in dopamine solution, rotating speed be 100r/min, temperature be 25 DEG C Concussion incubator shakes 24h, then alternately shakes cleaning with ethanol and deionized water, by the base with poly-dopamine composite bed Film soaks 4h in the amidized chitosan aqueous solution of the 0.5wt% that temperature is 40 DEG C, cleans with deionized water concussion;Then will 0.5% epoxychloropropane aqueous solution of the film immersion 60 DEG C obtained cross-links 5h;Clean with deionized water concussion, prepare infiltration vapour Change film.
Measuring this film dewatering to ethyl acetate, result is as follows.For the ethyl acetate solution of water content 3%, Under conditions of operation temperature is 50 DEG C, initial flux about 400g m-2·h-1, water content can be down to about 0.2%.Film is continuous Run 48h, swelling, deformation and the phenomenon separated with basement membrane do not occur, presents preferable combined strength bination.
Reference examples 1
By polyacrylonitrile basement membrane in 0.5%NaOH aqueous solution after static immersing 3h, then with ethanol and deionized water alternately Concussion is cleaned, and is subsequently placed in the 0.5wt% polyvinyl alcohol water solution that temperature is 40 DEG C immersion 4h, clear with deionized water concussion Wash;Then the film obtained is immersed in 0.5% glutaraldehyde water solution of 60 DEG C and cross-link 5h;Clean with deionized water concussion, prepare Infiltrating and vaporizing membrane, is illustrated in figure 4 the stereoscan photograph in its cross section.
Measuring this film dewatering to ethyl acetate, result is as follows.For the ethyl acetate solution of water content 3%, Under conditions of operation temperature is 50 DEG C, initial flux about 600g m-2·h-1, vacuum is operated when running about about 20min Reducing rapidly, sample detection display film, without separating effect, upon examination it is found that film surface composite layer departs from basement membrane.
Reference examples 2
By polyacrylonitrile basement membrane in 0.5%NaOH aqueous solution after static immersing 3h, then with ethanol and deionized water alternately Concussion is cleaned, and is subsequently placed in the amidized chitosan aqueous solution of 0.5wt% that temperature is 40 DEG C immersion 4h, shakes with deionized water Swing cleaning;Then the film obtained is immersed in the 0.5% epoxychloropropane aqueous solution of 60 DEG C and cross-link 5h;Clear with deionized water concussion Wash, prepare infiltrating and vaporizing membrane.
Measuring this film dewatering to ethyl acetate, result is as follows.For the ethyl acetate solution of water content 3%, Under conditions of operation temperature is 50 DEG C, initial flux about 550g m-2 h-1, equally, operate when running about about 20min Vacuum reduces rapidly, after upon examination it is found that film surface composite layer and basement membrane also there occurs disengaging.
Result shows, uses and has the poly-DOPA of special adhesion or poly-DOPA amine layer, has been greatly reinforced stratum disjunctum and base Combined strength bination between film, substantially prolongs the service life of film, and prepared infiltrating and vaporizing membrane has higher infiltration Flux and stability.

Claims (9)

1. an infiltration vaporization separation film, it is characterised in that be to be 0.01~1 μm, thickness by DOPA or dopamine autohemagglutination in aperture Degree is the membrane surface of 10~500 μm, form surface compact, thickness is the 1~200 poly-DOPA of μm or poly-dopamine composite bed point From film.
2. the preparation method of an infiltration vaporization separation film as claimed in claim 1, it is characterised in that preparation process is as follows:
(1) basement membrane being carried out pretreatment, by basement membrane static immersing 2~5h in the solution of 0.1~2mol/L, temperature is 20~60 DEG C, then alternately shake cleaning with ethanol and deionized water, and the most fully infiltrate;
(2) it is the 0.1~5mg/L mixing as solute with DOPA or dopamine that step (1) pretreated basement membrane is placed in concentration Solution carries out concussion reaction, then alternately shakes cleaning with ethanol and deionized water, obtain surface with poly-DOPA or poly-many The basement membrane of bar amine composite bed;The described concussion response time is 2~48h, temperature is 20~40 DEG C, concussion rotating speed is 100~200r/ min;
(3) surface that step (2) is obtained with the basement membrane of poly-DOPA or poly-dopamine composite bed in graft copolymer solution at immersion Reason, the basement membrane after being grafted;The concentration of described graft copolymer solution is 0.1~5wt%, and soak time is 2~48h, and temperature is 20 ~60 DEG C,;
(4) immersion treatment during the basement membrane after grafting step (3) obtained immerses cross-linking agent aqueous solution, obtains infiltration evaporation and separates Film;The concentration of described cross-linking agent aqueous solution is 0.1~2wt%, and soak time is 2~48h, and temperature is 20~80 DEG C.
The preparation method of a kind of infiltration vaporization separation film the most according to claim 2, it is characterised in that described basement membrane is for having Machine basement membrane or inorganic basement membrane;Described organic basement membrane is polyacrylonitrile, polyether sulfone, Kynoar, polysulfones, polypropylene or polytetrafluoro Ethylene;Described inorganic basement membrane is aluminium oxide, titanium oxide, zirconium oxide or silicon oxide.
The preparation method of a kind of infiltration vaporization separation film the most according to claim 2, it is characterised in that step (1) is described molten Liquid is sodium hydroxide solution, sulfuric acid solution, hydrochloric acid solution, liquor natrii hypochloritis or hydrogen peroxide solution.
The preparation method of a kind of infiltration vaporization separation film the most according to claim 2, it is characterised in that step (1) and (2) Described in number of times that alternately concussion is cleaned be 2~10 times, each scavenging period is 5~30min, and concussion rotating speed is 100~200r/ min。
The preparation method of a kind of infiltration vaporization separation film the most according to claim 2, it is characterised in that step (2) described with The solvent of DOPA or mixed solution that dopamine is solute be sea water, deionized water, pH be 6~10 Tris-hydrochloride buffer molten Liquid or the ethanol water that ethanol mass fraction is 5~40%.
The preparation method of a kind of infiltration vaporization separation film the most according to claim 2, it is characterised in that step connects described in (3) Branch solution is aqueous solution or the ethanol solution of the long-chain molecule of hydroxyl, amino or sulfydryl.
The preparation method of a kind of infiltration vaporization separation film the most according to claim 7, it is characterised in that described hydroxyl, ammonia The long-chain molecule of base or sulfydryl is tetraethyl orthosilicate, polymine, polyvinyl alcohol, sulfhydrylation or amidized Polyethylene Glycol Or amidized chitosan.
The preparation method of a kind of infiltration vaporization separation film the most according to claim 2, it is characterised in that step (4) described friendship Connection agent is glutaraldehyde, glycerin triglycidyl ether or epoxychloropropane.
CN201610461441.0A 2016-06-22 2016-06-22 A kind of infiltration vaporization separation film and preparation method thereof Pending CN106110910A (en)

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CN106492644A (en) * 2016-11-18 2017-03-15 北京建筑大学 A kind of ultrafilter membrane process for purifying water based on microemulsion modified Nano Zero-valent Iron Carbon Materials precoated shet
CN106750462A (en) * 2016-12-19 2017-05-31 大连理工大学 A kind of surface modifying method of dopamine and its derivative polymerization and crosslinking curing
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CN115152750A (en) * 2022-07-16 2022-10-11 杭州星空男孩新材料科技有限公司 Long-acting antibacterial spray and preparation method thereof
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Application publication date: 20161116