CN107158980A - Utilized thin film composite membranes reacted based on air liquid interface and its preparation method and application - Google Patents
Utilized thin film composite membranes reacted based on air liquid interface and its preparation method and application Download PDFInfo
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- CN107158980A CN107158980A CN201710425489.0A CN201710425489A CN107158980A CN 107158980 A CN107158980 A CN 107158980A CN 201710425489 A CN201710425489 A CN 201710425489A CN 107158980 A CN107158980 A CN 107158980A
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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
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
- B01D71/82—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74 characterised by the presence of specified groups, e.g. introduced by chemical after-treatment
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
- 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
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
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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
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The invention discloses a kind of preparation method for the utilized thin film composite membranes reacted based on air liquid interface, including：(1) hydrophobic polyalcohol stephanoporate basement membrane is swum in into deposition liquid surface, reacted 0.1~12 hour under the conditions of 10~90 DEG C, membrane structure is formed on the polyalcohol stephanoporate basement membrane at air liquid interface；Described deposition liquid is the polyphenol monomer of pH=6~10 and the solution of polyamine monomers；(2) reacted polyalcohol stephanoporate basement membrane in step (1) is placed in cross-linking reaction in cross-linking agent solution, membrane structure is cross-linked into selectivity function cortex on polyalcohol stephanoporate basement membrane, obtains the described utilized thin film composite membranes reacted based on air liquid interface.The preparation method controllability is strong.The invention also discloses the utilized thin film composite membranes prepared by above-mentioned preparation method, the utilized thin film composite membranes can be applied in nanofiltration, counter-infiltration, positive infiltration or seepage slope.
Description
Technical field
The present invention relates to technical field of membrane separation, more particularly to a kind of utilized thin film composite membranes reacted based on air liquid interface and
Its preparation method and application.
Background technology
Utilized thin film composite membranes refer to that, by porous support layer and the fine and close class separation membrane material for separating thin layer composite, it has
There are high pressure resistant, high flux, high selectivity, be widely used in fields such as nanofiltration, positive/negative infiltration, seepage slopes.Mesh
Before, preparing the method for utilized thin film composite membranes mainly has interfacial polymerization, LBL self-assembly, surface coating, chemical vapor deposition etc..
For example, Publication No. CN105498547A Chinese patent discloses a kind of preparation of hollow fiber compound nanofiltration membrane
Method, the fillers such as CNT are added in interface polymerization reaction, so as to be allowed to be embedded in the separating layer of NF membrane, improved
The performance of NF membrane.
Publication No. CN106268322A Chinese patent discloses a kind of LBL self-assembly graphene oxide/quaternized shell
Glycan Positively charged composite nanofiltration membrane and preparation method thereof, it utilizes graphene oxide on the surface of poly (ether-sulfone) ultrafiltration membrane and quaternized
Chitosan carries out electric charge assembling with opposite electric charge is thought.The thin layer composite nanofiltration that surface carries different electric charges is prepared
Film.
Publication No. CN106310977A Chinese patent discloses a kind of tannic acid and Fe3+Common coating prepares composite nanometer filter
The method of film, tannic acid and Fe are immersed by milipore filter3+Aqueous phase solution inside plant, using the coordination of the two, in milipore filter
Surface forms the network structure of densification, so as to prepare tannic acid and Fe3+Coat the composite nanometer filtering film of crosslinking.
Publication No. CN103212305A Chinese patent discloses a kind of preparation method of aligned carbon nanotube NF membrane,
The carbon nano pipe array arranged using chemical vapour deposition technique growth of vertical, two flat boards are clamped in by described carbon nano pipe array
Between, apply pressure, while promoting two flat boards along horizontal opposite direction, obtain the carbon nano-tube film of horizontal orientation arrangement；Leaching
Enter liquid flux, taken out after 5-30 minutes；Under the conditions of gravity-flow ventilation place 2-24 hours, after after solvent evaporating completely from flat board
Sur-face peeling, obtains the aligned carbon nanotube film of horizontal dense arrangement；Using the uniform pores between CNT as gas and liquid
The filtering duct of body molecule, obtains aligned carbon nanotube NF membrane.
It has been reported that thin layer composite membrane preparation method in, interface (including liquid/solid, gas/solid, liquid/liquid interface) is in film
Forming process in it is most important.As interfacial polymerization thing occurs in profit liquid/liquid interface, layer assembly and surface coating then need to be
Solid/liquid interfaces are carried out, and chemical vapour deposition technique then occurs at gas/solid interface.It there is no at present and prepare high-performance using air liquid interface
The method of thin-film composite membrane.
The content of the invention
The invention provides a kind of utilized thin film composite membranes reacted based on air liquid interface and its preparation method and application, the system
Preparation Method controllability is strong.
A kind of preparation method for the utilized thin film composite membranes reacted based on air liquid interface, is comprised the following steps：
(1) hydrophobic polyalcohol stephanoporate basement membrane is swum in into deposition liquid surface, react 0.1 under the conditions of 10~90 DEG C~
12 hours, membrane structure was formed on the polyalcohol stephanoporate basement membrane at air liquid interface；
Described deposition liquid is the polyphenol monomer of pH=6~10 and the solution of polyamine monomers；
Described polyphenol monomer is dopamine, DOPA, catechol, norepinephrine, pyrogallol, tannic acid, tea
At least one of polyphenol；
Described polyamine monomers are polyethyleneimine, polyallylamine hydrochlorides, chitosan, diethylenetriamine, triethylene four
At least one of amine, triethylamine, piperazine, m-phenylene diamine (MPD), p-phenylenediamine；
(2) reacted polyalcohol stephanoporate basement membrane in step (1) is placed in cross-linking reaction in cross-linking agent solution, polymer is more
Membrane structure is cross-linked into selectivity function cortex on the basement membrane of hole, obtains the described utilized thin film composite membranes reacted based on air liquid interface.
Hydrophobic polyalcohol stephanoporate basement membrane swims in polyphenol/polyamines solution surface in step (1), and oxygen passes through gas/liquid
Interface is spread downwards, the polyphenol oxidase formation quinoid in solution, and then anti-with polyamines generation Michael additions or Schiff
Should.On the one hand, oxygen concentration at air liquid interface is higher, and the extent of reaction is higher at air liquid interface；On the other hand, in reaction
The polyphenol of formation/many amine compounds have amphipathic, it is intended to aggregation is migrated to air liquid interface.Then, polyphenol/polyamines is multiple
Compound is further reacted at air liquid interface, and the membrane structure of crosslinking is formed at the air liquid interface of polyalcohol stephanoporate basement membrane.
In order to improve the compactness of membrane structure, step (2) is further reacted with polyphenol or polyamines residual group by crosslinking agent, passed through
The selectivity function cortex of densification is cross-linked to form, so as to obtain the described utilized thin film composite membranes reacted based on air liquid interface.
In step (1)：
Preferably, hydrophobic polyalcohol stephanoporate basement membrane is swum in into deposition liquid surface, it is anti-under the conditions of 40~60 DEG C
Answer 1~2 hour.Although reaction rate is raised and raised with temperature, middle dissolving hypoxgia in high temperature sinking hydrops, it is suppressed that phenol
Oxidation.The too short reaction time can not ensure the fine and close zero defect of the membrane structure to be formed, and the longer reaction time can cause
Membrane structure is thickening, significantly reduces final obtained thin layer composite membrane flux.
Preferably, in described deposition liquid, the concentration of polyphenol monomer and polyamine monomers is 1g/L~10g/L；Further
It is preferred that, the concentration of polyphenol monomer and polyamine monomers is 2g/L~4g/L.
In described deposition liquid, the mass ratioes of polyphenol monomer and polyamine monomers also has important to the performances of utilized thin film composite membranes
Influence, preferably, in described deposition liquid, the mass ratio of polyphenol monomer and polyamine monomers is 1: 0.25~4.Polyphenol ratio
Raising when, the film of formation is mainly the aggregation formed by polyphenol autoxidation and constituted, and film can be caused to become fragile, mechanical property
Can reduction；And the raising of polyamines ratio can then suppress film forming procedure.
It is further preferred that the mass ratio of polyphenol monomer and polyamine monomers is 1: 0.5~1.
The species of polyphenol monomer and polyamine monomers also has to the performance of utilized thin film composite membranes to be had a certain impact, preferably,
In described deposition liquid, described polyphenol monomer is dopamine and/or o-phenylenediamine, and described polyamine monomers are polyethyleneimine
Amine；
The concentration of polyphenol monomer and polyamine monomers is 2g/L~4g/L；
The mass ratio of polyphenol monomer and polyamine monomers is 1: 0.5~1.
The thickness of utilized thin film composite membranes is moderate as made from the sedimentary system, and performance is more excellent, with the same of preferable retention efficiency
When its water flux it is also higher.
It is further preferred that the weight average molecular weight of described polyethyleneimine is 600~10000Da.
The pH value of deposition liquid should be maintained in the range of 6~10, it is preferred that should be maintained at 8~10 scope, and described is heavy
It is molten that hydrops is dissolved in phosphate buffer, Tris buffer solutions, carbonate buffer solution, NaOH by polyphenol monomer and polyamine monomers
Liquid, KOH solution or Na2CO3Solution and be made.
The selection of hydrophobic polyalcohol stephanoporate basement membrane for utilized thin film composite membranes cutoff performance and do not make significant difference, this is
Because the cutoff performance of utilized thin film composite membranes is mainly determined by its selectivity function cortex.But, the species of basement membrane, pore size pair
It is notable in the water flux influence of composite membrane because basement membrane aperture and pore passage structure to water by when obstruction it is different.
Preferably, polyalcohol stephanoporate basement membrane is polypropylene, polyethylene, Kynoar, polyether sulfone, polysulfones or polychlorostyrene second
The microfiltration membranes or milipore filter of alkene.It is logical with higher water using composite nanometer filtering film made from the polyalcohol stephanoporate basement membrane of this kind of structure
Amount and preferable rejection effect.
In step (2)：
Preferably, described crosslinking agent is glutaraldehyde and/or pyromellitic trimethylsilyl chloride.
Preferably, the concentration of described cross-linking agent solution is 1~10wt%, cross-linking reaction temperature is 20~80 DEG C, is handed over
It is 10~120 minutes to join the reaction time.
Present invention also offers the utilized thin film composite membranes reacted based on air liquid interface prepared by above-mentioned preparation method；The thin layer
Composite membrane can be applied to the fields such as nanofiltration, counter-infiltration, positive infiltration or seepage slope.
Compared with prior art, beneficial effects of the present invention are：
(1) hydrophobic, macropore microfiltration membranes may be selected in the interfacial polymerization mainly used compared to industrial quarters, the preparation method
As support basement membrane, the scope of application of thin-film composite membrane is effectively increased, and be conducive to the lifting of membrane flux；
(2) preparation method is simple, and controllability is strong；
(3) the stronger positive electricity of utilized thin film composite membranes surface lotus prepared, the preparation method of current lotus positive electricity composite membrane is less, this hair
Bright preparation method is a useful supplement for this field.
Brief description of the drawings
Fig. 1 is the schematic flow sheet of the preparation method of the present invention；
Fig. 2 is the principle schematic of the preparation method of the present invention；
Fig. 3 is the cross-section morphology figure (SEM) for the utilized thin film composite membranes that embodiment 1 is prepared.
Embodiment
The preparation method of the present invention, will be hydrophobic as shown in figure 1, be first according to certain proportional arrangement polyphenol/many amine aqueous solutions
Basement membrane swim in the surface of solution.After the reaction some time, it is crosslinked if basement membrane is placed in glutaraldehyde water solution
The dry time, that is, obtain utilized thin film composite membranes.
The mechanism that it reacts is as shown in Fig. 2 oxygen is spread downwards by air liquid interface, and the polyphenol oxidase in solution is formed
Quinoid, and then occur Michael additions or Schiff reaction with polyamines, polyphenol/many amine compounds enter one at air liquid interface
Step reaction, forms the membrane structure of crosslinking at the air liquid interface of polyalcohol stephanoporate basement membrane；Membrane structure is by being cross-linked to form cause
Close selectivity function cortex, so as to obtain described utilized thin film composite membranes.
Utilized thin film composite membranes prepared by the present invention are used for desalination, and salt rejection rate and water flux are two of evaluating combined film properties
Important parameter.Wherein, salt rejection rate is defined as：
Wherein, Cf represents the concentration of salt ion in before processing water；CpAfter expression processing in solution salt ion concentration.Water leads to
The definition of amount is：Under the conditions of certain operating pressure, the volume of the water of per membrane area is passed through in the unit interval, its unit is
Lm-2h-1, formula is：
Wherein, V represents the volume of the solution passed through, and unit is L；A represents effective membrane area, and unit is m2；When t is represented
Between, unit is h.
Embodiment 1
From dopamine and polyethyleneimine (weight average molecular weight 600) as Polyphenols and many amine monomers, by dopamine
It is dissolved in polyethyleneimine according to 4: 1 mass concentration ratio in Tris-HCl cushioning liquid, wherein dopamine and polyethylene
The concentration of imines is respectively 2g/L and 0.5g/L.
Polyvinylidene fluoride microporous film is swum in into deposition liquid surface to deposit 4 hours under the conditions of 20 DEG C.
Finally the film prepared is put into 10% glutaraldehyde solution in crosslinking 2 hours at 70 DEG C.
Most cleaned afterwards through water, dry after obtain utilized thin film composite membranes.
The utilized thin film composite membranes cross-section morphology figure (SEM) of preparation is as shown in figure 1, the thickness of its epilamellar selectivity function cortex
Spend for 60nm or so.Its water flux is 53.3Lm-2h-1, magnesium chloride salt rejection rate is 95.1%.
Embodiment 2~4
Polyvinylidene fluoride microporous film is replaced with to polypropylene, polyethylene, polyvinyl chloride microfiltration membranes respectively, remaining condition is with real
Apply example 1.
Embodiment 5~7
The weight average molecular weight of the polyethyleneimine of selection is respectively 1200Da, 1800Da and 10000Da, and remaining condition is with real
Apply example 1.
Embodiment 8~13
Dopamine is replaced with to DOPA, catechol, norepinephrine, pyrogallol, tannic acid, Tea Polyphenols respectively,
Remaining condition be the same as Example 1.
Embodiment 14~21
Polyethyleneimine is replaced with to chitosan, polyallylamine, diethylenetriamine, triethylene tetramine, triethylamine, piperazine respectively
Piperazine, m-phenylene diamine (MPD), p-phenylenediamine, remaining condition be the same as Example 1.
Embodiment 22~25
From dopamine and polyethyleneimine (weight average molecular weight 600) as phenols and amine monomers, by dopamine and poly-
Aziridine is dissolved in Tris-HCl cushioning liquid according to 2: 1,1: 1,1: 2,1: 4 mass concentration ratio, wherein dopamine
Concentration be 2g/L, the concentration of polyethyleneimine is respectively 1g/L, 2g/L, 4g/L, 8g/L.Remaining condition be the same as Example 1.
Embodiment 26~33
From dopamine and polyethyleneimine (weight average molecular weight 600) as Polyphenols and many amine monomers, by dopamine
It is dissolved in polyethyleneimine according to 4: 1 mass concentration ratio in Tris-HCl cushioning liquid, wherein dopamine and polyethylene
The concentration of imines is respectively 2g/L and 0.5g/L.
By polyvinylidene fluoride microporous film swim in deposition liquid surface 10,30,40,50,60,70,80,90 DEG C of conditions sink
Product 4 hours.
Finally the film prepared is put into 10% glutaraldehyde solution in crosslinking 2 hours at 70 DEG C.
Most cleaned afterwards through water, dry after obtain utilized thin film composite membranes.
Embodiment 34~37
From dopamine and polyethyleneimine (weight average molecular weight 600) as Polyphenols and many amine monomers, by dopamine
It is dissolved in polyethyleneimine according to 4: 1 mass concentration ratio in Tris-HCl cushioning liquid, wherein dopamine and polyethylene
The concentration of imines is respectively 2g/L and 0.5g/L.
By polyvinylidene fluoride microporous film swim in deposition liquid surface deposit 0.5 under the conditions of 20 DEG C, 1,2,3 hours.
Finally the film prepared is put into 10% glutaraldehyde solution in crosslinking 2 hours at 70 DEG C.
Most cleaned afterwards through water, dry after obtain utilized thin film composite membranes.
Claims (10)
1. a kind of preparation method for the utilized thin film composite membranes reacted based on air liquid interface, it is characterised in that：Comprise the following steps：
(1) hydrophobic polyalcohol stephanoporate basement membrane is swum in into deposition liquid surface, 0.1~12 is reacted under the conditions of 10~90 DEG C small
When, membrane structure is formed on the polyalcohol stephanoporate basement membrane at air liquid interface；
Described deposition liquid is the polyphenol monomer of pH=6~10 and the solution of polyamine monomers；
Described polyphenol monomer is dopamine, DOPA, catechol, norepinephrine, pyrogallol, tannic acid, Tea Polyphenols
At least one of；
Described polyamine monomers are polyethyleneimine, polyallylamine hydrochlorides, chitosan, diethylenetriamine, triethylene tetramine, three
At least one of ethamine, piperazine, m-phenylene diamine (MPD), p-phenylenediamine；
(2) reacted polyalcohol stephanoporate basement membrane in step (1) is placed in cross-linking reaction in cross-linking agent solution, polyalcohol stephanoporate base
Membrane structure is cross-linked into selectivity function cortex on film, obtains the described utilized thin film composite membranes reacted based on air liquid interface.
2. the preparation method of the utilized thin film composite membranes according to claim 1 reacted based on air liquid interface, it is characterised in that：
Hydrophobic polyalcohol stephanoporate basement membrane is swum in into deposition liquid surface, reacted 1~2 hour under the conditions of 40~60 DEG C.
3. the preparation method of the utilized thin film composite membranes according to claim 1 reacted based on air liquid interface, it is characterised in that：
The concentration of described cross-linking agent solution be 1~10wt%, cross-linking reaction temperature be 20~80 DEG C, cross-linking reaction time be 10~
120 minutes.
4. the preparation method of the utilized thin film composite membranes according to claim 1 reacted based on air liquid interface, it is characterised in that：
In described deposition liquid, the concentration of polyphenol monomer and polyamine monomers is 1g/L~10g/L.
5. the preparation method of the utilized thin film composite membranes according to claim 4 reacted based on air liquid interface, it is characterised in that：
In described deposition liquid, the mass ratio of polyphenol monomer and polyamine monomers is 1: 0.25~4.
6. the preparation method of the utilized thin film composite membranes according to claim 1 reacted based on air liquid interface, it is characterised in that：
In described deposition liquid, described polyphenol monomer is dopamine and/or o-phenylenediamine, and described polyamine monomers are polyethyleneimine
Amine；
The concentration of polyphenol monomer and polyamine monomers is 2g/L~4g/L；
The mass ratio of polyphenol monomer and polyamine monomers is 1: 0.5~1.
7. according to the preparation method of the utilized thin film composite membranes according to claim 6 reacted based on air liquid interface, its feature exists
In：The weight average molecular weight of described polyethyleneimine is 600~10000Da.
8. according to the preparation method of the utilized thin film composite membranes according to claim 1 reacted based on air liquid interface, its feature exists
In：It is molten that described deposition liquid is dissolved in phosphate buffer, Tris buffer solutions, carbonate buffer by polyphenol monomer and polyamine monomers
Liquid, NaOH solution, KOH solution or Na2CO3Solution and be made.
9. a kind of utilized thin film composite membranes reacted based on air liquid interface, it is characterised in that as described in any one of claim 1~8
Preparation method is made.
10. a kind of utilized thin film composite membranes according to claim 9 reacted based on air liquid interface are in nanofiltration, counter-infiltration, just oozing
Application in saturating or seepage slope.
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