CN107789988A - Hollow fiber composite membrane of ultra-thin active layer and preparation method thereof - Google Patents
Hollow fiber composite membrane of ultra-thin active layer and preparation method thereof Download PDFInfo
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- CN107789988A CN107789988A CN201610789320.9A CN201610789320A CN107789988A CN 107789988 A CN107789988 A CN 107789988A CN 201610789320 A CN201610789320 A CN 201610789320A CN 107789988 A CN107789988 A CN 107789988A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/02—Hollow fibre modules
- B01D63/021—Manufacturing thereof
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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
- 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
-
- 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
- B01D69/122—Separate manufacturing of ultra-thin membranes
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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
- B01D71/08—Polysaccharides
- B01D71/12—Cellulose derivatives
- B01D71/14—Esters of organic acids
- B01D71/16—Cellulose acetate
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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
- B01D71/26—Polyalkenes
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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
- B01D71/30—Polyalkenyl halides
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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
- B01D71/58—Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
- B01D71/62—Polycondensates having nitrogen-containing heterocyclic rings in the main chain
- B01D71/64—Polyimides; Polyamide-imides; Polyester-imides; Polyamide acids or similar polyimide precursors
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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
- B01D2323/00—Details relating to membrane preparation
- B01D2323/02—Hydrophilization
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- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention belongs to functional high polymer material field, and in particular to a kind of hollow fiber composite membrane of ultra-thin active layer and preparation method thereof.The hollow fiber composite membrane is using the high-molecular porous film that inner surface and/or outer surface have dense layer surface as basement membrane, and the hydrophilic material of selectivity function is loaded with the outer wall of basement membrane as active separating layer.Active separating layer thickness is 0.2 1um.The present invention also provides its preparation method.Preparation process of the present invention is simple, easily operated；Composite membrane has high selectivity；Composite membrane preparation cost is low, is easily achieved industrialization production.The active separating layer thickness ultrathin of composite film surface, usage amount is seldom, being capable of industrialization production；The ultra-thin fine and close zero defect of active layer of the hollow fiber composite membrane, preparation method is simple, and thickness is controllable.
Description
Technical field
The invention belongs to functional high polymer material field, and in particular to a kind of hollow fiber composite membrane of ultra-thin active layer and
Its preparation method.
Background technology
Gaseous jet simulation be it is a kind of dissolved using each component in gas mixture in dense film, the difference of diffusion it is real
The process of existing gas separation.In order to improve permeability of the membrane energy, composite membrane is generally prepared as, i.e., one layer is covered on micropore basal membrane
Ultra-thin top layer with nano aperture, the centrifugation of composite membrane are mainly or entirely determined by ultra-thin cortex.Composite membrane cortex is most
It is thin to reach several nanometers, thus film possesses high flux.In addition, composite membrane top layer is ultra-thin, i.e., material amounts are few, Ke Yixuan
Select excellent performance, expensive high polymer material as composite membrane cortex.
The NS-300 that the research of composite membrane can trace back to JE Cadotte at the end of the seventies (US Pat.4812270) earliest is answered
Film exploitation is closed, using polysulfones as support basement membrane, is successfully made by interfacial polymerization, weak solution cladding process or Plasma Polymerization etc.
It is standby gone out ultra-thin composite membrane.The composite membrane of preparation will meet：Cortex is very thin；Separating property is good；Cortex is combined enough jails with basement membrane
It is Gu difficult for drop-off.Canadian Zenon companies (US Patent No.5,472,607, US2003/009827 5A1, WO 00/
78437 A1) the polymer composite hollow fibre microporous barrier for preparing, its thickness be 0.01~0.1mm, and film thickness is partially thick, unrealized
It is ultra-thin；Although the water flux of film is significantly improved, polymer separation film combined with basement membrane it is poor, film is carried out it is reverse
In cleaning process, polymer separation film is easily fallen off, and peeling resistance is low.United States Patent (USP) (US Pat.4857080) reports
For isolating and purifying " sandwich diaphragm for using silicon rubber-palldium alloy-polymer micro supporting layer " of hydrogen, although reducing
The defects of palldium alloy, but the infiltration rate of composite membrane reduces, thus the separating property of film is relatively low.T.A.Peters etc.
[T.A.Peters, C.H.S.Poeth, N.E.Benes, H.C.W.M.Buijs, F.F.Vercauteren,
(2006) 42-50 of J.T.F.Keurentjes.Journal of Membrane Science 276] report doughnut pottery
The polyvinyl alcohol permeation vaporization film of porcelain support, uses with 300nm macropore inorganic ceramic doughnut supporters, uses boehmite solution
Modify 4 times and form γ-Al2O3Intermediate layer, finally prepare the thin and flawless film layers of aperture 4nm, manufacture craft mistake
In complexity.
Existing gas separation membrane generally existing infiltration capacity is low, separation factor is small and the shortcomings of bad mechanical strength.With densification
For the hollow fiber polymer membrane material of cortex due to its hydrophobicity, separating property is poor, therefore is modified introducing with choosing
The hydrophilic material of sexual function is selected as active separating layer, the compactness of membrane surface is added, greatly improves composite membrane
Separation, permeance property.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of hollow fiber composite membrane of ultra-thin active layer,
The ultra-thin fine and close zero defect of active layer of the hollow fiber composite membrane, preparation method is simple, and thickness is controllable, and the present invention also provides its system
Preparation Method.
The hollow fiber composite membrane of ultra-thin active layer of the present invention, the hollow fiber composite membrane be with inner surface and/
Or it is basement membrane that outer surface, which has the high-molecular porous film of dense layer surface, and the hydrophilic of selectivity function is loaded with the outer wall of basement membrane
Property material is as active separating layer.
Wherein：
Active separating layer thickness is 0.2-1um.
High-molecular porous film is polysulfones, polyether sulfone, polyacrylonitrile, polypropylene, acetate fiber, polyimides or polyvinyl chloride
Any one in hollow-fibre membrane, polysulfones, polyether sulfone, polyacrylonitrile, polypropylene, acetate fiber, polyamides used in the present invention
Imines, polyvinyl chloride are the product that inner surface and/or outer surface have dense layer surface, purchased in market.
The hydrophilic material of selective function is in perfluorinated sulfonic resin, polyacrylic acid, polyvinyl alcohol or chitosan
Any one.
The present invention adds one layer of ultra-thin active layer material on the basement membrane outer wall with dense layer surface, reduces hollow fibre
The defects of Wiki hymeniderm layer, improve the selectivity of composite membrane.
The preparation method of the hollow fiber composite membrane of high selectivity ultra-thin active layer of the present invention, including following step
Suddenly：
(1) high-molecular porous film with dense layer surface is dipped in absolute ethyl alcohol and soaked, then taken out air-dried；
(2) hydrophilic material of selective function is dissolved in suitable solvent, stirring is completely dissolved it, prepares matter
Amount concentration is 3%-50%, and viscosity is 10-500mPas solution, that is, obtains preparation liquid；
(3) after preparation liquid standing and defoaming, preparation liquid is vertically dipped in by obtained high-molecular porous film is handled through step (1)
In, then by hollow-fibre membrane, using speed as 0.10-1.00m/s speed, the vertical at the uniform velocity lifting from preparation liquid comes out, and stands
Dry, obtain composite membrane；
(4) the composite membrane heating, drying that step (3) is prepared, obtains the hollow fiber composite membrane of ultra-thin active layer.
Solvent uses one or more of mixing in distilled water, ethanol, propyl alcohol, normal propyl alcohol, isopropanol or acetic acid.
The hydrophilic material of selective function and the mass ratio of solvent are 3-50：97-50；Preferably 3-20：97-80.
Preferably, the preparation method of the hollow fiber composite membrane of ultra-thin active layer of the present invention, comprises the following steps：
(1) basement membrane pre-processes
High-molecular porous basement membrane with dense layer surface is dipped in 10-30min in absolute ethyl alcohol, it is therefore an objective to remove fiber base
Organic impurities that film surface may be contained etc., then take out be placed on cleaning environment at least 24h make its natural air drying.
(2) preparation liquid is configured
The hydrophilic material of selective function is dissolved in suitable solvent, stirring is completely dissolved it, prepares quality
Concentration is 3%-50%, and viscosity is 10-500mPas solution；Preferred mass concentration is 3%-20%, viscosity 10-
200mPas solution, solution remove the impurity in solution by porous membrane press filtration purifying, that is, obtain preparation liquid.
(3) compound film preparation
After preparation liquid standing and defoaming, still preparation liquid is vertically dipped in by obtained high-molecular porous film is handled through step (1)
Middle stop 30s, then hollow-fibre membrane is vertically at the uniform velocity lifted out with the speed that speed is 0.10-1.00m/s from preparation liquid
Come, standing is dried；The preferred 0.10-0.50m/s of the basement membrane rate of pulling.
(4) composite membrane after air-drying is put into thermostatic drying chamber with vertical direction, 1-24h is being dried at 20-150 DEG C
The solvent in preparation liquid is removed, obtains the hollow fiber composite membrane of ultra-thin active layer.
The hollow fiber composite membrane of ultra-thin active layer of the present invention can be used for dehumidification of gas, especially suitable for natural
Gas, air and the dehydration of other industrial gasses.
In summary, the present invention has advantages below：
1st, preparation process is simple, easily operated.By modulating selective work(in preparation liquid on doughnut basement membrane outer wall
Content, viscosity, the rate of pulling and the drying condition of energy material carry out the thickness of regulation activity separating layer, and successfully obtaining ultrathin can
The hollow fiber composite membrane of control.
2nd, the basement membrane selection kind of composite membrane is more.High-molecular porous film with dense layer surface is polysulfones, polyether sulfone, gathered
Any one in acrylonitrile, polypropylene, acetate fiber, polyimides or PVC hollow fiber membrane, is not limited to certain
The basement membrane of certain material species, application are wide.
3rd, selectivity function material variation.Selectivity function material can be perfluorinated sulfonic resin, polyacrylic acid, poly- second
Any one in enol or chitosan.According to being actually needed in varied situations, required function material regulation and control thickness is selected
Demand parameter.
4th, composite membrane has peeling resistance height.The hollow fiber composite membrane of preparation carries out drying and watering cycle experiment, and dry and wet is followed
After ring 10-30 times, the cortex of film surface does not come off, and tunica fibrosa is also without being broken.
5. prepared by composite membrane, cost is low, is easily achieved industrialization production.The active separating layer thickness ultrathin of composite film surface,
Usage amount is seldom, being capable of industrialization production.
6. the ultra-thin fine and close zero defect of the active layer of the hollow fiber composite membrane, preparation method is simple, and thickness is controllable.
Brief description of the drawings
Fig. 1 is the SEM test charts for the hollow fiber composite membrane that the embodiment of the present invention 1 is prepared；
Fig. 2 is the SEM test charts for the hollow fiber composite membrane that the embodiment of the present invention 2 is prepared.
Embodiment
With reference to embodiment, the present invention will be further described.
Embodiment 1
1. a pair ps hollow fiber uf membrane surface with dense layer surface pre-processes：
Ps hollow fiber uf membrane with dense layer surface is placed in absolute ethyl alcohol and soaks 10min, it is therefore an objective to removes fiber
Organic impurities that film surface may be contained etc., then take out be placed on cleaning environment at least 24h make its natural air drying.
2. configure preparation liquid：
First, it is 80 perfluorinated sulfonic resin powder to be added into ethanol and distilled water mass ratio：In 20 dicyandiamide solution, stir
Mixing is completely dissolved it, and it is 5% to prepare mass concentration, viscosity 10mPas solution.Solution purifies by porous membrane press filtration
The impurity in solution is removed, that is, obtains preparation liquid.
3rd, compound film preparation
(1) after preparation liquid standing and defoaming, still film is vertically dipped in by obtained high-molecular porous film is handled through step (1)
30s is stopped in liquid, is then that 0.10m/s vertical at the uniform velocity liftings from solution come out with speed by hollow-fibre membrane, in cleaning
10min is stood in space, makes the active separating layer natural air drying formed in membrane surface.
(2) composite membrane after air-drying is put into thermostatic drying chamber with vertical direction, 1h is dried at 120 DEG C and removes film
Solvent in liquid, obtain the hollow fiber composite membrane of ultra-thin active layer.
To the hollow fiber composite membrane that embodiment 1 is prepared in liquid N2In quench it is disconnected, after metal spraying carry out SEM tests, test
As a result Fig. 1 is seen, the thickness of observation film section active separating layer is 0.3um, and thickness ultrathin is controllable.
Hollow fiber composite membrane that embodiment 1 is prepared carries out drying and watering cycle experiment, after drying and watering cycle 30 times, film surface
Cortex do not come off, tunica fibrosa is also without being broken.Thus, the better mechanical property of composite membrane is not torn, stripper-resistance
Can be also preferable.
Embodiment 2
1. a pair polyacrylonitrile hollow fiber membrane surface with dense layer surface pre-processes：
Polyacrylonitrile hollow fiber membrane with dense layer surface is placed in absolute ethyl alcohol and soaks 30min, it is therefore an objective to is removed
Organic impurities that tunica fibrosa surface may be contained etc., then take out be placed on cleaning environment at least 24h make its natural air drying.
2. configure preparation liquid：
First, it is 90 perfluorinated sulfonic resin powder to be added into ethanol and distilled water mass ratio：In 10 dicyandiamide solution, stir
Mixing is completely dissolved it, and it is 10% to prepare mass concentration, viscosity 100mPas solution.Solution is pure by porous membrane press filtration
The impurity in solution is eliminated, that is, obtains preparation liquid.
3rd, compound film preparation
(1) after preparation liquid standing and defoaming, still film is vertically dipped in by obtained high-molecular porous film is handled through step (1)
30s is stopped in liquid, is then that 0.25m/s vertical at the uniform velocity liftings from solution come out with speed by hollow-fibre membrane, in cleaning
10min is stood in space, makes the active separating layer natural air drying formed in membrane surface.
(2) composite membrane after air-drying is put into thermostatic drying chamber with vertical direction, 1h is dried at 150 DEG C and removes film
Solvent in liquid, obtain the hollow fiber composite membrane of ultra-thin active layer.
To the hollow fiber composite membrane that embodiment 1 is prepared in liquid N2In quench it is disconnected, after metal spraying carry out SEM tests, test
As a result Fig. 2 is seen, the thickness of observation film section active separating layer is 0.5um, and thickness ultrathin is controllable.
Hollow fiber composite membrane that embodiment 2 is prepared carries out drying and watering cycle experiment, after drying and watering cycle 30 times, film surface
Cortex do not come off, tunica fibrosa is also without being broken.Thus, the better mechanical property of composite membrane is not torn, stripper-resistance
Can be also preferable.
Claims (7)
- A kind of 1. hollow fiber composite membrane of ultra-thin active layer, it is characterised in that：The hollow fiber composite membrane be with inner surface and/ Or it is basement membrane that outer surface, which has the high-molecular porous film of dense layer surface, and the hydrophilic of selectivity function is loaded with the outer wall of basement membrane Property material is as active separating layer.
- 2. the hollow fiber composite membrane of ultra-thin active layer according to claim 1, it is characterised in that：Active separating layer thickness For 0.2-1um.
- 3. the hollow fiber composite membrane of ultra-thin active layer according to claim 1, it is characterised in that：High-molecular porous film is It is any one in polysulfones, polyether sulfone, polyacrylonitrile, polypropylene, acetate fiber, polyimides or PVC hollow fiber membrane Kind.
- 4. the hollow fiber composite membrane of ultra-thin active layer according to claim 1, it is characterised in that：Selective function Hydrophilic material is any one in perfluorinated sulfonic resin, polyacrylic acid, polyvinyl alcohol or chitosan.
- 5. a kind of preparation method of the hollow fiber composite membrane of any described ultra-thin active layers of claim 1-4, its feature exist In：Comprise the following steps：(1) high-molecular porous film with dense layer surface is dipped in absolute ethyl alcohol and soaked, then taken out air-dried；(2) hydrophilic material of selective function is dissolved in suitable solvent, stirring is completely dissolved it, and it is dense to prepare quality It is 10-500mPas solution to spend for 3%-50%, viscosity, that is, obtains preparation liquid；(3) after preparation liquid standing and defoaming, vertically it is dipped in obtained high-molecular porous film is handled through step (1) in preparation liquid, so By hollow-fibre membrane, using speed as 0.10-1.00m/s speed, the vertical at the uniform velocity lifting from preparation liquid is come out afterwards, and standing is dried, Obtain composite membrane；(4) the composite membrane heating, drying that step (3) is prepared, obtains the hollow fiber composite membrane of ultra-thin active layer.
- 6. the preparation method of the hollow fiber composite membrane of ultra-thin active layer according to claim 5, it is characterised in that：Solvent Mixed using the one or more in distilled water, ethanol, propyl alcohol, normal propyl alcohol, isopropanol or acetic acid.
- 7. the preparation method of the hollow fiber composite membrane of ultra-thin active layer according to claim 5, it is characterised in that：There is choosing The mass ratio of the hydrophilic material and solvent of selecting sexual function is 3-50：97-50.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108854602A (en) * | 2018-06-28 | 2018-11-23 | 江苏泓膜业科技有限公司 | A kind of enhanced hollow fiber ultrafiltration membrane and preparation method thereof |
| CN110975646A (en) * | 2019-12-18 | 2020-04-10 | 中海油节能环保服务有限公司 | Preparation method of hollow fiber composite membrane for separating carbon dioxide in mixed gas |
| CN111001307A (en) * | 2019-12-03 | 2020-04-14 | 广西大学 | Preparation method of composite film with replaceable active layer |
| CN112546875A (en) * | 2020-11-30 | 2021-03-26 | 江苏厚生新能源科技有限公司 | Water treatment multilayer composite membrane with ceramic coating and preparation process thereof |
| WO2021258130A1 (en) * | 2020-06-23 | 2021-12-30 | Commonwealth Scientific And Industrial Research Organisation | Dual-layer membrane |
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