CN107789986A - Enhanced hollow fiber ultrafiltration membrane and preparation method thereof - Google Patents
Enhanced hollow fiber ultrafiltration membrane and preparation method thereof Download PDFInfo
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- CN107789986A CN107789986A CN201610782462.2A CN201610782462A CN107789986A CN 107789986 A CN107789986 A CN 107789986A CN 201610782462 A CN201610782462 A CN 201610782462A CN 107789986 A CN107789986 A CN 107789986A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
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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
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
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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
- B01D69/08—Hollow fibre membranes
-
- 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
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
-
- 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
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/36—Polytetrafluoroethene
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- 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 enhanced hollow fiber ultrafiltration membrane and preparation method thereof.There is the polymeric hollow fiber of microcellular structure as basement membrane using surface, the hydrophilic material of selectivity function is coated with membrane surface, the hydrophilic material forms flawless dense layer surface structure as active separating layer while penetrating into basement membrane micropore in membrane surface.The thickness of active separating layer is 0.3 1um.The present invention also provides its preparation method.Preparation process is simple, easily operated；Milipore filter high mechanical strength；Milipore filter peel strength is high；Ultrafiltration Membrane Separation Character is high；Preparation cost is low, is easily achieved industrialization production.
Description
Technical field
The invention belongs to functional high polymer material field, and in particular to a kind of enhanced hollow fiber ultrafiltration membrane and its preparation
Method.
Background technology
Membrane separation technique have simple to operate, cost is low, without phase transformation, it is quick, save the energy and reduce the ability of pollutant,
Thus it is widely used in the fields such as water process, power industry, biomedical technology and food.During UF membrane use,
Due to the contamination resistance and bad mechanical strength of film, the large-scale application in water treatment field has been had a strong impact on.
The shortcomings that in order to overcome membrane separation technique to exist, mainly by improving the anti-soil of film to film modified increase hydrophily
Metachromia energy, the mechanical strength that the structure of composite membrane of dense layer surface improves film is formed by being coated on surface.United States Patent (USP) (US
Pat.2006177404) base is improved by crosslinking effect in pvdf membrane surface coating polymethyl vinyl ether (PVME) layer
The hydrophily of film, hydrophilic PVDF hyperfiltration/microfiltration film is prepared.By coating the structure of composite membrane of cortex outside pvdf membrane,
The mechanical strength of film can be improved.Chinese patent (the patent No.：201110138434.4) disclose hydrophilic PVDF doughnut
The preparation method of composite membrane, using the method that amphipathic copolymer is blended in casting solution, doughnut is introduced in preparation process
Supporting role of the pipe as PVDF, the hydrophily and mechanical strength of film are improved, pvdf membrane coating layer thickness is 0.1-0.4mm, thick
Degree is not thin enough.Chinese patent (201410690025.9) discloses a kind of the glass-fiber reinforced of raising interfacial adhesion strength
PVDF hollow fiber composite membrane preparation methods, be to occur interface polymerization reaction in glass fibre and active film liquid, organic film with
Chemical bond form is combined with inorganic supporting body, and monomer polymer uniform is embedded in fiberglass surfacing and pvdf membrane material,
Stable is present in hollow-fibre membrane, so that composite membrane peel strength, hydrophily and water flux all increase, prepares
Process is more complicated.
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 enhanced hollow fiber ultrafiltration membrane, this is hollow
The dense layer surface ultrathin of fiber ultrafiltration membrane is controllable, and preparation method is simple, good hydrophilic property, mechanical strength and peel strength
It is high；The present invention also provides its preparation method.
Enhanced hollow fiber ultrafiltration membrane of the present invention, using surface have the polymeric hollow fiber of microcellular structure as
Basement membrane, the hydrophilic material of selectivity function is coated with membrane surface, the hydrophilic material is being penetrated into basement membrane micropore
Flawless dense layer surface structure is formed as active separating layer in membrane surface simultaneously.
Wherein：The thickness of active separating layer is 0.3-1um.
Polymeric hollow fiber is in polysulfones, polyether sulfone, polypropylene, polyvinyl chloride, Kynoar or polytetrafluoroethylene (PTFE)
Any one.Polysulfones, polyether sulfone, polypropylene, polyvinyl chloride, Kynoar, polytetrafluoroethylene (PTFE) are with microcellular structure
And the commercially available prod without dense layer surface.
The hydrophilic material of selective function is that perfluorinated sulfonic resin, polyvinyl alcohol, polyvinylpyrrolidone or shell gather
Any one in sugar.
The selective function hydrophilic material of the present invention enters inside the hole of high-molecular porous basement membrane, adds basement membrane and skin
The adhesion of layer, the mechanical strength and peel strength for making milipore filter are improved；The introducing of selectivity function hydrophilic material
The hydrophily of milipore filter is added, the flux of milipore filter is greatly improved.
The preparation method of enhanced high flux hollow fibre milipore filter of the present invention, comprises the following steps：
(1) there is the polymeric hollow fiber of microcellular structure to be placed in absolute ethyl alcohol surface to soak, then take out nature
Air-dry；
(2) hydrophilic material of selective function is dissolved in suitable solvent, and stirring is completely dissolved it, prepares quality
Concentration is 2%-50%, and viscosity is 10-500mPas solution, that is, obtains preparation liquid；
(3) after preparation liquid standing and defoaming, will handle obtained surface through step (1) has the polymeric hollow of microcellular structure
Fiber basement membrane is vertically dipped in preparation liquid, is then 0.10-1.00m/s speed from preparation liquid using speed by doughnut basement membrane
In vertical at the uniform velocity lifting come out, standing is dried, and obtains composite membrane；
(4) the composite membrane heating, drying that step (3) is prepared, obtains enhanced hollow fiber ultrafiltration membrane.
Wherein：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 2-50：98-50；Preferably 3-20：97-80.
Described hollow fiber ultrafiltration membrane preparation process is simple, the controllable and fine and close zero defect of skin thickness.
Preferably, the preparation method of enhanced hollow fiber ultrafiltration membrane of the present invention, comprises the following steps：
(1) basement membrane pre-processes
The polymeric hollow fiber basement membrane that surface has microcellular structure is dipped in 10min in absolute ethyl alcohol, it is therefore an objective to remove
Organic impurities that fiber membrane surface may contain 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%-20%, and viscosity is 10-150mPas 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) ultrafiltration film preparation
After preparation liquid standing and defoaming, obtained surface will be handled through step (1) has the polymeric hollow of microcellular structure fine
Wiki film, which is vertically dipped in still preparation liquid, stops 30s, is then 0.10-0.50m/s from molten with speed by doughnut basement membrane
Vertical at the uniform velocity lifting comes out in liquid, the preferred 0.10-0.50m/s of the basement membrane rate of pulling, stands 15min in the space of cleaning, makes
In the active separating layer natural air drying that membrane surface is formed.
(4) milipore filter after air-drying is put into thermostatic drying chamber with vertical direction, 1-24h is dried at 20-200 DEG C and is removed
The solvent gone in preparation liquid, obtain enhanced hollow fiber ultrafiltration membrane.
Carry out drying and watering cycle experiment to the hollow fiber composite membrane for preparing of the present invention, after drying and watering cycle 10-30 times, film surface
Cortex does not come off, and tunica fibrosa is also without being broken.Thus, the better mechanical property of composite membrane is not torn, peeling resistance
Also it is preferable.
Enhanced hollow fiber ultrafiltration membrane of the present invention can be used for industry and municipal sewage treatment, drink water purifying
Or Treated sewage reusing.
In summary, the present invention has advantages below：
1st, preparation process is simple, easily operated.By changing the mass content of selectivity function material in preparation liquid, gluing
Degree, the rate of pulling and drying condition carry out the thickness of regulation activity separating layer, successfully obtain controllable hollow of ultra-thin active layer thickness
Fiber ultrafiltration membrane.
2nd, the basement membrane selection kind of milipore filter is more.It is poly- that surface, which has the polymeric hollow fiber basement membrane of microcellular structure,
Any one in sulfone, polyether sulfone, polyacrylonitrile, polypropylene, acetate fiber, polyimides or PVC hollow fiber membrane,
The basement membrane of certain certain material species is not limited to, application is wide.
3rd, selectivity function material variation.Selectivity function material can be perfluorinated sulfonic resin, polyvinyl alcohol, poly- second
Any one in alkene pyrrolidone or chitosan.According to being actually needed in varied situations, required function material is selected to adjust
Control thickness requirements index.
4th, milipore filter high mechanical strength.Ultra-thin dense layer surface is formed on basement membrane outer wall, improves the machinery of milipore filter
Intensity, prevent hollow fiber ultrafiltration membrane from producing fracture in use.
5th, milipore filter peel strength is high.Selectivity function hydrophilic material enters inside the hole of high-molecular porous basement membrane,
The adhesion of basement membrane and cortex is added, is improved the peel strength of milipore filter.
6th, preparation cost is low, is easily achieved industrialization production.The active separating layer thickness ultrathin of ultrafiltration membrane surface, usage amount
Seldom, it is possible to achieve industrialization production.
Brief description of the drawings
Fig. 1 is the SEM test charts for the enhanced hollow fiber ultrafiltration membrane that the embodiment of the present invention 1 is prepared；
Fig. 2 is the SEM test charts for the enhanced hollow fiber ultrafiltration 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. pair polysulfone hollow fibre basement membrane (have microcellular structure and do not have dense layer surface) pre-processes：
Ps hollow fiber uf membrane with microcellular structure and without dense layer surface is placed in absolute ethyl alcohol and soaked
10min, it is therefore an objective to remove organic impurities that tunica fibrosa surface may be contained etc., then take out and be placed in the environment of cleaning at least
24h makes its natural air drying.
2. configure preparation liquid：
First, it is 80 perfluorinated sulfonic resin powder to be added portionwise into ethanol and distilled water mass ratio on a small quantity：20 solvent
In system, stirring is completely dissolved it, and it is 5% to prepare mass concentration, viscosity 10mPas solution.Solution passes through porous membrane
Press filtration purifying removes the impurity in solution, that is, obtains preparation liquid.
3rd, ultrafiltration film preparation
(1) after preparation liquid standing and defoaming, will handle obtained surface through step (1) has the polymeric hollow of microcellular structure
Fiber basement membrane, which is vertically dipped in still preparation liquid, stops 30s, is then that 0.10m/s hangs down from solution with speed by hollow-fibre membrane
Directly at the uniform velocity lifting is come out, and 15min is stood in the space of cleaning, makes the active separating layer natural air drying formed in membrane surface.
(2) milipore filter after air-drying is put into thermostatic drying chamber with vertical direction, 2h is dried at 100 DEG C and removes film
Solvent in liquid, obtain enhanced hollow fiber ultrafiltration membrane.
The enhanced hollow fiber ultrafiltration membrane that embodiment 1 is prepared is in liquid N2In quench it is disconnected, after metal spraying carry out SEM surveys
Examination, test result are shown in Fig. 1, and the thickness of observation film section active separating layer is 0.45um, and thickness ultrathin is controllable.
The enhanced hollow fiber ultrafiltration membrane that embodiment 1 is prepared carries out drying and watering cycle experiment, drying and watering cycle 20 times
Afterwards, the cortex of film surface does not come off, and tunica fibrosa is also without being broken.Thus, the better mechanical property of milipore filter is not torn, is resisted
Stripping performance is also preferable.
Embodiment 2
1. pair polytetrafluoroethylhollow hollow fiber basement membrane (have microcellular structure and do not have dense layer surface) pre-processes：
Polytetrafluoroethylhollow hollow fiber membrane with microcellular structure and without dense layer surface is placed in absolute ethyl alcohol and soaked
Steep 10min, it is therefore an objective to remove organic impurities that tunica fibrosa surface may be contained etc., then take out and be placed in the environment of cleaning at least
24h makes its natural air drying.
2. configure preparation liquid：
First, it is 90 perfluorinated sulfonic resin powder to be added portionwise into ethanol and distilled water mass ratio on a small quantity：10 solvent
In system, stirring is completely dissolved it, and it is 10% to prepare mass concentration, viscosity 120mPas solution.Solution passes through porous filter
Mould filter purifying removes the impurity in solution, that is, obtains preparation liquid.
3rd, ultrafiltration film preparation
(1) after preparation liquid standing and defoaming, will handle obtained surface through step (1) has the polymeric hollow of microcellular structure
Fiber basement membrane, which is vertically dipped in still preparation liquid, stops 30s, is then that 0.30m/s hangs down from solution with speed by hollow-fibre membrane
Directly at the uniform velocity lifting is come out, and 15min is stood in the space of cleaning, makes the active separating layer natural air drying formed in membrane surface.
(2) milipore filter 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 enhanced high flux hollow fibre milipore filter.
The enhanced hollow fiber ultrafiltration membrane that embodiment 2 is prepared is in liquid N2In quench it is disconnected, after metal spraying carry out SEM surveys
Examination, test result are shown in Fig. 2, and the thickness of observation film section active separating layer is 0.60um, and thickness ultrathin is controllable.
The enhanced hollow fiber ultrafiltration membrane that embodiment 2 is prepared carries out drying and watering cycle experiment, drying and watering cycle 30 times
Afterwards, the cortex of film surface does not come off, and tunica fibrosa is also without being broken.Thus, the better mechanical property of milipore filter is not torn, is resisted
Stripping performance is also preferable.
Claims (7)
- A kind of 1. enhanced hollow fiber ultrafiltration membrane, it is characterised in that：There is the polymeric hollow fiber of microcellular structure with surface For basement membrane, the hydrophilic material of selectivity function is coated with membrane surface, the hydrophilic material is being penetrated into basement membrane micropore While in membrane surface form flawless dense layer surface structure as active separating layer.
- 2. enhanced hollow fiber ultrafiltration membrane according to claim 1, it is characterised in that：The thickness of active separating layer is 0.3-1um。
- 3. enhanced hollow fiber ultrafiltration membrane according to claim 1, it is characterised in that：Polymeric hollow fiber is poly- Any one in sulfone, polyether sulfone, polypropylene, polyvinyl chloride, Kynoar or polytetrafluoroethylene (PTFE).
- 4. enhanced hollow fiber ultrafiltration membrane according to claim 1, it is characterised in that：The hydrophily of selective function Material is any one in perfluorinated sulfonic resin, polyvinyl alcohol, polyvinylpyrrolidone or chitosan.
- A kind of 5. preparation method of any described enhanced hollow fiber ultrafiltration membranes of claim 1-4, it is characterised in that：Including Following steps：(1) there is the polymeric hollow fiber of microcellular structure to be placed in absolute ethyl alcohol surface to soak, then take out natural air drying；(2) hydrophilic material of selective function is dissolved in suitable solvent, and stirring is completely dissolved it, prepares mass concentration For 2%-50%, viscosity is 10-500mPas solution, that is, obtains preparation liquid；(3) after preparation liquid standing and defoaming, will handle obtained surface through step (1) has the polymeric hollow fiber of microcellular structure Basement membrane is vertically dipped in preparation liquid, then by doughnut basement membrane using speed as 0.10-1.00m/s speed from preparation liquid hang down Directly at the uniform velocity lifting is come out, and standing is dried, and obtains composite membrane；(4) the composite membrane heating, drying that step (3) is prepared, obtains enhanced hollow fiber ultrafiltration membrane.
- 6. the preparation method of enhanced hollow fiber ultrafiltration membrane according to claim 5, it is characterised in that：Solvent is using steaming One or more of mixing in distilled water, ethanol, propyl alcohol, normal propyl alcohol, isopropanol or acetic acid.
- 7. the preparation method of enhanced hollow fiber ultrafiltration membrane according to claim 5, it is characterised in that：Selective work( The hydrophilic material of energy and the mass ratio of solvent are 2-50：98-50.
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Cited By (6)
| 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 |
| CN112642301A (en) * | 2020-09-22 | 2021-04-13 | 迈博瑞生物膜技术（南通）有限公司 | PVDF/PS hollow fiber electropositive membrane for life straw |
| US20210354089A1 (en) * | 2020-05-18 | 2021-11-18 | Zhejiang Changxing Creflux Membrane Technology Co., Ltd. | Preparation method of high-performance mabr hollow fiber composite membrane |
| WO2021232649A1 (en) * | 2020-05-18 | 2021-11-25 | 浙江长兴求是膜技术有限公司 | Preparation method for high-performance mabr hollow fiber composite membrane |
| CN113766967A (en) * | 2019-05-30 | 2021-12-07 | 住友电气工业株式会社 | Hollow fiber membrane, filtration module, and drainage treatment device |
| CN114618321A (en) * | 2020-12-11 | 2022-06-14 | 中国科学院大连化学物理研究所 | Hollow fiber membrane, preparation and application in hydraulic oil degassing |
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Cited By (8)
| 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 |
| CN113766967A (en) * | 2019-05-30 | 2021-12-07 | 住友电气工业株式会社 | Hollow fiber membrane, filtration module, and drainage treatment device |
| CN113766967B (en) * | 2019-05-30 | 2024-02-23 | 住友电气工业株式会社 | Hollow fiber membrane, filtration module, and drainage treatment device |
| US20210354089A1 (en) * | 2020-05-18 | 2021-11-18 | Zhejiang Changxing Creflux Membrane Technology Co., Ltd. | Preparation method of high-performance mabr hollow fiber composite membrane |
| WO2021232649A1 (en) * | 2020-05-18 | 2021-11-25 | 浙江长兴求是膜技术有限公司 | Preparation method for high-performance mabr hollow fiber composite membrane |
| CN112642301A (en) * | 2020-09-22 | 2021-04-13 | 迈博瑞生物膜技术（南通）有限公司 | PVDF/PS hollow fiber electropositive membrane for life straw |
| CN114618321A (en) * | 2020-12-11 | 2022-06-14 | 中国科学院大连化学物理研究所 | Hollow fiber membrane, preparation and application in hydraulic oil degassing |
| CN114618321B (en) * | 2020-12-11 | 2023-07-25 | 中国科学院大连化学物理研究所 | Hollow fiber membrane, preparation and application thereof in hydraulic oil degassing |
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