CN106215725A - A kind of preparation method of multichannel hollow fiber nanofiltration membrane - Google Patents
A kind of preparation method of multichannel hollow fiber nanofiltration membrane Download PDFInfo
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- CN106215725A CN106215725A CN201610629858.3A CN201610629858A CN106215725A CN 106215725 A CN106215725 A CN 106215725A CN 201610629858 A CN201610629858 A CN 201610629858A CN 106215725 A CN106215725 A CN 106215725A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
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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
- B01D69/08—Hollow fibre 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
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/24—Mechanical properties, e.g. strength
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- Chemical Kinetics & Catalysis (AREA)
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- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The present invention relates to the preparation method of a kind of multichannel hollow fiber nanofiltration membrane, described method comprises the steps: step (1): by polymer, organic solvent, additive adds stirring in reactor by a certain percentage and forms the casting solution of stable homogeneous, spray through multichannel doughnut mould under air pressure drives after vacuum defoamation, enter in outer coagulating bath under the conditions of certain core flow velocity and air clearance and carry out inversion of phases, form multichannel doughnut basement membrane, take out after fully soaking under uniform temperature and dry, it is packaged in rustless steel assembly, two end plugs are with Cotton Gossypii blend compounds water-stop；Step (2): prepare certain density aqueous phase solution and oil-phase solution, first aqueous phase solution is injected multichannel endoporus and retains a period of time, employing keen draft purges, then oil-phase solution is injected and retain a period of time, empty gas flow purging a little, put into baking oven reaction, after taking-up, i.e. obtain multichannel hollow fiber nanofiltration membrane.The preparation method of the multichannel hollow fiber nanofiltration membrane of the present invention has higher toughness, higher intensity.
Description
Technical field
The present invention relates to the preparation method of a kind of multichannel hollow fiber nanofiltration membrane.Belong to technical field of membrane separation.
Background technology
Along with world today's science and technology and the continuous progress of civilization, isolation technics application in daily life is gradually extensive,
Membrane separation technique also receives more and more attention.Work is prepared in seawater and brackish water desalination and pure water, ultra-pure water except applying
In skill, in food, chemical industry, electronics, environmental protection, biology and medicine and other fields, membrane separation technique is widely used equally.
Nanofiltration (NF) is an important component part in membrane separation technique, pharmacy, metallurgy, decolouring, dyestuff reclaim and
The aspects such as concentration of juices suffer from being widely applied.The molecular cut off of NF membrane is more moderate (200-1000Da), is suitable for
Separate molecular weight at the small organic molecule of more than 200Da and multivalent salts (being equivalent to molecular dimension is about 1nm).Utilize difference
The NF membrane of molecular cut off, or can complete organic screening with its ultrafilter membrane combining PSPP, with
Time can also complete the separation between ion in conjunction with reverse osmosis membrane.The operation pressure of nanofiltration is low, typically 0.5-1.5MPa it
Between, and the operation pressure of reverse osmosis membrane is typically greater than 4.0MPa, therefore nanofiltration is also referred to as low pressure or loose reverse osmosis.Therefore,
In some cases, if using reverse osmosis membrane and NF membrane can meet process requirement, then can reduce if using NF membrane
Energy consumption, so that cost reduces.NF membrane is different to the rejection effect of different valence state ion, its to the rejection of ion by from
Sub-nature (such as valence charge number, ionic radius etc.) and the impact of membrane superficial tissue, typically to the rejection of monovalention relatively
Low, and high to the rejection of bivalence and high valence ion, such that it is able to the separation realized between monovalention and high valence ion.
Hollow fiber nanofiltration membrane has obvious flux and filling area advantage compared to the form such as Flat Membrane, tubular membrane,
But hollow fiber nanofiltration membrane is relatively low due to toughness and intensity, industrial scale application is very restricted.To this end, it is numerous
Researcher turns one's attention to the toughness of Hollow-fibre membranes material and the optimization of intensity and modification, by the industry of Hollow-fibre membranes material
Change application to become possible to.
Summary of the invention
It is an object of the invention to overcome above-mentioned deficiency, the multichannel doughnut proposing a kind of high intensity and high tenacity is received
Filter membrane, it is possible to scale is prepared and is applied to the fields such as the desalination of seawater and brackish water, sewage disposal, the preparation of ultra-pure water.
The present invention solves the technical scheme that the problems referred to above are used: the preparation side of a kind of multichannel hollow fiber nanofiltration membrane
Method, comprises the steps:
Step (1): polymer, organic solvent, additive are added by a certain percentage stirring in reactor and forms stable homogeneous
Casting solution, sprays through multichannel doughnut mould, at certain core flow velocity and sky after vacuum defoamation under air pressure drives
Enter under gas spacing condition in outer coagulating bath and carry out inversion of phases, form multichannel doughnut basement membrane, after fully soaking, take out one
Drying under fixed temperature, be packaged in rustless steel assembly, two end plugs are with Cotton Gossypii blend compounds water-stop.
Step (2): prepare certain density aqueous phase solution and oil-phase solution, first aqueous phase solution is injected multichannel endoporus
Retain a period of time, use keen draft purging, then oil-phase solution is injected and retain a period of time, empty gas flow purging a little,
Put into baking oven reaction, after taking-up, i.e. obtain multichannel hollow fiber nanofiltration membrane.
Described polymer is polyether sulfone or sulfonated polyether sulfone, and organic solvent is dimethyl acetylamide or N-crassitude
Ketone, additive is Polyethylene Glycol or polyvinylpyrrolidone.The mass ratio of polymer is 10-20%, the mass ratio of organic solvent
Example is 30-50%, and the mass ratio of additive is 40-60%.Casting solution mixing time in a kettle. is 18-24h, and vacuum takes off
A length of 12h during bubble, driving air pressure is 0.05-0.15MPa.Core liquid is water or ethanol, and flow velocity is 10-40ml/min, air clearance
For 0-20cm, outer coagulating bath is water or ethanol, and soak time is 24h, dries temperature and is 50-80 DEG C, and sealing glue is asphalt mixtures modified by epoxy resin
Fat glue.
Described aqueous phase solution is piperazine (PIP) solution, and solution concentration is 0.1-0.5%, and oil-phase solution is equal benzene three formyl
Chlorine (TMC) solution, solution concentration is 0.1-0.5%.The aqueous phase solution time of staying in multichannel doughnut basement membrane endoporus is
1-3min, the oil-phase solution time of staying in multichannel doughnut basement membrane endoporus is 10-20s.Described anti-in baking oven
Answering temperature to be 50-80 DEG C, the response time is 5-10min.
Compared with prior art, it is an advantage of the current invention that:
Multichannel hollow fiber nanofiltration membrane prepared by the present invention, mainly includes multichannel doughnut base membrane layer and ultra-thin nanofiltration
Layer.Multichannel doughnut basement membrane has higher toughness, higher intensity compared to single channel hollow-fibre membrane.Ultra-thin nanofiltration
Film layer is covered on multichannel doughnut inner hole wall, makes multichannel hollow fiber nanofiltration membrane retain the same of good salt rejection rate
Time possessed higher water flux.Present invention process is advantageously implemented continuous large-scale production, desalinates in seawater and brackish water, useless
The fields such as water process have a extensive future.
Detailed description of the invention
The detailed description of the invention of the preparation method of the present invention presented below a kind of multichannel hollow fiber nanofiltration membrane.
Embodiment 1:
24h shape is stirred in polyether sulfone, dimethyl acetylamide, Polyethylene Glycol are added reactor for 15%:40%:45% in mass ratio
Become the casting solution of stable homogeneous, spray through multichannel doughnut mould under 0.1MPa drives pressure after vacuum defoamation 12h, core
The flow velocity of liquid water is 10ml/min, and air clearance is 0cm, enters in outer solidification bath water and soaks 24h, takes out latter 50 DEG C and dry.
Embodiment 2
24h shape is stirred in polyether sulfone, dimethyl acetylamide, Polyethylene Glycol are added reactor for 15%:40%:45% in mass ratio
Become the casting solution of stable homogeneous, spray through multichannel doughnut mould under 0.1MPa drives pressure after vacuum defoamation 12h, core
The flow velocity of liquid water is 10ml/min, and air clearance is 5cm, enters in outer solidification bath water and soaks 24h, takes out latter 50 DEG C and dry.
Embodiment 3
24h shape is stirred in polyether sulfone, dimethyl acetylamide, Polyethylene Glycol are added reactor for 15%:40%:45% in mass ratio
Become the casting solution of stable homogeneous, spray through multichannel doughnut mould under 0.1MPa drives pressure after vacuum defoamation 12h, core
The flow velocity of liquid water is 10ml/min, and air clearance is 10cm, enters in outer solidification bath water and soaks 24h, takes out latter 50 DEG C and dry.
Embodiment 4:
(1) 24h is stirred in polyether sulfone, dimethyl acetylamide, Polyethylene Glycol being added reactor for 15%:40%:45% in mass ratio
Form the casting solution of stable homogeneous, spray through multichannel doughnut mould under 0.1MPa drives pressure after vacuum defoamation 12h,
The flow velocity of core liquid water is 10ml/min, and air clearance is 0cm, enters in outer solidification bath water and soaks 24h, takes out latter 50 DEG C and dry,
Being packaged in rustless steel assembly, two end plugs seal with Cotton Gossypii and with epoxide-resin glue.
(2) prepare PIP aqueous phase solution and the TMC oil-phase solution of 0.1% of 0.1%, aqueous phase solution is injected multichannel hollow
Fiber endoporus stops 2min, is injected by oil-phase solution and stop 15s after keen draft purging, and empty gas flow purging puts into baking oven 80 a little
DEG C reaction 8min, i.e. prepare multichannel hollow fiber nanofiltration membrane.
Embodiment 5:
(1) 24h is stirred in polyether sulfone, dimethyl acetylamide, Polyethylene Glycol being added reactor for 12%:42%:46% in mass ratio
Form the casting solution of stable homogeneous, spray through multichannel doughnut mould under 0.1MPa drives pressure after vacuum defoamation 12h,
The flow velocity of core liquid water is 10ml/min, and air clearance is 0cm, enters in outer solidification bath water and soaks 24h, takes out latter 50 DEG C and dry,
Being packaged in rustless steel assembly, two end plugs seal with Cotton Gossypii and with epoxide-resin glue.
(2) prepare PIP aqueous phase solution and the TMC oil-phase solution of 0.1% of 0.1%, aqueous phase solution is injected multichannel hollow
Fiber endoporus stops 2min, is injected by oil-phase solution and stop 15s after keen draft purging, and empty gas flow purging puts into baking oven 80 a little
DEG C reaction 8min, i.e. prepare multichannel hollow fiber nanofiltration membrane.
Embodiment 6:
(1) 24h is stirred in polyether sulfone, dimethyl acetylamide, Polyethylene Glycol being added reactor for 10%:40%:50% in mass ratio
Form the casting solution of stable homogeneous, spray through multichannel doughnut mould under 0.1MPa drives pressure after vacuum defoamation 12h,
The flow velocity of core liquid water is 10ml/min, and air clearance is 0cm, enters in outer solidification bath water and soaks 24h, takes out latter 50 DEG C and dry,
Being packaged in rustless steel assembly, two end plugs seal with Cotton Gossypii and with epoxide-resin glue.
(2) prepare PIP aqueous phase solution and the TMC oil-phase solution of 0.1% of 0.1%, aqueous phase solution is injected multichannel hollow
Fiber endoporus stops 2min, is injected by oil-phase solution and stop 15s after keen draft purging, and empty gas flow purging puts into baking oven 80 a little
DEG C reaction 8min, i.e. prepare multichannel hollow fiber nanofiltration membrane.
Embodiment 7:
(1) 24h is stirred in polyether sulfone, dimethyl acetylamide, Polyethylene Glycol being added reactor for 15%:40%:45% in mass ratio
Form the casting solution of stable homogeneous, spray through multichannel doughnut mould under 0.1MPa drives pressure after vacuum defoamation 12h,
The flow velocity of core liquid water is 10ml/min, and air clearance is 0cm, enters in outer solidification bath water and soaks 24h, takes out latter 50 DEG C and dry,
Being packaged in rustless steel assembly, two end plugs seal with Cotton Gossypii and with epoxide-resin glue.
(2) prepare PIP aqueous phase solution and the TMC oil-phase solution of 0.1% of 0.15%, aqueous phase solution is injected multichannel hollow
Fiber endoporus stops 2min, is injected by oil-phase solution and stop 15s after keen draft purging, and empty gas flow purging puts into baking oven 80 a little
DEG C reaction 8min, i.e. prepare multichannel hollow fiber nanofiltration membrane.
Embodiment 8:
(1) 24h is stirred in polyether sulfone, dimethyl acetylamide, Polyethylene Glycol being added reactor for 15%:40%:45% in mass ratio
Form the casting solution of stable homogeneous, spray through multichannel doughnut mould under 0.1MPa drives pressure after vacuum defoamation 12h,
The flow velocity of core liquid water is 10ml/min, and air clearance is 0cm, enters in outer solidification bath water and soaks 24h, takes out latter 50 DEG C and dry,
Being packaged in rustless steel assembly, two end plugs seal with Cotton Gossypii and with epoxide-resin glue.
(2) prepare PIP aqueous phase solution and the TMC oil-phase solution of 0.15% of 0.1%, aqueous phase solution is injected multichannel hollow
Fiber endoporus stops 2min, is injected by oil-phase solution and stop 15s after keen draft purging, and empty gas flow purging puts into baking oven 80 a little
DEG C reaction 8min, i.e. prepare multichannel hollow fiber nanofiltration membrane.
The test data such as table 1 below of multichannel doughnut basement membrane:
| Sample | External diameter (mm) | Water flux (L/m2.h) | Hot strength (MPa) |
| Embodiment 1 | 3.5 | 150 | 25 |
| Embodiment 2 | 3.6 | 165 | 22 |
| Embodiment 3 | 3.7 | 170 | 20 |
As can be seen from Table 1:
(1) water flux of multichannel doughnut basement membrane is relatively big, and basement membrane aperture belongs to ultrafiltration range.
(2) through the contrast of embodiment 1-3, the multichannel doughnut basement membrane of preparation is respectively provided with high hot strength, phase
Than single channel doughnut (usual hot strength < 5MPa), there is obvious strength advantage.
Multichannel hollow fiber nanofiltration membrane test result such as table 2 below:
As can be seen from Table 2:
(1) contrasting through embodiment 4-6, sodium chloride and magnesium sulfate are respectively provided with by three batch multichannel hollow fiber nanofiltration membranes of preparation
Higher removal efficiency, and the difference of casting solution proportioning has significant impact to film properties.
(2) contrasting through embodiment 4,7 and 8, three batches of NF membrane of preparation have the highest salt rejection rate, wherein embodiment equally
5 performances are optimal, and the concentration impact same on film properties of this explanation aqueous phase solution and oil-phase solution is notable.
(3) present invention process can form scale and prepares, and multichannel hollow fiber nanofiltration membrane intensity is high, and toughness is strong,
It is huge that seawater and brackish water desalination, sewage disposal and ultra-pure water such as prepare at the field application prospect.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
Member, without departing from the inventive concept of the premise, it is also possible to make some improvements and modifications, these improvements and modifications also should be regarded as
In protection scope of the present invention.
Claims (8)
1. the preparation method of a multichannel hollow fiber nanofiltration membrane, it is characterised in that: described method comprises the steps:
Step (1): polymer, organic solvent, additive are added by a certain percentage stirring in reactor and forms stable homogeneous
Casting solution, sprays through multichannel doughnut mould, at certain core flow velocity and sky after vacuum defoamation under air pressure drives
Enter under gas spacing condition in outer coagulating bath and carry out inversion of phases, form multichannel doughnut basement membrane, after fully soaking, take out one
Drying under fixed temperature, be packaged in rustless steel assembly, two end plugs are with Cotton Gossypii blend compounds water-stop；
Step (2): prepare certain density aqueous phase solution and oil-phase solution, first injects aqueous phase solution multichannel endoporus and retains
A period of time, using keen draft purging, then injected by oil-phase solution and retain a period of time, empty gas flow purging, puts into a little
In baking oven, reaction, i.e. obtains multichannel hollow fiber nanofiltration membrane after taking-up.
The preparation method of a kind of multichannel hollow fiber nanofiltration membrane the most according to claim 1, it is characterised in that: described poly-
Compound is polyether sulfone or sulfonated polyether sulfone, and organic solvent is dimethyl acetylamide or N-Methyl pyrrolidone, and additive is poly-second
Glycol or polyvinylpyrrolidone.
The preparation method of a kind of multichannel hollow fiber nanofiltration membrane the most according to claim 1, it is characterised in that: polymer
Mass ratio be 10-20%, the mass ratio of organic solvent is 30-50%, and the mass ratio of additive is 40-60%.
The preparation method of a kind of multichannel hollow fiber nanofiltration membrane the most according to claim 1, it is characterised in that: casting solution
Mixing time in a kettle. is 18-24h, a length of 12h during vacuum defoamation, and driving air pressure is 0.05-0.15MPa.
5. according to the preparation method of a kind of multichannel hollow fiber nanofiltration membrane described in claims 1, it is characterised in that: described
Core liquid be water or ethanol, flow velocity is 10-40ml/min, and air clearance is 0-20cm, and outer coagulating bath is water or ethanol, during immersion
Between be 24h, dry temperature and be 50-80 DEG C, sealing glue is epoxide-resin glue.
6. according to the preparation method of a kind of multichannel hollow fiber nanofiltration membrane described in claims 1, it is characterised in that: aqueous phase
Solution is piperazine (PIP) solution, and solution concentration is 0.1-0.5%, and oil-phase solution is pyromellitic trimethylsilyl chloride (TMC) solution, and solution is dense
Degree is 0.1-0.5%.
7. according to the preparation method of a kind of multichannel hollow fiber nanofiltration membrane described in claims 1, it is characterised in that: aqueous phase
The solution time of staying in multichannel doughnut basement membrane endoporus is 1-3min, and oil-phase solution is at multichannel doughnut basement membrane
The time of staying in endoporus is 10-20s.
8. according to the preparation method of a kind of multichannel hollow fiber nanofiltration membrane described in claims 1, it is characterised in that: described
Reaction temperature in baking oven is 50-80 DEG C, and the response time is 5-10min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108126528A (en) * | 2017-08-30 | 2018-06-08 | 江苏向阳科技有限公司 | A kind of preparation method of double-layer hollow fiber NF membrane |
| CN110523281A (en) * | 2019-08-26 | 2019-12-03 | 北京清鸥科技有限公司 | A kind of polyamide doughnut receives the preparation method of permeable membrane |
| CN114073900A (en) * | 2020-08-13 | 2022-02-22 | 中国科学院青岛生物能源与过程研究所 | Method for preparing hollow fiber membrane with one sealed end |
| CN114471181A (en) * | 2021-12-29 | 2022-05-13 | 北京工业大学 | Preparation method of high-permeability zwitterionic hollow fiber nanofiltration membrane |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103223300A (en) * | 2013-04-12 | 2013-07-31 | 清华大学 | Hollow fiber type composite nano-filtration membrane and preparation method thereof |
| CN105358238A (en) * | 2013-07-04 | 2016-02-24 | 巴斯夫欧洲公司 | Multiple channel membranes |
-
2016
- 2016-08-04 CN CN201610629858.3A patent/CN106215725A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103223300A (en) * | 2013-04-12 | 2013-07-31 | 清华大学 | Hollow fiber type composite nano-filtration membrane and preparation method thereof |
| CN105358238A (en) * | 2013-07-04 | 2016-02-24 | 巴斯夫欧洲公司 | Multiple channel membranes |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108126528A (en) * | 2017-08-30 | 2018-06-08 | 江苏向阳科技有限公司 | A kind of preparation method of double-layer hollow fiber NF membrane |
| CN110523281A (en) * | 2019-08-26 | 2019-12-03 | 北京清鸥科技有限公司 | A kind of polyamide doughnut receives the preparation method of permeable membrane |
| CN114073900A (en) * | 2020-08-13 | 2022-02-22 | 中国科学院青岛生物能源与过程研究所 | Method for preparing hollow fiber membrane with one sealed end |
| CN114471181A (en) * | 2021-12-29 | 2022-05-13 | 北京工业大学 | Preparation method of high-permeability zwitterionic hollow fiber nanofiltration membrane |
| CN114471181B (en) * | 2021-12-29 | 2023-09-26 | 北京工业大学 | Preparation method of high-permeability zwitterionic hollow fiber nanofiltration membrane |
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