CN107174969B - A kind of PET spun-bonded non-woven fabrics/PVDF composite porous film and preparation method thereof - Google Patents
A kind of PET spun-bonded non-woven fabrics/PVDF composite porous film and preparation method thereof Download PDFInfo
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- CN107174969B CN107174969B CN201710391103.9A CN201710391103A CN107174969B CN 107174969 B CN107174969 B CN 107174969B CN 201710391103 A CN201710391103 A CN 201710391103A CN 107174969 B CN107174969 B CN 107174969B
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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
- 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
- B01D67/0011—Casting solutions therefor
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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
- B01D67/0013—Casting processes
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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
- B01D67/0016—Coagulation
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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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- Dispersion Chemistry (AREA)
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- Manufacturing & Machinery (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The present invention relates to a kind of PET spun-bonded non-woven fabrics/PVDF composite porous films and preparation method thereof, and preparation step is successively are as follows: (a) PVDF, organic solvent, pore-foaming agent are mixed evenly, and then ultrasonic deaeration, obtains casting solution；(b) tetrahydrofuran (THF) solution spraying of PET spun-bonded non-woven fabrics amphipathic nature block polymer is dried afterwards completely；(c) it after the painting of modified PET spun-bonded non-woven fabrics being covered with casting solution, is put into coagulating bath and PVDF composite porous film is obtained by phase inversion.The method provided by the invention for preparing PVDF composite porous film is simple, easy to operate, with it is traditional prepare Kynoar film method compared with, the made pvdf membrane supporting layer of this method is combined closely with coat, and anti-high pressure backwash ability significantly improves, and application is wider.
Description
Technical field
The invention belongs to seperation film field, it is related to a kind of PET spun-bonded non-woven fabrics/PVDF composite porous film and its preparation side
Method.
Background technique
Undoubtedly, water resource is the primary condition that the mankind depend on for existence and develop.However, the water resource got worse
Short, serious water environment pollution has become an important factor for restricting Sustainable Socioeconomic Development.China is also a water money
The country of source shortage, the distribution of water resource are also very uneven.This severe status of water resources shortage is faced, saving is carried out and uses
Water is imperative, while needing to be strengthened waste water reclaiming and recycling.
Membrane separation technique be exactly using seperation film as interface, under the motive force of pressure difference, potential difference or concentration difference, each component
It is different through the rate of film, it is enriched with each component respectively in the two sides of film, with the mesh for reaching separation, concentration purification and recycling
's.It is in electroplating waste water resource processing, refuse leachate recycling treatment, paper waste recycling treatment, dyeing waste water
Outstanding contributions are made in the fields such as recycling treatment and sanitary sewage Treated sewage reusing.Separation membrane material can be divided into organic film and nothing
Machine film, wherein inoranic membrane is mainly based on ceramic membrane.Organic film is many kinds of, there is Kynoar, polysulfones, polyether sulfone, poly- four
Vinyl fluoride, polypropylene, polyamide, polycarbonate etc. can meet different use demands.Seperation film can be divided into micro- by pore size
Filter (MF), ultrafiltration (UF), nanofiltration (NF), reverse osmosis (RO) etc..If using the large pore materials such as microfiltration membranes or ultrafiltration membrane as branch
Supportting layer can be before guaranteeing film interception capacity in one layer of several hundred nanometer of its surface recombination or smaller film layer as separating layer
It puts, greatly improves permeation flux.Wherein, key technology is exactly to solve the problems, such as the binding force of separating layer Yu macropore backing material.
In the present invention, starting proposition and using has amphiphilic block copolymer-modified PET spun-bonded non-woven fabrics perforated material as base
Bottom, PVDF as separating layer are prepared for that the high-performance composite porous film of big pressure backwash can be carried out.
Summary of the invention
A kind of the purpose of the present invention is to provide methods simple, easy-operating PET spun-bonded non-woven fabrics/PVDF composite porous film
Preparation method.
The technical solution of the present invention is as follows:
A kind of preparation method of PET spun-bonded non-woven fabrics/PVDF composite porous film, the specific steps are as follows:
(a) PVDF, organic solvent, pore-foaming agent are mixed evenly, then ultrasonic deaeration, obtains casting solution；Described
PVDF: pore-foaming agent: the mass ratio of organic solvent is 10~25:3~8:67~87；
(b) by the tetrahydrofuran solution of PET spun-bonded non-woven fabrics amphipathic nature block polymer be sprayed to its it is completely drenched after
It is dry；
(c) it after the painting of modified PET spun-bonded non-woven fabrics being covered with casting solution, is put into coagulating bath and is obtained by phase inversion
PET spun-bonded non-woven fabrics/PVDF composite porous film.
Preparation method of the present invention preferably comprises following steps:
A) preparation of casting solution: PVDF, organic solvent, pore-foaming agent are mixed in a certain ratio, under certain temperature stir 3~
8h, then 0.5~5h of ultrasonic deaeration, obtains casting solution；The PVDF: pore-foaming agent: the mass ratio of organic solvent is 10~20:
3~8:75~87, preferably 10~18:3~6:78~86；
B) modification of PET spun-bonded non-woven fabrics: a certain amount of amphipathic nature block polymer is dissolved in THF, is prepared certain
The BCP solution of concentration；By PET spun-bonded non-woven fabrics amphipathic nature block polymer solution spraying to its completely drenched rear 80 DEG C of drying
30min~2h；
C) PET spun-bonded non-woven fabrics/PVDF composite porous film preparation: by casting solution knifing stick prepared in step a)
Coated on PET spun-bonded non-woven fabrics modified in step b), exposure after a certain period of time, is put into rapidly 10 in coagulating bath in air
Then~15min impregnates 45~48h in deionized water, obtains PVDF composite porous film.
In the present invention, PVDF molecular weight further preferred 300,000~700,000 described in step a).
In the present invention, the further preferred n,N-dimethylacetamide of solvent described in step a) (DMAc), N- methyl pyrrole
Pyrrolidone (NMP) or n,N-Dimethylformamide (DMF).
In the present invention, further preferred polyvinylpyrrolidone PVP K17 of pore-foaming agent described in step a), polyethylene pyrrole
Pyrrolidone PVP K30, polyvinylpyrrolidone PVP K60, polyvinylpyrrolidone PVP K90, lithium chloride (LiCl), poly- second two
One or more combinations of alcohol 400 (PEG 400), polyethylene glycol-800 (PEG 800), polyethylene glycol 2000 (PEG 2000).
In the present invention, further preferred 40 DEG C~95 DEG C of whipping temp described in step a).
In the present invention, amphipathic nature block polymer BCP described in step b) is further preferably by block A and B block group
At, the wherein preferred polystyrene of block A, B block preferably poly- (2- vinylpyridine) or P4VP；Wherein block
B accounts for the percentage preferably 9~25% of block copolymer total volume；Preferably 10,000~50,000 dongle of the total molecular weight of block copolymer
?.The type Amphiphilic Block Copolymer Micelles have patent report, such as 201210107974.0,201110192571.6,
201310066924.7.The present invention is the Canadian POLYMERSOURCE Products directly bought.But those skilled in the art
Both commercially available amphipathic nature block polymer can be bought, it can also the preparation of the method according to disclosed in the prior art.
In the present invention, BCP concentration of polymer solution further preferred 0.3%~7% described in step b).
In the present invention, the further preferred 10s~600s of exposure duration described in step c).
In the present invention, one of the further preferred deionized water of coagulating bath described in step c), ethyl alcohol, DMAc or several
Kind mixing.
PET spun-bonded non-woven fabrics/PVDF the composite porous film being prepared according to above-mentioned preparation method.
The PET spun-bonded non-woven fabrics/the application of PVDF composite porous film in the treatment of waste water.
The invention has the following advantages that
(1) in PET spun-bonded non-woven fabrics modifying process, amphipathic nature block polymer hydrophilic segment and hydrophobic segment pass through hydrogen bond
It is closely coupled with PET spun-bonded non-woven fabrics and PVDF respectively, " function served as bridge " is played between PET spun-bonded non-woven fabrics and PVDF.
(2) by being modified, the hydrophilic and hydrophobic on PET spun-bonded non-woven fabrics surface is changed, backward by original hydrophily
The hydrophobicity variation come.Based on the change of PET spun-bonded non-woven fabrics surface nature, the casting solution of polymer P VDF is coated to PET base
When on bottom, hydrophobicity PVDF segment can be sprawled preferably in PET base, to increase contact of the PVDF separating layer with substrate
Area improves the binding force of PVDF and substrate.
(3) in actual use, composite porous film can be cleaned with higher backwash pressure, more quickly restore film
Original flux, and the original interception capacity of film is maintained to the full extent.
(4) concentration that amphipathic nature block polymer uses is extremely dilute, only sprays very thin one layer on non-woven fabrics fiber surface layer, right
Influence caused by the permeance property of composite porous film is negligible, and the usage amount of amphipathic nature block polymer is few, there is utilization
Save the cost promotes the development of industrial applications.
The method provided by the invention for preparing PVDF composite porous film is simple, easy to operate, prepares polyvinylidene fluoride with traditional
Alkene film method is compared, and the made pvdf membrane supporting layer of this method is combined closely with coat, and anti-high pressure backwash ability significantly improves,
Using wider.
Specific embodiment
The present invention is further described below in conjunction with specific embodiment, but institute is not constituted to embodiment to the present invention
The limitation of claim saturation range.
Embodiment 1
A) PVDF, DMAc, LiCl that molecular weight is 300,000 are mixed, stirs 3h at 50 DEG C, then ultrasonic deaeration 1h, obtains
Casting solution；
Wherein, PVDF:LiCl:DMAc mass ratio is 10:4:86.
B) polystyrene-poly (2- vinylpyridine) amphipathic nature block polymer is dissolved in THF, prepares mass fraction
For 4% BCP solution；By the completely rear 80 DEG C of dryings of the amphipathic nature block polymer solution spraying of PET spun-bonded non-woven fabrics
30min；
It is 10% that wherein block poly- (2- vinylpyridine), which accounts for the percentage of block copolymer total volume,；Block copolymer
Total molecular weight is 2.5 ten thousand dalton.
C) casting solution prepared in step a) is coated in PET spun-bonded non-woven fabrics modified in step b) with knifing stick
On, after exposing 10s in air, it is put into 10min in alcohol solidification bath rapidly, then impregnates 48h in deionized water, obtains
PVDF composite porous film.
The PVDF perforated membrane is under 25 DEG C, 1bar pressure, flux 850Lm-2·h-1, film maximum backwash pressure
3.6bar。
Embodiment 2
A) PVDF, DMAc, LiCl that molecular weight is 500,000 are mixed, stirs 4h at 60 DEG C, then ultrasonic deaeration 1.5h, obtains
To casting solution；
Wherein, PVDF:LiCl:DMF mass ratio is 18:4:86.
B) polystyrene-poly (2- vinylpyridine) amphipathic nature block polymer is dissolved in THF, prepares mass fraction
For 3% BCP solution；By the completely rear 80 DEG C of dryings of the amphipathic nature block polymer solution spraying of PET spun-bonded non-woven fabrics
30min；
It is 13% that wherein block poly- (2- vinylpyridine), which accounts for the percentage of block copolymer total volume,；Block copolymer
Total molecular weight is 3.5 ten thousand dalton.
C) casting solution prepared in step a) is coated in PET spun-bonded non-woven fabrics modified in step b) with knifing stick
On, after exposing 20s in air, it is put into 10min in alcohol solidification bath rapidly, then impregnates 48h in deionized water, obtains
PVDF composite porous film.
The PVDF perforated membrane is under 25 DEG C, 1bar pressure, flux 113Lm-2·h-1, film maximum backwash pressure
3.4bar。
Embodiment 3
A) by molecular weight be 670,000 PVDF, NMP, PVP K30 mix, stir 4h at 70 DEG C, then ultrasonic deaeration 2h, obtains
To casting solution；
Wherein, PVDF:PVP K30:DMAc mass ratio is 16:6:78.
B) polystyrene-poly (4-vinylpridine) amphipathic nature block polymer is dissolved in THF, prepares mass fraction
For 6% BCP solution；By the completely rear 80 DEG C of dryings of the amphipathic nature block polymer solution spraying of PET spun-bonded non-woven fabrics
30min；
It is 13% that wherein block P4VP, which accounts for the percentage of block copolymer total volume,；Block copolymer
Total molecular weight is 4.5 ten thousand dalton.
C) casting solution prepared in step a) is coated in PET spun-bonded non-woven fabrics modified in step b) with knifing stick
On, after exposing 15s in air, it is put into 10min in alcohol solidification bath rapidly, then impregnates 48h in deionized water, obtains
PVDF composite porous film.
The PVDF perforated membrane is under 25 DEG C, 1bar pressure, flux 313Lm-2·h-1, film maximum backwash pressure
4.1bar。
Embodiment 4
A) PVDF, DMAc, PEG 800 that molecular weight is 430,000 is mixed, 4h is stirred at 55 DEG C, then ultrasonic deaeration 1h,
Obtain casting solution；
Wherein, PVDF:LiCl:DMAc mass ratio is 13:4:83.
B) polystyrene-poly (2- vinylpyridine) amphipathic nature block polymer is dissolved in THF, prepares mass fraction
For 4.5% BCP solution；By the completely rear 80 DEG C of dryings of the amphipathic nature block polymer solution spraying of PET spun-bonded non-woven fabrics
30min；
It is 15% that wherein block poly- (2- vinylpyridine), which accounts for the percentage of block copolymer total volume,；Block copolymer
Total molecular weight is 30,000 dalton.
C) casting solution prepared in step a) is coated in PET spun-bonded non-woven fabrics modified in step b) with knifing stick
On, after exposing 10s in air, it is put into 10min in alcohol solidification bath rapidly, then impregnates 48h in deionized water, obtains
PVDF composite porous film.
The PVDF perforated membrane is under 25 DEG C, 1bar pressure, flux 620Lm-2·h-1, film backwash pressure
3.8bar。
Embodiment 5
A) by molecular weight be 580,000 PVDF, DMAc, PVP K90 mix, stir 4h at 55 DEG C, then ultrasonic deaeration 1h,
Obtain casting solution；
Wherein, PVDF:PVP K90:DMAc mass ratio is 15:3:82.
B) polystyrene-poly (4-vinylpridine) amphipathic nature block polymer is dissolved in THF, prepares mass fraction
For 5% BCP solution；By the completely rear 80 DEG C of dryings of the amphipathic nature block polymer solution spraying of PET spun-bonded non-woven fabrics
30min；
It is 20% that wherein block P4VP, which accounts for the percentage of block copolymer total volume,；Block copolymer
Total molecular weight is 50,000 dalton.
C) casting solution prepared in step a) is coated in PET spun-bonded non-woven fabrics modified in step b) with knifing stick
On, after exposing 10s in air, it is put into 10min in alcohol solidification bath rapidly, then impregnates 48h in deionized water, obtains
PVDF composite porous film.
The PVDF perforated membrane is under 25 DEG C, 1bar pressure, flux 480Lm-2·h-1, film backwash pressure
4.3bar。
Claims (10)
1. a kind of preparation method of PET spun-bonded non-woven fabrics/PVDF composite porous film, characterized by comprising the steps of:
(a) PVDF, organic solvent, pore-foaming agent are mixed evenly, then ultrasonic deaeration, obtains casting solution；The PVDF:
Pore-foaming agent: the mass ratio of organic solvent is 10 ~ 25:3 ~ 8:67 ~ 87；
(b) tetrahydrofuran solution of PET spun-bonded non-woven fabrics amphipathic nature block polymer is sprayed to dry after it drenches completely；
(c) it after the painting of modified PET spun-bonded non-woven fabrics being covered with casting solution, is put into coagulating bath and PET is obtained by phase inversion
Spun-bonded non-woven fabrics/PVDF composite porous film.
2. preparation method according to claim 1, it is characterised in that comprise the steps of
A) preparation of casting solution: PVDF, organic solvent, pore-foaming agent are mixed in proportion, stir 3 ~ 8h, then ultrasonic deaeration 0.5 ~
5h obtains casting solution；
B) modification of PET spun-bonded non-woven fabrics: amphipathic nature block polymer is dissolved in tetrahydrofuran, and it is total to prepare amphipathic block
Copolymer solution；By PET spun-bonded non-woven fabrics amphipathic nature block polymer solution spraying to its completely drenched rear 80 DEG C of dry 30min
~2h；
C) casting solution prepared in step a) PET spun-bonded non-woven fabrics/PVDF composite porous film preparation: is coated in step b)
On the PET spun-bonded non-woven fabrics of middle modification, exposure after a certain period of time, is put into rapidly 10-15min in coagulating bath, then in air
45 ~ 48h is impregnated in deionized water, obtains PVDF composite porous film.
3. preparation method according to claim 2, it is characterised in that PVDF molecular weight described in step a) is 300,000 ~ 70
Ten thousand；The organic solvent is n,N-dimethylacetamide, N-Methyl pyrrolidone or n,N-Dimethylformamide；The cause
Hole agent is polyvinylpyrrolidone PVP K17, polyvinylpyrrolidone PVP K30, polyvinylpyrrolidone PVP K60, poly- second
Alkene pyrrolidone PVP K90, lithium chloride, polyethylene glycol 400, polyethylene glycol-800, one or more groups of polyethylene glycol 2000
It closes.
4. preparation method according to claim 2, it is characterised in that the temperature of stirring described in step a) is 40 DEG C ~ 95
℃。
5. preparation method according to claim 2, it is characterised in that amphipathic nature block polymer described in step b) by
Block A and B block composition, wherein block A is polystyrene, and B block is poly- (2- vinylpyridine) or poly- (4- ethylene
Yl pyridines)；The percentage that B block accounts for block copolymer total volume is 9 ~ 25%；The total molecular weight of block copolymer is 10,000 ~ 5
Ten thousand dalton.
6. preparation method according to claim 2, it is characterised in that amphipathic nature block polymer described in step b) is molten
Liquid mass concentration is 0.3% ~ 7%.
7. preparation method according to claim 2, it is characterised in that exposure duration described in step c) is 10s ~ 600s.
8. preparation method according to claim 1, it is characterised in that coagulating bath described in step c) is deionized water, second
One or more of alcohol, DMAc mixing.
9. compound more according to PET spun-bonded non-woven fabrics/PVDF that preparation method of any of claims 1-8 is prepared
Pore membrane.
10. the PET spun-bonded non-woven fabrics as claimed in claim 9/application of PVDF composite porous film in the treatment of waste water.
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| US10576429B1 (en) | 2019-04-17 | 2020-03-03 | King Saud University | Method of making an asymmetric polyvinylidene difluoride membrane |
| CN111871221A (en) * | 2020-07-09 | 2020-11-03 | 天津科技大学 | Hydrophobic/hydrophilic composite membrane with nuclear track etching membrane as base membrane and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1735666A (en) * | 2001-02-26 | 2006-02-15 | 罗狄亚化学公司 | Use of an amphiphilic block copolymers as adhesion promoters of film-forming aqueous compositions on a low-energy surface |
| CN102512972A (en) * | 2011-12-09 | 2012-06-27 | 西安建筑科技大学 | Method for preparing double-surface composite flat membrane |
| CN103088629A (en) * | 2012-12-18 | 2013-05-08 | 华南理工大学 | Method for carrying out super-hydrophobic modification on PET fabric surface |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1735666A (en) * | 2001-02-26 | 2006-02-15 | 罗狄亚化学公司 | Use of an amphiphilic block copolymers as adhesion promoters of film-forming aqueous compositions on a low-energy surface |
| CN102512972A (en) * | 2011-12-09 | 2012-06-27 | 西安建筑科技大学 | Method for preparing double-surface composite flat membrane |
| CN103088629A (en) * | 2012-12-18 | 2013-05-08 | 华南理工大学 | Method for carrying out super-hydrophobic modification on PET fabric surface |
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