CN110508160A - Kynoar filter membrane and preparation method thereof - Google Patents
Kynoar filter membrane and preparation method thereof Download PDFInfo
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- CN110508160A CN110508160A CN201810489669.XA CN201810489669A CN110508160A CN 110508160 A CN110508160 A CN 110508160A CN 201810489669 A CN201810489669 A CN 201810489669A CN 110508160 A CN110508160 A CN 110508160A
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- kynoar
- casting solution
- polyamide
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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
-
- 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
- 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
- B01D2325/00—Details relating to properties of membranes
- B01D2325/22—Thermal or heat-resistance properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/30—Chemical resistance
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
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- Chemical & Material Sciences (AREA)
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- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The present invention relates to field of membrane material, a kind of Kynoar filter membrane and preparation method thereof is disclosed.The method for preparing Kynoar filter membrane includes that casting solution is coated on substrate surface, prevapourising, film forming and solidification are carried out again, wherein, it is 100:(5-15 that the casting solution, which contains mass ratio): Kynoar, polyamide and the pore-foaming agent of (10-25).The invention also discloses Kynoar filter membranes made from the above method.Through the above technical solutions, present invention obtains hydrophily, rejection, thermal stability and chemical stability preferably Kynoar filter membranes.
Description
Technical field
The present invention relates to field of membrane material, and in particular, to Kynoar filter membrane and preparation method thereof.
Background technique
Membrane separation technique green high-efficient is widely used in Water warfare, chemical separating and field of biological pharmacy.Its
In, ultrafiltration membrane can be effectively removed biomolecule, high molecular polymer and colloidal substance etc., and loading density is big, low energy consumption,
It is easy to operate.Therefore, ultrafiltration membrane is widely used in the fields such as sewage treatment, chemical industry, biology, pharmacy.
Kynoar (PVDF) ultrafiltration membrane is because of its excellent thermal stability, chemical stability, heat radiation and excellent
Mechanical performance is concerned, but PVDF ultrafiltration membrane surface C-F key abundant and c h bond keep its hydrophily poor.Hydrone is difficult to attached
On pvdf membrane surface, cause water flux lower；On the other hand, organic matter is easily adsorbed on pvdf membrane surface, leads to membrane lifetime
It reduces.Generally, the hydrophily of film can be improved by physics and chemical means.Method of modifying be broadly divided into membrane surface modification and
It is membrane material modified.
Membrane surface modification is that polar group and hydrophilic molecule are introduced in the pvdf membrane surface and film inner hole prepared.Change
Property method includes that surface covering, chemical modification and ion are modifies etc..It is membrane material modified including membrane material chemical modification and total
Mixed modification.Wherein, blending and modifying is easy to operate, and hydrophilic radical is not easily to fall off, is convenient for large-scale promotion.In CN101703897A
Polyether sulfone is blended with PVDF to improve the anti-contracility energy of film and hydrophily.By cellulose acetate, poly- in CN102716677A
Methyl methacrylate is blended to improve the hydrophily and toughness of film.By hydrophilic nanoparticles and PVDF in CN101905123A
It is blended to improve the hydrophily of film.But the ultrafiltration membrane that above method obtains is difficult to meet hydrophily, rejection, heat simultaneously surely
The requirement of qualitative and chemical stability etc., use scope is limited, therefore, is improving hydrophilic while keeping as far as possible
Or rejection, thermal stability and the chemical stability of raising film have a very important significance.
Summary of the invention
The purpose of the invention is to overcome the presence of the prior art to be difficult to ensure hydrophily, rejection, thermostabilization simultaneously
The problem of property and chemical stability, provides a kind of PVDF filter membrane and preparation method thereof.
To achieve the goals above, the present invention provides a kind of method for preparing PVDF filter membrane, this method includes by casting film
Liquid is coated on substrate surface, then carries out prevapourising, film forming and solidification, wherein it is 100:(5- that the casting solution, which contains mass ratio,
15): Kynoar, polyamide and the pore-foaming agent of (10-25).
The present invention also provides Kynoar filter membranes made from the above method.
Through the above technical solutions, present invention obtains hydrophily, rejection, thermal stability and chemical stability are more excellent
Kynoar filter membrane, even if in casting solution do not include any surfactant in the case where.
Specific embodiment
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
The method provided by the invention for preparing Kynoar filter membrane includes casting solution being coated on substrate surface, then carry out
Prevapourising, film forming and solidification, which is characterized in that it is 100:(5-15 that the casting solution, which contains mass ratio): the poly- inclined fluorine of (10-25)
Ethylene, polyamide and pore-foaming agent.
In the present invention, the mass ratio between Kynoar and polyamide is preferably 100:(8-12).
In the present invention, the mass ratio between Kynoar and pore-foaming agent is preferably 100:(22-25).
In the present invention, the Kynoar can be commonly used in the Kynoar for preparing filter membrane for this field, excellent
Selection of land, the number-average molecular weight of the Kynoar are 40-80 ten thousand.
In the present invention, the polyamide can for this field common macromolecular main chain repetitive unit in contain amide groups
The high polymer of group, but under preferable case, the polyamide is at least one of fatty polyamide and aromatic polyamides, more excellent
It is selected as poly.The weight average molecular weight of poly can be 120-180 ten thousand.
In the present invention, the pore-foaming agent can common are for this field to help film and is formed in phase separation uniformly
The substance of pore structure.Preferably, the pore-foaming agent is polyvinylpyrrolidone (PVP) and/or polyethylene glycol.Wherein, described
Polyethylene glycol is preferably polyethylene glycol 200 (PEG-200) and/or polyethylene glycol 400 (PEG-400).
In the present invention, the concentration of Kynoar in casting solution is not required particularly, it is preferable that in the casting solution
Solvent and Kynoar between mass ratio be (250-350): 100, more preferably (280-320): 100.It is further excellent
Selection of land, the solvent in the casting solution are dimethylformamide (DMF), dimethyl acetamide (DMAc) and N-Methyl pyrrolidone
At least one of (NMP).
The present invention obtains performance preferably filter membrane in the case where can not including any surfactant in casting solution, because
This, the casting solution (spreads out without surfactant including various common carboxylates, sulfate, quaternary ammonium salt and polyethylene oxide
Biology).
In the present invention, the casting solution can be obtained by various conventional modes, still, the present inventor's hair
It is existing, Kynoar is first dissolved in a solvent, and adding polyamide and pore-foaming agent can make the filter membrane obtained have better property
Can, it is therefore preferable that in the case of, the casting solution is made by the following method:
It at 50-80 DEG C, is dissolved in Kynoar in solvent, then the solution of acquisition is mixed with polyamide and pore-foaming agent
It closes.Wherein, the order by merging of polyamide and pore-foaming agent is not required particularly, first solution can be made to mix with polyamide,
First solution can be made to mix with pore-foaming agent, solution can also be mixed with polyamide and pore-foaming agent simultaneously.According to a kind of specific
Embodiment, the method for preparing the casting solution include: to be dissolved in Kynoar in solvent at 50-80 DEG C, stir 1-5h
To being completely dissolved, blend A is made；Polyamide is added in blend A, blend B is made in stirring 1-5h；At 50-80 DEG C,
Pore-foaming agent is added in blend B, stirs 1-3h, obtains casting solution.
In the present invention, before coating, casting solution need to be subjected to deaeration, to remove bubble therein, consequently facilitating uniformly
Coating.Deaeration can be carried out by the way of conventional, the mode of deaeration preferably includes: casting solution is stood 12- at 20-40 DEG C
It is evacuated 3-5h for 24 hours and/or under vacuum.
In the present invention, it can be coated by the way of conventional, such as coated by scraper, knifing stick etc..Casting
The thickness of film liquid coating is preferably 100-500 μm, and more preferably 150-300 μm.
In the present invention, because solvent volatilization will form cortex construction during prevapourising.The condition of prevapourising preferably includes: temperature
It is 20-35 DEG C, more preferably 25-30 DEG C.The condition of prevapourising further preferably includes: that relative humidity is 50-80%, more preferably
60-70%.The condition of prevapourising further preferably include: the time be 20s-5min, more preferably 1-2min.
In the present invention, the film forming can carry out under conditions of routine, and such as mode of the film forming is to carry out water-bath.
Preferably, it is 20-40 DEG C that the condition of the water-bath (film forming), which includes: temperature,.It is further preferred that the water-bath
The condition of (film forming) further include: time 3-10min.
In the present invention, the solidification can carry out under conditions of routine, and such as cured mode is to carry out glycerol bath.
Preferably, it is 20-40 DEG C that the condition of the glycerol bath (solidification), which includes: temperature,.It is further preferred that the glycerol
Bathe the condition of (solidification) further include: time 5-20h.It is 20-40%'s that qualities of glycerin content, which can be used, in glycerol bath (solidification)
Glycerine water solution.
The present invention also provides Kynoar filter membranes made from foregoing method.
According to the present invention, the average pore size of the Kynoar filter membrane is 0.01-0.04 μm, and pure water flux reaches 510L
m-2·h-1(such as 440-510Lm-2·h-1), therefore can be used as ultrafiltration membrane use.
The present invention will be described in detail by way of examples below.In following embodiment, PVDF is Belgium Su Weigong
The commercially available product that the trade mark is 6020 is taken charge of, number-average molecular weight is 800,000；PA is the poly- isophthalic two that Sheng Ou aramid fiber limited liability company provides
Formyl m-phenylene diamine (MPD) industrial goods, weight average molecular weight are 1,400,000；PVP (K30), PEG-200 and PEG-400 are Chinese medicines group chemistry
The commercially available product of reagent Co., Ltd.
Embodiment 1
(1) mass ratio for controlling PVDF, PA, DMAc and PVP is 20:2:60:5.It is stirred 2 hours at 70 DEG C, by PVDF
Be dissolved completely in DMAc and obtain homogeneous solution A, PA is added in solution A, continue at 70 DEG C stirring obtain within 2 hours it is uniformly molten
Liquid B.
(2) PVP is added in solution B, is stirred 2 hours at 70 DEG C, obtains casting solution.By casting solution in 30 DEG C of insulating boxs
Middle standing 20h deaeration.
(3) casting solution is coated uniformly on clean glass plate with scraper, the glass plate for being coated with casting solution is placed in
Temperature and relative humidity are respectively 1min progress prevapourising in 30 DEG C and 60% climatic chamber.It is immersed into rapidly later
5min in 30 DEG C of water bath with thermostatic control；It is placed in the glycerine water solution (30 DEG C) of 20wt% again and impregnates 10h, taken out spontaneously dry later
Obtain PVDF ultrafiltration membrane.
Embodiment 2
(1) mass ratio for controlling PVDF, PA, DMAc and PEG-200 is 20:1:70:4.It is stirred 5 hours at 50 DEG C, it will
PVDF, which is dissolved completely in DMAc, obtains homogeneous solution A, and PA is added in solution A, continues stirring at 50 DEG C and obtains within 5 hours
Even solution B.
(2) PEG-200 is added in solution B, is stirred 3 hours at 50 DEG C, obtains casting solution.By casting solution in 40 DEG C of perseverances
12h deaeration is stood in incubator.
(3) casting solution is coated uniformly on clean glass plate with scraper, the glass plate for being coated with casting solution is placed in
Temperature and relative humidity are respectively 20s progress prevapourising in 35 DEG C and 50% climatic chamber.It is immersed into rapidly later
10min in 20 DEG C of water bath with thermostatic control；It is placed in the glycerine water solution (20 DEG C) of 40wt% again and impregnates 20h, it is dry to take out nature later
It is dry to obtain PVDF ultrafiltration membrane.
Embodiment 3
(1) mass ratio for controlling PVDF, PA, DMAc and PEG-400 is 20:3:50:2.It is stirred 1 hour at 80 DEG C, it will
PVDF, which is dissolved completely in DMF, obtains homogeneous solution A, and PA is added in solution A, continues stirring at 80 DEG C and obtains within 1 hour
Even solution B.
(2) PEG-400 is added in solution B, is stirred 2 hours at 80 DEG C, obtains casting solution.By casting solution in 20 DEG C of perseverances
Deaeration for 24 hours is stood in incubator.
(3) casting solution is coated uniformly on clean glass plate with scraper, the glass plate for being coated with casting solution is placed in
Temperature and relative humidity are respectively 5min progress prevapourising in 20 DEG C and 80% climatic chamber.It is immersed into rapidly later
3min in 40 DEG C of water bath with thermostatic control；It is placed in the glycerine water solution (40 DEG C) of 30wt% again and impregnates 5h, taken out spontaneously dry later
Obtain PVDF ultrafiltration membrane.
Embodiment 4
Filter membrane is prepared according to the method for embodiment 2, unlike, in step (1), solvent is added in PVDF and PA simultaneously
It is dissolved in DMAc, specifically:
At 50 DEG C, PVDF and PA is added in solvent DMAc simultaneously and is dissolved, stirring obtains homogeneous solution in 13 hours.
Embodiment 5
Filter membrane is prepared according to the method for embodiment 2, unlike, the temperature for controlling prevapourising is 15 DEG C, time 15s.
Embodiment 6
Filter membrane is prepared according to the method for embodiment 2, unlike, time of water-bath is 30min, and the time that glycerol impregnates is
4h。
Comparative example 1
(1) mass ratio for controlling PVDF, DMAc and PVP is 4:12:1.It is stirred 4 hours at 70 DEG C, PVDF and PVP is complete
Fully dissolved obtains preparation liquid in DMAc.
(2) casting solution is stood to 20h deaeration in 30 DEG C of insulating boxs.
(3) casting solution is coated uniformly on clean glass plate with scraper, the glass plate for being coated with casting solution is placed in
Temperature and relative humidity are respectively 1min progress prevapourising in 30 DEG C and 60% climatic chamber.It is immersed into rapidly later
5min in 30 DEG C of water bath with thermostatic control；It is placed in the glycerine water solution (30 DEG C) of 20wt% again and impregnates 10h, taken out spontaneously dry later
Obtain PVDF ultrafiltration membrane.
Comparative example 2
Filter membrane is prepared according to the method for embodiment 2, unlike, the mass ratio of PVDF and PA are 7:5.
Comparative example 3
Filter membrane is prepared according to the method for embodiment 2, unlike, PA is replaced with into polyimides (by equal four formyl chloride of benzene
140 ten thousand) it is synthesized with m-phenylene diamine (MPD), weight average molecular weight is.
Comparative example 4
Filter membrane is prepared according to the method for embodiment 2, unlike, PA is replaced with polyether sulfone, and (U.S.'s Su Wei trade mark is A-
100 commercially available product).
Test case 1
Filter membrane made from above embodiments and comparative example is tested for the property in accordance with the following methods:
Film average pore size is measured using the multi-functional filter sizes analyzer of 3H-2000PBL；
According to the pure water flux and rejection of the method measurement film recorded in HY/T050-1999, by filter membrane obtained 80
It is dry after being impregnated 3 months in DEG C pure water, test pure water flux and rejection again to examine or check the thermal stability of filter membrane.
Test result is as shown in table 1.
1 film properties test result of table
Can be seen that as the result of table 1 has excellent hydrophily, rejection using filter membrane made from the method for the present invention
And thermal stability.Though filter membrane made from comparative example 3 has more excellent hydrophily, rejection and thermal stability, polyimides
Backwash reagent is limited in facile hydrolysis under alkaline condition, use scope and use process.Particularly, comparing embodiment 2 and implementation
Example 4-6 can be seen that and prepare casting solution using preferred embodiment, implements prevapourising or solidify further improve gained
The performance of filter membrane.
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In skill of the invention
In art conception range, can with various simple variants of the technical solution of the present invention are made, including each technical characteristic with it is any its
Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, is belonged to
Protection scope of the present invention.
Claims (11)
1. a kind of method for preparing Kynoar filter membrane, this method includes that the casting solution after deaeration is coated on substrate surface,
Prevapourising, film forming and solidification are carried out again, which is characterized in that it is 100:(5-15 that the casting solution, which contains mass ratio): (10-25's)
Kynoar, polyamide and pore-foaming agent.
2. according to the method described in claim 1, wherein, the mass ratio between Kynoar, polyamide and pore-foaming agent is
100:(8-12):(22-25)。
3. method according to claim 1 or 2, wherein the number-average molecular weight of the Kynoar is 40-80 ten thousand；
And/or the polyamide is fatty polyamide and/or aromatic polyamide；
And/or the pore-foaming agent is polyvinylpyrrolidone and/or polyethylene glycol.
4. according to the method described in claim 3, wherein, the polyamide is poly；
And/or the polyethylene glycol is polyethylene glycol 200 and/or polyethylene glycol 400.
5. according to the method described in claim 1, wherein, the mass ratio between Kynoar and solvent in the casting solution
For 100:(250-350)；
And/or the solvent in the casting solution be dimethylformamide, dimethyl acetamide and N-Methyl pyrrolidone in extremely
Few one kind.
6. method according to claim 1 or 5, wherein the casting solution is made by the following method:
It at 50-80 DEG C, is dissolved in Kynoar in solvent, then the solution of acquisition is mixed with polyamide and pore-foaming agent.
7. according to the method described in claim 1, wherein, the casting solution carries out deaeration by the following method:
Casting solution is stood into 12-24h at 20-40 DEG C and/or is evacuated 3-5h under vacuum.
8. according to the method described in claim 1, wherein, the condition of prevapourising includes: that temperature is 20-35 DEG C, and relative humidity is
50-80%, time 20s-5min；
And/or the film forming carries out in a water bath, the condition of film forming includes: that temperature is 20-40 DEG C, time 3-10min.
9. according to the method described in claim 1, wherein, it is described be solidificated in the glycerol bath that glycerol content is 20-40wt% into
Row, cured condition include: that temperature is 20-40 DEG C, time 5-20h.
10. Kynoar filter membrane made from method described in any one of -9 according to claim 1.
11. Kynoar filter membrane according to claim 10, wherein the average pore size of the Kynoar filter membrane is
0.01-0.04μm。
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| CN201810489669.XA CN110508160A (en) | 2018-05-21 | 2018-05-21 | Kynoar filter membrane and preparation method thereof |
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| CN114130202A (en) * | 2021-12-15 | 2022-03-04 | 中国科学院长春应用化学研究所 | Microporous filter membrane and preparation method thereof |
| CN114230824A (en) * | 2020-09-09 | 2022-03-25 | 财团法人工业技术研究院 | Polyvinylidene fluoride film composition and polyvinylidene fluoride barrier film |
| CN115337788A (en) * | 2021-04-27 | 2022-11-15 | 南京工业大学 | Method for reducing membrane pollution in organic wastewater treatment process |
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