CN106693726A - Formula for preparing polyvinylidene fluoride and carbon nanotube composite film and preparation method of formula - Google Patents
Formula for preparing polyvinylidene fluoride and carbon nanotube composite film and preparation method of formula Download PDFInfo
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- CN106693726A CN106693726A CN201510800032.4A CN201510800032A CN106693726A CN 106693726 A CN106693726 A CN 106693726A CN 201510800032 A CN201510800032 A CN 201510800032A CN 106693726 A CN106693726 A CN 106693726A
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- film
- mwcnts
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- pvdf
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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
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
-
- 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
Abstract
The invention relates to a formula for preparing a polyvinylidene fluoride and carbon nanotube composite film and a preparation method of the formula. The method comprises the following steps: 1, weighing a certain amount of MWCNTs, taking dimethylformamide (DMF) as a solvent, and carrying out ultrasound treatment on MWCNTs in DMF for 40 minutes to enable MWCNTs to be dispersed fully; 2, drying polyvinylidene fluoride (PVDF) powder in an oven for a period of time before use to remove water; 3, adding the PVDF powder in a MWCNTs/DMF system to prepare a casting solution, violently stirring in constant-temperature water bath at the temperature of 70 DEG C for 4 hours, and enabling the PVDF powder to be dissolved fully to obtain a uniform solution; 4, sealing the obtained casting solution, and leaving the casting solution standstill during the whole night at room temperature to remove foam; 5, scraping the film on a clean glass plate with a 300 mu m film scraping bar, soaking a liquid film, together with the glass plate, in distilled water bath after 1 minute, and washing the film with deionized water to remove a residual solvent after the film is cured and is stripped from the glass plate automatically; and 6, finally, soaking the film in the deionized water for 48 hours, then taking part of the film and naturally air-drying the film at room temperature to obtain the PVDF/MWCNTs composite film. The preparation method is simple, high in operability, low in energy consumption and low in pollution.
Description
Technical field
The present invention relates to the masking formula and its preparation side of a kind of Kynoar and CNT flat composite membrane
Method.
Background technology
PVDF is a kind of line style semi-crystalline polymer, and glass transition temperature (Tg) is about -39 DEG C, melting
Temperature (Tm) is about 160 DEG C, and heat decomposition temperature is about 316 DEG C.The linear macromolecule chain structure of PVDF
It is-CH2-CF2-, polymer chain is surrounded by fluorine atom and hydrogen atom, therefore with excellent chemical stability,
Heat endurance and mechanical stability, while the features such as there is acid-alkali-corrosive-resisting, not degradable, easy film forming.By
In-CH2-CF2- be alternately arranged polarization, therefore some common polar solvents, such as N, N- can be dissolved in
Dimethylacetylamide, N-methyl pyrrolidones, dimethyl sulfoxide (DMSO), DMF, this causes it
The ideal material of film is prepared as phase conversion method.In recent years, pvdf membrane has been widely used in chemical industry, ring
The numerous areas such as guarantor, food, medicine and biochemistry.However, still having some problems to limit pvdf membrane enters one
The development and application of step, the especially purification in water and separation field, such as drinking water produce, wastewater treatment with
And bio-separation.Key issue is that the surface energy of PVDF is very low, causes film wetability poor, is dredged
It is aqueous stronger.When in the aqueous solution for the treatment of containing natural organic matter and protein, due to hydrophobic pvdf membrane
The almost effect without hydrogen bond between boundary layer and hydrone between, therefore during water is easily adsorbed on film surface
Protein or natural organic matter, and then the hole on film surface is blocked, water flux reduction, reduces the use longevity of film
Life, causes more operation costs changed and repair membrane module.And hydrophilic film surface has table high
Face tension force, can form hydrogen bond with the hydrone of surrounding, build a border between surface and hydrone
Layer, because the orderly structure in destruction boundary layer needs to increase extra energy, this cause in water protein or
Organic matter, it is difficult to close to film surface.Except the influence of the hydrophilic/hydrophobic on film surface, the electric charge on film surface and
Ionic strength, film topographical characteristics, including surface roughness, pore-size distribution, porosity, curvature are molten
Also the undeniable influence fouling membrane such as qualitative attribution and flow pattern.Therefore the parent for improving PVDF seperation films
It is aqueous, improve the anti-absorption pollution capacity of film and reduce the operating power consumption of film and ground as current seperation film
The focus studied carefully.
In recent years, by blending and modifying improve fluoropolymer antifouling property oneself increasingly cause researcher
Interest.Compared than traditional surface treatment method, blending and modifying do not need large-scale experiment instrument, into
Directly it is modified during film, and low cost, it is simple to operate.By the inorganic nano-particle that adulterates, can
To improve the performances such as the water flux of film, rejection, hydrophily.The embedded CNT in polymeric matrix,
As the development strategy of film, it is increasingly subject to pay attention to.First, the quick transport behavior of CNT has turned into and has ground
The focus studied carefully.Molecular dynamics simulations prediction finds due to the flatness of nanochannel, hydrophobicity and occurs to exist
Molecular order phenomenon in closed nanochannel, compares with known other porous materials, carbon nano-tube film tool
There are a permeation flux and selectivity of uniqueness, the lighter gas diffusion energy in the CNT of about 1 nanometer of internal diameter
Power is higher than more than the several orders of magnitude of other porous materials.Due to the unique combination property of CNT, by its letter
Single functionalization and dispersion is in the polymer, less filer content can strengthen mechanical strength and by hole
Size Control is in nanometer range.
The content of the invention
It is an object of the invention to provide a kind of Kynoar and CNT flat composite membrane masking formula and
Its preparation method.
The technical solution adopted by the present invention is to provide the system of a kind of Kynoar and CNT flat composite membrane
Film formulation and preparation method thereof, the method step is as follows：
1) a certain amount of MWCNTs is weighed, with dimethylformamide (DMF) as solvent, is made
MWCNTs ultrasound 40min in DMF, disperse MWCNTs abundant.
2) Kynoar (PVDF) powder is drying a period of time using preposition in baking oven, goes water removal
Point.
3) PVDF powder is added to and casting solution is made into MWCNTs/DMF systems, and in 70 DEG C of perseverance
4h is stirred vigorously in tepidarium, PVDF powder is fully dissolved, obtain uniform solution.
4) by gained casting solution sealing preserve, standing deaeration overnight at room temperature
5) liquid film is soaked together with glass plate after 1min with 300 μm of knifing rod knifing on clean glass plate
Enter in distilled water water-bath, treat that film solidifies and automatically strips glass plate, use deionized water wash and remove residual
Solvent.
6) after film finally being soaked into 48h in deionized water, it is placed in and dries naturally at room temperature, that is, obtains
PVDF/MWCNTs composite membranes.
Kynoar and CNT flat composite membrane are prepared using the technique of blending and modifying, material therefor is
Kynoar, dimethylformamide, unmodified multi-walled carbon nano-tubes, 0.49% carboxylated multi-wall carbon nano-tube
Pipe, 2% functionalized multi-wall carbonnanotubes, 3.86% functionalized multi-wall carbonnanotubes and deionized water etc..
Described method is simple blending and modifying technique.
It is solvent that described method uses dimethylformamide.
The coagulating bath that described method is constituted using deionized water.
The beneficial effects of the invention are as follows：
1) preparation process is simple, serialization and easily industrialization.
2) composition of coagulating bath is common deionized water, and temperature is room temperature, is easily controlled, and save energy
Consumption, reduces cost.
3) tension test shows that adding certain CNT can strengthen the intensity of pure pvdf membrane, and containing 0.49
% carboxy-modified MWCNTs improves 16% than unmodified MWCNTs intensity, and 21% is improve than pure pvdf membrane.
But as carboxy-modified degree increases, compound film strength first rises and declines afterwards, i.e. addition changes containing 0.49% carboxyl
Property MWCNTs the compound film strength highests of PVDF.
4) TG and DTG curves show that five kinds of films are to start to decompose at about 420 DEG C, pvdf membrane
Heat decomposition temperature be 450 DEG C, MWCNT/PVDF films bring up to 454 DEG C, and with carboxylated degree
Increase, the heat decomposition temperature of composite membrane rises 4-5 DEG C successively.
Brief description of the drawings
Fig. 1 is that Kynoar prepared by embodiment 1 is schemed with the SEM of CNT flat composite membrane.
Specific embodiment
Using simple blending and modifying technique, with Kynoar as matrix, dimethylformamide is used as molten
Agent, prepares the process of Kynoar and CNT flat composite membrane.
With reference to embodiment, the invention will be further described, so that those skilled in the art can be more
Good understanding is of the invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
Embodiment 1
A kind of use blending and modifying technique prepares the preparation side of Kynoar and CNT flat composite membrane
Method, the method step is as follows：
1) a certain amount of MWCNTs is weighed, with dimethylformamide (DMF) as solvent, is made
MWCNTs ultrasound 40min in DMF, disperse MWCNTs abundant.
2) Kynoar (PVDF) powder is drying a period of time using preposition in baking oven, goes water removal
Point.
3) PVDF powder is added to and casting solution is made into MWCNTs/DMF systems, and in 70 DEG C of perseverance
4h is stirred vigorously in tepidarium, PVDF powder is fully dissolved, obtain uniform solution.
4) by gained casting solution sealing preserve, deaeration overnight at room temperature is stood.
5) liquid film is soaked together with glass plate after 1min with 300 μm of knifing rod knifing on clean glass plate
Enter in distilled water water-bath, treat that film solidifies and automatically strips glass plate, use deionized water wash and remove residual
Solvent.
6) after film finally being soaked into 48h in deionized water, it is placed in and dries naturally at room temperature, that is, obtains
PVDF/MWCNTs composite membranes.
Fig. 1 is that Kynoar prepared by embodiment 1 is schemed with the SEM of CNT flat composite membrane.Pass through
ESEM is to pvdf membrane (a) and four kinds of p-MWCNT/PVDF (b), 0.49%MWCNT-COOH
(c), 2%MWCNT-COOH/PVDF (d), 3.86%MWCNT-COOH/PVDF (e) composite membranes
Surface, the CNT for adding different modification degrees is can be seen that from film exterior view to pure pvdf membrane table
The size in the aperture in face, obvious influence is distributed with.As carboxylated degree increases, the aperture and hole on surface
Gap rate gradually increases, and there is a small amount of CNT group on the surface of the compound pvdf membrane of unmodified CNT
It is poly- so that film surface becomes fine and close, uneven, the carbon nano-tube compound film surface of corresponding carboxylated
Aperture and porosity increase, and uniformly.
Claims (9)
1. the masking of a kind of Kynoar and carbon nano-tube compound film is formulated and preparation method thereof, and its feature exists
In, the method step is as follows,
1) a certain amount of MWCNTs is weighed, with dimethylformamide (DMF) as solvent, is made
MWCNTs ultrasound 40min in DMF, disperse MWCNTs abundant.
2) Kynoar (PVDF) powder is drying a period of time using preposition in baking oven, goes water removal
Point.
3) PVDF powder is added to and casting solution is made into MWCNTs/DMF systems, and in 70 DEG C of perseverance
4h is stirred vigorously in tepidarium, PVDF powder is fully dissolved, obtain uniform solution.
4) by gained casting solution sealing preserve, standing deaeration overnight at room temperature.
5) liquid film is soaked together with glass plate after 1min with 300 μm of knifing rod knifing on clean glass plate
Enter in distilled water water-bath, treat that film solidifies and automatically strips glass plate, use deionized water wash and remove residual
Solvent
6) after film finally being soaked into 48h in deionized water, it is placed in and dries naturally at room temperature, that is, obtains
PVDF/MWCNTs composite membranes.
2. the masking formula of a kind of Kynoar according to claim 1 and carbon nano-tube compound film and
Its preparation method, it is characterised in that material therefor is Kynoar, dimethylformamide, unmodified
Multi-walled carbon nano-tubes, 0.49% functionalized multi-wall carbonnanotubes, 2% functionalized multi-wall carbonnanotubes, 3.86% carboxylic
Base multi-walled carbon nano-tube and deionized water etc..
3. the masking formula of a kind of Kynoar according to claim 1 and carbon nano-tube compound film and
Its preparation method, it is characterised in that during with casting solution, makes MWCNTs ultrasound 40min in DMF,
Disperse MWCNTs abundant.
4. the masking formula of a kind of Kynoar according to claim 1 and carbon nano-tube compound film and
Its preparation method, it is characterised in that during with casting solution, 4h is stirred vigorously in 70 DEG C of waters bath with thermostatic control, is made
PVDF powder fully dissolves, and obtains uniform solution.
5. the masking formula of a kind of Kynoar according to claim 1 and carbon nano-tube compound film and
Its preparation method, it is characterised in that casting solution sealing preserve, stands deaeration overnight at room temperature.
6. the masking formula of a kind of Kynoar according to claim 1 and carbon nano-tube compound film and
Its preparation method, it is characterised in that with 300 μm of knifing rod knifing on clean glass plate, after 1min
By liquid film together with glass plate immersion distilled water water-bath.
7. the masking formula of a kind of Kynoar according to claim 1 and carbon nano-tube compound film and
Its preparation method, it is characterised in that wash off the residual solvent on composite membrane with deionized water, and by film
48h in deionized water is soaked, preservation is dried afterwards.
8. the masking formula of a kind of Kynoar according to claim 1 and carbon nano-tube compound film and
Its preparation method, it is characterised in that surface and cross-section morphology feature from composite membrane, unmodified carbon
The carbon nano-tube compound film section of nanotube and 0.49% carboxyl-content is all fine and close aperture, relative with surface
Answer, as carboxylated degree increases, porosity increases, and mechanical property is improved.
9. the masking formula of a kind of Kynoar according to claim 1 and carbon nano-tube compound film and
Its preparation method, it is characterised in that from TG and DTG curves, five kinds of films are at about 420 DEG C
Place starts to decompose, and the heat decomposition temperature of pvdf membrane is 450 DEG C, and MWCNT/PVDF films bring up to 454
DEG C, and with the increase of carboxylated degree, the heat decomposition temperature of composite membrane rises 4-5 DEG C successively.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510800032.4A CN106693726A (en) | 2015-11-18 | 2015-11-18 | Formula for preparing polyvinylidene fluoride and carbon nanotube composite film and preparation method of formula |
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| CN201510800032.4A CN106693726A (en) | 2015-11-18 | 2015-11-18 | Formula for preparing polyvinylidene fluoride and carbon nanotube composite film and preparation method of formula |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108097223A (en) * | 2017-10-30 | 2018-06-01 | 天津工业大学 | A kind of ultrasonic wave added phase inversion prepares multi-walled carbon nanotube/polyvinylidene fluoride porous film MATERIALS METHODS |
| CN108201795A (en) * | 2017-12-22 | 2018-06-26 | 江苏大学 | A kind of preparation method of Selective Separation Enoxacin molecularly imprinted composite membrane material |
| CN108251072A (en) * | 2018-03-05 | 2018-07-06 | 北京科技大学 | A kind of preparation method of liquid metal composite phase-change material |
| CN108854595A (en) * | 2018-06-28 | 2018-11-23 | 华南师范大学 | Modified PVDF plate membrane of a kind of nano biological charcoal and the preparation method and application thereof |
| CN109621756A (en) * | 2019-01-28 | 2019-04-16 | 沈阳建筑大学 | The preparation method of high-throughput resistant to pollution PVDF ultrafiltration membrane |
| CN110141975A (en) * | 2019-05-17 | 2019-08-20 | 李文国 | A kind of multi-walled carbon nanotube-polyacrylonitrile (MWCNT-PAN) composite hyperfiltration membrane and preparation method thereof |
| CN110143851A (en) * | 2019-06-06 | 2019-08-20 | 太仓沪试试剂有限公司 | A method of n-butanol is purified using membrane separation technique |
| CN110961132A (en) * | 2019-11-14 | 2020-04-07 | 济南市环境研究院 | C3N4Preparation method and application of modified organic membrane |
| CN112316558A (en) * | 2020-10-28 | 2021-02-05 | 鄂尔多斯市清科紫荆技术开发有限公司 | High-efficiency integrated water purification equipment polymer and CNTs (carbon nanotubes) composite filter material for sewage treatment and preparation method thereof |
| CN116889857A (en) * | 2023-07-11 | 2023-10-17 | 四川农业大学 | Film gradient diffusion method for in-situ selective monitoring lead effective state |
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| CN104530614A (en) * | 2014-12-25 | 2015-04-22 | 武汉工程大学 | Porous polyvinylidene fluoride-carbon nanotube composite material and preparation method thereof |
| CN104829976A (en) * | 2015-05-27 | 2015-08-12 | 陕西科技大学 | Method for manufacturing composite dielectric materials from polyvinylidene fluoride and end carboxyl multi-walled carbon nano-tubes |
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| CN104530614A (en) * | 2014-12-25 | 2015-04-22 | 武汉工程大学 | Porous polyvinylidene fluoride-carbon nanotube composite material and preparation method thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108097223A (en) * | 2017-10-30 | 2018-06-01 | 天津工业大学 | A kind of ultrasonic wave added phase inversion prepares multi-walled carbon nanotube/polyvinylidene fluoride porous film MATERIALS METHODS |
| CN108201795A (en) * | 2017-12-22 | 2018-06-26 | 江苏大学 | A kind of preparation method of Selective Separation Enoxacin molecularly imprinted composite membrane material |
| CN108251072B (en) * | 2018-03-05 | 2020-08-25 | 北京科技大学 | Preparation method of liquid metal composite phase-change material |
| CN108251072A (en) * | 2018-03-05 | 2018-07-06 | 北京科技大学 | A kind of preparation method of liquid metal composite phase-change material |
| CN108854595A (en) * | 2018-06-28 | 2018-11-23 | 华南师范大学 | Modified PVDF plate membrane of a kind of nano biological charcoal and the preparation method and application thereof |
| CN109621756A (en) * | 2019-01-28 | 2019-04-16 | 沈阳建筑大学 | The preparation method of high-throughput resistant to pollution PVDF ultrafiltration membrane |
| CN110141975A (en) * | 2019-05-17 | 2019-08-20 | 李文国 | A kind of multi-walled carbon nanotube-polyacrylonitrile (MWCNT-PAN) composite hyperfiltration membrane and preparation method thereof |
| CN110143851A (en) * | 2019-06-06 | 2019-08-20 | 太仓沪试试剂有限公司 | A method of n-butanol is purified using membrane separation technique |
| CN110143851B (en) * | 2019-06-06 | 2022-06-07 | 太仓沪试试剂有限公司 | Method for purifying n-butanol by membrane separation technology |
| CN110961132A (en) * | 2019-11-14 | 2020-04-07 | 济南市环境研究院 | C3N4Preparation method and application of modified organic membrane |
| CN112316558A (en) * | 2020-10-28 | 2021-02-05 | 鄂尔多斯市清科紫荆技术开发有限公司 | High-efficiency integrated water purification equipment polymer and CNTs (carbon nanotubes) composite filter material for sewage treatment and preparation method thereof |
| CN116889857A (en) * | 2023-07-11 | 2023-10-17 | 四川农业大学 | Film gradient diffusion method for in-situ selective monitoring lead effective state |
| CN116889857B (en) * | 2023-07-11 | 2024-04-02 | 四川农业大学 | Film gradient diffusion method for in-situ selective monitoring lead effective state |
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Application publication date: 20170524 |