CN105056775B - A kind of CNT activeness and quietness PSF hollow-fibre membranes and preparation method thereof - Google Patents
A kind of CNT activeness and quietness PSF hollow-fibre membranes and preparation method thereof Download PDFInfo
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- CN105056775B CN105056775B CN201510545741.2A CN201510545741A CN105056775B CN 105056775 B CN105056775 B CN 105056775B CN 201510545741 A CN201510545741 A CN 201510545741A CN 105056775 B CN105056775 B CN 105056775B
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Abstract
The present invention provides a kind of CNT activeness and quietness PSF hollow-fibre membranes and preparation method thereof, and described hollow-fibre membrane includes each component of following parts by weight, 5~20 parts of multi-walled carbon nanotube, PSF10~30 part, 60~85 parts of solvent, additive 5~25；The PSF is polysulfones.Using CNT as micromolecule additive, it can not only suppress macropore and be formed, moreover it is possible to because of the property of itself, great activeness and quietness PS membrane, and permeability of the membrane is influenceed little.Doughnut of the present invention has good intensity, elasticity, fatigue resistance, and permeability of the membrane can be preferably.
Description
Technical field
The invention belongs to doughnut technical field of membrane, more particularly, to a kind of hollow fibres of CNT activeness and quietness PSF
Tie up film and preparation method thereof.
Background technology
Polysulfones material is a kind of membrane material for applying a lot, due to its good chemical stability, water resistance, heat-resisting
Property, dimensional stability, and preferably film forming and mechanical strength, micro-filtration, counter-infiltration, ultrafiltration, electrodialysis, gas separation,
Bioengineering, medical treatment etc. are widely used.Polysulfones resinoid be one kind on main chain containing sulfuryl and aromatic ring
High-molecular compound, mainly there are bisphenol-a polysulfone, polyarylsulfone (PAS), polyether sulfone, PPSS etc..As can be seen that sulfone from structure
The both sides of base have phenyl ring to form conjugated system, and because sulphur atom is in highest oxidation state, sulfuryl both sides are highly conjugated in addition,
So this resinoid has excellent inoxidizability, heat endurance and high-temperature fusion stability.
At present, the conventional preparation method of PS membrane is immersion precipitation phase inversion process (NIPS).The method is first will be by polysulfones, molten
The homogeneous casting solution that agent, non-solvent additive are formed at a certain temperature is cast to backing material or by spinning head extruded shape
Into nascent state film, then it is immersed in non-solvent coagulating bath rapidly, by non-in the solvent and coagulating bath in nascent state film
Solvent is exchanged with each other, and constantly reduces the ratio of film internal solvent so that system is separated, final gel solidification film forming.
Polysulfones casting solution occurs to relate generally to thermodynamics and kineticses in phase separation, and the two factors finally determine poly-
The morphosis and performance of sulfone film.The process that is exchanged with each other of the non-solvent in solvent and coagulating bath in nascent state film is power
Process, its speed largely have impact on membrane pore structure：On the premise of other no additives, both get in exchange
It hurry up, the finger-like pore that easier formation is big, penetrating is on the contrary, it is possible to create small and thin finger-like pore even sponge hole.From broad perspectives
For on energy, form, the size in hole, the tensile strength and elongation at break of film, i.e. film strength and toughness can be influenceed.Hole is thinner
Pine is penetrating, aperture is bigger, and the tensile strength and elongation at break of film are smaller；On the contrary, if fenestra is tiny, closely knit, or even form sea
Continuous structure, the tensile strength and elongation at break of film are higher, and intensity and toughness are also better.
Kim, Chakrabarty, Ma etc. have studied performance impact of the additives polyethylene glycol (PEG) to PS membrane.With
The increase of PEG molal weights and content, the viscosity increase of system, the diffusion coefficient between non-solvent and solvent reduce so that poly-
The rate of settling of compound is reduced, and the finger-like pore in membrane structure, which is suppressed, to be gradually decreased, fenestra number and porosity increase, aquifer yield
Decrease.Tsai etc. with the addition of small molecule sorbester p17 in polysulfones casting solution, and research finds that sorbester p17 can suppress finger-like pore
Generation, when its addition progressively increases to 15%, film section structure gradually becomes spongy hole from a large amount of finger-like pores, and film oozes
Permeability can reduce.Equally, viscosity of the non-ionic surfactant Tween 80 due to casting solution can be increased so that the time that is separated prolongs
Long, the aperture of film reduces, and permeance property reduces.As can be seen here, either macromolecular additive or Small molecular surfactant
Addition, formed although macropore can be suppressed, also reduce permeability of the membrane energy.
The content of the invention
In view of this, the present invention is directed to propose a kind of CNT activeness and quietness PSF hollow-fibre membranes and preparation method,
The advantages that its hollow-fibre membrane has that intensity is high, toughness is good, and permeance property is good.
To reach above-mentioned purpose, the technical proposal of the invention is realized in this way：
A kind of CNT activeness and quietness PSF hollow-fibre membranes, include each component of following parts by weight, multi-wall carbon nano-tube
5~20 parts of pipe, 10~30 parts of PSF, 60~85 parts of solvent, 5~25 parts of additive；The PSF is polysulfones.
Using CNT as micromolecule additive, it can not only suppress macropore and be formed, moreover it is possible to because of the property of itself, greatly
Activeness and quietness PS membrane, and permeability of the membrane is influenceed little.
CNT, also known as Baji-tube, it is a kind of One-dimensional Quantum material with special construction, in January, 1991 by day
This physicist Sumio Iijima is found.Mainly be made up of the carbon atom of hexagonal arrangement several layers to tens of layers of CNT
Coaxial pipe is formed.Fixed distance, about 0.34nm are kept between layers, and diameter is generally 2~20nm.
CNT has good mechanical property, and tensile strength reaches 50~200GPa, is 100 times of steel, density is but
Only the 1/6 of steel, an order of magnitude at least higher than ordinary graphite fiber；Its modulus of elasticity is up to 1TPa, the bullet with diamond
Property modulus is suitable, about 5 times of steel.For the CNT of the solid wall with ideal structure, its tensile strength about 800GPa.
Although the structure of CNT is similar to the structure of high polymer material, its structure is more more stable than high polymer material.Carbon is received
Mitron is the material with highest specific strength that can be prepared at present.If PSF and CNT are made into composite, can make multiple
Condensation material shows good intensity, elasticity, fatigue resistance and isotropism, and the performance to composite, which is brought, greatly to be changed
It is kind.
Preferably, the solvent is in dimethyl acetamide, 1-METHYLPYRROLIDONE, dimethylformamide, tetrahydrofuran
One or more.
Preferably, the additive be PEG-4000, PEG-8 00, polyvinylpyrrolidone PVP, ethanol,
The one or more of lithium chloride, acetone.
Preferably, the polysulfones is bisphenol-a polysulfone.
Present invention also offers a kind of method for preparing CNT activeness and quietness PSF hollow-fibre membranes as described above,
First multi-walled carbon nanotube and additive are dissolved in solvent, 1~3h is stirred at 45~60 DEG C, adds PSF, stirring 12~
24h, the feed liquid after stirring is placed into the storage tank of hollow-fibre membrane spinning-drawing machine, 2~5h of vacuum defoamation；Feed liquid after deaeration
Spinning head is delivered to by storage tank under the constant pressure effect that liquid nitrogen provides, while core liquid is also under constant pressure source from the center of spinning head
Hole enters the cavity of doughnut as support and interior coagulating bath；Dynamic analysis of spinning leaves spinning head, by dry-spinning path, into solidifying
Gu groove, through solidification in coagulating basin, into wrapping wire groove, it is wrapped on wire wrapping wheel, hollow-fibre membrane is formed after solidifying completely；Institute
State the air gap of the dry-spinning path between spinning head and coagulating basin；Preferably, the core liquid is distilled water；The constant pressure source is liquid
Nitrogen.
Preferably, the height of the dry-spinning path is 1~15cm.
Preferably, the feed liquid after the deaeration is delivered to spinning head under 0.05MPa~0.3MPa constant pressures by storage tank, and
The temperature of feed liquid is 50 DEG C~60 DEG C.
Preferably, the core liquid enters hollow fibre under 0.05MPa~0.2MPa constant pressure from the center cavity of spinning head
The cavity of dimension, and the temperature of core liquid is 30 DEG C~50 DEG C.
Preferably, the rotating speed of the wire wrapping wheel is 17-37m/min.
Preferably, the temperature of the coagulating basin and wrapping wire groove is 25 DEG C~45 DEG C.
Relative to prior art, CNT activeness and quietness PSF hollow-fibre membranes of the present invention and preparation method thereof,
Have the advantage that：Doughnut of the present invention has good intensity, elasticity, fatigue resistance, and permeability of the membrane energy
Preferably.
Embodiment
The DMAC being previously mentioned in the embodiment of the invention, refers to dimethyl acetamide；NMP is N- crassitudes
Ketone；DMF is dimethylformamide；THF is tetrahydrofuran；PEG-400 is PEG-4000；PEG-800 be polyethylene glycol-
800；PVP is polyvinylpyrrolidone.
The present invention will be described in detail by embodiment below.
Embodiment one
A kind of CNT activeness and quietness PSF hollow-fibre membranes, include each component of following parts by weight, multi-wall carbon nano-tube
8 parts of pipe, 17 parts of PSF, 68 parts of NMP, 5 parts of PVP, 2 parts of ethanol.The polysulfones PSF is bisphenol-a polysulfone.
By the following method, hollow-fibre membrane is prepared：First multi-walled carbon nanotube, PVP, ethanol are mixed with NMP, added
Heat stirs 1h to 45 DEG C, adds PSF, stirs 24h, and the feed liquid after stirring is placed into the storing of hollow-fibre membrane spinning-drawing machine
In tank, vacuum defoamation 2h；Feed liquid after deaeration is delivered to spinneret under the 0.15MPa constant pressures effect that liquid nitrogen provides by storage tank
Head, and the temperature of feed liquid is 50 DEG C, while core liquid also enters under the 0.1MPa that constant pressure source provides from the center cavity of spinning head
The cavity of doughnut is as support and interior coagulating bath, and the temperature of core liquid is 40 DEG C；Dynamic analysis of spinning leaves spinning head, through overdrying
Journey is spun, into coagulating basin, through solidification in coagulating basin, into wrapping wire groove, is wrapped on wire wrapping wheel, in being formed after solidifying completely
Empty fiber membrane；The air gap of the dry-spinning path between spinning head and coagulating basin；The core liquid is distilled water；The constant pressure source
For liquid nitrogen.The dry-spinning path is highly 10cm；The linear velocity of wire wrapping wheel is 17m/min；The temperature of coagulating basin and wrapping wire groove is
40℃。
The intensity of the present embodiment institute wire vent is 0.45kg power, and elongation at break 165%, monofilament flux is 268L/m2·
h；Wherein intensity and elongation at break with reference to " plastic tensile method for testing performance GB/T1040-92 ", monofilament flux with reference to " in
Fibre ultrafiltration film method of testing HYT 050-1999 ".
Embodiment two
A kind of CNT activeness and quietness PSF hollow-fibre membranes, include each component of following parts by weight, multi-wall carbon nano-tube
12 parts of pipe, 18 parts of PSF, 65 parts of NMP, 5 parts of PEG-4000.The polysulfones is bisphenol-a polysulfone.
By the following method, hollow-fibre membrane is prepared：First multi-walled carbon nanotube, NMP and PEG-4000 are mixed
Close, be heated to 45 DEG C, stir 1h, add PSF, stir 24h, the feed liquid after stirring is placed into hollow-fibre membrane spinning-drawing machine
In storage tank, vacuum defoamation 2h；Feed liquid after deaeration is delivered to spray under the 0.05MPa constant pressures effect that liquid nitrogen provides by storage tank
Silk head, and the temperature of feed liquid is 60 DEG C, while core liquid also enters under the 0.1MPa that constant pressure source provides from the center cavity of spinning head
Enter the cavity of doughnut as support and interior coagulating bath, and the temperature of core liquid is 50 DEG C；Dynamic analysis of spinning leaves spinning head, passes through
Dry-spinning path, into coagulating basin, through solidification in coagulating basin, into wrapping wire groove, it is wrapped on wire wrapping wheel, is formed after solidifying completely
Hollow-fibre membrane；The air gap of the dry-spinning path between spinning head and coagulating basin.The core liquid is distilled water；The constant pressure
Source is liquid nitrogen；The dry-spinning path is highly 5cm；The linear velocity of wire wrapping wheel is 26m/min；The temperature of coagulating basin and wrapping wire groove is
50℃。
The intensity of the present embodiment institute wire vent is 0.65kg power, and elongation at break 180%, monofilament flux is 245L/m2·
h；Wherein intensity and elongation at break with reference to " plastic tensile method for testing performance GB/T1040-92 ", monofilament flux with reference to " in
Fibre ultrafiltration film method of testing HYT 050-1999 ".
Embodiment three
A kind of CNT activeness and quietness PSF hollow-fibre membranes, include each component of following parts by weight, multi-wall carbon nano-tube
10 parts of pipe, 18 parts of PSF, 65 parts of NMP, 00 7 parts of PEG-8.The polysulfones is bisphenol-a polysulfone.
By the following method, hollow-fibre membrane is prepared：First multi-walled carbon nanotube, PEG-8 00 and NMP are mixed
Close, be heated to 45 DEG C, stir 1h, add PSF, stir 24h, the feed liquid after stirring is placed into hollow-fibre membrane spinning-drawing machine
In storage tank, vacuum defoamation 2h；Feed liquid after deaeration is delivered to spray under the 0.1MPa constant pressures effect that liquid nitrogen provides by storage tank
Silk head, and the temperature of feed liquid is 50 DEG C, while core liquid also enters under the 0.1MPa that constant pressure source provides from the center cavity of spinning head
Enter the cavity of doughnut as support and interior coagulating bath, and the temperature of core liquid is 40 DEG C；Dynamic analysis of spinning leaves spinning head, passes through
Dry-spinning path, into coagulating basin, through solidification in coagulating basin, into wrapping wire groove, it is wrapped on wire wrapping wheel, is formed after solidifying completely
Hollow-fibre membrane；The air gap of the dry-spinning path between spinning head and coagulating basin.The core liquid is distilled water；The constant pressure
Source is liquid nitrogen；The dry-spinning path is highly 10cm；Wrapping wire wheel speed is 20m/min；The temperature of coagulating basin and wrapping wire groove is 35
℃。
The intensity of the present embodiment institute wire vent is 0.5kg power, and elongation at break 210%, monofilament flux is 256L/m2·h。
Wherein intensity and elongation at break are with reference to " plastic tensile method for testing performance GB/T1040-92 ", monofilament flux is with reference to " hollow
Fiber ultrafiltration membrane method of testing HYT 050-1999 ".
Contrast experiment
A kind of PSF hollow-fibre membranes, include each component of following parts by weight, 68 parts of 18 parts of PSF, NMP, 4 parts of PVP,
8 parts of PEG-400,2 parts of ethanol.The polysulfones is bisphenol-a polysulfone.
By the following method, hollow-fibre membrane is prepared：PVP, PEG-400, ethanol are mixed with NMP, are heated to 45
DEG C, 1h is stirred, adds PSF, 24h is stirred, the feed liquid after stirring is placed into the storage tank of hollow-fibre membrane spinning-drawing machine, very
Empty deaeration 2h；Feed liquid after deaeration is delivered to spinning head, and feed liquid under the 0.15MPa constant pressures effect that liquid nitrogen provides by storage tank
Temperature be 50 DEG C, while core liquid also enters doughnut under the 0.1MPa that constant pressure source provides from the center cavity of spinning head
Cavity is as support and interior coagulating bath, and the temperature of core liquid is 40 DEG C；Dynamic analysis of spinning leaves spinning head, by dry-spinning path, enters
Coagulating basin, through solidification in coagulating basin, into wrapping wire groove, it is wrapped on wire wrapping wheel, hollow-fibre membrane is formed after solidifying completely；
The core liquid is distilled water；The constant pressure source is liquid nitrogen；The air gap of the dry-spinning path between spinning head and coagulating basin.Institute
It is highly 10cm to state dry-spinning path；The linear velocity of wire wrapping wheel is 17r/min；The temperature of coagulating basin and wrapping wire groove is 40 DEG C.
The intensity of this contrast experiment institute wire vent is 0.35kg power, and elongation at break 35%, monofilament flux is 260L/m2·
h.Wherein intensity and elongation at break with reference to " plastic tensile method for testing performance GB/T1040-92 ", monofilament flux with reference to " in
Fibre ultrafiltration film method of testing HYT 050-1999 ".
The preferred embodiment of the invention is the foregoing is only, is not intended to limit the invention creation, it is all at this
Within the spirit and principle of innovation and creation, any modification, equivalent substitution and improvements made etc., the invention should be included in
Protection domain within.
Claims (7)
- A kind of 1. CNT activeness and quietness PSF hollow-fibre membranes, it is characterised in that：Include each component of following parts by weight, 5~20 parts of multi-walled carbon nanotube, 10~30 parts of PSF, 60~85 parts of solvent, 5~25 parts of additive；The PSF is polysulfones, institute It is bisphenol-a polysulfone to state polysulfones；The solvent is dimethyl acetamide, 1-METHYLPYRROLIDONE, dimethylformamide, tetrahydrochysene furan More than one or both of muttering；The additive be PEG-4000, PEG-8 00, polyvinylpyrrolidone PVP, Ethanol, lithium chloride, the one or more of acetone.
- 2. a kind of method for preparing CNT activeness and quietness PSF hollow-fibre membranes according to claim 1, its feature exist In：First multi-walled carbon nanotube and additive are dissolved in solvent, 1~3h is stirred at 45~60 DEG C, adds PSF, is stirred 12~24h, the feed liquid after stirring is placed into the storage tank of hollow-fibre membrane spinning-drawing machine, 2~5h of vacuum defoamation；After deaeration Feed liquid is delivered to spinning head under the constant pressure effect that liquid nitrogen provides by storage tank, while core liquid is also under constant pressure source from spinning head Center cavity enters the cavity of doughnut as support and interior coagulating bath；Dynamic analysis of spinning leaves spinning head, by dry-spinning path, enters Enter coagulating basin, through solidification in coagulating basin, into wrapping wire groove, be wrapped on wire wrapping wheel, doughnut is formed after solidifying completely Film；The air gap of the dry-spinning path between spinning head and coagulating basin；The core liquid is distilled water；The constant pressure source is liquid Nitrogen.
- 3. preparation method according to claim 2, it is characterised in that：The height of the dry-spinning path is 1~15cm.
- 4. preparation method according to claim 2, it is characterised in that：Feed liquid after the deaeration 0.05MPa~ Spinning head is delivered to by storage tank under 0.3MPa constant pressures, and the temperature of feed liquid is 50 DEG C~60 DEG C.
- 5. preparation method according to claim 2, it is characterised in that：Constant pressure of the core liquid in 0.05MPa~0.2MPa Under enter the cavity of doughnut from the center cavity of spinning head, and the temperature of core liquid is 30 DEG C~50 DEG C.
- 6. preparation method according to claim 2, it is characterised in that：The linear velocity of the wire wrapping wheel is 17-37m/min.
- 7. preparation method according to claim 2, it is characterised in that：The temperature of the coagulating basin and wrapping wire groove for 25 DEG C~ 45℃。
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| CN105597571B (en) * | 2016-02-29 | 2018-05-01 | 天津大学 | High intensity self-supporting ultrafiltration membrane and preparation method prepared by vacuum aided self assembly |
| CN106334461A (en) * | 2016-09-26 | 2017-01-18 | 天津华清健坤膜科技有限公司 | PVDF and PSF binary blended ultrafiltration membrane and preparation method thereof |
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