CN104437120A - Polyvinyl chloride ultrafiltration membrane based on ordered arrangement of carbon nano tubes and preparation method and application thereof - Google Patents

Polyvinyl chloride ultrafiltration membrane based on ordered arrangement of carbon nano tubes and preparation method and application thereof Download PDF

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CN104437120A
CN104437120A CN201410660229.8A CN201410660229A CN104437120A CN 104437120 A CN104437120 A CN 104437120A CN 201410660229 A CN201410660229 A CN 201410660229A CN 104437120 A CN104437120 A CN 104437120A
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ultrafiltration membrane
ordered arrangement
preparation
polyvinyl chloride
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CN104437120B (en
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牛晓君
吴浩
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South China University of Technology SCUT
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Abstract

The invention belongs to the technical field of composite materials and discloses a polyvinyl chloride ultrafiltration membrane based on ordered arrangement of carbon nano tubes and a preparation method and an application of the polyvinyl chloride ultrafiltration membrane. The preparation method comprises the following steps: carrying out reaction on FeCl3.6H2O, FeSO4.7H2O and carbon nano tubes to obtain a magnetic carbon nano tube under an alkaline condition, carrying out ultrasonic dispersion in the solvent, stirring for 8-20h with polyvinyl chloride and a pore-forming agent, and dissolving and blending uniformly to form a casting solution; defoaming the prepared casting solution and placing onto a support and coating; acting on the coated membrane for 5-10min under the magnetic field intensity of 200-400Oe, and immersing into deionized water for solvent exchange to obtain the polyvinyl chloride ultrafiltration membrane based on ordered arrangement of carbon nano tubes. The ultrafiltration membrane has the advantage of good separating capacity, and can be applied to the fields of protein separation, industrial waste water treatment, recycling of reclaimed water and the like.

Description

A kind of Pvc Ultrafiltration Membrane based on CNT ordered arrangement and preparation method thereof and application
Technical field
The invention belongs to technical field of composite materials, be specifically related to a kind of Pvc Ultrafiltration Membrane based on CNT ordered arrangement and preparation method thereof and application.
Background technology
CNT, due to performances such as the one dimension tubular structure of its uniqueness, the optical, electrical, hot of excellence, is considered to the perfect additive of novel nanocomposite materials, has many potential application in bioengineering, catalytic chemistry, biochemistry, material science.CNT is studied as membrane material additive is also existing, but by the rare research of CNT ordered arrangement on film.
Compared with the CNT of random orientation, arrange performance and functional characteristic that orderly CNT has many excellences, it has better nanoaperture structure and higher specific area, show electricity and the optical property of some uniquenesses, as the anisotropy of electric property, polarisation of light effect and higher light transmission, in optics and photoelectric device, there is extensive use.CNT ordered arrangement on film then makes film define better conductive network passage, realizes good dynamic changes process, substantially increases the performance of film.
Orderly carbon nano-tube compound film preparation method can be divided into two kinds, and a kind of is first prepare unordered carbon nano-tube compound film, then makes disordered carbon nanotube ordered arrangement by post processing; Another kind is first synthesizing ordered carbon nano pipe array, then with polymer monomer generation home position polymerization reaction, obtains composite membrane.A kind of front method is simple to operate, and the method that post processing realizes CNT ordered arrangement has magnetic field orientating method, electric field orientation method, liquid crystalline phase induced orientation method etc.
Summary of the invention
For above prior art, primary and foremost purpose of the present invention is the preparation method providing a kind of Pvc Ultrafiltration Membrane based on CNT ordered arrangement.
Another object of the present invention is to provide a kind of Pvc Ultrafiltration Membrane based on CNT ordered arrangement prepared by above-mentioned preparation method.
Another object of the present invention is to provide the above-mentioned application of Pvc Ultrafiltration Membrane in the fields such as Separation of Proteins, Industrial Wastewater Treatment, Treated sewage reusing based on CNT ordered arrangement.
The object of the invention is achieved through the following technical solutions:
Based on a preparation method for the Pvc Ultrafiltration Membrane of CNT ordered arrangement, comprise following operating procedure:
(1) by FeCl 36H 2o, FeSO 47H 2o and CNT mixing, add deionized water, under room temperature, ultrasonic process 10 ~ 60min, obtains black suspension, then under nitrogen protection, stirring is warming up to 55 ~ 70 DEG C, drip NaOH solution to pH>12, reaction 1 ~ 1.5h, cold filtration, sediment spends deionized water to neutral final vacuum drying 12 ~ 24 hours, and grinding obtains the magnetic CNT of tool;
(2) by magnetic for tool CNT ultrasonic disperse in solvent, successively polyvinyl chloride, pore former are added, stir 8 ~ 20h dissolve evenly blended, formed casting solution;
(3) by after the casting solution deaeration for preparing, being placed on supporter and carrying out film, then perpendicular to the direction of supporter applying the magnetic field that intensity is 200 ~ 400Oe, making film act on 5 ~ 10min under magnetic field;
(4) carry out exchange of solvent to become with liquid level the angle of 60 ~ 90 ° to immerse in deionized water after the film after step (3) being processed stops 30 ~ 60s in atmosphere, obtain the Pvc Ultrafiltration Membrane of CNT ordered arrangement.
FeCl described in step (1) 36H 2o, FeSO 47H 2the mass parts ratio that O and CNT add is: FeCl 36H 2o 0.97 ~ 4.48 part, FeSO 47H 2o 0.50 ~ 2.30 part, CNT 0.1 ~ 2 part.
The preferred external diameter of CNT described in step (1) is 10 ~ 40nm, length <2 μm, purity >97%, and specific area is 100 ~ 210m 2the CNT of/g.
Polyvinyl chloride preferred degree of polymerization described in step (2) is the polyvinyl chloride of 1000 ~ 3000.
Solvent described in step (2) is selected from one or more the mixture in DMF, DMA and 1-METHYLPYRROLIDONE.
Pore former described in step (2) is selected from one or more the mixture in polyvinylpyrrolidone, polyethylene glycol, glycerine, propane diols, ethylene glycol, acetone, oxalic acid and lithium chloride; Preferred mean molecule quantity is the polyvinylpyrrolidone of 5000 ~ 200000.
Ultrasonic disperse described in step (2) refers to ultrasonic disperse 0.5 ~ 1.5h under frequency is the condition of 20 ~ 60kHz.
The mass percentage of the magnetic CNT of tool, polyvinyl chloride, pore former and the solvent described in step (2) is the magnetic CNT 0.05 ~ 5% of tool, polyvinyl chloride 5 ~ 22%, pore former 1 ~ 10%, and surplus is solvent.
Deaeration described in step (3) refers to standing 12 ~ 30h deaeration; The polyester non-woven fabric that described supporter is preferably level and smooth, carbon fiber or glass plate; The thickness of described film is 150 ~ 450 μm.
Based on a Pvc Ultrafiltration Membrane for CNT ordered arrangement, prepared by above-mentioned preparation method.
The above-mentioned application of Pvc Ultrafiltration Membrane in the fields such as Separation of Proteins, Industrial Wastewater Treatment, Treated sewage reusing based on CNT ordered arrangement.
Preparation principle of the present invention is for passing through FeCl 36H 2o and FeSO 47H 2o generates Fe in the basic conditions 3o 4, Fe 3o 4be carried on CNT and make it have magnetic, then by externally-applied magnetic field, magnetic carbon nano-tube is produced and align, obtain the Pvc Ultrafiltration Membrane based on CNT ordered arrangement.
Had the following advantages and beneficial effect by preparation method of the present invention and the product tool that obtains:
(1) magnetic ferroferric oxide is generated by chemical coprecipitation, it is made to be carried on carbon nano tube surface, not only flexibly simple, convenient, make CNT orientations under magnetic fields, and the existence of the tri-iron tetroxide more excellent performance that also made film have;
(2) pass through the content regulating the CNT added in preparation method of the present invention, casting solution concentration, the ratio of pore former, can control efficiently to the pore structure of film, hydrophily, charge etc., and then optimizes the separating property of film.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that the film of embodiment 1 acts under magnetic field.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
(1) by FeCl 36H 2o 0.97g, FeSO 47H 2(external diameter is 40nm, length <2 μm, purity >97% to O 0.50g and CNT 0.1g, and specific area is 100m 2/ g) mixing, add deionized water, under room temperature, ultrasonic process 30min, obtains black suspension, then under nitrogen protection, stirring is warming up to 65 DEG C, drip NaOH to pH>12, reaction 1h, cold filtration, sediment spends deionized water to neutral final vacuum drying 12 hours, and grinding obtains the magnetic CNT of tool;
(2) magnetic for the tool of 0.5wt% CNT is added the N of 80wt%, in N-dimethylacetylamide, ultrasonic disperse 0.5h under supersonic frequency is 60kHz, be the polyvinyl chloride of 1000 again by the 13wt% degree of polymerization, 6.5wt% mean molecule quantity be 5000 polyvinylpyrrolidone join ultrasonic after solution in, stir 16h at ambient temperature, obtain dissolving the casting solution mixed;
(3) after casting solution standing and defoaming 24h, be coated in by casting solution on plate glass, the THICKNESS CONTROL of coat film is at 350 μm, and the speed of coating is 1.2m/min; Then perpendicular to the direction of plate glass applying the magnetic field that intensity is 400Oe, make film act on 5min under magnetic field, its schematic diagram acted under magnetic field as shown in Figure 1;
(4) to become the angle of 60 ° to immerse in deionized water with liquid level after the film after step (3) being processed stops 60s in atmosphere, exchange of solvent 24h, taking-up is dried, and obtains the Pvc Ultrafiltration Membrane based on CNT ordered arrangement.
Pure water flux and bisphenol-A (BPA) rejection of the polyvinyl chloride-CNT composite hyperfiltration membrane of the present embodiment all adopt dead-end filtration to measure on YL-300 ultrafiltration cup.When ultrafiltration pressure is 100kpa, pure water flux is 601.6L/m 2h, BPA rejection is 56.8%.
Embodiment 2
(1) by FeCl 36H 2o 2.24g, FeSO 47H 2(external diameter is 10nm, length <2 μm, purity >97% to O 1.15g and CNT 1.0g, and specific area is 210m 2/ g) mixing, add deionized water, under room temperature, ultrasonic process 10min, obtains black suspension, then under nitrogen protection, stirring is warming up to 55 DEG C, drip NaOH to pH>12, reaction 1.5h, cold filtration, sediment spends deionized water to neutral final vacuum drying 12 hours, and grinding obtains the magnetic CNT of tool;
(2) magnetic for the tool of 0.08wt% CNT is added the N of 83wt%, in N-dimethylacetylamide, ultrasonic disperse 1.5h under supersonic frequency is 50kHz, be the polyvinyl chloride of 3000 again by the 14wt% degree of polymerization, 2.92wt% mean molecule quantity be 200000 polyvinylpyrrolidone join ultrasonic after solution in, stir 12h at ambient temperature, obtain dissolving the casting solution mixed;
(3) after casting solution standing and defoaming 22h, be coated in by casting solution on plate glass, the THICKNESS CONTROL of coat film is at 350 μm, and the speed of coating is 1.2m/min; Then perpendicular to the direction of plate glass applying the magnetic field that intensity is 200Oe, film is made to act on 10min under magnetic field;
(4) immerse in deionized water with the angle in 90 ° with liquid level after the film after step (3) being processed stops 30s in atmosphere, exchange of solvent 24h, taking-up is dried, and obtains the Pvc Ultrafiltration Membrane based on CNT ordered arrangement.
Pure water flux and bisphenol-A (BPA) rejection of the polyvinyl chloride-CNT composite hyperfiltration membrane of the present embodiment all adopt dead-end filtration to measure on YL-300 ultrafiltration cup.When ultrafiltration pressure is 100kpa, pure water flux is 210.2L/m 2h, BPA rejection is 68.2%.
Embodiment 3
(1) by FeCl 36H 2o 4.48g, FeSO 47H 2(external diameter is 30nm, length <2 μm, purity >97% to O 2.30g and CNT 2.0g, and specific area is 180m 2/ g) mixing, add deionized water, under room temperature, ultrasonic process 60min, obtains black suspension, then under nitrogen protection, stirring is warming up to 70 DEG C, drip NaOH to pH>12, reaction 1h, cold filtration, sediment spends deionized water to neutral final vacuum drying 24 hours, and grinding obtains the magnetic CNT of tool;
(2) magnetic for the tool of 2.5wt% CNT is added the N of 80wt%, in N-dimethylacetylamide, ultrasonic disperse 1.0h under supersonic frequency is 60kHz, be the polyvinyl chloride of 2000 again by the 15wt% degree of polymerization, 2.5wt% mean molecule quantity be 50000 polyvinylpyrrolidone join ultrasonic after solution in, stir 18h at ambient temperature, obtain dissolving the casting solution mixed;
(3) after casting solution standing and defoaming 30h, be coated in by casting solution on plate glass, the THICKNESS CONTROL of coat film is at 350 μm, and the speed of coating is 1.2m/min; Then perpendicular to the direction of plate glass applying the magnetic field that intensity is 300Oe, film is made to act on 10min under magnetic field;
(4) to become the angle of 75 ° to immerse in deionized water with liquid level after the film after step (3) being processed stops 60s in atmosphere, exchange of solvent 24h, taking-up is dried, and obtains the Pvc Ultrafiltration Membrane based on CNT ordered arrangement.
Pure water flux and bisphenol-A (BPA) rejection of the polyvinyl chloride-CNT composite hyperfiltration membrane of the present embodiment all adopt dead-end filtration to measure on YL-300 ultrafiltration cup.When ultrafiltration pressure is 100kpa, pure water flux is 489.9L/m 2h, BPA rejection is 57.7%.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.

Claims (10)

1., based on a preparation method for the Pvc Ultrafiltration Membrane of CNT ordered arrangement, it is characterized in that comprising following operating procedure:
(1) by FeCl 36H 2o, FeSO 47H 2o and CNT mixing, add deionized water, under room temperature, ultrasonic process 10 ~ 60min, obtains black suspension, then under nitrogen protection, stirring is warming up to 55 ~ 70 DEG C, drip NaOH solution to pH>12, reaction 1 ~ 1.5h, cold filtration, sediment spends deionized water to neutral final vacuum drying 12 ~ 24 hours, and grinding obtains the magnetic CNT of tool;
(2) by magnetic for tool CNT ultrasonic disperse in solvent, successively polyvinyl chloride, pore former are added, stir 8 ~ 20h dissolve evenly blended, formed casting solution;
(3) by after the casting solution deaeration for preparing, being placed on supporter and carrying out film, then perpendicular to the direction of supporter applying the magnetic field that intensity is 200 ~ 400Oe, making film act on 5 ~ 10min under magnetic field;
(4) carry out exchange of solvent to become with liquid level the angle of 60 ~ 90 ° to immerse in deionized water after the film after step (3) being processed stops 30 ~ 60s in atmosphere, obtain the Pvc Ultrafiltration Membrane of CNT ordered arrangement.
2. the preparation method of a kind of Pvc Ultrafiltration Membrane based on CNT ordered arrangement according to claim 1, is characterized in that: the FeCl described in step (1) 36H 2o, FeSO 47H 2the mass parts that O and CNT add is: FeCl 36H 2o 0.97 ~ 4.48 part, FeSO 47H 2o 0.50 ~ 2.30 part, CNT 0.1 ~ 2 part.
3. the preparation method of a kind of Pvc Ultrafiltration Membrane based on CNT ordered arrangement according to claim 1, it is characterized in that: the CNT described in step (1) refers to that external diameter is 10 ~ 40nm, length <2 μm, purity >97%, specific area is 100 ~ 210m 2the CNT of/g.
4. the preparation method of a kind of Pvc Ultrafiltration Membrane based on CNT ordered arrangement according to claim 1, it is characterized in that: the solvent described in step (2) refers to N, one or more mixture in dinethylformamide, DMA and 1-METHYLPYRROLIDONE; Described polyvinyl chloride refers to that the degree of polymerization is the polyvinyl chloride of 1000 ~ 3000; Described pore former refers to one or more the mixture in polyvinylpyrrolidone, polyethylene glycol, glycerine, propane diols, ethylene glycol, acetone, oxalic acid and lithium chloride.
5. the preparation method of a kind of Pvc Ultrafiltration Membrane based on CNT ordered arrangement according to claim 4, is characterized in that: described pore former refers to that mean molecule quantity is the polyvinylpyrrolidone of 5000 ~ 200000.
6. the preparation method of a kind of Pvc Ultrafiltration Membrane based on CNT ordered arrangement according to claim 1, is characterized in that: the ultrasonic disperse described in step (2) refers to ultrasonic disperse 0.5 ~ 1.5h under frequency is the condition of 20 ~ 60kHz.
7. the preparation method of a kind of Pvc Ultrafiltration Membrane based on CNT ordered arrangement according to claim 1, it is characterized in that: the mass percentage of the magnetic CNT of tool, polyvinyl chloride, pore former and the solvent described in step (2) is: the magnetic CNT 0.05 ~ 5% of tool, polyvinyl chloride 5 ~ 22%, pore former 1 ~ 10%, surplus is solvent.
8. the preparation method of a kind of Pvc Ultrafiltration Membrane based on CNT ordered arrangement according to claim 1, is characterized in that: the deaeration described in step (3) refers to standing 12 ~ 30h deaeration; Described supporter refers to level and smooth polyester non-woven fabric, carbon fiber or glass plate; The thickness of described film is 150 ~ 450 μm.
9. based on a Pvc Ultrafiltration Membrane for CNT ordered arrangement, it is characterized in that: prepared by the preparation method described in any one of claim 1 ~ 8.
10. the application of Pvc Ultrafiltration Membrane in Separation of Proteins, Industrial Wastewater Treatment, Treated sewage reusing field based on CNT ordered arrangement according to claim 9.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108970421A (en) * 2018-08-21 2018-12-11 成都市水泷头化工科技有限公司 A kind of carbon nanotube-cellulose acetate film and preparation method efficiently to desalinize seawater
CN110052169A (en) * 2019-04-25 2019-07-26 武汉大学 A kind of method that magnetic carbon nano-tube is modified to complex reverse osmosis membrane
CN114653209A (en) * 2022-03-21 2022-06-24 东南大学 Preparation method and application of magnetic conductive microfiltration membrane

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* Cited by examiner, † Cited by third party
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WO2022010941A1 (en) * 2020-07-06 2022-01-13 Lawrence Livermore National Security, Llc Nanoporous membranes for fast diffusion of ions and small molecules

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104117292A (en) * 2014-08-01 2014-10-29 天津工业大学 Preparation method of polymer/inorganic nano-material composite ultrafiltration membrane

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104117292A (en) * 2014-08-01 2014-10-29 天津工业大学 Preparation method of polymer/inorganic nano-material composite ultrafiltration membrane

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108970421A (en) * 2018-08-21 2018-12-11 成都市水泷头化工科技有限公司 A kind of carbon nanotube-cellulose acetate film and preparation method efficiently to desalinize seawater
CN108970421B (en) * 2018-08-21 2020-11-20 义乌市富顺箱包有限公司 Method for efficiently desalinating seawater by using carbon nano tube-cellulose acetate membrane
CN110052169A (en) * 2019-04-25 2019-07-26 武汉大学 A kind of method that magnetic carbon nano-tube is modified to complex reverse osmosis membrane
CN114653209A (en) * 2022-03-21 2022-06-24 东南大学 Preparation method and application of magnetic conductive microfiltration membrane

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