CN103301756A - Preparation method of nanometer TiO2-PA laminated film - Google Patents
Preparation method of nanometer TiO2-PA laminated film Download PDFInfo
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- CN103301756A CN103301756A CN201310271122XA CN201310271122A CN103301756A CN 103301756 A CN103301756 A CN 103301756A CN 201310271122X A CN201310271122X A CN 201310271122XA CN 201310271122 A CN201310271122 A CN 201310271122A CN 103301756 A CN103301756 A CN 103301756A
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Abstract
The invention discloses a preparation method of a nanometer TiO2-PA laminated film. According to the method, nanometer TiO2 particles are effectively scattered in the film through interfacial polymerization, so that the filtration flux of a PA film is effectively improved; moreover, the nanometer TiO2 particles can be effectively adhered to the PA film for a long time, so that the problem that the TiO2 particles easily drop off to cause the situation the TiO2 concentration of the film during the using process is reduced in the traditional preparation method is solved, and the stability of the nanometer TiO2-PA laminated film is ensured; and therefore, the preparation method has good application prospect and important research significance.
Description
Technical field
The invention belongs to the synthesis of polymer material field, relate in particular to a kind of nano-TiO
2The preparation method of-PA laminated film.
Background technology
Nanofiltration (nanofiltration, NF are called for short nanofiltration) is a kind of Aspect of some new membrane processes take pressure as driving force between counter-infiltration and ultrafiltration, and the pore diameter range of nano-filtration membrane (abbreviation NF membrane) is about several nanometers.Can hold back organic molecule and most of inorganic salts are seen through, operating pressure is low, good application prospect is arranged in food industry, biochemical industry and water treatment etc. aspect many.Nano-filtration membrane block relative molecular mass less than 1000, greater than 100, filled up the blank between milipore filter and the reverse osmosis membrane.NF membrane can be held back the solute that can see through milipore filter; And can not hold back the solute (such as water) that can see through reverse osmosis membrane.
Nano-filtration membrane is considered to the most effectively instrument of water treatment procedure gradually.The nanofiltration film preparation generally is divided into two large classes: a kind of method by dipper precipitation; Another kind is to prepare by interfacial polymerization.The NF film has advantages of a lot, and is low such as running cost, filtration flux is high and to filterability of salt and organic matter excellence etc.Nano-filtration membrane has shown huge application prospect in isolated by filtration, but the film pollution remains nano-filtration membrane in the required significant problem that overcomes of commercialization process, and film pollutes the filter efficiency that will cause film and descends.Therefore research prevents that the method for modifying of NF film pollution is very important.
Titanium dioxide (TiO
2) have widely at photocatalysis, sensor, the aspect such as antibiotic and to use.Relevant studies have shown that, because titanium dioxide has a good light catalytic activity, therefore promotion organic substance decomposing that can be effectively, utilizes the composite nano titanium dioxide particle to prepare filter membrane and can effectively solve the problem that film pollutes.
Traditional preparation TiO
2-PA laminated film (TiO
2-polyamide laminated film) method generally is with TiO
2Directly deposit at PA film (PA membrane) matrix, in order to allow TiO
2Particle is attached on the PA film, however this preparation TiO
2-PA laminated film method is easy to make TiO
2Particle causes TiO in the PA film because the not strong problem of adhesive force breaks away from the PA film surface
2Granule density descends, and then affects the performance of composite membrane; In addition, adopt the method for this direct impregnation also to have TiO
2The problem that distribution of particles is inhomogeneous.Therefore in order to prepare the more TiO of stability and high efficiency
2-PA laminated film is developed new preparation method and technology and is just seemed particularly important, and the present invention therefore.
Summary of the invention
The problem that the present invention solves is to provide a kind of nano-TiO for preparing
2The method of-PA laminated film.Nano-TiO by this method preparation
2-PA complex thin film structure is stable, has solved TiO among traditional preparation method
2Particle easily comes off and causes in use TiO of film
2The problem that concentration reduces.
In order to solve these problems of the prior art, concrete technical scheme provided by the invention is as follows:
A kind of nano-TiO for preparing
2The method of-PA laminated film is characterized in that described method comprises following two steps:
(1) preparation of porous polyether sulfone (PES) carrier: polyether sulfone is dissolved in forms solution in the DMF, then in water-bath, precipitating on the nonwoven, use again the unnecessary solvent of distilled water flush away, form porous polyether sulfone (PES) carrier;
(2) nano-TiO
2The preparation of-PA laminated film: the polyether sulfone carrier of preparation immersed carry out surface coating in the mixed aqueous solution contain NaOH and m-phenylene diamine (MPD), then with nano-TiO
2Particle is dispersed in the mixed solution of 1,1-, two chloro-1-fluoroethanes and 1,3,5-benzene, three formyl chlorides, and the polyether sulfone carrier after then the surface being coated is immersed in and is dispersed with nano-TiO
2Carry out interfacial polymerization in the mixed solution of particle, make the polyether sulfone carrier surface form nano-TiO
2-PA laminated film; With prepared nano-TiO
2The curing of-PA laminated film obtains final nano-TiO
2-PA laminated film.
Preferably, the molecular weight of polyether sulfone is 58000g/mol in the described method step (1).
Preferably, in the mixed solution of the polyether sulfone described in the described method step (1) and DMF, the mass fraction of polyether sulfone is 10-20%.
The THICKNESS CONTROL of the porous polyether sulfone carrier layer that preferably, prepares in the described method step (1) is at 100-200 μ m.
Preferably, the preparation whole process of porous polyether sulfone carrier needs to carry out under 20-25 ℃ the constant temperature in the described method step (1).
Preferably, nano-TiO in the described method step (2)
2The particle diameter of particle is 20-30nm.
Preferably, the mass fraction that contains m-phenylene diamine (MPD) in the mixed aqueous solution of NaOH and m-phenylene diamine (MPD) in the described method step (2) is 1-3%; The mass fraction of NaOH is 0.03-0.06%.
Preferably, nano-TiO in the described method step (2)
2The dispersion steps of particle adopts ultrasonic dispersion, and ultrasonic jitter time is 1-2h, disperses to carry out at ambient temperature.
Preferably, 1 described in the described method step (2), the mass fraction of TMC is 0.1-0.5% in the mixed solution of 1-two chloro-1-fluoroethanes (HCFC) and 1,3,5-benzene, three formyl chlorides (TMC).
Preferably, the polyether sulfone carrier impregnation time is 1-3 minute in the described method step (2).
Preferably, nano-TiO in the described method step (2)
2The condition of cure of-PA laminated film is: temperature is 60-80 ℃, and the time is 1-5 minute.
Preferably, TiO described in the described method step (2)
2Nano-TiO in the-PA laminated film
2The mass fraction of particle is no more than 6%.
Nano-filtration membrane is low because of running cost, filtration flux is high and the advantages such as filterability of salt and organic excellence have been obtained great concern.The invention provides a kind of nano-TiO
2The method of-PA laminated film, the method by interfacial polymerization so that nano-TiO
2Particle is dispersed in the film effectively, has not only effectively improved the filtration flux of PA film, and nano-TiO
2Particle can be attached on the PA film for a long time, has solved TiO among traditional preparation method
2Particle easily comes off and causes in use TiO of film
2The problem that concentration reduces.Method of the present invention improved divided thin film from permeability and selective; And nanomaterials and nanotechnology given polymeric material new character and purposes, has good widely application prospect and important Research Significance.
Preparation method of the present invention is divided into two steps: a) preparation of porous polyether sulfone (PES) carrier; B) nano-TiO
2The preparation of-PA laminated film.Wherein a) middle porous polyether sulfone carrier is that polyether sulfone prepares in DMF (DMF) solvent.As preferably, described a) in the molecular weight of polyether sulfone be 58000g/mol.As preferably, solution is that precipitation makes porous polyether sulfone carrier under water bath condition on the nonwoven.As preferably, in the mixed solution of described polyether sulfone and DMF, the mass fraction of polyether sulfone is 10-20%.As preferably, the THICKNESS CONTROL of prepared porous polyether sulfone carrier layer is at 100-200 μ m.As preferably, prepared porous polyether sulfone carrier need to be with distilled water with the residual solvent of thorough flush away.As preferably, the preparation whole process of described porous polyether sulfone carrier needs to carry out under 20-25 ℃ the constant temperature.
B) nano-TiO
2The preparation of-PA laminated film is first the polyether sulfone carrier to be carried out the surface to coat in containing NaOH and m-phenylene diamine (MPD) (m-MPD) aqueous solution; Then with nano-TiO
2Particle is dispersed in the mixed solution of 1,1-, two chloro-1-fluoroethanes (HCFC) and 1,3,5-benzene, three formyl chlorides (TMC).The polyether sulfone carrier of handling well is immersed in nano-TiO
2In the dispersion soln of particle.The polyether sulfone carrier impregnation time is 1-3 minute, by interfacial polymerization so that form nano-TiO at the polyether sulfone carrier
2-PA laminated film.Be described b) middle polyether sulfone carrier and nano-TiO
2Be 1-3 minute interface recombination time of particle.
As preferably, described b) particle diameter of TiO2 is 20-30nm in.As preferably, the mass fraction of m-MPD is 1-3% in the described aqueous solution that contains NaOH and m-phenylene diamine (MPD) (MPD); The mass fraction of NaOH is 0.03-0.06%.
As preferably, in order to guarantee nano-TiO
2Particle is uniformly dispersed, and adopts ultrasonic dispersion, and ultrasonic jitter time is 1-2h, disperses to carry out at ambient temperature.As preferably, described 1, the mass fraction of TMC is 0.1-0.5% in the mixed solution of 1-two chloro-1-fluoroethanes (HCFC) and 1,3,5-benzene, three formyl chlorides (TMC).
As preferably, the nano-TiO for preparing
2-PA laminated film need be cured.As preferably, described condition of cure is: temperature is 60-80 ℃, and the time is 1-5 minute.As preferably, TiO
2Nano-TiO in the-PA laminated film
2The mass fraction of particle is no more than 6%.
Therefore, all things considered the invention provides a kind of method for preparing nano TiO 2-PA laminated film, may further comprise the steps:
(1) preparation polyether sulfone carrier.Polyether sulfone is dissolved in forms solution in the DMF, then in water-bath, precipitating on the nonwoven, then use the residual solvent of distilled water flush away.
(2) the polyether sulfone carrier of preparation in (1) is immersed carry out surface in the mixed aqueous solution that contains NaOH and m-phenylene diamine (MPD) and coat, then remove surperficial excessive m-phenylene diamine (MPD) solution by rotation.
(3) with nano-TiO
2Particle is ultrasonic to be dispersed in the mixed solution of 1,1-, two chloro-1-fluoroethanes and 1,3,5-benzene, three formyl chlorides, then the polyether sulfone carrier is immersed in and carries out interfacial polymerization in the mixed solution, so that nano-TiO
2-PA laminated film forms at the polyether sulfone carrier surface.
(4) prepared laminated film is worn out in air furnace obtain TiO
2-PA laminated film.
With respect to scheme of the prior art, advantage of the present invention is:
The invention provides a kind of nano-TiO for preparing
2The method of-PA laminated film has not only improved the filtration flux of PA film and nano-TiO effectively
2Particle can be attached on the PA film for a long time effectively, has solved TiO among traditional preparation method
2Particle easily comes off and causes in use TiO of film
2The problem that concentration reduces has guaranteed nano-TiO
2Therefore the stability of-PA laminated film have a good application prospect and important Research Significance.
The specific embodiment
Below in conjunction with specific embodiment such scheme is described further.Should be understood that these embodiment are not limited to limit the scope of the invention for explanation the present invention, all equivalent transformations that Spirit Essence is done according to the present invention or modification all should be encompassed within protection scope of the present invention.The implementation condition that adopts among the embodiment can be done further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in the normal experiment.
Embodiment 1 nano-TiO
2The preparation of-PA laminated film
(1) preparation of polyether sulfone carrier.
Under 25 ℃ constant temperature and good stirring condition, polyether sulfone is dissolved in forms solution in the DMF, the mass fraction of polyether sulfone is 17%, then precipitates at nonwoven under water bath condition.The THICKNESS CONTROL of carrier layer is removed the residual solvent of carrier with the distilled water washing at last at 160 μ m, obtains the carrier of porous.
(2) nano-TiO
2The preparation of-PA laminated film.
First the polyether sulfone carrier is soaked 2min in the aqueous solution that contains NaOH and m-phenylene diamine (MPD) (m-MPD), carry out the surface and coat, wherein the mass fraction of m-phenylene diamine (MPD) is 2%; The mass fraction of NaOH is 0.04%.
With nano-TiO
2Particle joins in the mixed solution of 1,1-, two chloro-1-fluoroethanes (HCFC) and 1,3,5-benzene, three formyl chlorides (TMC), and wherein 1,3, the mass fraction of 5-benzene three formyl chlorides is 0.3%, ultrasonic 1.5h makes its Uniform Dispersion.
The polyether sulfone carrier of handling well is immersed in nano-TiO
2In the dispersion soln of particle, by interfacial polymerization so that form nano-TiO at the polyether sulfone carrier
2-PA laminated film.The interfacial polymerization time is 2 minutes.With the TiO that makes
2-PA laminated film is put into air furnace and is cured, and solidification temperature is 60 ℃, and the time is 5 minutes, obtains final nano-TiO
2-PA laminated film.
Embodiment 2 nano-TiOs
2The preparation of-PA laminated film
(1) preparation of polyether sulfone carrier.
Under 25 ℃ constant temperature and good stirring condition, polyether sulfone is dissolved in forms solution in the DMF, the mass fraction of polyether sulfone is 17%, then precipitates at nonwoven under water bath condition.The THICKNESS CONTROL of carrier layer is removed the residual solvent of carrier with the distilled water washing at last at 160 μ m, obtains the carrier of porous.
(2) nano-TiO
2The preparation of-PA laminated film.
First the polyether sulfone carrier is soaked 2min in the aqueous solution that contains NaOH and m-phenylene diamine (MPD) (m-MPD), carry out the surface and coat, wherein the mass fraction of m-phenylene diamine (MPD) is 3%; The mass fraction of NaOH is 0.05%.
With nano-TiO
2Particle joins in the mixed solution of 1,1-, two chloro-1-fluoroethanes (HCFC) and 1,3,5-benzene, three formyl chlorides (TMC), and wherein 1,3, the mass fraction of 5-benzene three formyl chlorides is 0.5%, ultrasonic 1.5h makes its Uniform Dispersion.
The polyether sulfone carrier of handling well is immersed in nano-TiO
2In the dispersion soln of particle, by interfacial polymerization so that form nano-TiO at the polyether sulfone carrier
2-PA laminated film.The interfacial polymerization time is 3 minutes.With the TiO that makes
2-PA laminated film is put into air furnace and is cured, and solidification temperature is 60 ℃, and the time is 5 minutes, obtains final nano-TiO
2-PA laminated film.
Embodiment 3 nano-TiOs
2The preparation of-PA laminated film
(1) preparation of polyether sulfone carrier.
Under 25 ℃ constant temperature and good stirring condition, polyether sulfone is dissolved in forms solution in the DMF, the mass fraction of polyether sulfone is 17%, then precipitates at nonwoven under water bath condition.The THICKNESS CONTROL of carrier layer is removed the residual solvent of carrier with the distilled water washing at last at 180 μ m, obtains the carrier of porous.
(2) nano-TiO
2The preparation of-PA laminated film.
First the polyether sulfone carrier is soaked 1min in the aqueous solution that contains NaOH and m-phenylene diamine (MPD) (m-MPD), carry out the surface and coat, wherein the mass fraction of m-phenylene diamine (MPD) is 2%; The mass fraction of NaOH is 0.04%.
With nano-TiO
2Particle joins in the mixed solution of 1,1-, two chloro-1-fluoroethanes (HCFC) and 1,3,5-benzene, three formyl chlorides (TMC), and wherein 1,3, the mass fraction of 5-benzene three formyl chlorides is 0.3%, ultrasonic 1.5h makes its Uniform Dispersion.
The polyether sulfone carrier of handling well is immersed in nano-TiO
2In the dispersion soln of particle, by interfacial polymerization so that form nano-TiO at the polyether sulfone carrier
2-PA laminated film.The interfacial polymerization time is 3 minutes.With the TiO that makes
2-PA laminated film is put into air furnace and is cured, and solidification temperature is 60 ℃, and the time is 6 minutes, obtains final nano-TiO
2-PA laminated film.
MgSO with 2000ppm
4The aqueous solution of solution, the character of detection film under the 1MPa condition.
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Salt rejection rate | 93.6% | 98.3% | 95.6% |
| Flux (L/m 2h） | 24.6 | 15.5 | 21.6 |
Simultaneously under this condition, carry out follow-on test, through 3 days, the nano-TiO in the NF membrane
2Content substantially do not have to reduce, and adopt the NF membrane nano particle of general sedimentation preparation to lose 30%.
Resulting NF membrane has good rejection effect for salt, and good stability is arranged.
Above to a kind of nano-TiO for preparing provided by the present invention
2The method of-PA laminated film has been described in detail and introduces.Above-mentioned example only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the people who is familiar with technique can understand content of the present invention and according to this enforcement, can not limit protection scope of the present invention with this.All equivalent transformations that Spirit Essence is done according to the present invention or modification all should be encompassed within protection scope of the present invention.
Claims (12)
1. one kind prepares nano-TiO
2The method of-PA laminated film is characterized in that described method comprises following two steps:
(1) preparation of porous polyether sulfone (PES) carrier: polyether sulfone is dissolved in forms solution in the DMF, then in water-bath, precipitating on the nonwoven, use again the unnecessary solvent of distilled water flush away, form porous polyether sulfone (PES) carrier;
(2) nano-TiO
2The preparation of-PA laminated film: the polyether sulfone carrier of preparation immersed carry out surface coating in the mixed aqueous solution contain NaOH and m-phenylene diamine (MPD), then with nano-TiO
2Particle is dispersed in the mixed solution of 1,1-, two chloro-1-fluoroethanes and 1,3,5-benzene, three formyl chlorides, and the polyether sulfone carrier after then the surface being coated is immersed in and is dispersed with nano-TiO
2Carry out interfacial polymerization in the mixed solution of particle, make the polyether sulfone carrier surface form nano-TiO
2-PA laminated film; With prepared nano-TiO
2The curing of-PA laminated film obtains final nano-TiO
2-PA laminated film.
2. method according to claim 1 is characterized in that the molecular weight of polyether sulfone in the described method step (1) is 58000g/mol.
3. method according to claim 1 is characterized in that in the mixed solution of the polyether sulfone described in the described method step (1) and DMF, the mass fraction of polyether sulfone is 10-20%.
4. method according to claim 1 is characterized in that the THICKNESS CONTROL of the porous polyether sulfone carrier layer for preparing in the described method step (1) is at 100-200 μ m.
5. method according to claim 1, the preparation whole process that it is characterized in that porous polyether sulfone carrier in the described method step (1) need to carry out under 20-25 ℃ the constant temperature.
6. method according to claim 1 is characterized in that nano-TiO in the described method step (2)
2The particle diameter of particle is 20-30nm.
7. method according to claim 1, the mass fraction that it is characterized in that containing in the described method step (2) m-phenylene diamine (MPD) in the mixed aqueous solution of NaOH and m-phenylene diamine (MPD) is 1-3%; The mass fraction of NaOH is 0.03-0.06%.
8. method according to claim 1 is characterized in that nano-TiO in the described method step (2)
2The dispersion steps of particle adopts ultrasonic dispersion, and ultrasonic jitter time is 1-2h, disperses to carry out at ambient temperature.
9. method according to claim 1 is characterized in that 1 described in the described method step (2), and the mass fraction of TMC is 0.1-0.5% in the mixed solution of 1-two chloro-1-fluoroethanes (HCFC) and 1,3,5-benzene, three formyl chlorides (TMC).
10. method according to claim 1 is characterized in that the polyether sulfone carrier impregnation time is 1-3 minute in the described method step (2).
11. method according to claim 1 is characterized in that nano-TiO in the described method step (2)
2The condition of cure of-PA laminated film is: temperature is 60-80 ℃, and the time is 1-5 minute.
12. method according to claim 1 is characterized in that TiO described in the described method step (2)
2Nano-TiO in the-PA laminated film
2The mass fraction of particle is no more than 6%.
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Application publication date: 20130918 |