CN104624066A - Preparation method of high-flux mixed matrix composite film - Google Patents
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Abstract
The invention relates to a preparation method of a mixed matrix composite film, and particularly relates to a preparation method of a high-flux mixed matrix composite film. The preparation method comprises the following steps: preparing a polysulfone supporting layer from a polysulfone-containing N,N-dimethylformamide (DMF) solution, soaking in an m-phenylenediamine water solution, removing the excessive solution, then coating a titanate organic solution by a certain thickness, enabling a coated polysulfone supporting film to be in contact with an organic solution of trimesoyl chloride, finally, keeping the film in a vacuum drying oven with a temperature of 50-100 DEG C for a certain period of time, and washing with water to obtain the mixed matrix composite film. The preparation method has the advantages that the adopted raw materials are low in price, the method is simple and convenient, under the same operation conditions, the higher the prepared mixed matrix composite film is, the higher the retention rate is, and the higher the efficiency-to-cost of the mixed matrix composite film is.
Description
Technical field
The present invention relates to a kind of preparation method of mixed-matrix composite membrane, specifically refer to a kind of preparation method of high-flux reverse osmosis membrane.
Background technology
Reverse osmosis membrane, is widely used in the aspects such as bitter desalination, desalinization and ultra-pure water production, and organic-inorganic mixed-matrix reverse osmosis composite membrane is a focus of current reverse osmosis membrane research.Because the thickness of ultra-thin composite membrane is very little, therefore, the inorganic material of employing is all nano-scale.At present, more inorganic material is used to have TiO
2nano particle, CNT, Nano Silver, Nano-meter SiO_2
2, zeolite etc.Inorganic material add the hydrophily and roughness that can change film surface, improve membrane flux, strengthen contamination resistance, improve service life of diffusion barrier.
TiO2 nanoparticle dispersion in organic phase TMC solution, adopts the method for original position interfacial polymerization to prepare polyamide-TiO by Hyun Soo Lee etc.
2hybridization compounding NF membrane, experiment finds, works as TiO
2when content is more than 5%, due to TiO
2become more remarkable for polymerizing polyamide interference, the degree of polymerization of hybridized film and mechanical strength decline obviously, and the separating property of hybridized film significantly declines; Also there are certain influence heat treatment temperature and time to separating property simultaneously, and 70 DEG C of process 5 minutes, operating pressure was 0.6MPa, and the rejection of hybridized film to Adlerika reaches more than 95%, and flux is 9.1Lm-2h-1; XPS analysis confirms after the continued operation of 2 days, and in hybridized film, TiO2 content does not change substantially, and TiO is described
2nano particle is combined with polyamide closely, shows that hybridized film has good stability simultaneously.[Hyun Soo Lee,Se Joon Im,Jong Hak Kim,et al,Polyamide thin-film nanofiltration membranes containing TiO2 nanoparticles[J].Desalination 219(2008)48–56].
Kwak and Kim etc. adopt interfacial polymerization method to obtain polyamide ultrathin reverse osmosis membrane, are then immersed and are hydrolyzed by isopropyl titanate the TiO got
2in colloidal sol, make the nano-TiO of positively charged
2in composite film surface self assembly, thus obtained hybridized film.TiO
2under the action of uv light, OH and O2-with strong oxidizing property can be produced, the microorganism on film surface can be killed, turn improve the hydrophily on film surface.Experiment confirms that the antibacterial pollution capacity of hybridized film under illumination condition is significantly improved than under dark condition, is equally also better than the organic film of non-hydridization, and simultaneously when salt rejection rate is identical, flux improves.[Seung–Yeop Kwak,Sung Ho Kim,et al.Hybrid organic/inorganic reverse osmosis(RO)membrane for bactericidal anti-Fouling.1.preparation and characterization of TiO2 nanoparticle self-assembled aromatic polyamide thin-film-composite (TFC)membrane[J],Environmental Science and Technology 2001,35,2388-2394.]
Zhang etc. adopt multi-walled carbon nano-tubes to prepare hydridization polyamide reverse osmosis composite film as dopant material, wherein CNT and the mixing of MPD aqueous phase solution, research finds, due to the multi-pore channel of multi-walled carbon nano-tubes self, hybridized film improves more than 2 times for the flux of the terephthalic acid (TPA) (PTA) of 200ppm, rejection remains on more than 98% simultaneously, and be original 3 times for the flux of the NaCl solution of 2000ppm, but rejection declines obviously, when doping reaches 0.1%, to the rejection of NaCl solution lower than 80%; Contact angle and SEM test result also illustrate, the hydrophily of hybridized film is better, but surface roughness obviously increases.The decline of salt rejection rate shows, the multi-walled carbon nano-tubes in aqueous phase should create impact to the density of film superficial cortical layers, makes superficial cortical layers be not so good as pure polyamide composite film consolidation.In addition, this hybridized film, for the good separation effect of organic matter-aqueous solution, shows potential using value.[Lin Zhang,Guo-Zhong Shi,Shi Qiu,,Li-Hua Cheng,Huan-Lin Chen.Preparation of high-flux thin film nanocomposite reverse osmosis membranes by incorporating functionalized multi-walled carbon nanotubes[J],Desalination and Water Treatment 34(2011)19–24.]
Hang Dong etc. use octadecyl trichlorosilane alkane modified nano-zeolite molecular sieve, have prepared zeolite-polyamide reverse osmosis nano composite membrane, and contact angle experiments confirms, the hydrophily of modified hybridized film with unmodified changing; Counter-infiltration results of property shows, under the same conditions, the flux of modified zeolite hybridization compounding film is higher than unmodified hybridized film, and salt rejection rate also slightly improves.Zeolite doping is that the flux 28.5Lm-2h-1 of 0.05% (w/v) hybridized film is increased to 40.9Lm-2h-1, and salt rejection rate also brings up to 98.5% by from 97.8%.Experimental result shows, the modification of octadecyl trichlorosilane alkane makes zeolite molecular sieve nanocrystal can be dispersed in polyamide cortex well, therefore improves the permeability of water, also maintains high solute rejection.Hang Dong,[Xin-Ying Qu,Lin Zhang,Li-Hua Cheng,Huan-Lin Chen,Cong-Jie Gao,Preparation and characterization of surface-modified zeolite-polyamide thin film nanocomposite membranes for desalination[J],Desalination and Water Treatment 34(2011)6–12.]
Generally speaking, the preparation method of current mixed-matrix reverse osmosis membrane is the oil phase or the aqueous phase that nano particle are mixed into interfacial polymerization, being obtained by interface polymerization reaction. the feature of interface polymerization reaction is that oil phase and aqueous phase all require excessive use, this makes, nano particle has a certain amount of waste, and the dispersion of nano particle is also a difficult point.
Summary of the invention
The deficiency that the preparation method that the present invention is directed to mixed-matrix reverse osmosis membrane at present exists, proposes a kind of efficiency higher, more economical mixed-matrix reverse osmosis membrane preparation method.
The present invention is achieved by following technical proposals:
A preparation method for high flux mixed-matrix composite membrane, is characterized in that comprising the steps:
(1) with the polysulfone supporting layer that DMF (DMF) solution containing mass content 14-16% polysulfones is prepared from, the m-phenylene diamine (MPD) aqueous solution soaking 0.5-5 minute that mass concentration is 1.0-2.5% is put into;
(2) the polysulfones support membrane rubber rollers roll extrusion after m-phenylene diamine (MPD) aqueous solution soaking, removes unnecessary solution;
(3) on polysulfones support membrane, coating is 0.001-0.1% titanate ester organic solution containing mass concentration, the thickness of coating is 10-50 micron, coating duration controlled in 5-20 second, and organic solvent is wherein the one in cyclohexane, n-hexane or heptane;
(4) then the polysulfones support membrane after coating is contacted 10-300 second with the organic solution containing mass concentration being 0.05-0.5% pyromellitic trimethylsilyl chloride, organic solvent is wherein the one in trifluorotrichloroethane, n-hexane or heptane;
(5) above-mentioned film is placed in the vacuum drying oven of 50-100 DEG C keeps 10-15 minute again, obtain mixed-matrix reverse osmosis membrane through washing.
As preferably, in the m-phenylene diamine (MPD) aqueous solution in the step (1) of above-mentioned preparation method, add solution quality than the dodecyl sodium sulfate being 0.1%.Although in the present invention, also object of the present invention can be realized not adding dodecyl sodium sulfate, but after adding the certain amount of dodecyl sodium sulfate, the film prepared by discovery has better effect, this has sufficient embodiment in the performance test process of film.
As preferably, in the step (3) of above-mentioned preparation method, titanate ester refers to one or more mixtures in metatitanic acid methyl esters, tetraethyl titanate, titanium propanolate or butyl titanate, and its mass concentration is 0.04-0.05%.Material in the present invention in titanate ester is a lot, and the present invention considers from many factors such as the performances of economy, film, above-mentioned selected material has comprehensive good result, wherein concentration is also larger on the impact of film properties, so inventor, show that this concentration of 0.04-0.05% has good effect by a large amount of experiments, relative to other concentration clearly.
As preferably, in the step (3) of above-mentioned preparation method, the thickness of coating is 25-30 micron, although certain thickness must be had after coating, but also extremely important for the control of thickness, after verification experimental verification repeatedly, inventor thinks that 25-30 micron has comprehensive performance advantage, if too thick, then obviously can affect water energy, but too thin, then affect rejection equally.
As preferably, polysulfones support membrane in the step (4) of above-mentioned preparation method after coating and control the time of contact of organic solution in 60-80 second, and organic solvent used is trifluorotrichloroethane, and the mass concentration of the organic solution of pyromellitic trimethylsilyl chloride is 0.10-0.15%, control time of contact in 30-40 second.Obviously, in the present invention, control for time of contact is also to realize better effect, although in other time of contact, also have corresponding effect to embody, but inventor is in order to more fully realize the performance of film, can realize on general basis, determine time of contact further, can draw better effect, the selection for organic solvent is the same, although relative to prior art, have multi-solvents to select, when this multiple organic solvent comprehensive, wherein trifluorotrichloroethane is better selection.
As preferably, in the step (5) of above-mentioned preparation method, oven temperature controls at 80 DEG C, and baking time controls at 10-11 minute.Because the temperature in post processing controls to have for the change of group more directly to affect, therefore when repeatedly determining control temperature, inventor thinks 80 DEG C, and baking time controls, when 10-11 minute, to have optimum efficiency.
Beneficial effect: material that the present invention adopts is cheap, and method is easy, the mixed-matrix reverse osmosis membrane of preparation, and under equal service condition, flux is higher, and rejection is higher, the efficiency cost of this film is than higher.
Detailed description of the invention
Example below for setting forth the present invention, and is not used in explanation and limits the scope of the invention.
Embodiment 1
Use the polysulfone supporting layer of DMF solution composition containing 16% polysulfones, put into the m-phenylene diamine (MPD) aqueous solution about two minutes of 1.0%, wherein in the m-phenylene diamine (MPD) aqueous solution containing the dodecyl sodium sulfate (SDS) of 0.1%.Support membrane rubber rollers after m-phenylene diamine (MPD) solution soaks removes the unnecessary solution in front and the back side.On polysulfones support membrane, coating is the cyclohexane solution of 0.05% butyl titanate containing mass concentration, thickness is 25 microns, stop 20 seconds, then this support membrane is contacted 30 seconds with the organic solution containing 0.2% pyromellitic trimethylsilyl chloride, organic solvent is wherein trifluorotrichloroethane; Form ultra-thin titanium dioxide-aramid layer, then this film is put in the vacuum drying oven of 80 DEG C and keep 10 minutes, form titanium dioxide-polyamide mixed-matrix reverse osmosis membrane.
With the NaCl aqueous solution of 2000ppm (millionth mass concentration), the initial performance of test membrane under the pressure of 1MPa.Acquired results is as follows: the initial salt rejection rate of reverse osmosis membrane is 90.39%, and water flux is 58.63 (L/m
2h).
Embodiment 2
Use the polysulfone supporting layer of DMF solution composition containing 16% polysulfones, put into the m-phenylene diamine (MPD) aqueous solution about two minutes of 2%, wherein in the m-phenylene diamine (MPD) aqueous solution containing the dodecyl sodium sulfate (SDS) of 0.1%.Support membrane rubber rollers after m-phenylene diamine (MPD) solution soaks removes the unnecessary solution in front and the back side.On polysulfones support membrane, coating is the cyclohexane solution of 0.05% butyl titanate containing mass concentration, thickness is 25 microns, stop 20 seconds, then this support membrane is contacted 30 seconds with the organic solution containing 0.1% pyromellitic trimethylsilyl chloride, organic solvent is wherein trifluorotrichloroethane; Form ultra-thin titanium dioxide-aramid layer, then this film is put in the vacuum drying oven of 80 DEG C and keep 10 minutes, form titanium dioxide-polyamide mixed-matrix reverse osmosis membrane.
With the NaCl aqueous solution of 2000ppm (millionth mass concentration), the initial performance of test membrane under the pressure of 1MPa.Acquired results is as follows: the initial salt rejection rate of reverse osmosis membrane is 97.39%, and water flux is 45.20 (L/m
2h).
Embodiment 3
Use the polysulfone supporting layer of DMF solution composition containing 16% polysulfones, put into the m-phenylene diamine (MPD) aqueous solution about two minutes of 2.5%, wherein in the m-phenylene diamine (MPD) aqueous solution containing the dodecyl sodium sulfate (SDS) of 0.1%.Support membrane rubber rollers after m-phenylene diamine (MPD) solution soaks removes the unnecessary solution in front and the back side.On polysulfones support membrane, coating is the cyclohexane solution of 0.05% butyl titanate containing mass concentration, thickness is 25 microns, stop 20 seconds, then this support membrane is contacted 30 seconds with the organic solution containing 0.1% pyromellitic trimethylsilyl chloride, organic solvent is wherein trifluorotrichloroethane; Form ultra-thin titanium dioxide-aramid layer, then this film is put in the vacuum drying oven of 80 DEG C and keep 10 minutes, form titanium dioxide-polyamide mixed-matrix reverse osmosis membrane.
With the NaCl aqueous solution of 2000ppm (millionth mass concentration), the initial performance of test membrane under the pressure of 1MPa.Acquired results is as follows: the initial salt rejection rate of reverse osmosis membrane is 98.99%, and water flux is 40.15 (L/m
2h).
Embodiment 4-8
Except the butyl titanate concentration difference of second step coating, the method for operating identical with embodiment 1 is adopted to prepare composite nanometer filtering film.Adopt the method for testing identical with embodiment 3, it the results are shown in following table:
| Embodiment | 4 | 5 | 6 | 7 | 8 |
| Butyl titanate concentration | 0.01％ | 0.04％ | 0.06％ | 0.08％ | 0.1％ |
| Salt rejection rate | 99.09％ | 98.95％ | 98.06％ | 92.08％ | 81.11％ |
| Flux (L/m 2h) | 31.5 | 37.72 | 40.55 | 41.83 | 45.12 |
Embodiment 9-13
Except the butyl titanate thickness difference of second step coating, the method for operating identical with embodiment 1 is adopted to prepare composite nanometer filtering film.Adopt the method for testing identical with embodiment 3, it the results are shown in following table:
| Embodiment | 9 | 10 | 11 | 12 | 13 |
| Coating thickness (micron) | 10 | 15 | 25 | 30 | 40 |
| Salt rejection rate | 97.09％ | 97.95％ | 99.06％ | 99.08％ | 91.11％ |
| Flux (L/m 2h) | 45.12 | 43.72 | 40.55 | 40.83 | 31.5 |
Embodiment 14-16
Except organic solvent difference in step (4), the method for operating identical with embodiment 1 is adopted to prepare composite nanometer filtering film.Adopt the method for testing identical with embodiment 3, it the results are shown in following table:
| Embodiment | 14 | 15 | 16 |
| Organic solvent | Trifluorotrichloroethane | N-hexane | Heptane |
| Salt rejection rate | 97.09％ | 95.95％ | 93.06％ |
| Flux (L/m 2h) | 45.12 | 43.72 | 40.55 |
Embodiment 17-21
Except temperature difference in step (5), the method for operating identical with embodiment 1 is adopted to prepare composite nanometer filtering film.Adopt the method for testing identical with embodiment 3, it the results are shown in following table:
| Embodiment | 17 | 18 | 19 | 20 | 21 |
| Temperature DEG C | 60 | 70 | 80 | 85 | 95 |
| Salt rejection rate | 95.09％ | 96.95％ | 99.06％ | 97.08％ | 96.11％ |
| Flux (L/m 2h) | 41.12 | 42.72 | 45.55 | 43.83 | 39.5 |
Embodiment 22-24
Except time difference in step (5), the method for operating identical with embodiment 1 is adopted to prepare composite nanometer filtering film.Adopt the method for testing identical with embodiment 3, it the results are shown in following table:
| Embodiment | 22 | 23 | 24 |
| Time (minute) | 10 | 12 | 14 |
| Salt rejection rate | 98.02％ | 95.75％ | 94.36％ |
| Flux (L/m 2h) | 45.32 | 41.72 | 38.55 |
Claims (6)
1. a preparation method for high flux mixed-matrix composite membrane, is characterized in that comprising the steps:
(1) with the polysulfone supporting layer that DMF (DMF) solution containing mass content 14-16% polysulfones is prepared from, the m-phenylene diamine (MPD) aqueous solution soaking 0.5-5 minute that mass concentration is 1.0-2.5% is put into;
(2) the polysulfones support membrane rubber rollers roll extrusion after m-phenylene diamine (MPD) aqueous solution soaking, removes unnecessary solution;
(3) on polysulfones support membrane, coating is 0.001-0.1% titanate ester organic solution containing mass concentration, the thickness of coating is 10-50 micron, coating duration controlled in 5-20 second, and organic solvent is wherein the one in cyclohexane, n-hexane or heptane;
(4) then the polysulfones support membrane after coating is contacted 10-300 second with the organic solution containing mass concentration being 0.05-0.5% pyromellitic trimethylsilyl chloride, organic solvent is wherein the one in trifluorotrichloroethane, n-hexane or heptane;
(5) above-mentioned film is placed in the vacuum drying oven of 50-100 DEG C keeps 10-15 minute again, obtain mixed-matrix reverse osmosis membrane through washing.
2. the preparation method of a kind of high flux mixed-matrix composite membrane according to claim 1, is characterized in that adding solution quality than the dodecyl sodium sulfate being 0.1% in the m-phenylene diamine (MPD) aqueous solution in step (1).
3. the preparation method of a kind of high flux mixed-matrix composite membrane according to claim 1, it is characterized in that in step (3), titanate ester refers to one or more mixtures in metatitanic acid methyl esters, tetraethyl titanate, titanium propanolate or butyl titanate, its mass concentration is 0.04-0.05%.
4. the preparation method of a kind of high flux mixed-matrix composite membrane according to claim 1, is characterized in that the thickness of coating in step (3) is 25-30 micron.
5. the preparation method of a kind of high flux mixed-matrix composite membrane according to claim 1, it is characterized in that controlling the time of contact of polysulfones support membrane in step (4) after coating and organic solution in 60-80 second, and organic solvent used is trifluorotrichloroethane, and the mass concentration of the organic solution of pyromellitic trimethylsilyl chloride is 0.10-0.15%, control time of contact in 30-40 second.
6. the preparation method of a kind of high flux mixed-matrix composite membrane according to claim 1, it is characterized in that in step (5), oven temperature controls at 80 DEG C, and baking time controls at 10-11 minute.
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| CN109847597A (en) * | 2018-12-20 | 2019-06-07 | 浙江工业大学 | A kind of high throughput high desalination reverse osmosis membrane and preparation method thereof |
| CN110801737A (en) * | 2019-11-25 | 2020-02-18 | 徐业华 | Preparation method of high-dispersion titanium dioxide doped polyamide reverse osmosis membrane |
| CN110801738A (en) * | 2019-11-25 | 2020-02-18 | 徐业华 | Preparation method of high-dispersion titanium dioxide doped polyamide nanofiltration membrane |
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| C06 | Publication | ||
| PB01 | Publication | ||
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Application publication date: 20150520 |