CN104548945A - After-treatment method for increasing flux of ultra-filtration membrane - Google Patents
After-treatment method for increasing flux of ultra-filtration membrane Download PDFInfo
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- CN104548945A CN104548945A CN201310504737.2A CN201310504737A CN104548945A CN 104548945 A CN104548945 A CN 104548945A CN 201310504737 A CN201310504737 A CN 201310504737A CN 104548945 A CN104548945 A CN 104548945A
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Abstract
The invention discloses an after-treatment method for increasing the flux of an ultra-filtration membrane. The after-treatment method comprises the following steps: after the ultra-filtration membrane is prepared and formed, carrying out solution impregnation on the ultra-filtration membrane, wherein the solution is an aqueous solution of one or more of tetrahydrofuran, N,N-dimethyl formamide, N,N-dimethyl acetamide, N,N-dimethyl acrylamide, N-methyl pyrrolidone, 2-methyl pyrrolidone, dimethyl sulfoxide, tetramethyl sulfoxide, sulfolane, pyridine, methyl pyridine, dimethyl pyridine, dioxane, acetonitrile, hexamethylene amide, morpholine, hydrochloric acid, sulfuric acid, sodium hydroxide and chloroform. The after-treatment method disclosed by the invention has the advantages that the interception rate is maintained, and simultaneously the flux is increased. The after-treatment process is easy to operate and relatively low in increased cost, and conforms to the development direction of high performance and low cost in the membrane industry.
Description
Technical field
The present invention relates to technical field of membrane, furtherly, relate to a kind of post-processing approach improving milipore filter flux.
Background technology
Along with the industrialized high speed development of China, the situation of water resource pollutes aggravation day by day, water resources shortage and water pollutions have day by day seriously become the bottleneck of restriction Chinese society progress and economic development, Membrane Separation for Water Treatment is the important technology solving resource-type lack of water and water quality type water shortage problem, and the development of high performance membrane material obtains the great attention of global range.The development of current global high performance membrane product presents following several respects feature: film industry is to high-performance, low cost and greenization future development.
With regard to current most of business optimal experimental design technique, the performance of its film, rejection and flux phase separation step is shaping complete after namely determine, to select so focus mostly on to the modified technique of milipore filter at the additive of casting solution.Such as: Chinese patent CN102512998A adds flux and the rejection that molecular sieve has improved milipore filter in casting solution; Chinese patent CN102921317A adds certain density surfactant in casting solution, and the performance of its milipore filter is not less than the prerequisite of prior art in rejection under, flux increases.And the technique related to for milipore filter post processing employs the technology of ultra-violet radiation or Plasma-Modified more, such as: Chinese patent CN102921316A, Chinese patent CN102029117A and Chinese patent CN102512998A, it by adding after reactant monomer by ultraviolet radiation graft modification in casting solution; Chinese patent CN102722844A has then selected and added hydrophilic block copolymers in casting solution, afterwards with surface ionizing technology modification, the hydrophilicity of film is improved.Above patent all needs to add property-modifying additive in casting solution, easily causes and increases the difficulty of casting solution quality control; Ultra-violet radiation and surface ionizing technology easily bring the raising of preparation cost, the problem of complex operation.
Summary of the invention
For solving produced problem in prior art, the invention provides a kind of post-processing approach improving milipore filter flux.Flux can be improved while its rejection of maintenance.After this process operations is simple, increases cost lower.Meet the high-performance of film industry, low cost developing direction.
The object of this invention is to provide a kind of post-processing approach improving milipore filter flux.
Comprise:
After optimal experimental design is shaping, solution impregnation is carried out to it,
Described solution is oxolane (THF), N, dinethylformamide (DMF), N, the aqueous solution of one or more in N-dimethylacetylamide (DMAc), N, N-dimethylpropionamide, 1-METHYLPYRROLIDONE (NMP), 2-methyl pyrrolidone, dimethyl sulfoxide (DMSO) (DMSO), tetramethyl sulfoxide, sulfolane, pyridine, picoline, lutidines, dioxane, acetonitrile, hexa-methylene acid amides, morpholine, hydrochloric acid, sulfuric acid, NaOH, chloroform.
Wherein, preferred:
The aqueous solution is 10-600 second to milipore filter infiltrating time, and infiltration temperature is 15-45 DEG C.
Milipore filter, after solution impregnation, spends deionized water.Deionized water wash time is preferably 10 ~ 60 seconds.
The water flux of handled milipore filter improves a lot, and rejection remains unchanged.
Method of the present invention is applicable with the performance improvement process to membrane material in tubular filter, hollow fiber form filter and spiral winded type filter.
The present invention breaches the constraint of existing theory, inventor thinks, milipore filter is contacted with the aqueous solution having the preparation of reagents of certain solvability to become to it, can cause ultrafiltration membrane surface separating layer membrane structure that slight to dissolve and swelling occurs under the action of the solvent, reduce the separating layer thickness of milipore filter, thus improve flux; By the concentration of control treatment liquid and with the microcellular structure that can ensure film surface time of contact of milipore filter, obvious change can not occur, thus ensure that its rejection.
Detailed description of the invention
Below in conjunction with embodiment, further illustrate the present invention.
Embodiment is raw materials used as follows:
Polysulfones
U.S. solvay Udel solid particle
Oxolane (THF), N, dinethylformamide (DMF), N, N-dimethylacetylamide (DMAc), N, N-dimethylpropionamide, 1-METHYLPYRROLIDONE (NMP), 2-methyl pyrrolidone, dimethyl sulfoxide (DMSO) (DMSO), tetramethyl sulfoxide, sulfolane, pyridine, picoline, lutidines, dioxane, acetonitrile, hexa-methylene acid amides, morpholine, hydrochloric acid, sulfuric acid, NaOH, chloroform Beijing Chemical Plant analyze pure
Embodiment 1-3
In this group embodiment, list the test performance adopting milipore filter obtained by different solutions post processing.The liquor capacity concentration of post processing in embodiment is 10%, and compound method is measure selected reagent to be placed in volumetric flask, then adds deionized water to scale.Be specially embodiment 1, embodiment 2, the volumetric concentration that embodiment 3 selects oxolane (THF), DMA (DMAc), N-ethyl pyrrolidone (NMP) to be mixed with respectively is the solution of 10%.The solution prepared is preserved under room temperature (22 DEG C).
Use and retain the polysulphone super-filter membrane that PEG molecular weight is 100,000, contact 60 seconds with under the solution normal temperature configured, then in the water of 25 DEG C, rinsing was preserved in deionized water after 10 minutes.
Milipore filter good for post processing is tested flux with pure water under the pressure of 0.1MPa, add afterwards PEG molecular weight be 100,000 solution carry out rejection test, test result is in table 1.
Comparative example 1
Comparative example 1 adopts and identical with embodiment 1-3 retains the polysulphone super-filter membrane that PEG molecular weight is 100,000, but does not carry out the post processing of milipore filter, and in the experiment tested at water flux and rejection, also all adopts identical condition with embodiment.Test result is in table 1.
Table 1
The test result of table 1 shows, through post processing milipore filter experiment selected by test condition under, flux is significantly improved, and rejection remains unchanged substantially.
Comparative example 2
In contrast milipore filter moulding process in phase separation step, coagulating bath add organic solvent and with organic solvent post processing after the difference of milipore filter performance:
1) milipore filter casting solution is configured.Be dissolved in DMF by polysulfones at 80 DEG C, stir until dissolve, the Polymer Solution of obtained transparent and homogeneous, leave standstill 24h deaeration after dissolving completely, the concentration of polymer solution controls at 20wt%.
2) milipore filter is prepared with phase inversion.Casting solution scraper is evenly distributed on chemical fiber non-woven fabric surface, primary film is (25 2 DEG C, soil in atmosphere, relative humidity 40-60%) after standing a period of time, film is immersed (coagulating bath is respectively the mixed solution of deionized water and deionized water and 10%wt THF) in coagulating bath, after 10 minutes, milipore filter taking-up is placed in a large amount of deionized water and preserves to remove residual solvent completely.
3) coagulating bath be the mixed solution post processing 60 second of milipore filter at deionized water and 10%wt THF of deionized water, test with polyethylene glycol PEG100000 solution under the pressure of 0.2MPa afterwards, the pure water flux of this film is 258L/m
2the rejection of h, PEG100000 is 92.8%.Be that the milipore filter of deionized water and 10%wt THF is tested with polyethylene glycol PEG100000 solution under the pressure of 0.2MPa coagulating bath, the pure water flux of this film is 136L/m
2the rejection of h, PEG100000 is 93.3%
Embodiment 4-6
In this group embodiment, list the test performance of the milipore filter adopted obtained by different THF concentration post-treatment solution.In embodiment, selected experimental procedure and method, experiment condition are all identical with described in embodiment 1-3.
Test result is in table 2.
Table 2
As can be seen from the data of table 2, the concentration no matter infiltrating solution is how many, and the water flux of the milipore filter after solution impregnation rises all to some extent, and infiltrate solution concentration larger, water flux ascensional range is larger; And while water flux rises, rejection remains unchanged substantially.
Embodiment 7-9
In this group embodiment, list the results of property of milipore filter post processing different time.In this group embodiment, the THF aqueous solution of 10% is all adopted to process milipore filter.Selected experimental procedure is all identical with described in embodiment 1-3 with method, experiment condition.
Test result is in table 3
Table 3
As can be seen from the data of table 3, milipore filter is longer through the time of solution impregnation, and water flux ascensional range is larger.
Embodiment 10-12
In this group embodiment, list the milipore filter post processing result that molecular cut off is different, be specially embodiment 10, embodiment 11, embodiment 12 select respectively molecular cut off be 200,000,50,000 and 20,000 milipore filter.In this group embodiment, the THF aqueous solution of 10% is all adopted to process milipore filter.Selected experimental procedure is all identical with described in embodiment 1-3 with method, experiment condition.
Test result is in table 4
Table 4
Claims (4)
1. improve a post-processing approach for milipore filter flux, it is characterized in that described method comprises:
After optimal experimental design is shaping, solution impregnation is carried out to it,
Described solution is oxolane (THF), N, dinethylformamide (DMF), N, the aqueous solution of one or more in N-dimethylacetylamide (DMAc), N, N-dimethylpropionamide, 1-METHYLPYRROLIDONE (NMP), 2-methyl pyrrolidone, dimethyl sulfoxide (DMSO) (DMSO), tetramethyl sulfoxide, sulfolane, pyridine, picoline, lutidines, dioxane, acetonitrile, hexa-methylene acid amides, morpholine, hydrochloric acid, sulfuric acid, NaOH, chloroform.
2. the post-processing approach improving milipore filter flux as claimed in claim 1, is characterized in that:
The aqueous solution is 10-600 second to milipore filter infiltrating time, and infiltration temperature is 15-45 DEG C.
3. the post-processing approach improving milipore filter flux as claimed in claim 1, is characterized in that:
Milipore filter, after solution impregnation, spends deionized water.
4. the post-processing approach improving milipore filter flux as claimed in claim 3, is characterized in that:
Deionized water wash time is 10 ~ 60 seconds.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105032220A (en) * | 2015-09-08 | 2015-11-11 | 南京工业大学 | Preparation method of permanent hydrophilic type polysulfone ultrafiltration membrane |
| CN106621829A (en) * | 2015-10-28 | 2017-05-10 | 中国石油化工股份有限公司 | Composite reverse osmosis membrane preparation method and composite reverse osmosis membrane |
| CN107056298A (en) * | 2016-12-01 | 2017-08-18 | 西安科技大学 | A kind of production method of the high-intensity high-density Delanium with low-resistivity |
| CN107899436A (en) * | 2017-11-24 | 2018-04-13 | 贵阳时代沃顿科技有限公司 | A kind of preparation method of the alkaline-resisting NF membrane of high-performance |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105032220A (en) * | 2015-09-08 | 2015-11-11 | 南京工业大学 | Preparation method of permanent hydrophilic type polysulfone ultrafiltration membrane |
| CN106621829A (en) * | 2015-10-28 | 2017-05-10 | 中国石油化工股份有限公司 | Composite reverse osmosis membrane preparation method and composite reverse osmosis membrane |
| CN107056298A (en) * | 2016-12-01 | 2017-08-18 | 西安科技大学 | A kind of production method of the high-intensity high-density Delanium with low-resistivity |
| CN107056298B (en) * | 2016-12-01 | 2020-02-21 | 西安科技大学 | Production method of high-strength high-density artificial graphite with low resistivity |
| CN107899436A (en) * | 2017-11-24 | 2018-04-13 | 贵阳时代沃顿科技有限公司 | A kind of preparation method of the alkaline-resisting NF membrane of high-performance |
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Application publication date: 20150429 |