CN103585891A - Compression-resistant microporous membrane and preparation method thereof - Google Patents
Compression-resistant microporous membrane and preparation method thereof Download PDFInfo
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- CN103585891A CN103585891A CN201310566662.0A CN201310566662A CN103585891A CN 103585891 A CN103585891 A CN 103585891A CN 201310566662 A CN201310566662 A CN 201310566662A CN 103585891 A CN103585891 A CN 103585891A
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Abstract
The invention relates to the technical field of a membrane, in particular to a compression-resistant microporous membrane and a preparation method thereof. The preparation method comprises the steps as follows: a polymer and a structural compound are added in a microporous membrane forming solution, the polymer accounts for 10%-25% of the weight of an overall solution, and the structural compound accounts for 0.05%-2% of the weight of the polymer and comprises a component A and a component B, wherein the component A is a carbon nano tube and/or a carbon fiber, the component B is graphene, a weight ratio of the component A to the component B is 0-1, and the components are stirred for 48 hours at the temperature of 40 DEG C, is subjected to still standing for 4 hours, and is defoamed; and the membrane forming solution is scraped on a membrane support with a tape casting method, the microporous membrane is prepared with a phase inversion method, and specifically, a film casing liquid is exposed in the air for 0.5-3 min, soaked in non-solvent water and cured to form the membrane. With the adoption of the compression-resistant microporous membrane and the preparation method thereof, the compression resistance can be improved, and meanwhile, separation properties such as water flux and the like of the membrane is not lost absolutely.
Description
Technical field
The present invention relates to membrane technology field, be specifically related to a kind of resistance to compression microporous barrier and preparation method thereof.
Background technology
The membrane technology such as ultrafiltration and micro-filtration is widely applied in chemical industry, environmental protection, medicine and other fields in recent years.Meanwhile, milipore filter is also the supporting layer of the composite membranes such as counter-infiltration or nanofiltration.Micro-filtration, ultrafiltration, nanofiltration and counter-infiltration all belong to pressure-actuated membrane process, in running, film is for a long time in pressured state, film can be gradually by densification, cause flux to decline with the prolongation of running time, particularly, as the support membrane of counter-infiltration or nanofiltration, institute's pressure that bears is very high, so the crushing resistance of film is extremely important.
Conventionally, the microcellular structure of film is divided into finger-like pore and spongy hole, and the film of finger-like pore has larger water permeable ability, and the crushing resistance in spongy hole is better, and therefore a lot of research has been reported by changing the pore structure of film and improved its crushing resistance.Application number is that 200710072442.7 patent has been announced and in pvdf membrane, added molysite, and the section structure that changes film improves the close property of resistance to compression of film; It is spongelike structure that Zhou Haiping has obtained section by adjustment preparation liquid composition in the preparation research > > of the polysulphone super-filter membrane of Master's thesis < < density gradient structure, fenestra size is the PS membrane of density gradient, and the crushing resistance of this film is also very good; Model is for also forming by optimizing preparation liquid the poly (ether sulfone) film that has obtained spongy hole in the influence factor in Master's thesis < < structure of polyethersulfone ultrafiltration membranes and performance study > >, and the close property of resistance to compression of this film is significantly improved.
Summary of the invention
Goal of the invention: in order to prepare the better microporous barrier of a kind of compressive property.
The effect that the present invention has clear improvement to the mechanical property of high molecular polymer according to CNT or carbon fiber and Graphene, and they belong to respectively a peacekeeping two-dimensional nano material, after mixing, can form unique microstructure, to adding in Polymer Solution after its modification, by inversion of phases, prepare the microporous barrier of high crushing resistance.
The following scheme of concrete employing:
Scheme 1:
: a kind of crushing resistance microporous barrier preparation method, it is characterized in that, comprise following steps,
In microporous barrier film making solution, add polymer and textural association thing, described polymer accounts for the 10-25wt% of whole solution, described textural association thing accounts for the 0.05-2wt% of polymer weight ratio, comprise A component and B component: A CNT and/or carbon fiber, B Graphene, wherein the weight ratio of A component and B component is 0-1, stirs deaeration in standing 4 hours at 40 ℃ 48 hours;
Film making solution is scraped on masking supporter by the tape casting, utilizes phase inversion to prepare microporous barrier, and concrete grammar is: casting solution immerses in non-solvent water expose 0.5-3min in air after, film-forming.
The further technical scheme of the present invention is, the preferred multi-walled carbon nano-tubes of described CNT.
The further technical scheme of the present invention is, the preferred Graphene of described carbon fiber.
The further technical scheme of the present invention is, the solvent of described microporous barrier film making solution is any one of following solvent, 1-METHYLPYRROLIDONE, DMF, DMA, triethyl phosphate, dimethyl sulfoxide (DMSO), acetone, oxolane.
The further technical scheme of the present invention is, in described microporous barrier film making solution, can comprise as follows one or more as additive, lithium chloride, polyvinylpyrrolidone, polyethylene glycol, water, methyl alcohol, ethanol, formic acid, acetic acid, acetone, oxolane, addition be take amount of polymers and is counted 1-10wt% as benchmark;
The further technical scheme of the present invention is, also comprises prepared film is immersed in to step stand-by in water.
Scheme 2:
A microporous barrier, is characterized in that, the skeleton that comprises CNT or carbon fiber and Graphene structure.
Scheme 3:
The purposes of multi-walled carbon nano-tubes in preparing microporous barrier.
Conclusion is expressed as follows: a kind of crushing resistance microporous barrier preparation method, comprises the following steps:
(1) CNT of organic modification or carbon nano-fiber are mixed with the Graphene of organic modification, add in the microporous barrier film making solution of various routines, comprise that in the solution such as Kynoar (PVDF), polysulfones (PSf), polyether sulfone (PES), polyacrylonitrile (PAN) and cellulose acetate (CA), wherein the ratio of CNT or carbon fiber and Graphene is 0-1;
(2) the polymer concentration scope that consists of of film making solution is 10-25wt%, and the addition of nanometer hybrid particles be take amount of polymers and counted 0.05-2wt% as benchmark;
(3) solvent of film making solution comprises 1-METHYLPYRROLIDONE (NMP), or N, dinethylformamide (DMF), or DMA (DMAc), or triethyl phosphate (TEP), or dimethyl sulfoxide (DMSO) (DMSO), or acetone (AC), or oxolane (THF) etc., can dissolve above-mentioned high molecular polymer, and and the water organic matter that can dissolve each other;
(4) in film making solution, can comprise as follows one or more as additive: lithium chloride, polyvinylpyrrolidone (PVP), polyethylene glycol (PEG), water, methyl alcohol, ethanol, formic acid, acetic acid, acetone, oxolane etc., addition be take amount of polymers and is counted 1-10wt% as benchmark;
(5) film making solution is scraped on masking supporter by the tape casting, utilizes phase inversion to prepare microporous barrier, and concrete grammar is: casting solution immerses in non-solvent water expose 0.5-3min in air after, film-forming;
(6) prepared film is immersed in water stand-by;
(7) prepared film is measured to pure water flux under 0.4MPa, then press down 30min at 1.0MPa, and then measure pure water flux under 0.4MPa, the crushing resistance of comparative film.
Based on this, the present invention utilizes CNT or carbon fiber and Graphene mixture to add in the Polymer Solutions such as Kynoar, polysulfones, polyether sulfone, prepares microporous barrier, improves the crushing resistance of film, obtains a kind of new method of preparing compressive film.
The method that the present invention prepares compressive film is simple, and the mixture that only need to add a certain amount of CNT/fiber and Graphene in former material of preparing can be realized the raising of crushing resistance, and the separating properties such as water flux of film are without any loss simultaneously.
The specific embodiment
embodiment 1
(1) dry PVDF resin (Su Wei 6010) is dissolved in the mixed solvent of DMAc and acetone, PVDF concentration is that the mixing ratio of 15%, DMAc and acetone is 85:15, then at 40 ℃, stirs 48 hours, deaeration in standing 4 hours;
(2) above-mentioned PVDF casting solvent is scraped on nonwoven, the 1min that volatilizees under room temperature, is then placed in pure water and bathes, and soaks 48 hours, then be placed in new pure water bathe soak stand-by;
(3) measure the crushing resistance of prepared film, its performance is as shown in table 1.
embodiment 2
(1) dry PVDF resin (Su Wei 6010) is dissolved in the mixed solvent of DMAc and acetone, PVDF concentration is 15%, the mixing ratio of DMAc and acetone is 85:15, add wherein more organically-modified multi-walled carbon nano-tubes (MWNT), addition is 0.05% of PVDF, strong agitation 48 hours at 40 ℃ again, deaeration in standing 4 hours;
(2) above-mentioned PVDF casting solvent is scraped on nonwoven, the 1min that volatilizees under room temperature, is then placed in pure water and bathes, and soaks 48 hours, then be placed in new pure water bathe soak stand-by;
(3) measure the crushing resistance of prepared film, its performance is as shown in table 1.
embodiment 3
(1) dry PVDF resin (Su Wei 6010) is dissolved in containing in the TEP of LiCl and the mixed solvent of ethanol, PVDF concentration is 15%, LiCl is 1% of PVDF, the mixing ratio of TEP and ethanol is 90:10, add wherein respectively more organically-modified carbon nano-fiber and Graphene), addition is respectively 0.5% and 1.5% of PVDF, then at 40 ℃ strong agitation 48 hours, deaeration in standing 4 hours;
(2) above-mentioned PVDF casting solvent is scraped on nonwoven, the 1min that volatilizees under room temperature, is then placed in pure water and bathes, and soaks 48 hours, then be placed in new pure water bathe soak stand-by;
(3) measure the crushing resistance of prepared film, its performance is as shown in table 1.
embodiment 4
(1) by dry PSf resin dissolves in containing in the DMSO of PVP, wherein PSf concentration is 20%, PVP is 10% of PVDF amount, add wherein respectively more organically-modified multi-walled carbon nano-tubes (MWNT) and Graphene, the addition of MWNT and Graphene is respectively the 0.05wt% of PSf, strong agitation 48 hours at 40 ℃ again, deaeration in standing 4 hours;
(2) above-mentioned PSf casting solvent is scraped on nonwoven, the 1min that volatilizees under room temperature, is then placed in pure water and bathes, and soaks 48 hours, then be placed in new pure water bathe soak stand-by;
(3) measure the crushing resistance of prepared film, its performance is as shown in table 1.
embodiment 5
(1) by dry PES resin dissolves in containing in the DMF of PEG, wherein PES concentration is 25%, PEG is 10% of PVDF amount, add wherein respectively more organically-modified multi-walled carbon nano-tubes (MWNT) and Graphene, the addition of MWNT and Graphene is respectively the 1wt% of PSf, strong agitation 48 hours at 40 ℃ again, deaeration in standing 4 hours;
(2) above-mentioned PES casting solvent is scraped on nonwoven, the 1min that volatilizees under room temperature, is then placed in pure water and bathes, and soaks 48 hours, then be placed in new pure water bathe soak stand-by;
(3) measure the crushing resistance of prepared film, its performance is as shown in table 1.
embodiment 6
(1) by dry PES resin dissolves in containing in the DMF of PEG, wherein PES concentration is that 25%, PEG is 10% of PES amount, then at 40 ℃ strong agitation 48 hours, deaeration in standing 4 hours;
(2) above-mentioned PES casting solvent is scraped on nonwoven, the 1min that volatilizees under room temperature, is then placed in pure water and bathes, and soaks 48 hours, then be placed in new pure water bathe soak stand-by;
(3) measure the crushing resistance of prepared film, its performance is as shown in table 1.
embodiment 7
(1) by dry PAN resin dissolves in containing in the DMF of PEG, wherein PAN concentration is 20%, PEG is 10% of PAN amount, add wherein respectively more organically-modified multi-walled carbon nano-tubes (MWNT) and Graphene, the addition of MWNT and Graphene is respectively the 1wt% of PSf, strong agitation 48 hours at 40 ℃ again, deaeration in standing 4 hours;
(2) above-mentioned PAN casting solvent is scraped on nonwoven, the 3min that volatilizees under room temperature, is then placed in pure water and bathes, and soaks 48 hours, then be placed in new pure water bathe soak stand-by;
(3) measure the crushing resistance of prepared film, its performance is as shown in table 1.
embodiment 8
(1) dry cellulose acetate (degree of acetylation 39.8) is dissolved in moisture acetone, wherein cellulose acetate concentration is 18%, the ratio of acetone and water is 90:10, add wherein respectively more organically-modified multi-walled carbon nano-tubes (MWNT) and Graphene, the addition of MWNT and Graphene is respectively the 1wt% of cellulose acetate, strong agitation 48 hours at 40 ℃ again, deaeration in standing 4 hours;
(2) above-mentioned cellulose acetate casting solvent is scraped on nonwoven, the 0.5min that volatilizees under room temperature, is then placed in pure water and bathes, and soaks 48 hours, then be placed in new pure water bathe soak stand-by;
(3) measure the crushing resistance of prepared film, its performance is as shown in table 1.
The microporous barrier pure water flux that table 1 embodiment prepares and the rejection to bovine serum albumin
?more than show and described basic principle of the present invention, principal character and advantage of the present invention.Those skilled in the art should understand the present invention and not be restricted to the described embodiments; that in above-described embodiment and description, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in claimed scope.
Claims (8)
1. a crushing resistance microporous barrier preparation method, is characterized in that, comprises following steps,
In microporous barrier film making solution, add polymer and textural association thing, described polymer accounts for the 10-25wt% of whole solution, described textural association thing accounts for the 0.05-2wt% of polymer weight ratio, comprise A component and B component: A CNT and/or carbon fiber, B Graphene, wherein the weight ratio of A component and B component is 0-1, stirs deaeration in standing 4 hours at 40 ℃ 48 hours;
Film making solution is scraped on masking supporter by the tape casting, utilizes phase inversion to prepare microporous barrier, and concrete grammar is: casting solution immerses in non-solvent water expose 0.5-3min in air after, film-forming.
2. a kind of crushing resistance microporous barrier preparation method as claimed in claim 1, is characterized in that the preferred multi-walled carbon nano-tubes of described CNT.
3. a kind of crushing resistance microporous barrier preparation method as claimed in claim 1, is characterized in that the preferred Graphene of described carbon fiber.
4. a kind of crushing resistance microporous barrier preparation method as claimed in claim 1, it is characterized in that, the solvent of described microporous barrier film making solution is any one of following solvent, 1-METHYLPYRROLIDONE, N, dinethylformamide, DMA, triethyl phosphate, dimethyl sulfoxide (DMSO), acetone, oxolane.
5. a kind of crushing resistance microporous barrier preparation method as claimed in claim 4, it is characterized in that, in described microporous barrier film making solution, can comprise as follows one or more as additive, lithium chloride, polyvinylpyrrolidone, polyethylene glycol, water, methyl alcohol, ethanol, formic acid, acetic acid, acetone, oxolane, addition be take amount of polymers and is counted 1-10wt% as benchmark.
6. a kind of crushing resistance microporous barrier preparation method as claimed in claim 1, is characterized in that, also comprises prepared film is immersed in to step stand-by in water.
7. a crushing resistance microporous barrier, is characterized in that, the skeleton that comprises CNT or carbon fiber and Graphene structure.
8. the purposes of multi-walled carbon nano-tubes in preparing microporous barrier.
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| CN106163630A (en) * | 2014-02-28 | 2016-11-23 | 洛克希德马丁公司 | For obtaining syringe and the correlation technique that submicron material property for you to choose measures |
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| CN106345309A (en) * | 2016-10-20 | 2017-01-25 | 合肥创想能源环境科技有限公司 | PVDF organic membrane modifying method |
| CN107158967A (en) * | 2017-06-16 | 2017-09-15 | 上海海事大学 | A kind of carbon containing composite semipermeable membrane, preparation method and the usage that water is evaporated for light |
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