CN101829508A - Novel polyamide nanofiltration membrane and preparation method thereof - Google Patents
Novel polyamide nanofiltration membrane and preparation method thereof Download PDFInfo
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- CN101829508A CN101829508A CN201010172208A CN201010172208A CN101829508A CN 101829508 A CN101829508 A CN 101829508A CN 201010172208 A CN201010172208 A CN 201010172208A CN 201010172208 A CN201010172208 A CN 201010172208A CN 101829508 A CN101829508 A CN 101829508A
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Abstract
The invention discloses a polymeric membrane and a preparation method thereof, in particular to a polyamide nanofiltration membrane and a preparation method thereof. The membrane comprises a porous support layer membrane and a polyamide ultrathin functional layer, wherein the polyamide ultrathin functional layer simultaneously contains sulfonyl amino, amide, carboxylic and sulfonic functional groups. The preparation method comprises the following step of compounding an aromatic polyamide ultrathin functional layer on a polysulfone support membrane through the interfacial polycondensation between aromatic polyhydric acyl chloride or other aromatic polyhydric acyl chloride mixture with modified acyl chloride groups on aromatic rings and a 4-amino piperidine water solution. The invention has the advantages that: the preparation method is novel and simple; and the nanofiltration membrane has better hydrophilcity and chlorine resistance and keeps higher removal ratio to bivalent ions while maintaining higher reflux. The invention has wide application in liquid separation industry.
Description
Technical field
The present invention relates to a kind of polymeric membrane and preparation method, specifically be meant a kind of polyamide nanofiltration membrane and preparation method.
Technical background
NF membrane is the new membrane isolation technics between ultrafiltration and counter-infiltration.Its technical characterstic is to realize selective permeation to dissolved constituent by sterically hindered and electrostatic interaction, and operating system pressure is well below reverse osmosis process (operating pressure is generally 0.4-1MPa), NF membrane to divalent ion and molecular weight greater than the rejection of 200 solute greater than 90%, and the rejection of monovalent ion and low molecular weight solutes generally is lower than 50%, thereby can realize Selective Separation to material.The charge of material, ion valence mumber and concentration have a significant impact the nanofiltration membrane separation efficiency, the separating effect of NF membrane uniqueness is widened its range of application rapidly, be widely used in the bitter desalination, industries such as medicine, food and biology, simultaneously, nanofiltration is more suitable for some special occasions than counter-infiltration, replaces counter-infiltration by NF membrane, can save lot of energy.
Nano filtering composite membrane is that one deck ultrathin functional layer is deposited to suitable micropore support membrane surface, aperture, and preparation technology roughly has following several: phase inversion, weak solution coating, interfacial polymerization, thermal induction phase inversion and chemic modified method etc.
NF membrane commonly used has: poly aromatic amide-type, polyamide-based, SPSF class, polyvinyl alcohol etc.The aromatic polyamides class, polyamide-based be to adopt interfacial polymerization method to prepare charged top layer; SPSF class, polyvinyl alcohol are to adopt coating process to prepare charged top layer.
At present, the composite nanometer filtering film that occurs in the world mainly contains four kinds of series:
(1) aromatic polyamides class composite membrane: this class film mainly contains the NF-50 and two kinds of the NF-70 (bear) of U.S. Film Tec company.
(2) polyamide-based composite nanometer filtering film: this class film mainly contains the NF-40 (negative electricity) and the Minneapolis of U.S. Film Tec company, the NF-40HF film of MN company, UTC-60 (both sexes) film of the UTC-20HF of toray company (negative electricity), the ATF-30 and the ATF-50 of U.S. AMT company.
(3) sulfonated polyether sulfone class composite nanometer filtering film: this class film has the serial NF membrane of NFR 1 (negative electricity) of Japanese eastern electrician company exploitation.
(4) mixed type composite nanometer filtering film: NTR 1 (negative electricity) film as Japan eastern electrician company (belongs to polyamide-based film, added polyvinyl alcohol at aqueous phase during preparation, heat down at 110 ℃ behind the interface polymerization reaction, and make it crosslinked by radiation, to obtain cooperative effect), the Desaal-5 film of U.S. Desalination company exploitation (adopts coating process, directly blow down casting solution on the basement membrane, utilize phase inversion to form composite bed, its structural formula is compound ultra-thin aramid layer on the SPSF layer).
Except that organic film, also have NF membrane with the inorganic material preparation, as being deposited on, Quadrafos and polysiloxanes be prepared into the composite inorganic NF membrane on the inorganic micro filtering membrane.
At present commercial general polyamide nanofiltration membrane is to prepare by interfacial polycondensation by pyromellitic trimethylsilyl chloride or its mixture and piperidines or its mixture.Although nanofiltration has been obtained great advance, existing membrane material can not satisfy people's demand, and under the condition of not losing rejection, the flux of film needs further to improve, and needs new monomer, the appearance of new material.
Summary of the invention
The present invention is directed to deficiency of the prior art, proposed a kind of novel NF membrane, better chlorine resistance, bigger water flux etc.
The present invention is achieved by following proposal:
A kind of novel polyamide nanofiltration membrane is made up of porous support layer film and polyamide ultrathin functional layer, contains sulfoamido, amide groups, carboxylic acid group and sulfonic group functional group in the described polyamide ultrathin functional layer simultaneously.
A kind of novel compound nanometer filtering membrane of polyamide of the present invention's preparation, composite membrane is made up of polysulfone supporting layer and polyamide ultrathin functional layer, and described polyamide ultrathin functional layer (CO-N), also contains sulfonamide functional group (SO except having the acid amides functional group
2-N), mix back and piperidines by the polynary acyl chlorides of the aromatic series that contains the sulfonic acid chloride group or with other aromatic polycarboxylic acyl chlorides by the interfacial polycondensation preparation.
A kind of preparation method of novel polyamide nanofiltration membrane is characterized in that comprising the steps,
(1) the 4-amino piperidine aqueous solution is poured into porous support layer film surface, covered porous support layer film surface 1～5 minute; Wherein the quality volumetric concentration of 4-amino piperidine is 0.1～2% in the 4-amino piperidine aqueous solution, and concentration unit is g/ml;
Porous support membrane described in the above-mentioned preparation method is PS membrane, poly (ether sulfone) film or the polyacrylonitrile porous membrane of molecular cut off 2～30,000;
As preferably, the above-mentioned piperidines aqueous solution with hydrochloric acid, formic acid or acetate as pH value conditioning agent; Wherein be best with hydrochloric acid.
As preferably, add certain sodium phosphate in the used piperidine solution among the above-mentioned preparation method and be mixed into solution, wherein be dissolved as the highest limit fully with sodium phosphate.
(2) this unnecessary 4-amino piperidine solution in film surface is outwelled, in air, dry, carried out interfacial polymerization in 10～300 seconds with having the aromatic polycarboxylic acyl chlorides of modification acid chloride groups on the aromatic rings or pouring into the film surface reaction again with other aromatic polycarboxylic acyl chlorides mixture solutions; Solvent for use is a kind of in trifluorotrichloroethane, n-hexane, normal heptane or the isopar solvent naphtha; The quality volumetric concentration of aromatic polycarboxylic acyl chlorides in solution that has the modification acid chloride groups on the aromatic rings is 0.03～0.3%; The quality volumetric concentration of other aromatic polycarboxylic acyl chlorides mixtures in solution is 0.2～0.5%; The quality volumetric concentration of 4-amino piperidine is 0.1～4%; Concentration unit is g/ml;
(3) subsequently it is carried out first step heat treatment, heat treatment is to handle 3～10 minutes down at 40-70 ℃;
(4) carry out two step rinsings then, described rinsing comprises, the first step: at 30～60 ℃ methyl alcohol part by weight is rinsing 10～40 minutes in 15% the aqueous solution, second step: be rinsing 10～40 minutes in 30-60 ℃ water;
(5) and then carry out the second step heat treatment, heat treatment is to handle 3～9 minutes down at 80～110 ℃, obtains polyamide nanofiltration membrane.
As preferably, describedly have the aromatic polycarboxylic acyl chlorides of modification acid chloride groups and the part by weight of other aromatic polycarboxylic acyl chlorides is 1: 1～9, pour into the film surface and react.
As preferably, the described aromatic polycarboxylic acyl chlorides that has the modification acid chloride groups contains at least one sulfonic acid chloride group and two acid chloride groups.
As preferably, described other aromatic polycarboxylic acyl chlorides are pyromellitic trimethylsilyl chloride.
As preferably, used organic solvent isopar solvent naphtha in the described step (2).
As preferably, the concentration of solution is in the described step (2): the quality volumetric concentration of other aromatic polycarboxylic acyl chlorides mixtures in solution is 0.3%.
Beneficial effect: the preparation method's novelty among the present invention, simple, NF membrane has hydrophily and chlorine resistance preferably, when higher flux, has kept bivalent ions higher removal efficiency.
The specific embodiment
Following examples provide explanation and their desalting performance and the water flux of nanofiltration composite membrane.Yet these embodiment only provide as an illustration rather than limit the present invention.
Embodiment 1
UDEL P3500 polysulfones with 16%, 0.3% water and 0.1% polyoxyethylene nonyl phenyl Acetoxon acid esters are dissolved in N, N-dimethylacetylamide, be coated with and scrape on polyester non-woven fabric, immerse in the water gel then and remove and obtain the support membrane that molecular cut off is 2-3 ten thousand after desolvating, hygrometric state is preserved standby.
It is 0.1% that the polysulfones support membrane single face of hygrometric state is immersed in the piperidines part by weight, the NaOH part by weight is in 0.25% the aqueous solution two minutes, after extracting with squeegee roll extrusion support membrane surface, with fragrant acyl chlorides part by weight is that 0.1% isopar solvent naphtha solution single face contacts and carries out interface polymerization reaction 20-40 second, composite membrane dried in the shade in air 2 minutes, handled 3-10 minute down through 40-70 ℃ again.Then carry out two step rinsings again: the first step is to be in 15% the aqueous solution rinsing 10-40 minute at 30-60 ℃ methyl alcohol part by weight, and second step was in 30-60 ℃ water rinsing 10-40 minute.The composite membrane of preparation is kept in the solution of sodium bisulfite.
At the saline solution of 2000ppm (millionth mass concentration), operating pressure 1MPa, operating temperature is its desalting performance of test under 25 ℃ the condition, the result is as shown in table 1
Table 1
Embodiment 2-9
Other conditions are all identical with embodiment 1, TMC and CSIC proportioning in the admixture solvent oil solution of change different peptide acyl chlorides of 5-sulfonic acid chloride and pyromellitic trimethylsilyl chloride, result such as following table 2
Table 2
CSIC among the present invention is meant 5-chlorine sulfonic acid chloride isophthaloyl chlorine, and the isopar solvent naphtha is a C11-C13 aliphatic solvent oil.
Claims (7)
1. a novel polyamide nanofiltration membrane is made up of porous support layer film and polyamide ultrathin functional layer, it is characterized in that, contains sulfoamido, amide groups, carboxylic acid group and sulfonic group functional group in the described polyamide ultrathin functional layer simultaneously.
2. the preparation method of a novel polyamide nanofiltration membrane is characterized in that comprising the steps,
(1) the 4-amino piperidine aqueous solution is poured into porous support layer film surface, covered porous support layer film surface 1～5 minute; Wherein the quality volumetric concentration of 4-amino piperidine is 0.1～2% in the 4-amino piperidine aqueous solution, and concentration unit is g/ml;
(2) this unnecessary 4-amino piperidine solution in film surface is outwelled, in air, dry, carried out interfacial polymerization in 10～300 seconds with having the aromatic polycarboxylic acyl chlorides of modification acid chloride groups on the aromatic rings or pouring into the film surface reaction again with other aromatic polycarboxylic acyl chlorides mixture solutions; Solvent for use is a kind of in trifluorotrichloroethane, n-hexane, normal heptane or the isopar solvent naphtha; The quality volumetric concentration of aromatic polycarboxylic acyl chlorides in solution that has the modification acid chloride groups on the aromatic rings is 0.03～0.3%; The quality volumetric concentration of other aromatic polycarboxylic acyl chlorides mixtures in solution is 0.2～0.5%; The quality volumetric concentration of 4-amino piperidine is 0.1～4%; Concentration unit is g/ml;
(3) subsequently it is carried out first step heat treatment, heat treatment is to handle 3～10 minutes down at 40-70 ℃;
(4) carry out two step rinsings then, described rinsing comprises, the first step: at 30～60 ℃ methyl alcohol part by weight is rinsing 10～40 minutes in 15% the aqueous solution, second step: be rinsing 10～40 minutes in 30-60 ℃ water;
(5) and then carry out the second step heat treatment, heat treatment is to handle 3～9 minutes down at 80～110 ℃, obtains polyamide nanofiltration membrane.
3. preparation method according to claim 2 is characterized in that, describedly has the aromatic polycarboxylic acyl chlorides of modification acid chloride groups and the part by weight of other aromatic polycarboxylic acyl chlorides is 1: 1～9, pours into the film surface and reacts.
4. preparation method according to claim 3 is characterized in that, the described aromatic polycarboxylic acyl chlorides that has the modification acid chloride groups contains at least one sulfonic acid chloride group and two acid chloride groups.
5. preparation method according to claim 2 is characterized in that, described other aromatic polycarboxylic acyl chlorides are pyromellitic trimethylsilyl chloride.
6. preparation method according to claim 2 is characterized in that, used organic solvent isopar solvent naphtha in the step (2).
7. preparation method according to claim 2 is characterized in that, the concentration of solution is in the step (2): the quality volumetric concentration of other aromatic polycarboxylic acyl chlorides mixtures in solution is 0.3%.
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Cited By (17)
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|---|---|---|---|---|
| CN102120149A (en) * | 2011-01-30 | 2011-07-13 | 杭州方然滤膜技术有限公司 | Method for preparing acid-proof polysulfonamide nanofiltration composite film |
| CN102151499A (en) * | 2011-02-28 | 2011-08-17 | 浙江理工大学 | Polyamide composite nanofiltration membrane and preparation method thereof |
| CN102210986A (en) * | 2011-06-10 | 2011-10-12 | 南京帝膜净水材料开发有限公司 | Method for preparing nanofiltration composite membrane |
| CN102500244A (en) * | 2011-11-30 | 2012-06-20 | 杭州水处理技术研究开发中心有限公司 | Preparation method of reverse osmosis composite membrane for sea water desalinization |
| CN103272486A (en) * | 2013-06-18 | 2013-09-04 | 天津工业大学 | Composite film containing calixarene structure on surface layer |
| CN103480284A (en) * | 2013-09-03 | 2014-01-01 | 株洲时代新材料科技股份有限公司 | Pollution-resistant polyamide composite membrane and preparation method thereof |
| CN103933881A (en) * | 2013-01-18 | 2014-07-23 | 中国科学院宁波材料技术与工程研究所 | Method for preparing composite nanofiltration membrane by employing interfacial polymerization process |
| CN104379243A (en) * | 2013-06-07 | 2015-02-25 | Lg化学株式会社 | Prolyamide-based water treatment separation membrane having excellent oxidation resistance and chlorine resistance and manufacturing method therefor |
| CN107899437A (en) * | 2017-11-21 | 2018-04-13 | 贵阳时代沃顿科技有限公司 | A kind of high-performance water-oil separationg film based on interfacial polymerization and preparation method thereof |
| CN110404419A (en) * | 2019-08-14 | 2019-11-05 | 东华大学 | A kind of sulfonation polyphenol nanofiltration membrane and preparation method thereof |
| CN110743394A (en) * | 2019-09-12 | 2020-02-04 | 三达膜科技（厦门）有限公司 | Preparation method of aliphatic polyamide nanofiltration membrane |
| CN111603948A (en) * | 2020-05-21 | 2020-09-01 | 杭州科百特科技有限公司 | Nylon membrane and preparation method and application thereof |
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| CN112397848A (en) * | 2020-12-11 | 2021-02-23 | 宁波启新精合新能源研究院有限公司 | High-performance lithium ion battery diaphragm and preparation thereof |
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| CN114870629A (en) * | 2022-06-06 | 2022-08-09 | 天津工业大学 | High-selectivity nanofiltration membrane and preparation method and application thereof |
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| CN112316752A (en) * | 2020-11-04 | 2021-02-05 | 天津工业大学 | Sulfonamide micromolecule surface modified polyamide composite membrane and preparation method thereof |
| CN112397848A (en) * | 2020-12-11 | 2021-02-23 | 宁波启新精合新能源研究院有限公司 | High-performance lithium ion battery diaphragm and preparation thereof |
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| CN112717712A (en) * | 2020-12-15 | 2021-04-30 | 中国科学院过程工程研究所 | Acid-resistant nanofiltration membrane and preparation method and application thereof |
| CN112717712B (en) * | 2020-12-15 | 2022-02-25 | 中国科学院过程工程研究所 | Acid-resistant nanofiltration membrane and preparation method and application thereof |
| CN114870629A (en) * | 2022-06-06 | 2022-08-09 | 天津工业大学 | High-selectivity nanofiltration membrane and preparation method and application thereof |
| CN114870629B (en) * | 2022-06-06 | 2023-06-30 | 天津工业大学 | High-selectivity nanofiltration membrane and preparation method and application thereof |
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Application publication date: 20100915 |