CN103272499A - Dopamine-polyethersulfone composite membrane and preparation method thereof - Google Patents
Dopamine-polyethersulfone composite membrane and preparation method thereof Download PDFInfo
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- CN103272499A CN103272499A CN2013101712210A CN201310171221A CN103272499A CN 103272499 A CN103272499 A CN 103272499A CN 2013101712210 A CN2013101712210 A CN 2013101712210A CN 201310171221 A CN201310171221 A CN 201310171221A CN 103272499 A CN103272499 A CN 103272499A
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Abstract
The invention discloses a preparation method of a dopamine-polyethersulfone composite membrane. The preparation method mainly comprises the following steps of: preparing a polyethersulfone basal membrane, sequentially soaking the polyethersulfone basal membrane in an aqueous phase monomer, namely dopamine and an organic phase monomer, namely trimesoyl chloride, and carrying out interfacial polymerization to prepare the dopamine composite membrane. Compared with a conventional polyethersulfone composite nanofiltration membrane prepared through the interfacial polymerization, the dopamine-polyethersulfone composite membrane has the advantages that as the dopamine is used as the aqueous phase monomer, the dopamine-polyethersulfone composite membrane shows excellent antioxidant capacity, for instance, after a polypiperazine-amide composite membrane is soaked for 4 days in 10ppm of sodium hypochlorite, the retention rate of the polypiperazine-amide composite membrane to orange sodium salt is reduced to 30.4% from 99.7%, and after the dopamine-polyethersulfone composite membrane is soaked for 4 days in 20ppm of sodium hypochlorite through experiments, the retention rate of the dopamine-polyethersulfone composite membrane to the orange sodium salt is reduced to 89.27% from 91.04%.
Description
Technical field
The present invention relates to a kind of diffusion barrier and preparation method, especially dopamine composite membrane and preparation method thereof.
Background technology
Nanofiltration is a kind of pressure-driven type membrane separation technique between counter-infiltration and ultrafiltration, the aperture of NF membrane is at 0.5-2nm, its cutoff performance is also between counter-infiltration and milipore filter, characteristics are to have the nanoscale aperture, and operating pressure is low, preferably pressure tightness, can replace a plurality of steps in the conventional process, be mainly used in the water for industrial use purifying, purification of waste water, valuable components the aspect such as concentrates in the technological process.
At present, NF membrane is divided into anisotropic membrane and composite membrane two classes by textural classification.Composite membrane is the porous basement membrane and covers epilamellar fine and close active layer composition.Wherein, active layer is used for holding back divalent ion or organic molecule, and porous support layer provides film required mechanical strength.Advantages such as interfacial polymerization is simple to operate with it, controllability is strong are widely used in the membrane technology field, and interfacial polymerization can prepare ultra-thin active layer, cause composite membrane under low pressure to have higher selective and permeability concurrently.
It is to utilize the very high monomer of two kinds of reactivities at two immiscible solvents polymerization reaction take place at the interface that interfacial polymerization prepares composite membrane, thereby (milipore filter or micro-filtration membrane) forms very thin compacted zone on porous supporting body.Activated monomer commonly used has polyamine, polyalcohol, polyhydric phenols and polynary acyl chlorides etc.Form polymeric surface layers such as polyamide, polyester, polyureas or polyurethane after the reaction respectively.Interfacial polymerization is easy to control with simple to operate, and the interfacial polymerization layer that forms can have been realized extensive use to 20nm.
The aromatic polyamides base polymer is typical composite nanometer filter membrane material, but the easy oxidative degradation of this base polymer.Often contain the free oxygen of low concentration in natural water and the waste water solution, thereby influenced the service life of film, limited its range of application.Development of new functional polymer membrane material, reinforcement prepare oxidation resistant composite membrane and have very important and practical meanings the ultra-thin cortex of film and activating technology research.
Dopamine (DOPA) is a kind of material with biological stickiness, is present in the mussel of ocean.Since Lee in 2007 etc. by since forming the multifunctional polymeric coating at organic (comprising inert metal, oxide, polymer, semiconductor and pottery) surface recombination dopamine, utilize the biological adhesive dopamine extremely strong stick characteristic, it is often longer that preparation dopamine composite membrane more and more is subjected to sedimentation experiment time of people's attention dopamine, and short rejection of autohemagglutination time is low especially.Contain two phenolic hydroxyl groups and amido in the dopamine molecule, these two kinds of groups can with the acid chloride groups effect, so adopt interfacial polymerization to prepare the dopamine composite nanometer filtering film, organic dyestuff is reached certain holding back, and the ester bond that forms has excellent oxidation resistance with respect to amido link.
Summary of the invention
The object of the present invention is to provide a kind of preparation method with oxidation resistance composite membrane, this preparation method's process is simple to operation, prepared composite membrane has good oxidation resistance, and under ultralow operating pressure, have the flux height, selective high characteristic.
The present invention is achieved through the following technical solutions, and a kind of preparation method of composite membrane is characterized in that may further comprise the steps:
1, the preparation of polyether sulfone basement membrane
Polyether sulfone is dissolved in N, dinethylformamide, be mixed with that to contain the polyether sulfone mass concentration be 18% casting solution, stir 4h down at 60 ℃, and at 60 ℃ of following standing and defoaming 4h, casting solution is poured on knifing on the glass plate after being cooled to room temperature, put into 25 ℃ of water-bath freezing films again, take off the back from glass plate and soak 24h with deionized water, obtain the polyacrylonitrile basement membrane;
2, the preparation of dopamine (DOPA) composite membrane
After homemade poly (ether-sulfone) ultrafiltration membrane is immersed in the phosphate buffer solution 10min of pH=6 of dopamine that mass fraction is 0.5-5wt%, take out and remove residual droplets, be immersed in again in the n-heptane solution of the pyromellitic trimethylsilyl chloride that mass fraction is 0.1-0.5wt% (TMC), taking-up is immersed in the deionized water after 1 to 10min, obtains composite membrane.
The invention has the advantages that: with respect to the polyamide composite film of former interfacial polymerization preparation, this composite membrane demonstrates excellent oxidation resistance, the clorox that is immersed in 10ppm as poly-piperazine amide composite membrane dropped to 30.4% to the rejection of orange sodium from original 99.7% after 4 days, in this experiment the clorox of composite membrane immersion 20ppm after 4 days the rejection to orange sodium drop to 89.27% by 91.04%.The film of the present invention's preparation is held back for the separation of salt in the saline solution and holding back of organic pigment has excellent effect.
Description of drawings
Fig. 1 is the embodiment of the invention 3 made anti-oxidant NF membrane are soaked the rejection of pure water flux and orange sodium after 5 days in the liquor natrii hypochloritis of variable concentrations change curve.
The specific embodiment
Embodiment 1
Polyether sulfone is dissolved in N, dinethylformamide, be mixed with that to contain the polyether sulfone mass concentration be 18% casting solution, stir 4h down at 60 ℃, and at 60 ℃ of following standing and defoaming 4h, casting solution is poured on knifing on the glass plate after being cooled to room temperature, put into 25 ℃ of water-bath freezing films again, take off the back from glass plate and soak 24h with deionized water, obtain the polyether sulfone basement membrane.
The phosphate buffer solution of configuration pH=6 is used for the phosphoric acid solution that dissolving water monomer DOPA prepares DOPA, the poly (ether-sulfone) ultrafiltration membrane that makes is immersed in 5min in the DOPA phosphoric acid solution of 1wt%, make DOPA can fully spread and be adsorbed onto fenestra and film surface, taking-up is blotted with filter paper and is guaranteed that the surface does not have residual solution.Be immersed in again in the n-heptane solution of pyromellitic trimethylsilyl chloride of 0.2wt%, take out behind the 2min, be immersed in the deionized water, obtain composite membrane 1.
The water flux of prepared composite membrane 1 is 80L/ (m
2HMPa).Filtration concentration is that the orange sodium water solution rejection of 100mg/L is 91.04%, and concentration is that the rejection of the Congo red aqueous solution of 100mg/L is 97.59%.
Embodiment 2
Mode as embodiment 1 prepares the polyether sulfone basement membrane.
The phosphate buffer solution of configuration pH=6 is used for the phosphoric acid solution that dissolving water monomer DOPA prepares DOPA, the poly (ether-sulfone) ultrafiltration membrane that makes is immersed in 5min in the phosphoric acid solution of DOPA of 3wt%, make DOPA can fully spread and be adsorbed onto fenestra and film surface, taking-up is blotted with filter paper and is guaranteed that the surface does not have residual solution.Be immersed in again in the n-heptane solution of pyromellitic trimethylsilyl chloride of 0.2wt%, take out behind the 2min, be immersed in the deionized water, obtain composite membrane 2.
The water flux of prepared composite membrane 2 is 33.5L/ (m
2HMPa).Filtration concentration is that the orange sodium water solution rejection of 100mg/L is 94.96%, and concentration is that the rejection of the Congo red aqueous solution of 100mg/L is 98.56%.
Embodiment 3
Mode as embodiment 1 prepares the polyether sulfone basement membrane.
The phosphate buffer solution of configuration pH=6 is used for the phosphoric acid solution that dissolving water monomer DOPA prepares DOPA, the poly (ether-sulfone) ultrafiltration membrane that makes is immersed in 5min in the phosphoric acid solution of DOPA of 5wt%, make DOPA can fully spread and be adsorbed onto fenestra and film surface, taking-up is blotted with filter paper and is guaranteed that the surface does not have residual solution.Be immersed in again in the n-heptane solution of pyromellitic trimethylsilyl chloride TMC of 0.2wt%, take out behind the 2min, be immersed in the deionized water, obtain composite membrane 3.
The water flux of prepared composite membrane 3 is 20.9L/ (m
2HMPa).Filtration concentration is that the orange sodium water solution rejection of 100mg/L is 95.54%, and concentration is that the rejection of the Congo red aqueous solution of 100mg/L is 98.07%.
Embodiment 4
Mode as embodiment 1 prepares the polyether sulfone basement membrane.
The phosphate buffer solution of configuration pH=6 is used for the phosphoric acid solution that dissolving water monomer DOPA prepares DOPA, the poly (ether-sulfone) ultrafiltration membrane that makes is immersed in 5min in the phosphoric acid solution of DOPA of 1wt%, make DOPA can fully spread and be adsorbed onto fenestra and film surface, taking-up is blotted with filter paper and is guaranteed that the surface does not have residual solution.Be immersed in again in the n-heptane solution of pyromellitic trimethylsilyl chloride of 0.3wt%, take out behind the 2min, be immersed in the deionized water, obtain composite membrane 4.
The water flux of prepared composite membrane 4 is 69L/ (m
2HMPa).Filtration concentration is that the orange sodium water solution rejection of 100mg/L is 95.06%, and concentration is that the rejection of the Congo red aqueous solution of 100mg/L is 99.03%.
Embodiment 5
Mode as embodiment 1 prepares the polyether sulfone basement membrane.
The phosphate buffer solution of configuration pH=6 is used for the phosphoric acid solution that dissolving water monomer DOPA prepares DOPA, the poly (ether-sulfone) ultrafiltration membrane that makes is immersed in 5min in the phosphoric acid solution of DOPA of 1wt%, make DOPA can fully spread and be adsorbed onto fenestra and film surface, taking-up is blotted with filter paper and is guaranteed that the surface does not have residual solution.Be immersed in again in the n-heptane solution of pyromellitic trimethylsilyl chloride of 0.5wt%, take out behind the 2min, be immersed in the deionized water, obtain composite membrane 5.
The water flux of prepared composite membrane 5 is 83.5L/ (m
2HMPa).Filtration concentration is that the orange sodium water solution rejection of 100mg/L is 93.76%, and concentration is that the rejection of the Congo red aqueous solution of 100mg/L is 98.09%.
Comparative Examples 1
Mode as embodiment 1 prepares the polyether sulfone basement membrane.
The phosphate buffer solution of configuration pH=6 is used for the phosphoric acid solution that dissolving water monomer DOPA prepares DOPA, the poly (ether-sulfone) ultrafiltration membrane that makes is immersed in 5min in the phosphoric acid solution of DOPA of 1wt%, make DOPA can fully spread and be adsorbed onto fenestra and film surface, taking-up is blotted with filter paper and is guaranteed that the surface does not have residual solution, be immersed in the deionized water, obtain comparative film 1.
The water flux of prepared comparative film is 959.6 L/ (m
2HMPa), for orange sodium with Congo redly all do not hold back.
The performance of the comparative film that the prepared stimulating responsive composite membrane of the embodiment of the invention and Comparative Examples make is relatively classified table 1 as.
Claims (8)
1. the preparation method of dopamine-polyether sulfone composite separating film is characterized in that comprising the step of soaking the polyether sulfone basement membrane with dopamine solution.
2. preparation method as claimed in claim 1 is characterized in that: at first the polyether sulfone basement membrane is immersed in the dopamine phosphate buffer solution of pH=6, takes out and blot residual water solution with filter paper, be immersed in the n-heptane solution of pyromellitic trimethylsilyl chloride again.
3. preparation method as claimed in claim 2, the mass fraction that it is characterized in that dopamine solution is 0. 5-5%, the mass fraction of pyromellitic trimethylsilyl chloride in n-heptane solution is 0.1-0.5%.
4. preparation method as claimed in claim 2 is characterized in that polyether sulfone basement membrane soak time in dopamine solution is 10min, and soak time is 2min in the n-heptane solution of pyromellitic trimethylsilyl chloride.
5. preparation method as claimed in claim 3 is characterized in that polyether sulfone basement membrane soak time in dopamine solution is 10min, and soak time is 2min in the n-heptane solution of pyromellitic trimethylsilyl chloride.
6. as each described preparation method among the claim 1-5, the preparation process that it is characterized in that the polyether sulfone basement membrane is as follows: polyether sulfone is dissolved in N, dinethylformamide, be mixed with and contain the casting solution that the polyether sulfone mass concentration is 15-18%, stir 4h down at 60 ℃, and at 60 ℃ of following standing and defoaming 4h, after being cooled to room temperature casting solution is poured on knifing on the glass plate, put into 25 ℃ of water-bath freezing films, take off the back from glass plate and soak 24h with deionized water, obtain the polyether sulfone basement membrane.
7. the dopamine for preparing as each method among the claim 1-6-polyether sulfone composite separating film.
Described in claim 7 dopamine-polyether sulfone composite separating film in saline solution salt hold back or the holding back of organic pigment in purposes.
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| CN104368244A (en) * | 2014-09-24 | 2015-02-25 | 浙江大学 | Making method of catechol compound nanoparticle modified polymeric composite membrane |
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| CN105013340A (en) * | 2014-11-01 | 2015-11-04 | 中国海洋大学 | Preparation method for novel carbon-nanotube-doped composite membrane with double selective layers |
| CN105013336A (en) * | 2015-06-30 | 2015-11-04 | 天津大学 | Preparation method of nano silver/poly dopamine composite membrane |
| CN105169970A (en) * | 2015-09-08 | 2015-12-23 | 武汉大学 | Preparation method for polydopamine-modified polyamide composite forward osmosis membrane |
| CN105492109A (en) * | 2013-10-04 | 2016-04-13 | Lg电子株式会社 | Surface-modified separation membrane and method for modifying surface of separation membrane |
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| CN104368244A (en) * | 2014-09-24 | 2015-02-25 | 浙江大学 | Making method of catechol compound nanoparticle modified polymeric composite membrane |
| CN105013340A (en) * | 2014-11-01 | 2015-11-04 | 中国海洋大学 | Preparation method for novel carbon-nanotube-doped composite membrane with double selective layers |
| CN104474925A (en) * | 2014-12-12 | 2015-04-01 | 杭州水处理技术研究开发中心有限公司 | Preparation method of composite high-water-flux polyamide reverse-osmosis membrane |
| CN105013336A (en) * | 2015-06-30 | 2015-11-04 | 天津大学 | Preparation method of nano silver/poly dopamine composite membrane |
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| CN105688691A (en) * | 2016-03-07 | 2016-06-22 | 东南大学 | Preparation method and application of anti-pollution polyethersulfone membrane |
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| CN105797585B (en) * | 2016-05-27 | 2018-01-12 | 中国科学院生态环境研究中心 | A kind of graphene oxide is modified organic polymer NF membrane and preparation method thereof |
| CN108031311A (en) * | 2017-12-21 | 2018-05-15 | 贵州省材料产业技术研究院 | The preparation method of durable hydrophilic property composite nanometer filtering film |
| CN108636142A (en) * | 2018-05-07 | 2018-10-12 | 万华化学集团股份有限公司 | A kind of preparation method of composite nanometer filtering film |
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Application publication date: 20130904 |