CN108854603A - A kind of preparation method coating modified ultrafiltration membrane altogether using dopamine and functionalized carbon nano-tube - Google Patents
A kind of preparation method coating modified ultrafiltration membrane altogether using dopamine and functionalized carbon nano-tube Download PDFInfo
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- CN108854603A CN108854603A CN201810746202.9A CN201810746202A CN108854603A CN 108854603 A CN108854603 A CN 108854603A CN 201810746202 A CN201810746202 A CN 201810746202A CN 108854603 A CN108854603 A CN 108854603A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/48—Antimicrobial properties
Abstract
The problems such as the invention discloses a kind of preparation methods for coating modified ultrafiltration membrane altogether using dopamine and functionalized carbon nano-tube, belong to membrane material preparation field, and the present invention is to solve fouling membrane present in ultrafiltration membrane operation and low flux.Additive and polymeric film material are added in organic solvent first for the method for the present invention, and heating stirring is uniform, and vacuum defoamation obtains casting solution;Casting solution is uniformly scraped on non-woven fabrics, obtains ultrafiltration membrane into coagulation bath;By carbon nanotube carboxylated, ultrasonic disperse is in deionization, by dispersion to film surface in the way of vacuum filter;Followed by Fe2+/ persulfate oxidation system promotes dopamine polymerization, and modified carbon nano-tube is secured firmly to film surface, to realize that dopamine and modified carbon nano-tube coat modified ultrafiltration membrane preparation altogether.The adsorptivity, hydrophily and antibiotic property of carbon nanotube is utilized in the preparation method well, greatly improves the antifouling property of ultrafiltration membrane.
Description
Technical field
The invention belongs to membrane material preparation fields;It is coated altogether more particularly to a kind of using dopamine and functionalized carbon nano-tube
The preparation method of modified ultrafiltration membrane.
Background technique
With risk of drinking water pollution aggravation and guidelines for drinking water quality it is increasingly stringent, traditional water treatment technology cannot answer
To increasingly prominent water pollution problems, the upgrading of traditional water factory becomes one of the change direction of drinking water treatment technique.It is super
Filter technology can effectively retain particulate matter, colloid, macromolecular organic pollutant and microorganism in water body etc., therefore become and drink
The research hotspot of water water treatment field, and scale application has successfully been obtained in Large Water Works.In actual moving process, surpass
Some problems existing for filter technology also gradually find by people, as operation energy consumption is larger and longtime running present in fouling membrane
Problem, this is greatly related to the economy and stability of water factory's production run.The optimization of service condition can be to a certain extent
Operation energy consumption increase and membrane pollution problem are solved, but final solution must start with from membrane material itself, prepare high pass
Amount and antipollution ultrafiltration membrane are only the core content solved these problems.
The development of nano material provides new freedom degree for the preparation of novel film materials, in polymer material self-characteristic
Under limitation, introducing nano material can greatly improve the performance of film, such as hydrophily, flux and mechanical strength.
In conjunction with the characteristics of carbon nanotube own material, ultrafiltration membrane can effectively be solved in reality by carbon nano-tube modification ultrafiltration membrane
The problem of border is applied.Carbon nanotube sheet is as hydrophobic material, but its tube wall and opening existing defects, utilizes this
Design feature can be modified carbon nanotube, prepare the functionalized carbon nano-tube with guide function.Patent
CN104437120B discloses a kind of preparation method of Pvc Ultrafiltration Membrane based on carbon nanotube ordered arrangement, but realizes carbon
The ordered arrangement process of nanotube is complicated, although improving the performance of film to a certain extent, large-scale application presence is very big
The problem of.Patent CN105478018B and CN102961981B disclose a kind of preparation of functionalized carbon nano-tube blended ultrafiltration membrane
Method, blending and modifying improve the antipollution and antibacterial characteristics of film, but compared with carbon nanotube is directly anchored to film surface, film
Hydrophily and antibacterial characteristics seem slightly insufficient.Patent CN105080361B and CN104923082A disclose a kind of macromolecule
The method for coating ultrafiltration membrane, compared with nano material, the presence of polymer coating layer significantly increases the resistance of film, reduces
Membrane flux.
Summary of the invention
Compared with organic polymer coating, existing surface coating modified general use organic polymer coating, and macromolecule
Coating can have some problems, and nano material is different from macromolecule organic material, and the present invention is applied using hydrophilic nano material
It covers and can solve existing problem, the present invention can provide water passage by hydrophilic nano material, in terms of film properties regulation
With bigger freedom degree;Meanwhile nano-material surface coating can play absorption and the antibacterial spy of carbon nanotube to the greatest extent
Property, Pollution of Ultrafiltration Membrane is substantially reduced, to improve the flux of film in longtime running.Coat can be impregnated by chemical agent or height
It presses backwash process to remove, provides new thinking for the regeneration of film.
The invention solves fouling membrane present in ultrafiltration membrane operation and the technical problems such as flux is low, for existing carbon nanometer
The anti-microbial property of film is poor in pipe blending and modifying, macromolecule organic layer coats dramatically increase membrane resistance and independent carbon nanotube coats
The problem that falls off of carbon nanotube, provides a kind of Fe in modified ultrafiltration membrane preparation method2+/ persulfate quick catalysis dopamine is poly-
It closes, realizes that dopamine and functionalized carbon nano-tube coat modified ultrafiltration membrane altogether, deposited when effectively improving surface carbon nano-tube coating
The problem that falls off, enhance the antipollution and antibacterial characteristics energy of film.
In order to solve the above technical problems, a kind of in the present invention coat modified surpass using dopamine and functionalized carbon nano-tube altogether
The preparation method of filter membrane carries out in the steps below:
Step 1: polymer and pore-foaming agent are added in organic solvent, heating stirring, standing and defoaming, is formed equal at room temperature
Phase casting solution;
Step 2: by step 1 formed casting solution uniformly scratch on PET non-woven fabrics, at room temperature stop 10s~
30s is placed in coagulation bath and carries out Gel Treatment, then impregnated with deionized water, obtain ultrafiltration membrane;
Step 3: then carbon nanotube carboxylated is added in deionization, ultrasonic treatment, vacuum filter is coated in through step
The ultrafiltration membrane surface of rapid two processing, is placed in the Tris-HCl buffer solution of dopamine, is then respectively adding identical molar ratio
Fe2+And persulfate, at least 5min is shaken, deionized water is cleaned after taking-up, obtains dopamine and functionalized carbon nano-tube applies altogether
Cover modified ultrafiltration membrane.
Tris-HCl buffer solution configures in the present invention:Accurately weigh 1.2114g trishydroxymethylaminomethane Tris in
In 800mL deionized water, pH to 8.5 is adjusted with the HCl of 1moL/L, deionized water is settled to 1L.
Fe in the present invention2+/ persulfate is to weigh a certain amount of respective substance respectively to be dissolved in above-mentioned Tris-HCl, is made
Fe2+It is 0.05-0.2mmol/L, Fe with persulfate concentration2+It is identical with the molar ratio of persulfate, it is ready-to-use, make
Used time mixing.
It further limits, carbon nanotube carboxylated described in step 3 is completed in the steps below:By original carbon nanometer
Pipe first passes through 70 DEG C of the concentrated sulfuric acid and concentrated nitric acid (v:V=3:1) it after mixed strong acids solution reaction 3h, is diluted with ultrapure water dissolved with carbon
The acid solution of nanotube, then carbon nanotube is collected by filtration through 0.45 μm of polytetrafluoroethylene film is sufficiently rinsed to dispersion liquid pH about etc.
In 7, the carbon nanotube after cleaning for 24 hours, is stored stand-by in dry environment in 80 DEG C of vacuum drying.
Above-mentioned original carbon nanotubes are single-walled carbon nanotube or multi-walled carbon nanotube.
Further limit, in step 1 under the conditions of 60~80 DEG C, 400~600r/min heating stirring 8h~12h.
It further limits, in step 1 in casting solution, the mass concentration of the polymer is 12%~18%, the cause
The mass concentration of hole agent is 3%~7%, and surplus is solvent.
It further limits, polymer described in step 1 is in polysulfones, polyether sulfone, Kynoar and polyvinyl chloride
One kind or in which several any combination.
Further limit, pore-foaming agent described in step 1 be one of PEG 200, PVPk30 and lithium chloride or its
In several any combination.
It further limits, organic solvent described in step 1 is n,N-Dimethylformamide, N, N- dimethylacetamide
One or more are combined in amine and N-Methyl pyrrolidone with arbitrary proportion.
It further limits, coagulation bath described in step 2 is prepared by N-Methyl pyrrolidone and deionized water, institute
The concentration for stating N-Methyl pyrrolidone is 3wt%~7wt%, and the temperature of the coagulating bath is controlled at 25 ± 0.2 DEG C, and described is solidifying
The glue time controls in 10min.
It further limits, step 3 is that deionization is added in 0.5%-2.0% by the mass concentration of carboxylic carbon nano-tube
In.
It further limits, Fe described in step 32+In/persulfate, Fe2+For FeCl2Or FeSO4;Persulfate is
One of permonosulphuric acid potassium, permonosulphuric acid sodium, permonosulphuric acid ammonium or in which several combinations in any proportion.
It further limits, dopamine concentration 2.0mg/mL, Fe2+/ persulfate concentration is 0.05-0.2mmol/L
(Fe2+/ persulfate molar ratio is 1:1).
Carbon nanotube is hydrophobic material, but its tube wall and opening existing defects can be right using this design feature
Carbon nanotube is modified.The concentrated sulfuric acid and concentrated nitric acid mixed liquor have stronger oxidisability, in a heated condition can be in film surface
A large amount of carboxylic group is formed, to realize that the carboxylated of carbon nanotube is modified.The hydrophily of original carbon nanotubes is poor, dispersion
It is easy to appear agglomeration in water, after hydrophilically modified, can be uniformly dispersed in water, to realize equal in film surface
Even coating.The preparation of ultrafiltration membrane is completed by traditional phase inversion, and whole process is not related to modifying process, in ultrafiltration film preparation
After completion, by vacuum filter or high-pressure filteration mode, carboxylic carbon nano-tube is uniformly coated to film surface, but film surface with
Adsorption capacity between carbon nanotube is weaker, it cannot be guaranteed that carbon nanotube is still secured to film surface under cross-current flow.Dopamine
The characteristic of itself determines that it can be coated in the film surface of different hydrophilic, but the polymerization process of dopamine itself is slower, logical
It needs to significantly increase the modification time of film for 24 hours under the conditions of often.Ferrous ion can activate peroxy-monosulfate while generate three
Valence iron ion (Fe3+) and potentiometric titrations (SO4 ·-), SO4 ·-Can be converted in water body hydroxyl radical free radical (·OH), SO4 ·-
With·OH can accelerate the auto polymerization process of dopamine, realize the quick adherency of poly bar amine, thus the carbon that will be coated in film surface
Nanotube is secured firmly to ultrafiltration membrane surface.
The invention has the advantages that:
(1) the required modified device of the present invention is simple, easy to operate, and management service is convenient.
(2) present invention makes full use of ferrous ion activation persulfate to generate SO4 ·-With·OH accelerates dopamine auto polymerization
Journey shortens traditional dopamine polymerization time, accelerates film preparation process, to realize that carbon nanotubes are coated in film table
Face.
(3) the present invention overcomes the absorption of the crown_interception for having given full play to ultrafiltration membrane and carbon nanotube and antibacterial characteristics,
Significantly improve ultrafiltration membrane antipollution and purification efficiency.
(4) present invention in total coat can chemical reagent impregnate or condition of high voltage under fall off, film effluent quality compared with
When poor, regenerated offline use is being carried out, the service life of film is substantially prolonged, is reducing film operating cost.
Detailed description of the invention
Fig. 1 is the modified schematic diagram of carbon nanotube carboxylated of the invention;
Fig. 2 is original carbon nanotubes of the invention and carboxylic carbon nano-tube transmission electron microscope picture;
Original ultrafiltration membrane and dopamine-carbon nanotube Fig. 3 of the invention coats modified ultrafiltration Surface scan electron microscope altogether.
Specific embodiment
Embodiment 1, the present embodiment coat the preparation method of modified ultrafiltration membrane using dopamine and functionalized carbon nano-tube altogether
It carries out in the steps below:
Step 1: 12g polysulfones and 4g PEG200 and 84g n,N-Dimethylformamide are added in 250mL conical flask, bottle
Mouth is sealed with preservative film, conical flask is placed in magnetic heating stirrer, magnetic agitation 8h under the conditions of 60 DEG C, 400r/min,
Standing and defoaming for 24 hours, forms homogeneous casting solution at room temperature;
Step 2: adjusting knifing knife up degree for being sticked on smooth glass plate with a thickness of 40 μm of PET non-woven fabrics with adhesive plaster
It is 80 μm, the casting solution that step 1 is formed uniformly is coated on non-woven fabrics with scraper, stops 1min at room temperature, then will
Entire glass plate is placed in the N-Methyl pyrrolidone deionized water that 25 DEG C of concentration are 3wt% and completes gel process;Gel 10min
Afterwards, the film prepared is placed in 25 DEG C of deionized waters for 24 hours, continues to complete inversion of phases process, complete the preparation of ultrafiltration membrane;
Step 3: take 0.5g (carboxylic carbon nano-tube) to be added in 100mL deionization carbon nanotube carboxylated, ultrasound
Processing 30min obtains dispersion liquid, is set dispersion in the ultrafiltration membrane surface handled through step 2 in the way of vacuum filter
In the Tris-HCl buffer (pH=8.5) that 100mL concentration is 2mg/mL dopamine, it is 1 that molar ratio, which is then added,:1
FeCl2Make Fe in reaction system with permonosulphuric acid potassium2+It is 0.05mmol/L with permonosulphuric acid potassium concn, shakes 5min, takes out
Deionized water is cleaned afterwards, obtains dopamine and functionalized carbon nano-tube coats modified ultrafiltration membrane altogether, be placed in 4 DEG C of deionized waters
It saves;
Wherein, carbon nanotube carboxylated described in step 3 is completed in the steps below:1g single armed carbon nanotube is mixed
In the 100mL concentrated sulfuric acid and concentrated nitric acid (v:V=3:1) in solution, 70 DEG C are heated with stirring to, after reacting 3h, dissolved with carbon nanotube
Acid solution is diluted with ultrapure water, and collects carbon nanotube with 0.45 μm of polytetrafluoroethylene film, is cleaned carbon with a large amount of ultrapure waters and is received
Carbon nanotube several times, until dispersion liquid pH is approximately equal to 7, is then placed in drying in 80 DEG C of drying boxes and for 24 hours, stores dry environment by mitron
In it is stand-by, complete carboxyl function carbon nano tube and prepare (as shown in Figure 1).
Figure it is seen that after carboxylated is modified, the dispersibility of carbon nanotube in water more evenly, agglomeration
It is unobvious, avoid the modified film surface of coating it is uneven caused by defect.
From figure 3, it can be seen that coating altogether through dopamine and carboxylic carbon nano-tube modified, modified layer is firmly adhered to film
Surface, compared with unmodified, the roughness for coating modified caudacoria increases.
Embodiment 2, the present embodiment coat the preparation method of modified ultrafiltration membrane using dopamine and functionalized carbon nano-tube altogether
It carries out in the steps below:
Step 1: 12g polyether sulfone and 4g PVPk30 and 84g N-Methyl pyrrolidone are added in 250mL conical flask, bottle
Mouth is sealed with preservative film, conical flask is placed in magnetic heating stirrer, magnetic agitation 8h under the conditions of 60 DEG C, 400r/min,
Standing and defoaming for 24 hours, forms homogeneous casting solution at room temperature;
Step 2: adjusting knifing knife up degree for being sticked on smooth glass plate with a thickness of 80 μm of PET non-woven fabrics with adhesive plaster
It is 120 μm, the casting solution that step 1 is formed uniformly is coated on non-woven fabrics with scraper, stops 1min at room temperature, then
Entire glass plate is placed in the N-Methyl pyrrolidone deionized water that 25 DEG C of concentration are 3wt% and completes gel process;Gel
After 10min, the film prepared is placed in 25 DEG C of deionized waters for 24 hours, inversion of phases process is continued to complete, completes the system of ultrafiltration membrane
It is standby;
Step 3: take 2.0g (carboxylic carbon nano-tube) to be added in 100mL deionization carbon nanotube carboxylated, ultrasound
Processing 30min obtains dispersion liquid, is set dispersion in the ultrafiltration membrane surface handled through step 2 in the way of vacuum filter
In the Tris-HCl buffer (pH=8.5) that 100mL concentration is 2mg/mL dopamine, it is 1 that molar ratio, which is then added,:1
FeCl2Make Fe in reaction system with permonosulphuric acid potassium2+It is 0.2mmol/L with permonosulphuric acid potassium concn, 5min is shaken, after taking-up
Deionized water cleaning, obtains dopamine and functionalized carbon nano-tube coats modified ultrafiltration membrane altogether, be placed in 4 DEG C of deionized waters and protect
It deposits.
Claims (10)
1. a kind of preparation method for coating modified ultrafiltration membrane altogether using dopamine and functionalized carbon nano-tube, it is characterised in that described
Preparation method carry out in the steps below:
Step 1: polymer and pore-foaming agent are added in organic solvent, heating stirring, standing and defoaming, forms homogeneous casting at room temperature
Film liquid;
Step 2: uniformly scratching the casting solution that step 1 is formed on PET non-woven fabrics, 10s~30s is stopped at room temperature, is set
Gel Treatment is carried out in coagulation bath, is then impregnated with deionized water, obtains ultrafiltration membrane;
Step 3: then carbon nanotube carboxylated is added in deionization, ultrasonic treatment, vacuum filter is coated in through step 2
The ultrafiltration membrane surface of processing is placed in the Tris-HCl buffer solution containing dopamine, is then respectively adding identical molar ratio
Fe2+And persulfate, at least 5min is shaken, deionized water is cleaned after taking-up, obtains dopamine and functionalized carbon nano-tube applies altogether
Cover modified ultrafiltration membrane.
2. a kind of preparation side for coating modified ultrafiltration membrane altogether using dopamine and functionalized carbon nano-tube according to claim 1
Method, it is characterised in that carbon nanotube carboxylated described in step 3 is completed in the steps below:Original carbon nanotubes are first passed through
70 DEG C of the concentrated sulfuric acid and concentrated nitric acid (v:V=3:1) it after mixed strong acids solution reaction 3h, is diluted with ultrapure water dissolved with carbon nanotube
Acid solution, then carbon nanotube is collected by filtration through 0.45 μm of polytetrafluoroethylene film, it sufficiently rinses to dispersion liquid pH and is approximately equal to 7, clean
Carbon nanotube afterwards for 24 hours, is stored stand-by in dry environment in 80 DEG C of vacuum drying.
3. a kind of preparation side for coating modified ultrafiltration membrane altogether using dopamine and functionalized carbon nano-tube according to claim 2
Method, it is characterised in that original carbon nanotubes are single-walled carbon nanotube or multi-walled carbon nanotube.
4. a kind of preparation side for coating modified ultrafiltration membrane altogether using dopamine and functionalized carbon nano-tube according to claim 1
Method, it is characterised in that in step 1 under the conditions of 60~80 DEG C, 400~600r/min heating stirring 8h~12h.
5. a kind of preparation side for coating modified ultrafiltration membrane altogether using dopamine and functionalized carbon nano-tube according to claim 1
Method, it is characterised in that in step 1 in casting solution, the mass concentration of the polymer is 12%~18%, the matter of the pore-foaming agent
Measuring concentration is 3%~7%, and surplus is solvent.
6. a kind of preparation side for coating modified ultrafiltration membrane altogether using dopamine and functionalized carbon nano-tube according to claim 1
Method, it is characterised in that polymer described in step 1 be one of polysulfones, polyether sulfone, Kynoar and polyvinyl chloride or
Wherein several any combination;The pore-foaming agent is one of PEG 200, PVP k30 and lithium chloride or in which several
Any combination;The organic solvent is in N,N-dimethylformamide, DMAC N,N' dimethyl acetamide and N-Methyl pyrrolidone
One or more are combined with arbitrary proportion.
7. a kind of preparation side for coating modified ultrafiltration membrane altogether using dopamine and functionalized carbon nano-tube according to claim 1
Method, it is characterised in that coagulation bath described in step 2 is prepared by N-Methyl pyrrolidone and deionized water, the N- methyl
The concentration of pyrrolidones is 3wt%~7wt%, and the temperature of the coagulating bath controls the gel time control at 25 ± 0.2 DEG C
System is in 10min.
8. a kind of preparation side for coating modified ultrafiltration membrane altogether using dopamine and functionalized carbon nano-tube according to claim 1
Method, it is characterised in that step 3 is that 0.5%-2.0% is added in deionization by the mass concentration of carboxylic carbon nano-tube.
9. a kind of preparation side for coating modified ultrafiltration membrane altogether using dopamine and functionalized carbon nano-tube according to claim 1
Method, it is characterised in that Fe described in step 32+In/persulfate, Fe2+For FeCl2Or FeSO4;Persulfate is permonosulphuric acid
One of potassium, permonosulphuric acid sodium, permonosulphuric acid ammonium or in which several combinations in any proportion.
10. a kind of preparation for coating modified ultrafiltration membrane altogether using dopamine and functionalized carbon nano-tube according to claim 1
Method, it is characterised in that dopamine concentration 2.0mg/mL, Fe2+It is 0.05mmol/L-0.2mmol/ with persulfate concentration
L, Fe2+Molar ratio with persulfate is 1:1.
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CN111203107A (en) * | 2020-02-19 | 2020-05-29 | 东华大学 | Polyphenol-iron nano film and preparation method and application thereof |
CN111701464A (en) * | 2020-06-30 | 2020-09-25 | 福州大学 | Super-hydrophilic beta-FeOOH/PDAus/PVDF composite membrane and preparation and application thereof |
CN113121859A (en) * | 2021-04-22 | 2021-07-16 | 哈尔滨工业大学 | Preparation method of electropolymerized polydopamine-carbon nanotube composite membrane |
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