CN110548418A - preparation of carbon nano tube/polyaniline/polysulfone conductive ultrafiltration membrane and membrane pollution online monitoring technology - Google Patents
preparation of carbon nano tube/polyaniline/polysulfone conductive ultrafiltration membrane and membrane pollution online monitoring technology Download PDFInfo
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- CN110548418A CN110548418A CN201810553425.3A CN201810553425A CN110548418A CN 110548418 A CN110548418 A CN 110548418A CN 201810553425 A CN201810553425 A CN 201810553425A CN 110548418 A CN110548418 A CN 110548418A
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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
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/10—Testing of membranes or membrane apparatus; Detecting or repairing leaks
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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
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
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- 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
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0013—Casting processes
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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
- B01D69/06—Flat membranes
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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
- B01D69/12—Composite membranes; Ultra-thin membranes
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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
- B01D71/02—Inorganic material
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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
- B01D71/58—Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
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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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Abstract
The invention discloses a preparation and on-line monitoring technology of a carbon nano tube/polyaniline/polysulfone conductive ultrafiltration membrane. The invention takes polysulfone as a film forming material and carbon nano tubes and polyaniline nano fibers as fillers, and prepares the carbon nano tube/polyaniline/polysulfone conductive ultrafiltration membrane by a blending method and immersion phase inversion. The polysulfone membrane is non-conductive, so that the addition of the conductive materials of the carbon nano tube and the polyaniline improves the performances of the membrane such as flux, hydrophilicity, mechanical strength and the like, and improves the conductivity of the membrane. The change of the membrane flux is reflected by the change of the membrane resistance, so that the membrane pollution condition can be monitored in real time. The preparation method and the process flow of the conductive ultrafiltration membrane are simple and easy to operate, the cost is low, the prepared membrane has excellent performance, the real-time monitoring method of membrane pollution is sensitive and simple, the service life of the membrane is prolonged, and the conductive ultrafiltration membrane can be used in the industrial fields of sewage treatment, protein separation and the like.
Description
Technical Field
The invention belongs to the technical field of preparation of modified ultrafiltration membranes and membrane pollution monitoring, and relates to a preparation and on-line membrane pollution monitoring technology of a carbon nano tube/polyaniline/polysulfone conductive ultrafiltration membrane with high permeability, high rejection rate, hydrophilicity and conductivity.
Background
With the increasing demand of people on the demand and quality of drinking water, water treatment membranes are more concerned by researchers in the separation field. However, membrane fouling has been an inevitable problem in membrane separation processes, which results in a decrease in permeability and service life of the membrane, thereby limiting the development and application of the membrane. In order to overcome the defect, the membrane needs to be modified to improve the anti-pollution performance of the membrane, and a simple and sensitive method is searched for online real-time monitoring of membrane pollution, so that the pollution degree of the membrane can be timely found and timely treated.
the preparation of a novel modified conductive film provides possibility for monitoring film pollution. The conductive film can be used as a conductive device in a conductive loop, so that the conductive film can have response current after continuously changing voltage is applied, and the conductive film is converted into the change of film resistance through the electrical signal, namely the film pollution condition is reflected through the change of the film resistance, so that the purpose of monitoring the film pollution in real time is achieved.
The conductive film modification method mainly comprises two methods of blending modification and surface modification. Wherein the blending modification is widely applied due to the advantages of simple operation, low cost and the like. The conductive film prepared by the blending method has the advantages that the conductivity of the film is improved by adding the conductive nano-filler, and meanwhile, the permeability, the retention rate, the mechanical strength and other properties of the film are improved. Polyaniline has a high specific surface area and hydrophilic groups, and is widely applied to ultrafiltration membranes, and meanwhile, polyaniline also becomes an ideal conductive polymer due to simple preparation and chemical stability. Carbon nanotubes have been used as conductive nanofillers to improve various properties of films due to their excellent mechanical properties and electrical conductivity. The carbon nanotubes and polyaniline migrate to the surface of the membrane during the phase inversion process, thereby constructing mutually connected conductive channels on the surface of the membrane and inside the membrane, and improving the conductivity of the membrane.
Disclosure of Invention
the invention aims to prepare a carbon nano tube/polyaniline/polysulfone conductive ultrafiltration membrane with excellent performance by a blending method, wherein the membrane has the advantages of good permeability, interception, hydrophilicity, pollution resistance, mechanical strength and the like, the resistance change of the membrane is monitored by a simple and sensitive method, and the pollution condition of the membrane is reflected by combining the permeation quantity of the membrane.
The technical scheme of the invention is as follows:
A carbon nano tube/polyaniline/polysulfone conductive ultrafiltration membrane is prepared by using polysulfone as a matrix film forming material and using carbon nano tubes and polyaniline as conductive nanofillers through a blending method and an immersion phase inversion method, so that the carbon nano tube/polyaniline/polysulfone conductive ultrafiltration membrane is applied to real-time monitoring of membrane pollution.
The preparation and pollution monitoring of the carbon nano tube/polyaniline/polysulfone conductive ultrafiltration membrane can be divided into the following steps:
(1) preparation of carbon nano tube/polyaniline/polysulfone conductive ultrafiltration membrane
Firstly, preparing polyaniline nano-fiber by a rapid mixing method, dissolving the polyaniline nano-fiber and carbon nano-tubes as conductive nano-fillers in an organic solvent, stirring and ultrasonically dispersing for a period of time to obtain uniform dispersion liquid, then adding a certain amount of polysulfone into the dispersion liquid, heating and stirring to prepare a membrane casting solution, placing the membrane casting solution into a vacuum oven for defoaming for a certain period of time after the membrane casting solution is ultrasonically treated, then scraping a membrane on a glass plate by a membrane scraping rod with a certain thickness to form a membrane, and stably placing the membrane on a coagulating bath for phase conversion to prepare a flat membrane.
(2) Membrane resistance testing
The prepared carbon nano tube/polyaniline/polysulfone conductive ultrafiltration membrane is placed between two titanium electrode plates and connected to an electrochemical workstation, and the conductivity of the membrane is tested by a linear sweep voltammetry method in a testing method.
(3) Membrane contamination monitoring
And (3) placing the conductive film in a film pool, connecting the conductive film to an electrochemical workstation, and recording the change of film resistance and permeation quantity in a certain time so as to perform real-time online monitoring on film pollution.
The invention has the main innovation points that:
(1) Adding carbon nano tube and polyaniline conductive nano filler, and preparing the conductive ultrafiltration membrane by a blending method and an immersion phase conversion method.
(2) The conductivity of the membrane was characterized by measuring the resistance of the membrane by linear sweep voltammetry in an electrochemical workstation.
(3) The change of membrane resistance in the separation process is responded in real time through a linear sweep voltammetry method in an electrochemical workstation, and the pollution degree of the membrane is monitored in real time on line by combining the BSA flux change.
The beneficial technical effects of the invention are as follows: according to the carbon nano tube/polyaniline/polysulfone conductive ultrafiltration membrane, the polyaniline with excellent hydrophilicity and mechanical properties and the property of the carbon nano tube modified polysulfone base membrane are added, and the nano composite membrane with excellent performances is prepared by a blending method and an immersion phase conversion method.
In the preparation process of the membrane, the polyaniline is added not only into a conductive material, but also can be used as a pore-forming agent, so that the conductivity of the membrane is improved, and the permeability of the membrane is improved. With the addition of carbon nanotubes, the permeability and conductivity of the film are improved. Under the synergistic effect of polyaniline and carbon nano tubes, compared with a pure polysulfone membrane, the flux is improved by 56%, and the conductivity is obviously improved.
The preparation method of the carbon nano tube/polyaniline/polysulfone conductive ultrafiltration membrane and the online monitoring of membrane pollution have the advantages of simple and easy operation of experimental methods, low cost, sensitive and efficient method for monitoring membrane pollution and hopeful industrial application in the field of membrane separation.
Drawings
FIG. 1 shows pure water flux of the prepared pure polysulfone membrane, polyaniline/polysulfone membrane, carbon nanotube/polysulfone membrane, and carbon nanotube/polyaniline/polysulfone membrane at 0.1 MPa.
Figure 2 is a diagram of a test membrane resistance device.
FIG. 3 is a linear sweep voltammogram of pure polysulfone film, polyaniline/polysulfone film, carbon nanotube/polyaniline/polysulfone film.
FIG. 4 is a membrane fouling monitoring device.
FIG. 5 shows the results of membrane fouling monitoring.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1: a preparation method of a pure polysulfone ultrafiltration membrane and online monitoring of membrane pollution comprise the following specific steps:
(1) Preparation of pure polysulfone ultrafiltration membrane. Weighing 6.8g of polysulfone and 0.4g of polyvinylpyrrolidone, adding the polysulfone and the polyvinylpyrrolidone into 36.5ml of N, N-dimethylformamide, heating and stirring at 60 ℃ for 7h to prepare a membrane casting solution, placing the membrane casting solution in an ultrasonic and vacuum oven for defoaming treatment, scraping the membrane by using a membrane scraping rod with the thickness of 200 mu m, and placing the membrane scraping rod in a water coagulation bath for phase conversion to obtain the flat-plate polysulfone ultrafiltration membrane.
(2) And (3) a membrane pollution online monitoring technology. The prepared pure polysulfone ultrafiltration membrane is placed in a membrane pool with a titanium electrode, is connected with an electrochemical workstation at the same time, and filters 1g/L bovine serum albumin solution under 0.1 MPa. The change of membrane resistance in the pollution process is recorded through a linear scanning voltammetry method, meanwhile, the permeation quantity of bovine serum albumin is recorded, and the membrane pollution condition is reflected through the change of the two signals.
Example 2: a preparation method of a carbon nano tube/polyaniline/polysulfone conductive ultrafiltration membrane and online monitoring of membrane pollution comprise the following specific steps:
(1) The polyaniline nano-fiber is prepared by oxidation-reduction reaction by adopting a rapid mixing method. Weighing 3ml of aniline monomer, and dissolving the aniline monomer in 100ml of 1mol/L HCl solution, and marking as solution A; 2g of ammonium persulfate was weighed out and dissolved in 100ml of 1mol/L HCl solution and recorded as solution B. The A, B solutions were mixed rapidly, stirred vigorously for 2min, and allowed to stand for 6 h. Filtering the polymerization solution with 0.22 μm microfiltration membrane, washing with methanol, acetone and deionized water for several times, and oven drying at 60 deg.C in vacuum oven.
(2) A carbon nano tube/polyaniline/polysulfone ultrafiltration membrane is prepared. Weighing 0.085g of carbon nano tube, 0.5g of polyaniline and 0.5g of polyvinylpyrrolidone, putting the carbon nano tube, the polyaniline and the polyvinylpyrrolidone into 44ml of N, N-dimethylformamide, stirring for 20min, then carrying out ultrasound for 1h, setting the ultrasound power to be 100W, thus obtaining uniformly dispersed carbon nano tube and polyaniline dispersion liquid, weighing 8.5g of polysulfone, adding the polysulfone into the dispersion liquid, heating and stirring for 7h at 60 ℃ to prepare membrane casting solution, carrying out defoaming treatment on the membrane casting solution in an ultrasound and vacuum oven at room temperature, scraping the membrane by using a membrane scraping rod with the thickness of 200 mu m, putting the membrane into a water coagulation bath for phase transformation, and obtaining the carbon nano tube/polyaniline composite conductive membrane after the phase transformation is completed.
(3) Conducting film pollution on-line monitoring technology. The prepared carbon nano tube/polyaniline/polysulfone conductive ultrafiltration membrane is placed in a membrane pool with a titanium electrode, is connected with an electrochemical workstation at the same time, and filters 1g/L bovine serum albumin solution under 0.1 MPa. The change of membrane resistance in the pollution process is recorded through a linear scanning voltammetry method, meanwhile, the permeation quantity of bovine serum albumin is recorded, and the membrane pollution condition is reflected through the change of the two signals.
Claims (9)
1. a preparation method of a carbon nano tube/polyaniline/polysulfone conductive ultrafiltration membrane and an on-line membrane pollution monitoring technology are characterized by comprising the following steps:
(1) Preparation of polyaniline
The polyaniline nano-fiber is prepared by a rapid mixing method. Weighing a certain amount of aniline to dissolve in an acid solution with a certain concentration, weighing a certain amount of initiator to dissolve in an acid solution with the same concentration, quickly mixing the two solutions, stirring for a certain time, standing for 5 hours, separating the prepared polyaniline by using a suction filtration device, washing with acetone, diluted acid solution and deionized water, and finally putting into a vacuum oven to dry and grind for later use.
(2) Preparation of carbon nano tube/polyaniline/polysulfone conductive ultrafiltration membrane
Dissolving carbon nano tubes and prepared polyaniline which are used as nano fillers and additives into a solvent, stirring for a period of time, and then carrying out ultrasonic dispersion for a certain period of time in a water bath to obtain a uniform dispersion liquid. Adding a certain amount of polysulfone into the dispersion liquid, heating and stirring for a certain time to form a uniform membrane casting solution, and then placing the membrane casting solution into a vacuum oven for defoaming after carrying out ultrasonic treatment for a period of time. And (3) scraping the membrane on a glass plate by using a membrane scraping rod with a certain thickness, and stably putting the glass plate into a coagulating bath for solvent exchange, namely a phase inversion process, so as to obtain the carbon nano tube/polyaniline/polysulfone conductive ultrafiltration membrane.
(3) Membrane resistance testing
The prepared carbon nano tube/polyaniline/polysulfone conductive ultrafiltration membrane is placed between two titanium electrode plates and connected to an electrochemical workstation, and a current-voltage curve is obtained under a certain voltage range and scanning rate through a linear sweep voltammetry method in a testing method, so that a membrane resistance is obtained, and the quality of the conductivity of the membrane is represented.
(4) on-line monitoring of membrane fouling conditions
The change relation between the membrane surface resistance and the membrane flux is established by measuring the values of the membrane surface resistance and the membrane flux in the membrane filtration process, so that the electrical signals are converted into real-time monitoring of the membrane pollution condition. The membrane pollution condition can be timely detected by monitoring the change of the membrane resistance on line, and the next treatment is carried out according to the membrane pollution condition, so that the service life of the membrane is prolonged, the cost is saved, and the real-time monitoring technology has great application potential in the field of membrane separation.
2. The process (1) according to claim 1, wherein the acid solution is selected from hydrochloric acid, sulfuric acid, perchloric acid or dodecylbenzenesulfonic acid, and has a concentration of 0.1 to 3 mol/L; the initiator can be selected from ammonium persulfate, ferric trichloride or potassium persulfate.
3. The process (1) according to claim 1, wherein the molar ratio of aniline and initiator is 1: 1 to 10: 1, thereby preparing the nanofibrous polyaniline.
4. Step (2) according to claim 1, wherein the additive is selected from polyvinylpyrrolidone, polyethylene glycol, titanium dioxide, in an amount of 1-3%; the solvent can be N-N-dimethylacetamide, N-dimethylformamide and N-methylpyrrolidone, and the content is 70-90%; the film forming material can be selected from polysulfone, polyethersulfone, polyvinylidene fluoride and polypropylene, and the content is 10-20%.
5. Step (2) according to claim 1, characterized in that the stirring time is 10-40 min; the ultrasonic power of the water bath is 60-100W; the ultrasonic time is 1-3 h; stirring in water bath for 4-8 h; the heating temperature is 50-80 ℃; the ultrasonic defoaming time of the casting solution is 10-30min, and the ultrasonic power is 60-100W; the defoaming temperature of the vacuum oven is 20-50 ℃, and the time is 10-15 h; the temperature of the coagulating bath is 20-40 ℃.
6. Step (3) according to claim 1, wherein the linear sweep voltammetry is used by applying a linearly varying voltage to the electrode while measuring the response current of the working electrode or the reference electrode to obtain a current versus electrode potential curve (I-V curve); the voltage range is-5V-5V; scanning rate: 1-50 mV/s.
7. Step (4) according to claim 1, wherein the prepared conductive membrane is placed in a membrane cell with a titanium electrode, wherein the conductive membrane is in contact with the titanium ring and connected to a working electrode in an electrochemical workstation, and another titanium sheet electrode is connected to a reference electrode and a counter electrode, and a conductive loop is constructed to monitor changes in membrane resistance in real time.
8. Step (4) according to claim 1, wherein a Bovine Serum Albumin (BSA) solution is used as the contaminating solution, and the concentration thereof is 1g/L, and the operating pressure is 0.1 MPa. Under the pressure, the polluted solution is filtered within a certain time, the change of the membrane resistance and the BSA flux along with the time is recorded, and the membrane pollution condition is found in time, so that the membrane is cleaned or treated in other ways, and the efficient utilization of the membrane is realized.
9. Step (4) according to claim 1, characterized in that the change of current with electrode potential, i.e. the change of membrane resistance, over time is acquired using linear sweep voltammetry. The method is convenient, quick, sensitive and wide in applicability.
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| CN114558461A (en) * | 2022-03-21 | 2022-05-31 | 合肥九号线传媒科技有限公司 | Organic-inorganic composite conductive filter membrane and preparation method thereof |
| CN117101419A (en) * | 2023-10-23 | 2023-11-24 | 山东卫康生物医药科技有限公司 | Medical functional food production control system |
| CN117431587A (en) * | 2023-12-22 | 2024-01-23 | 烟台泰和新材高分子新材料研究院有限公司 | Composite diaphragm and preparation method and application thereof |
| CN117504607A (en) * | 2024-01-08 | 2024-02-06 | 武汉工程大学 | Method, device and system for detecting anti-pollution performance of forward osmosis membrane and electronic equipment |
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| CN117431587A (en) * | 2023-12-22 | 2024-01-23 | 烟台泰和新材高分子新材料研究院有限公司 | Composite diaphragm and preparation method and application thereof |
| CN117504607A (en) * | 2024-01-08 | 2024-02-06 | 武汉工程大学 | Method, device and system for detecting anti-pollution performance of forward osmosis membrane and electronic equipment |
| CN117504607B (en) * | 2024-01-08 | 2024-03-22 | 武汉工程大学 | Method, device and system for detecting anti-pollution performance of forward osmosis membrane and electronic equipment |
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Application publication date: 20191210 |