CN114832633A - Preparation method and application of nanofiltration membrane based on hydrogel coated stainless steel wire mesh - Google Patents
Preparation method and application of nanofiltration membrane based on hydrogel coated stainless steel wire mesh Download PDFInfo
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- CN114832633A CN114832633A CN202210378447.7A CN202210378447A CN114832633A CN 114832633 A CN114832633 A CN 114832633A CN 202210378447 A CN202210378447 A CN 202210378447A CN 114832633 A CN114832633 A CN 114832633A
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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
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
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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
- B01D65/02—Membrane cleaning or sterilisation ; Membrane regeneration
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/22—Electrical effects
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
Abstract
The invention belongs to the technical field of membrane separation, and particularly relates to a preparation method and application of a nanofiltration membrane based on a hydrogel coated stainless steel wire mesh. The stainless steel wire mesh, the Kevlar fiber for preparing hydrogel, the piperazine for interfacial polymerization, the trimesoyl chloride and other raw materials are cheap, and the integral preparation method does not need complex equipment and is simple and easy to implement. In addition, the invention innovatively proposes that hydrogel is precoated on the stainless steel wire mesh supporting layer to construct a reaction interface convenient for polyamide growth, overcomes the problem that the large gap of the stainless steel wire mesh is not beneficial to interfacial polymerization to generate a continuous polyamide layer, and successfully prepares the novel conductive nanofiltration membrane on the stainless steel wire mesh.
Description
Technical Field
The invention belongs to the technical field of membrane separation, and particularly relates to a preparation method and application of a nanofiltration membrane based on a hydrogel coated stainless steel wire mesh.
Background
Nanofiltration is used as a novel pressure-driven membrane separation technology, can realize effective removal of multivalent ions and organic small molecules (molecular weight is larger than 200Da), has the advantages of high separation efficiency, adjustable selectivity and the like, and has wide application prospects in the fields of seawater desalination, wastewater treatment, sewage recycling and the like. Commercial nanofiltration membranes are generally based on a polyamide thin-layer composite structure, although the membrane surface is negatively charged at neutral pH and has electrostatic repulsion on negatively charged pollutants in a water body, the pollutants are inevitably deposited on the membrane surface due to the driving force generated in the membrane filtration process, so that membrane pollution is caused. The membrane pollution can obviously reduce the membrane flux and increase the operation energy consumption, and is a main technical bottleneck for limiting the long-term stable use of the nanofiltration membrane.
The charged pollutants are driven to move reversely by coupling an external field in a hydraulic field, and the method is a potential way for preventing the pollutants from depositing on the membrane surface and relieving membrane pollution. Novel electrically conductive nanofiltration membrane has separation characteristic and electrically conductive function simultaneously, increases the repulsion between the pollutant in conducting film and the water through applying external voltage at the membrane separation in-process, makes the pollutant remove to the direction of keeping away from the membrane surface, thereby it alleviates the membrane pollution to hopefully reduce the deposit of pollutant on the membrane surface. Therefore, the invention aims to prepare the nanofiltration membrane with conductive performance, and the rejection of the membrane and charged pollutants is enhanced through the action of an external electric field, so that the problem of membrane pollution in the process of a nanofiltration membrane separation process is solved.
The stainless steel wire mesh support layer has good electric conductivity and mechanical property, is an ideal support layer material for preparing the composite novel electric conduction nanofiltration membrane, but has larger gap and is difficult to directly form a polyamide interception layer on the stainless steel wire mesh support layer through interfacial polymerization. The invention innovatively provides that hydrogel is pre-coated on a stainless steel wire mesh supporting layer, a reaction interface convenient for polyamide growth is constructed, a polyamide nanofiltration interception layer is formed on a hydrogel-stainless steel wire mesh complex through interface polymerization, and the novel nanofiltration membrane based on the hydrogel coated stainless steel wire mesh is prepared, so that the membrane can play the nanoscale separation performance and simultaneously shows the anti-pollution characteristic to charged pollutants under the action of an external electric field.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defect that the pollution of the nanofiltration membrane cannot be controlled in the prior art, so that the preparation method and the application of the nanofiltration membrane based on the hydrogel coated stainless steel wire mesh are provided.
Therefore, the invention provides the following technical scheme,
the invention provides a method for preparing a nanofiltration membrane based on a hydrogel coated stainless steel wire mesh, which comprises the following steps of,
(1) placing a stainless steel wire mesh in a nitric acid solution for pretreatment, then cleaning the stainless steel wire mesh by using deionized water, then soaking the stainless steel wire mesh in an isopropanol solution for treatment, cleaning the stainless steel wire mesh by using the deionized water, and finally drying the stainless steel wire mesh to obtain a stainless steel wire mesh precursor;
(2) pouring the hydrogel solution on a stainless steel wire mesh precursor for soaking, and cleaning and exchanging with deionized water to obtain a stainless steel wire mesh with the surface coated with hydrogel;
(3) and (2) immersing the stainless steel wire mesh with the hydrogel coated on the surface into a water solution containing piperazine, then immersing the stainless steel wire mesh into a n-hexane solution containing trimesoyl chloride for reaction, and carrying out heat treatment after the reaction to obtain the target nanofiltration membrane.
Optionally, the average pore diameter of the stainless steel wire mesh is 0.5-2 μm;
and/or the concentration of the nitric acid solution is 3-5 mol/L.
Optionally, the pretreatment time is 30-60 min;
and/or the concentration of the isopropanol is 20-25 v%.
Optionally, the treatment time is 10-30 min;
and/or the drying temperature is 50 ℃.
Optionally, the preparation method of the hydrogel solution comprises the following steps,
s1: commercial Kevlar fiber was cut into 3-6mm long pieces, which were then soaked overnight in a mixed solution containing 5-10 v% ethanol and 5-10 v% dimethylacetamide. Then the mixture is thoroughly washed by deionized water and is placed in a blast drying oven for drying at 40 ℃.
S2: and (2) weighing 1-3g of Kevlar fiber and 1-3g of potassium hydroxide obtained in the step (S1), dissolving in a mixed solution containing 0-6.0mL of deionized water and 98mL of dimethyl sulfoxide, stirring at the rotating speed of 300rpm, stirring at room temperature for 1 week, and standing for 24 hours to obtain a hydrogel solution.
Optionally, the pouring amount of the hydrogel solution in the step (2) is 5-10 mL;
and/or, the soaking time is 5-10 min.
Optionally, the time of the cleaning exchange in the step (2) is 10-60 min;
and/or the mass volume fraction of the piperazine water solution in the step (3) is 0.1-0.3 wt/v%.
Optionally, the mass volume fraction of the trimesoyl chloride contained in the step (3) is 0.08-0.24 wt/v%;
And/or the immersion time is 10 min.
Optionally, the reaction time is 30-90 s;
and/or the time of the heat treatment is 5 min;
and/or the temperature of the heat treatment is X-X ℃.
The invention also provides an application of the nanofiltration membrane prepared by the preparation method in controlling membrane pollution;
the method comprises the following steps of taking the nanofiltration membrane as a cathode and taking a titanium net as an anode, increasing the repulsive force between charged pollutants and the surface of the nanofiltration membrane under the condition of external voltage, and slowing down the deposition rate of the negatively charged pollutants on the membrane surface, thereby realizing membrane pollution control.
The technical proposal provided by the invention has the advantages that,
1. the invention uses stainless steel wire net, Kevlar fiber for preparing hydrogel, piperazine for interfacial polymerization, trimesoyl chloride and other raw materials with low price, and the integral preparation method does not need complex equipment and is simple and easy to implement. In addition, the invention innovatively proposes that hydrogel is precoated on the stainless steel wire mesh supporting layer to construct a reaction interface convenient for polyamide growth, overcomes the problem that the large gap of the stainless steel wire mesh is not beneficial to interfacial polymerization to generate a continuous polyamide layer, and successfully prepares the novel conductive nanofiltration membrane on the stainless steel wire mesh.
2. The novel nanofiltration membrane prepared by the invention based on the hydrogel coated stainless steel wire mesh can exert the nanoscale separation performance, and simultaneously can show the anti-pollution characteristic to charged pollutants under the action of an external electric field, thereby providing an innovative scheme for solving the problem of membrane pollution in the practical application of the nanofiltration membrane.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1(a) is a scanning electron microscope photograph of a stainless steel wire mesh produced in example 1;
FIG. 1(b) is a scanning electron microscope photograph of the hydrogel-stainless steel wire mesh composite prepared in example 2;
FIG. 1(c) is a scanning electron microscope image of the novel nanofiltration membrane based on hydrogel coated stainless steel wire mesh prepared in example 3;
FIG. 2 is a plot of linear voltammetric scans (LSV) for examples 1, 2, and 3;
FIG. 3 is a graph of water permeability and retention of Na2SO4, MgSO4, MgCl2, CaCl2 and NaCl for a novel conductive nanofiltration membrane;
fig. 4 is a graph of normalized membrane flux over time for the prepared novel conductive nanofiltration membrane in a 300min filtration cycle.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Example 1
Cutting a stainless steel wire mesh with the average aperture of 1 mu m into a circular sheet with the diameter of 7.5cm, cleaning the circular sheet by using deionized water, soaking the circular sheet in a nitric acid solution of 5mol/L for 30min, and then thoroughly cleaning the circular sheet by using the deionized water. Then the mixture is soaked in 25 v% isopropanol solution for 10min, then is thoroughly washed by deionized water, and is placed in a blast drying oven for drying at 40 ℃.
Fig. 1(a) is a scanning electron microscope image of the stainless steel wire mesh support layer prepared as described above, and it is found that the surface of the pretreated stainless steel wire mesh is smoother. The conductivity of the conductive coating is 140252S/m by adopting a four-probe method.
Example 2
A stainless steel wire mesh support layer was obtained in the same manner as in example 1. Preparing a hydrogel solution, wherein the specific preparation method comprises the following steps: (1) commercial Kevlar fibers were cut into 6 mm-length pieces and then soaked overnight in a mixed solution containing 5 v% ethanol and 5 v% dimethylacetamide. Then thoroughly washed with deionized water and dried in a forced air drying oven at 40 ℃. (2) 2.0g of Kevlar fiber and 2.0g of potassium hydroxide were dissolved in a mixed solution containing 2mL of deionized water and 98mL of dimethyl sulfoxide, and the mixture was stirred at room temperature at 300rpm for 1 week and then allowed to stand for 24 hours to obtain a hydrogel solution. (3) Putting a stainless steel wire mesh supporting layer into a polytetrafluoroethylene mold, pouring 5mL of hydrogel solution into the stainless steel wire mesh for 10min, removing the redundant solution on the surface, pouring a large amount of deionized water immediately, exchanging dimethyl sulfoxide in the hydrogel solution with the aqueous solution for 30min to promote phase conversion to form hydrogel, and then thoroughly cleaning with deionized water to remove the redundant substances on the surface.
Fig. 1(b) is a scanning electron microscope image of the hydrogel-stainless steel wire mesh composite prepared as described above, and it is found that the continuous hydrogel layer is successfully coated on the stainless steel wire mesh, which is beneficial for the subsequent interfacial polymerization reaction to form a polyamide layer.
Example 3
The hydrogel-stainless steel wire mesh composite is obtained by the same method as the embodiment 2, and then is immersed in 0.2 wt/v% piperazine water solution for 10min, the obtained composite is taken out and then placed on the back of a stainless steel wire mesh supporting layer to absorb the redundant liquid drops on the surface of the hydrogel, then the composite membrane attached with the piperazine water solution is immersed in 0.16 wt/v% trimesoyl chloride/n-hexane solution to carry out interfacial polymerization reaction for 60s to obtain a polyamide interception layer, and after the reaction is finished, the polyamide interception layer is placed in a blast drying oven for heat treatment at 60 ℃ for 5min to obtain the target nanofiltration membrane.
Fig. 1(c) is a scanning electron microscope image of the novel nanofiltration membrane based on hydrogel-coated stainless steel mesh prepared as described above, and it was found that a continuous polyamide layer had been formed on the hydrogel-stainless steel mesh composite.
Fig. 2 is a plot of linear voltammetric scans (LSV) for examples 1, 2, and 3, and it can be seen that the topcoat hydrogel and the subsequently formed polyamide layer have no significant effect on the conductivity of the stainless steel wire mesh.
Test example 1
The prepared novel conductive nanofiltration membrane is loaded into a cross-flow filtering device and pre-pressed for 2 hours at 6bar, and then the water permeability and Na pair of the conductive nanofiltration membrane are tested at 6bar 2 SO 4 、MgSO 4 、MgCl 2 、CaCl 2 And the interception effect of five salts of NaCl, and figure 3 shows the water permeability of the novel conductive nanofiltration membrane and the water permeability of the novel conductive nanofiltration membrane on Na2SO4, MgSO4 and MgCl 2 、CaCl 2 And NaCl interception effect chart, and the water permeability of the novel conductive nanofiltration membrane is 25L m -2 h -1 bar -1 To Na 2 SO 4 、MgSO 4 、MgCl 2 、CaCl 2 And the rejection rates of NaCl are 95.3%, 71.9%, 13.0%, 11.5% and 15.5% respectively, which shows that the novel conductive nanofiltration membrane has good nanoscale separation performance and ideal selectivity to sulfate radicals/chloride ions.
Test example 2
The titanium mesh is used as an anode, the novel conductive nanofiltration membrane is used as a cathode, the distance between the two electrodes is 1.0mm, and the two electrodes are connected to a direct-current stabilized power supply through titanium leads. Starting a charged cross-flow filtration system by using a 200mg/L bovine serum albumin (pH 7.2) solution containing 2g/L sodium chloride electrolyte as a pollutant solution, and applying voltages of 0, 1.5 and 2.0V respectively after the membrane flux is stable to monitor the change of the membrane flux. Fig. 4 is a graph of normalized membrane flux over time for the prepared novel conductive nanofiltration membrane over a 300min filtration cycle. When the voltage is 2.0V, the membrane flux of the novel conductive nanofiltration membrane in the filtering process is higher than that of the novel conductive nanofiltration membrane without the voltage, which shows that the novel nanofiltration membrane based on the hydrogel coated stainless steel wire mesh shows certain pollution resistance under the voltage application condition.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A method for preparing a nanofiltration membrane based on a hydrogel coated stainless steel wire mesh is characterized by comprising the following steps of,
(1) placing a stainless steel wire mesh in a nitric acid solution for pretreatment, then cleaning the stainless steel wire mesh by using deionized water, then soaking the stainless steel wire mesh in an isopropanol solution for treatment, cleaning the stainless steel wire mesh by using the deionized water, and finally drying the stainless steel wire mesh to obtain a stainless steel wire mesh precursor;
(2) pouring the hydrogel solution on a stainless steel wire mesh precursor for soaking, and cleaning and exchanging with deionized water to obtain a stainless steel wire mesh with the surface coated with hydrogel;
(3) and (2) immersing the stainless steel wire mesh with the hydrogel coated on the surface into a water solution containing piperazine, then immersing the stainless steel wire mesh into a n-hexane solution containing trimesoyl chloride for reaction, and carrying out heat treatment after the reaction to obtain the target nanofiltration membrane.
2. The method for preparing a nanofiltration membrane based on a hydrogel coated stainless steel screen according to claim 1, wherein the stainless steel screen has an average pore size of 0.5-2 μm;
and/or the concentration of the nitric acid solution is 3-5 mol/L.
3. The method for preparing a nanofiltration membrane based on a hydrogel coated stainless steel screen according to claim 1 or 2, wherein the pretreatment time is 30-60 min;
and/or the concentration of the isopropanol is 20-25 v%.
4. The method for preparing nanofiltration membranes based on hydrogel coated stainless steel screens according to any one of claims 1 to 3, wherein the treatment time is 10 to 30 min;
and/or the drying temperature is 50 ℃.
5. The method for preparing nanofiltration membrane based on a hydrogel coated stainless steel screen according to any one of claims 1 to 4, wherein the hydrogel solution is prepared by a method comprising the following steps,
s1: commercial Kevlar fiber was cut into 3-6mm long pieces, which were then soaked overnight in a mixed solution containing 5-10 v% ethanol and 5-10 v% dimethylacetamide. Then the mixture is thoroughly washed by deionized water and is placed in a blast drying oven for drying at 40 ℃.
S2: and (3) weighing 1-3g of Kevlar fiber and 1-3g of potassium hydroxide obtained in the step (S1), dissolving the Kevlar fiber and the potassium hydroxide in a mixed solution containing 0-6.0mL of deionized water and 98mL of dimethyl sulfoxide, stirring at the rotating speed of 300rpm, stirring at room temperature for 1 week, and standing for 24 hours to obtain a hydrogel solution.
6. The method for preparing nanofiltration membranes based on hydrogel coated stainless steel screens according to any one of claims 1 to 5, wherein the amount of the hydrogel solution poured in the step (2) is 5 to 10 mL;
and/or the soaking time is 5-10 min.
7. The method for preparing nanofiltration membranes based on hydrogel coated stainless steel screens according to any one of claims 1 to 6, wherein the time for the cleaning exchange in the step (2) is 10 to 60 min;
and/or the mass volume fraction of the piperazine water solution in the step (3) is 0.1-0.3 wt/v%.
8. The method for preparing a nanofiltration membrane based on a hydrogel coated stainless steel screen according to any one of claims 1 to 7, wherein the mass volume fraction of trimesoyl chloride in the step (3) is 0.08 to 0.24 wt/v%;
and/or the immersion time is 10 min.
9. The method for preparing nanofiltration membranes based on hydrogel coated stainless steel screens according to any one of claims 1 to 8, wherein the reaction time is 30 to 90 s;
and/or the time of the heat treatment is 5 min;
and/or the temperature of the heat treatment is X-X ℃.
10. The application of the nanofiltration membrane prepared by the preparation method of any one of claims 1 to 9 in controlling membrane pollution;
The method comprises the following steps of taking the nanofiltration membrane as a cathode and taking a titanium net as an anode, increasing the repulsive force between charged pollutants and the surface of the nanofiltration membrane under the condition of external voltage, and slowing down the deposition rate of the negatively charged pollutants on the membrane surface, thereby realizing membrane pollution control.
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110288199A1 (en) * | 2010-05-19 | 2011-11-24 | Hospital For Special Surgery | Fiber-Hydrogel Composite for Tissue Replacement |
| CN103463999A (en) * | 2013-09-06 | 2013-12-25 | 烟台绿水赋膜材料有限公司 | Preparation method of novel ultrathin salt-cutting separation membrane |
| CN104888496A (en) * | 2015-05-04 | 2015-09-09 | 江苏大学 | Method for coating surface of underwater oleophobic net film with nano-material |
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