CN112473372B - Conductive forward osmosis membrane and preparation method thereof - Google Patents

Conductive forward osmosis membrane and preparation method thereof Download PDF

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CN112473372B
CN112473372B CN202011431341.6A CN202011431341A CN112473372B CN 112473372 B CN112473372 B CN 112473372B CN 202011431341 A CN202011431341 A CN 202011431341A CN 112473372 B CN112473372 B CN 112473372B
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王新华
徐梦思
周倩
赵频
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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
    • B01D61/002—Forward osmosis or direct osmosis
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    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
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    • B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
    • B01D71/68—Polysulfones; Polyethersulfones
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • C02F1/445—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by forward osmosis
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Abstract

The invention discloses a conductive forward osmosis membrane and a preparation method thereof, belonging to the technical field of water treatment. The method takes a polymer film as a supporting layer, and firstly, MXene powder is fully dispersed into deionized water in a short time in an ultrasonic dispersion mode to obtain uniform MXene dispersion liquid; and then, carrying out suction filtration on the dispersion liquid to the surface of the polyether sulfone support layer, and preparing the conductive forward osmosis membrane through interfacial polymerization. The conductive forward osmosis membrane prepared by the invention has good conductivity, can combine the membrane separation process with the electrochemical process in the sewage treatment process, and effectively relieves the organic pollution of the FO membrane.

Description

Conductive forward osmosis membrane and preparation method thereof
Technical Field
The invention relates to a conductive forward osmosis membrane and a preparation method thereof, belonging to the technical field of water treatment.
Background
Forward Osmosis (FO) is a membrane separation process in which water permeates from a feed liquid side (low osmotic pressure side) through an osmotic membrane to a draw liquid side (high osmotic pressure side) driven by an osmotic pressure difference. In recent years, the FO technology has shown good application potential in the fields of seawater desalination, salt difference power generation, sewage treatment and reuse, farmland irrigation and the like. However, the lower water flux limits the widespread application of FO technology. There are many reasons for the low water flux during FO operation, and among them, membrane fouling (especially organic fouling caused by alginate, protein, natural organic substances, etc.) is one of the main factors causing flux attenuation, so that slowing down the organic fouling of FO membrane is of great significance to improve the operation performance of FO.
Currently, there is an increasing interest in controlling organic contamination by means of FO membrane modification, and alleviating organic contamination by means of an external electric field under the action of electrostatic repulsion on the basis of preparing a conductive membrane is a commonly used way of membrane modification and then alleviating organic contamination. While it has been proposed by researchers to introduce a nanomaterial layer on the FO membrane to improve membrane performance, in view of the high conductivity and hydrophilicity of MXene, we associate the introduction of an MXene layer with conductive properties to prepare a conductive FO membrane and study the feasibility of conductive FO membranes to mitigate organic contamination.
Disclosure of Invention
The invention aims to provide a conductive FO membrane and a preparation method thereof, wherein the conductive FO membrane takes a polymer membrane as a carrier, namely MXene (Ti)3C2) And as a conductive material, MXene dispersion is deposited on a support layer in a vacuum filtration mode, and the conductive FO membrane is prepared through interfacial polymerization. The conductive FO membrane prepared by the invention has conductive performance, and can combine the membrane separation process with the electrochemical process in the sewage treatment process, thereby effectively relieving the organic pollution of the FO membrane.
First, it is a first object of the present invention to provide a method for making a conductive FO membrane using a polymer membrane as a support layer, MXene (Ti) membrane3C2) And (3) as a conductive material, depositing the MXene dispersion liquid on the surface of the polymer support layer in a vacuum filtration mode, and preparing the conductive FO membrane through interfacial polymerization.
In one embodiment of the present invention, the preparation method specifically includes the following steps:
(1) preparing MXene (Ti) with the concentration of 0.1-0.5 mg/mL3C2) A dispersion liquid;
(2) preparing an MXene layer: depositing a certain volume of the dispersion liquid obtained in the step (1) on a polyether sulfone or polysulfone supporting layer in a vacuum filtration mode under a certain pressure, drying the membrane, and soaking the membrane in water after drying;
(3) preparation of conductive FO membranes: fixing the film obtained in the step (2), pouring a certain mass fraction of m-phenylenediamine solution onto the surface of the film, and removing the m-phenylenediamine solution remained on the surface of the film after soaking; and then pouring a trimesoyl chloride solution with a certain mass fraction onto a membrane surface for reaction, draining, and placing the membrane in a hot water bath for thermal crosslinking to obtain the conductive FO membrane.
In one embodiment of the present invention, the preparation method of the dispersion liquid of step (1) is specifically: taking a certain amount of MXene (Ti)3C2) Ultrasonically dispersing the powder in water, and centrifuging to remove undispersed MXene powder to obtain MXene componentAnd (4) dispersing.
In one embodiment of the invention, MXene powder is subjected to ultrasonic treatment for 0.5 to 1 hour at a power of 200 to 600W, and then centrifuged at a rotation speed of 3000 to 6000r for 0.2 to 0.5 hour to obtain a dispersion.
In one embodiment of the invention, in the step (1), the ratio of the MXene powder to water in mg of mass to volume (mL) is (1-7): 40.
in one embodiment of the present invention, in step (1), the water is preferably deionized water or purified water.
In one embodiment of the invention, in the step (2), the MXene dispersion liquid is filtered on the polyether sulfone membrane supporting layer under the pressure of 0.1-1 MPa.
In one embodiment of the present invention, in the step (2), the concentration of the MXene dispersion is 0.1 to 0.5mg/mL, and the volume ratio of the dispersion to water is (1 to 1.5): 7, the MXene content on the film is 0.03-0.20 mg/cm2And drying the mixture in an oven at the temperature of between 60 and 100 ℃ for 0.3 to 0.5 hour.
In one embodiment of the invention, in the step (3), the conductive FO membrane is prepared based on the membrane sheet obtained in the step (2), the mass fraction of m-phenylenediamine is 2-4%, the soaking time is 1-10 min, the mass fraction of trimesoyl chloride is 0.1-0.2%, and the reaction is 1-10 min.
In one embodiment of the present invention, the step (3) is performed by thermal crosslinking in a hot water bath at 80-100 ℃ for 2-5 min to obtain the conductive FO membrane.
A second object of the present invention is to provide a conductive FO membrane prepared by the above method.
It is a third object of the present invention to provide a water treatment device or apparatus comprising the above-described conductive FO membrane.
A fourth object of the present invention is to provide the above production method or the use of the above conductive FO membrane in water treatment.
Compared with the prior art, the invention has the following advantages:
(1) when the conductive FO membrane is prepared, MXene powder is fully dispersed into deionized water in a short time by an ultrasonic dispersion mode to obtain uniform MXene dispersion liquid; and then, carrying out suction filtration on the surface of the polyether sulfone support layer to prepare the conductive FO membrane through interfacial polymerization. MXene is a two-dimensional transition metal carbide with strong metal conductivity, the existence of a terminal group (such as-OH) of MXene enables MXene to have a hydrophilic surface, and the combination of hydrophilicity and metal conductivity is one of the advantages of MXene over graphene materials. In addition, the MXene surface is negatively charged because the O and F atoms in the MXene end group have large electronegativity. These properties of MXene enhance the anti-fouling properties of the membrane itself.
(2) The membrane prepared by the invention has an active layer with high permeability and selectivity, and can realize the high-efficiency interception of organic matters in the FO process; meanwhile, the conductive MXene material forms a conductive network in the polyether sulfone membrane, so that the membrane can be used as an electrode under the condition of an external electric field, and the deposition of organic pollutants on the membrane surface is reduced. The invention applies the preparation technology of the conductive FO membrane to the field of sewage treatment, combines the membrane separation process with the electrochemical process in the sewage treatment process, is a brand-new subject in the fields of environmental engineering, material chemistry and electrochemistry, simultaneously achieves the aims of sewage treatment, membrane pollution reduction and FO membrane performance improvement, and has great theoretical significance and application value.
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Fig. 1 is a schematic diagram of the fabrication of a conductive FO membrane.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
A method of making a conductive FO membrane comprising the steps of:
(1) preparation of MXene (Ti)3C2) Dispersion liquid: 10mg of Ti were weighed3C2Ultrasonic dispersion of the powder (300W, 0.5h) at 200mL deionizationAdding water, and centrifuging (6000r, 0.2 hr) to remove undispersed Ti3C2Powder, i.e. uniform MXene (Ti) is obtained3C2) The concentration of the dispersion liquid is 0.15 mg/mL;
(2) preparing an MXene layer: depositing 35mL of MXene dispersion liquid on a polyether sulfone support layer in a vacuum filtration mode under the pressure of 0.2MPa, drying the membrane in a 60 ℃ drying oven for 0.5h, taking out, and fully soaking in deionized water;
(3) preparation of conductive FO membranes: fixing the film obtained in the step (2), pouring a proper amount of m-phenylenediamine solution with the mass fraction of 2% onto the surface of the film, soaking for 1min, and removing the m-phenylenediamine solution remained on the film surface by using a rubber roller after soaking; and then pouring 0.1 mass percent of trimesoyl chloride solution onto the membrane surface for reaction for 2min, draining, and then placing the membrane in a hot water bath at 100 ℃ for thermal crosslinking for 5min to obtain the conductive FO membrane.
The water flux and the salt flux were measured by equation (1) and equation (2), respectively.
Figure BDA0002820756580000031
In the formula, JWRepresents the water flux of the membrane, L/(m)2H), abbreviated as LMH; Δ V represents the volume of the raw material solution that permeates the membrane, L; Δ t represents the time of the test experiment, h; a. themRepresents the effective area of the film, m2。
Figure BDA0002820756580000032
In the formula, JsIs the reverse salt flux of the membrane, g/(m)2·h)；C0And CtAnd the salt concentrations of the starting and ending starting solutions, mg/L, respectively; v0And V0The volume of the starting and ending feed solution, L, respectively; Δ t represents the experimental time, h; a. themRepresents the effective area of the film, m2。
The conductive FO membrane was found to have a water flux of 13.5 L.m-2·h-1Reverse salt flux of 1.8 g.m-2·h-1。
Example 2
A method of making a conductive FO membrane, differing from example 1 in that: weighing 15mg of Ti3C2The powder was ultrasonically dispersed (300W, 0.5h) in 200mL deionized water and the undispersed Ti was removed by centrifugation (6000r, 0.2h)3C2Powder, i.e. uniform MXene (Ti) is obtained3C2) The concentration of the dispersion was 0.23 mg/mL. And then, under the pressure of 0.2MPa, taking 35mL of dispersion liquid, carrying out suction filtration on the polyether sulfone support layer, placing the membrane in a 60 ℃ oven, drying for 0.5h, taking out, and placing in deionized water for infiltration. Fixing the fully soaked membrane by using a plate frame, pouring a proper amount of 2% m-phenylenediamine solution onto the surface of the membrane for soaking for 1min, removing the m-phenylenediamine solution remained on the membrane surface by using a rubber roller after soaking, then taking a proper amount of 0.1% trimesoyl chloride solution for reacting for 2min, draining, and then placing the membrane in a hot water bath at 100 ℃ for thermal crosslinking for 5min to obtain the conductive FO membrane.
According to the test method of example 1, the water flux of the conductive forward osmosis membrane was measured to be 15.6 L.m-2·h-1Reverse salt flux of 1.5 g.m-2·h-1。
Sodium alginate was used as a simulated organic contaminant to examine the flux change and membrane fouling behavior of conventional and conductive FO membranes, respectively, in the absence and application of an electric field. With extended operating time (10h), the conventional FO membrane (comparative example 1) and the conductive FO membrane had similar flux decay rates (38% and 40%) under no applied field conditions. The conductive FO membrane has the lowest flux decay rate (less than 30%) when an electric field is applied. This demonstrates that the anti-fouling performance of the conductive FO membrane is greatly enhanced in the presence of an electric field.
In addition, the rejection performance of the FO membrane for organics was determined by a total organic carbon analyzer. The conductive FO membrane has a greater rejection rate (greater than 94%) for sodium alginate than the conventional FO membrane (90%) regardless of the applied electric field. After an electric field is applied, the retention rate of the conductive FO membrane on sodium alginate is also slightly improved.
Example 3
A method for preparing a conductive forward osmosis membrane, which is different from example 2 in that: weighing 20mg of Ti3C2The powder was ultrasonically dispersed (300W, 0.5h) in 200mL deionized water and the undispersed Ti was removed by centrifugation (6000r, 0.2h)3C2Powder, i.e. uniform MXene (Ti) is obtained3C2) The concentration of the dispersion was 0.35 mg/mL. And then, under the pressure of 0.2MPa, taking 35mL of dispersion liquid, carrying out suction filtration on the polyether sulfone support layer, placing the membrane in a 60 ℃ oven, drying for 0.5h, taking out, and placing in deionized water for infiltration. Fixing the fully soaked membrane by using a plate frame, pouring a proper amount of 2% m-phenylenediamine solution onto the surface of the membrane for soaking for 1min, removing the m-phenylenediamine solution remained on the membrane surface by using a rubber roller after soaking, then taking a proper amount of 0.1% trimesoyl chloride solution for reacting for 2min, draining, and then placing the membrane in a hot water bath at 100 ℃ for thermal crosslinking for 5min to obtain the conductive FO membrane.
According to the test method of example 1, the conductive FO membrane was found to have a water flux of 14.1 L.m-2·h-1Reverse salt flux of 1.6 g.m-2·h-1。
Example 4
A method for preparing a conductive forward osmosis membrane, which is different from example 3 in that: 25mg of Ti were weighed3C2The powder was ultrasonically dispersed (300W, 0.5h) in 200mL deionized water and the undispersed Ti was removed by centrifugation (6000r, 0.2h)3C2Powder, i.e. uniform MXene (Ti) is obtained3C2) The concentration of the dispersion was 0.42 mg/mL. And then, under the pressure of 0.2MPa, taking 35mL of dispersion liquid, carrying out suction filtration on the polyether sulfone support layer, placing the membrane in a 60 ℃ oven, drying for 0.5h, taking out, and placing in deionized water for infiltration. Fixing the fully soaked membrane by using a plate frame, pouring a proper amount of 2% m-phenylenediamine solution onto the surface of the membrane for soaking for 1min, removing the m-phenylenediamine solution remained on the membrane surface by using a rubber roller after soaking, then taking a proper amount of 0.1% trimesoyl chloride solution for reacting for 2min, draining, and then placing the membrane in a hot water bath at 100 ℃ for thermal crosslinking for 5min to obtain the conductive FO membrane.
The conductive FO membrane was tested for a water flux of 13 following the test method of example 1.9L·m-2·h-1Reverse salt flux of 1.5 g.m-2·h-1。
Example 5
Preparation of MXene (Ti)3C2) Dispersion liquid: 10mg of Ti were weighed3C2The powder was dispersed ultrasonically (200W, 1h) in 200mL of deionized water and the undispersed Ti was removed by centrifugation (4000r, 0.4h)3C2Powder, i.e. uniform MXene (Ti) is obtained3C2) The concentration of the dispersion liquid is 0.10 mg/mL; depositing 35mL of MXene dispersion liquid on a polyether sulfone support layer in a vacuum filtration mode under the pressure of 0.2MPa, drying the membrane in a 60 ℃ drying oven for 0.5h, taking out, and fully soaking in deionized water; fixing the obtained film, pouring a proper amount of m-phenylenediamine solution with the mass fraction of 2% onto the surface of the film, soaking for 1min, and removing the m-phenylenediamine solution remained on the film surface by using a rubber roller after soaking; and then pouring 0.1 mass percent of trimesoyl chloride solution onto the membrane surface for reaction for 2min, draining, and then placing the membrane in a hot water bath at 100 ℃ for thermal crosslinking for 2min to obtain the conductive FO membrane.
The conductive FO membrane was tested for a water flux of 12.9L · m according to the test method of example 1-2·h-1Reverse salt flux of 1.7 g.m-2·h-1。
Comparative example 1
A method of making a conventional FO membrane comprising the steps of:
fixing the fully soaked polyether sulfone support layer by using a plate frame, pouring a proper amount of 2% m-phenylenediamine solution onto the surface of the membrane for soaking for 1min, removing the m-phenylenediamine solution remained on the membrane surface by using a rubber roller after soaking, then taking a proper amount of 0.1% trimesoyl chloride solution for reacting for 2min, draining, and then placing the membrane in a hot water bath at 100 ℃ for thermal crosslinking for 5min to obtain the conventional FO membrane.
The water flux of the conventional FO membrane was measured to be 12.5L · m according to the test method of example 1-2·h-1Reverse salt flux of 2.0 g.m-2·h-1。
Comparative example 2
MXene material is deposited onto the active layer during FO membrane preparation, resulting in active layer breakage and leakage of salts from the draw solution into the feed solution.
Comparative example 3
When MXene is deposited on the intermediate layer during the FO membrane production process, the active layer is directly peeled off, and the FO membrane cannot be produced.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (3)

1. The preparation method of the conductive FO membrane is characterized in that a polymer membrane is used as a supporting layer, MXene is used as a conductive material, MXene dispersion liquid is deposited on the surface of the polymer supporting layer in a vacuum filtration mode, and the conductive FO membrane is prepared through interfacial polymerization;
the method comprises the following steps:
(1) preparing MXene dispersion liquid with the concentration of 0.1-0.5 mg/mL: ultrasonically dispersing a certain amount of MXene powder in water, and centrifuging to remove undispersed MXene to obtain MXene dispersion liquid; wherein the ratio of MXene powder to water in terms of mass mg and volume mL is (1-7): 40;
(2) preparing an MXene layer: depositing a certain volume of dispersion liquid obtained in the step (1) on a polyether sulfone or polysulfone supporting layer in a vacuum filtration mode under the pressure of 0.1-1 MPa, drying the membrane in an oven at the temperature of 60-100 ℃ for 0.3-0.5 h, wherein the MXene content on the membrane is 0.03-0.20 mg/cm2Drying and then soaking in water, wherein the volume ratio of the dispersion liquid to the water is (1-1.5): 7;
(3) preparation of conductive FO membranes: fixing the film obtained in the step (2), pouring a certain mass fraction of m-phenylenediamine solution onto the surface of the film, and removing the m-phenylenediamine solution remained on the surface of the film after soaking; pouring a trimesoyl chloride solution with a certain mass fraction onto a membrane surface for reaction, draining, and then placing the membrane in a hot water bath at the temperature of 80-100 ℃ for thermal crosslinking for 2-5 min to obtain the conductive FO membrane; wherein the mass fraction of the m-phenylenediamine is 2-4%, the soaking time is 1-10 min, the mass fraction of the trimesoyl chloride is 0.1-0.2%, and the reaction time is 1-10 min.
2. The conductive FO membrane produced by the method of claim 1.
3. Use of the electrically conductive FO membrane of claim 2 in water treatment.
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