CN109046042B - Composite nanofiltration membrane and preparation and application thereof - Google Patents

Composite nanofiltration membrane and preparation and application thereof Download PDF

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CN109046042B
CN109046042B CN201810940479.5A CN201810940479A CN109046042B CN 109046042 B CN109046042 B CN 109046042B CN 201810940479 A CN201810940479 A CN 201810940479A CN 109046042 B CN109046042 B CN 109046042B
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nanofiltration membrane
graphene oxide
composite nanofiltration
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CN109046042A (en
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聂华丽
杨慧琴
王家齐
宋禹昊
陈德强
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Donghua University
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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
    • 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
    • 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
    • B01D67/0081—After-treatment of organic or inorganic membranes
    • B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
    • 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
    • B01D71/40—Polymers of unsaturated acids or derivatives thereof, e.g. salts, amides, imides, nitriles, anhydrides, esters
    • B01D71/42—Polymers of nitriles, e.g. polyacrylonitrile
    • 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
    • C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
    • 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

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  • Engineering & Computer Science (AREA)
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  • Nanotechnology (AREA)
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Abstract

The invention relates to a composite nanofiltration membrane, and preparation and application thereof, wherein the composite nanofiltration membrane is a graphene oxide modified composite nanofiltration membrane, and the number of layers modified by graphene oxide is 0-10. The composite nanofiltration membrane is used for desalination treatment. The method disclosed by the invention is simple to operate, mild in reaction conditions, non-toxic and pollution-free, and the prepared composite nanofiltration membrane has certain nanofiltration performance on four salts, can be widely applied to the fields of biomedicine, environmental protection, water treatment and the like, and has good practical value and potential value.

Description

Composite nanofiltration membrane and preparation and application thereof
Technical Field
The invention belongs to the field of nanofiltration membrane materials and preparation and application thereof, and particularly relates to a composite nanofiltration membrane and preparation and application thereof.
Background
With the ever-increasing number of economy and population in China and the development requirement of industry, the problem of water resource is continuously concerned by people, so that the research on the nanofiltration membrane technology is greatly promoted by ensuring the safe water use of people and meeting the industrial water use requirement. The application of the nanofiltration membrane mainly relates to the aspects of sewage treatment, food processing, hard water softening and the like, and the performance of the nanofiltration membrane is between an ultrafiltration membrane and a reverse osmosis membrane. Compared with the traditional nanofiltration membrane, the membrane has the defects of low strength, easy peeling and the like due to the limitation of the preparation method, and the structure and performance stability of the membrane are poor. However, Polyacrylonitrile (PAN) is commonly used for preparing separation membranes due to its own good thermal and chemical properties, but its mechanical properties and toughness are insufficient, thereby limiting its application in many fields. Nowadays, the compounding and modification of polymers become a trend for researching nanofiltration membranes, and Graphene Oxide (GO) has good hydrophilicity, higher specific surface area and mechanical properties, and is commonly used for researching nanofiltration membranes in recent years, wherein the research generally comprises a blending method, a spin coating method and the like. In contrast, the LB self-assembled membrane can control the membrane structure and thickness on a molecular scale, and constantly improve the chemical stability and separation characteristics of the composite membrane. In some studies by current scientists, the direction of enhancing the selective permeability, permeability and the like of composite nanofiltration membranes by introducing new nano materials or inorganic molecules has been continuously developed and utilized by researchers.
Disclosure of Invention
The invention aims to solve the technical problem of providing a composite nanofiltration membrane and preparation and application thereof, and overcomes the defect that the structure and thickness of the membrane can not be adjusted on a molecular scale in the prior art, the composite nanofiltration membrane adopts a Langmuir-Blodgett self-assembly technology to self-assemble GO on a PAN nanofiltration membrane layer by layer, the number of layers and the thickness of GO/PAN nanofiltration membranes with high flux can be controllably prepared, meanwhile, the nanofiltration performance of the nanofiltration membrane on four salts is found, the preparation process is non-toxic and pollution-free, and the composite nanofiltration membrane has good nanofiltration performance, is a brand new composite nanofiltration membrane, and has wide application prospects in the fields of water treatment, medical treatment, environmental protection, cosmetics and the like.
The composite nanofiltration membrane modified by graphene oxide comprises graphene oxide and a substrate, wherein the graphene oxide is loaded on the substrate.
The number of layers modified by the graphene oxide is 0-10, and the thickness is 0-15 nm.
The thickness of the composite nanofiltration membrane is 20-80um, the thickness of the substrate nanofiber membrane is 10-70 um, and the porosity is 10% -40%.
The composite nanofiltration membrane is a graphene oxide/polyacrylonitrile nanofiltration membrane.
The preparation method of the composite nanofiltration membrane comprises the following steps:
(1) preparing a graphene oxide film by utilizing a Langmuir-Blodgett LB technology and transferring the graphene oxide film to a substrate;
(2) and dipping and pulling, and repeating the steps to obtain the composite nanofiltration membrane.
The preferred mode of the above preparation method is as follows:
the substrate in the step (1) is a polyacrylonitrile nanofiber membrane, the thickness is 10-70 um, and the porosity is 10% -40%.
The LB technology in the step (1) is specifically as follows: and (3) spreading the graphene oxide spreading solution on the water surface, standing, compressing the sliding barrier, standing for self-assembly to form a graphene oxide film, and then transferring the graphene oxide film to the substrate through a film drawing machine.
In the graphene oxide spreading solution, the concentration of the graphene oxide spreading solution is 0.05-1.0 mg/mL; the spreading solvent is a mixed solvent of methanol and deionized water, and the volume ratio of the methanol to the deionized water is 1: 3-1: 8.
the dipping speed in the step (2) is 8-15 mm/min; the pulling speed is 0.3-0.8 mm/min.
The preparation method of the graphene oxide modified polyacrylonitrile nanofiltration membrane by utilizing the Langmuir-Blodgett (LB) technology comprises the following steps:
(a) preparing a graphene oxide spreading solution and spreading a monolayer on a water surface: carefully spreading the graphene oxide spreading solution on the water surface through an injector to obtain sparse monomolecular layer graphene oxide floating on the water surface, reducing the area of the water surface through compressing a sliding barrier, and compressing the graphene oxide on the water surface to form a compact film to obtain a graphene oxide film arranged on the monomolecular layer floating on the water surface; (b) transferring the compact graphene oxide film floating on the water surface to a substrate of an electrostatic spinning polyacrylonitrile nanofiber film by using an LB (Langmuir-Blodgett) technology through a film drawing machine to obtain the single-layer graphene oxide coated polyacrylonitrile nanofiltration membrane; (c) and repeating the steps to obtain the composite polyacrylonitrile nanofiltration membrane sample containing 2, 3 and 4 layers of graphene oxide.
The invention relates to application of a composite nanofiltration membrane.
The composite nanofiltration membrane is used for desalination treatment.
The salt is Na2SO4、MgSO4、NaCl、MgCl2。
The concentration of the salt solution is as follows: 0.5 mg/mL-2.0 mg/mL.
And (3) testing the salt nanofiltration performance of the composite nanofiltration membrane:
preparing a salt solution with a certain concentration: accurately measuring four kinds of Na respectively2SO4、MgSO4、NaCl、MgCl2500mg of salt solution is continuously stirred to be completely dissolved, and the salt solution is respectively added into a volumetric flask to be constant volume and stored at room temperature for later use; the concentration of the salt solution is 0.5 mg/mL-2.0 mg/mL;
calculating the nanofiltration performance of the composite nanofiltration membrane on salt through a nanofiltration device: cpAnd CfMeasuring, namely measuring C of four salt solutions by a DDS-11C type conductivity meterp(solute concentration in permeate), Cf(solute concentration in four salts).
Advantageous effects
(1) According to the invention, the graphene oxide/polyacrylonitrile nanofiltration membrane is prepared by using an LB method, the preparation method is simple, the experimental conditions are mild, the thickness of the functional layer can be controlled to be in a nanometer level, and the thickness range value is 0-15 nm;
(2) the graphene oxide/polyacrylonitrile nanofiltration membrane functional layer prepared by the method is not easy to strip from the substrate;
(3) the graphene oxide/polyacrylonitrile nanofiltration membrane prepared by the method has a good nanofiltration effect on salt, and Na is contained when the graphene oxide reaches four layers2SO4The rejection rate reaches more than 80 percent, and the nanofiltration membrane prepared by the invention has Na-ion exchange capacity2SO4、MgSO4、NaCl、MgCl2Much higher than other related documents, see fig. 1.
Drawings
Figure 1 is a graph comparing the nanofiltration performance of salts between the present invention and prior research literature;
FIG. 2 shows the nanofiltration performance and flux of a graphene oxide/polyacrylonitrile nanofiltration membrane on NaCl;
FIG. 3 shows a graphene oxide/polyacrylonitrile nanofiltration membrane pair Na2SO4The nanofiltration performance and flux of the membrane;
FIG. 4 shows the graphene oxide/polyacrylonitrile nanofiltration membrane vs. MgCl2The nanofiltration performance and flux of the membrane;
FIG. 5 shows graphene oxide/polyacrylonitrile nanofiltration membrane vs MgSO4The nanofiltration performance and flux of the membrane;
figure 6 is a graph comparing the nanofiltration performance of a graphene oxide/polyacrylonitrile nanofiltration membrane against four salts;
FIG. 7 is a schematic view of a membrane test apparatus according to the present invention.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
Step 1: firstly, 3.0mL of Graphene Oxide (GO) aqueous solution of 1.0mg/mL is prepared, then 15.0mL of methanol is added into the solution, and stirring is carried out for 20min, so as to obtain graphene oxide spreading solution with the final concentration of 0.167 mg/mL.
Step 2: and (3) taking 10.0mL of the graphene oxide spreading solution, spreading the graphene oxide spreading solution on the water surface in an LB water tank carefully by using one drop of injection, wherein the area of the water tank is 10 x 20cm, standing for 20 minutes, moving the sliding barrier at the speed of 0.8cm/min after methanol on the water surface is completely volatilized, stopping moving when the distance from the sliding barrier to the sliding barrier is 1cm, standing, and waiting for the formation of a monolayer graphene oxide film through self-assembly.
And step 3: cutting the polyacrylonitrile nanofiltration membrane into samples with the specification of 5cm x 2.5cm, soaking polyacrylonitrile nanofibers in an LB water tank at a soaking speed of 10mm/min by controlling the parameters of a membrane drawing machine, wherein the length below the liquid level is 4.0cm, and after the liquid level is stabilized for 20 minutes, drawing the polyacrylonitrile nanofibers at a drawing speed of 0.5mm/min to transfer graphene oxide on a monolayer on the water surface to the surface of the polyacrylonitrile nanofiltration membrane.
And 4, step 4: cutting the obtained sample into 2cm x 2.5cm specifications, carrying out secondary impregnation at the impregnation speed of 10mm/min, and carrying out lifting at the same speed to obtain the two-layer graphene oxide coating polyacrylonitrile nanofiltration membrane. And (4) repeating the step (4) to obtain a sample of the three-layer and four-layer composite polyacrylonitrile nanofiltration membrane.
Example 2
Preparation of four salt solutions: the method comprises the following steps:
accurately measuring four kinds of Na respectively2SO4、MgSO4、NaCl、MgCl2And (3) continuously stirring the salt solution 500mg to completely dissolve, adding the salt solution into a 500mL volumetric flask to a constant volume, and storing at room temperature for later use.
The concentration of the four salt solutions was 1.0 mg/ml.
Example 3
The nanofiltration performance of the nanofiltration membrane on salt is tested at room temperature by adopting a self-made flux testing device (shown in figure 7), and the specific nanofiltration experimental steps are as follows:
step 1: pre-pressing: fixing the sample in the filter, keeping the speed of the peristaltic pump at 5rpm, and pressing the membrane by deionized water until the water flux reaches a stable state.
Step 2: pure water flux determination: the deionized water flux J was tested, i.e. the volume of liquid permeated was recorded and the test was terminated after stabilization.
And step 3: measurement of feed liquid interception: the test was performed again by changing to the salt solution, and both the permeated solution and the raw material solution were sampled and tested.
And 4, step 4: the rejection performance of the nanofiltration membrane is evaluated by adopting the rejection rate R, and the calculation formula is as follows:
R＝(1—Cp/Cf)
in the formula, R is the rejection rate (%) of four salts by the GO/PAN nanofiltration membrane, and C ispIs the concentration of solute in the permeate, CfIs the solute concentration in the four salts.
And 5: c of four saltspAnd CfAnd (3) determination: testing the conductivity of the solution penetrated by the four salt solutions and the conductivity of the original salt solution by a DDS-11C type conductivity meter, and calculating by a formulaTo the retention of four salts.
As can be seen from fig. 2-6, among the four salts, all of the different numbers of graphene oxide nanofiltration membranes were paired with Na2SO4The salt rejection rate of (2) is the highest, Na when the graphene oxide reaches four layers2SO4The retention rate reaches more than 80 percent. Meanwhile, the nanofiltration performance of the nanofiltration membrane on salt is contrastively analyzed with that of the prior literature, and as can be seen from figure 1, the 4-layer nanofiltration membrane prepared by the invention can be used for four kinds of salt Na2SO4、MgSO4、NaCl、MgCl2The flux of the method is far higher than other related documents, but the retention rate of the four salts is equivalent to that of the documents, and the method is shown in figure 1 and has important significance for the desalination treatment of industrial brine.
Example 4
Bovine Serum Albumin (BSA) aqueous solution is used as a simulated dye system, so that a series of anti-pollution performance indexes of the nanofiltration membrane are evaluated.
The preparation method of the BSA solution comprises the following steps: 1000mg of BSA is accurately weighed, then deionized water is added, stirring is continuously carried out until the BSA is dissolved, the obtained solution is placed in a 1000mL volumetric flask, the volume is constant, a BSA aqueous solution with the concentration of 1000mg/L is prepared, and the BSA aqueous solution is stored at room temperature for standby application.
The main steps for evaluating the anti-pollution performance of the composite nanofiltration membrane are as follows:
(1) pre-pressing: fixing the sample in a filtering device, keeping the rotating speed of a peristaltic pump at 5r/min, and pressing the membrane for 20min by using deionized water until the water flux reaches a stable state.
(2) Pure water flux determination: measuring the flux J of deionized water, i.e. recording the volume of liquid permeated, measuring the flux Jw1And terminating the test until stable.
(3) BSA aqueous solution assay: the BSA aqueous solution was tested in place of the original deionized water and the flux of the solution was measured to be Jp。
(4) Cleaning a nanofiltration membrane sample: the BSA solution was poured out, and then deionized water was added and washed for 15 min.
(5) Second test water flux: pouring off the washed solution, adding deionized water again,testing secondary pure water flux Jw2。
Four parameters for evaluating the anti-pollution index of the GO/PAN nanofiber membrane, namely Flux Recovery Rate (FRR) and flux attenuation rate (R) after water cleaning are introducedt) Reversible flux decay Rate (R)r) Irreversible flux attenuation Rate (R)ir) And the formula is calculated as follows:
FRR(％)＝Jw2/Jw1×100％
Rt(％)＝(1—Jp/Jw1)×100％
Rr(％)＝(Jw2—Jp)/Jw1×100％
Rir(％)＝(1—Jw2/Jw1)×100％
TABLE 1 anti-pollution index of BSA solution filtered by graphene oxide coating films with different layers
Figure BDA0001768925220000051
As can be seen from the table above, the nanofiltration membrane of the invention has excellent anti-pollution performance and can be practically applied to desalination treatment of wastewater.

Claims (9)

1. The composite nanofiltration membrane is characterized in that the composite nanofiltration membrane is a graphene oxide modified composite nanofiltration membrane, wherein the components comprise graphene oxide and a substrate, and the graphene oxide is loaded on the substrate; the composite nanofiltration membrane is prepared by the following steps:
(1) preparing a graphene oxide film by utilizing a Langmuir-Blodgett LB technology and transferring the graphene oxide film to a substrate;
(2) dipping and pulling, and repeating the steps to obtain the composite nanofiltration membrane; the number of layers modified by graphene oxide in the composite nanofiltration membrane is 2 or 4.
2. The composite nanofiltration membrane of claim 1, wherein the modification layer has a thickness of 0 to 15 nm.
3. The composite nanofiltration membrane according to claim 1, wherein the composite nanofiltration membrane has a thickness of 20-80 um.
4. A method for preparing a composite nanofiltration membrane as claimed in any one of claims 1 to 3, comprising the following steps:
(1) preparing a graphene oxide film by utilizing a Langmuir-Blodgett LB technology and transferring the graphene oxide film to a substrate;
(2) and dipping and pulling, and repeating the steps to obtain the composite nanofiltration membrane.
5. The preparation method according to claim 4, wherein the substrate in the step (1) is a polyacrylonitrile nanofiber membrane, the thickness is 10-70 um, and the porosity is 10% -40%.
6. The preparation method according to claim 4, wherein the LB technology in the step (1) is specifically: and (3) spreading the graphene oxide spreading solution on the water surface, standing, compressing the sliding barrier, standing for self-assembly to form a graphene oxide film, and then transferring the graphene oxide film to the substrate through a film drawing machine.
7. The preparation method according to claim 6, wherein in the graphene oxide spreading solution, the concentration of the graphene oxide spreading solution is 0.05-1.0 mg/mL; the spreading solvent is a mixed solvent of methanol and deionized water, and the volume ratio of the methanol to the deionized water is 1: 3-1: 8.
8. the production method according to claim 6, wherein the dipping speed in the step (2) is 8 to 15 mm/min; the pulling speed is 0.3-0.8 mm/min.
9. Use of a composite nanofiltration membrane according to claim 1.
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Citations (1)

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CN107059248A (en) * 2017-03-29 2017-08-18 东华大学 A kind of graphene oxide monolayer modifies the preparation method of polyacrylonitrile nanofiber film

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CN107059248A (en) * 2017-03-29 2017-08-18 东华大学 A kind of graphene oxide monolayer modifies the preparation method of polyacrylonitrile nanofiber film

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Title
A large-area free-standing graphene oxide multilayer membrane with high stability for nanofiltration applications;Long Chen et al.;《Chemical Engineering Journal》;20180326;第345卷;第536-544页 *
Membranes prepared from graphene-based nanomaterials for sustainable applications: a review;Xiaoying Zhu et al.;《Environ. Sci. Nano》;20171005(第4期);第2267-2285页 *

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