CN114259891B - Graphene oxide nanofiltration membrane as well as preparation method and application thereof - Google Patents
Graphene oxide nanofiltration membrane as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a graphene oxide nanofiltration membrane as well as a preparation method and application thereof, wherein the preparation method comprises the following steps: and coating the dispersion liquid containing the graphene oxide on a base membrane, crosslinking polyamine, and performing post-treatment by using sodium hypochlorite to obtain the graphene oxide nanofiltration membrane. According to the invention, polyamine is adopted to crosslink graphene oxide, so that the structural stability and performance stability of the graphene oxide membrane are improved, and sodium hypochlorite is further adopted for post-treatment, so that the flux of the nanofiltration membrane is greatly improved, and the retention rate of the dye is kept, so that the nanofiltration membrane can be successfully applied to the decolorization treatment of wastewater.
Description
Technical Field
The invention relates to the technical field of nanofiltration membranes, and particularly relates to a graphene oxide nanofiltration membrane as well as a preparation method and application thereof.
Background
The procedures of the processing, weaving and printing and dyeing processes of cotton spinning products are very complicated, each process can generate different pollutant components, especially, the waste water discharged in the printing and dyeing process contains a large amount of undyed dyes and hydrolysates thereof, and the undyed dyes discharged in the dyeing process cause the waste water to have high chroma and are difficult to biochemically treat. The reuse of the printing and dyeing wastewater can not reach the reuse standard until the color of the wastewater finally discharged by a sewage plant is completely removed by carrying out advanced treatment on the color of the wastewater. The traditional treatment method is that dyeing wastewater is mixed with wastewater produced in other production links, the salt content and the chromaticity are diluted, and then the wastewater is treated by physical and chemical treatment, biochemical treatment or physical and chemical combination, and the like, and then the wastewater reaches the standard and is discharged; the discharged wastewater reaching the standard can make the color of the final effluent meet the requirement of recycling only by advanced oxidation or activated carbon adsorption. However, these steps inevitably bring about secondary pollution to the environment.
The aperture of the nanofiltration membrane is between that of the ultrafiltration membrane and that of the reverse osmosis membrane, the separation precision is 1-10nm, molecules and multivalent ions with the molecular mass of 150-2000Da can be effectively removed, the molecular weight of the active dye is generally 800-2000Da, the interception of the dye can be achieved by applying certain pressure to the water inlet end, and effluent with extremely low chroma can be obtained. Therefore, the dye-containing wastewater is decolorized by the nanofiltration membrane, and the method has high economic value and social benefit. The preparation of the traditional nanofiltration membrane mainly continues the conventional interfacial polymerization process, and the flux of the traditional nanofiltration membrane is small and the pollution resistance is poor. Therefore, the development of a membrane material which has simple preparation process and excellent separation performance when treating dye-containing wastewater is very important for improving the application of the nanofiltration membrane technology in the field of wastewater decolorization, and has very important economic value and social value.
Graphene oxide is a derivative of graphene, and is also a single-layer two-dimensional sheet-like carbon material. Recent research shows that water molecules can rapidly flow on the surface of graphene oxide, and the graphene oxide has excellent separation performance. The graphene oxide film is rich in oxygen-containing functional groups such as hydroxyl, carboxyl, epoxy, carbonyl and the like on the surface, has good hydrophilicity, is easy to disperse in water to form uniform dispersion liquid, and is easy to prepare into a graphene oxide film. At present, graphene oxide membranes can be prepared by methods such as vacuum filtration, dip coating, spray coating, layer-by-layer self-assembly, coating and the like, and show excellent salt/dye separation performance. For example, chinese patent application No. 201910847802.9 discloses a graphene oxide nanofiltration membrane and a preparation method thereof, wherein the preparation method comprises the steps of uniformly coating a coating rod with a graphene oxide dispersion liquid, drying, and partially reducing by ultraviolet irradiation. For example, chinese patent application No. 202010662479.0 discloses a self-supporting reduced graphene oxide nanofiltration membrane, and a preparation method and application thereof, wherein the preparation method comprises uniformly coating graphene oxide slurry on the polymer substrate, and then reducing by ultraviolet lamp irradiation. Although the technical scheme of the patent application provides an attempt scheme for the batch production of the graphene oxide film, the graphene oxide film is very easy to expand after the prepared graphene oxide film is contacted with water due to the strong hydrophilicity of the graphene oxide, so that the graphene oxide film is damaged, decomposed or falls off from a base film, the film separation performance is unstable, the performance of different solutions can be greatly changed during testing, and the application value of the graphene oxide film is greatly reduced. Therefore, the development of the graphene oxide nanofiltration membrane which is simple to prepare, easy to produce in batches, stable in structure and performance and has excellent salt/dye separation performance is very important.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a graphene oxide nanofiltration membrane, and a preparation method and application thereof.
In order to achieve the purpose, the invention provides a preparation method of a graphene oxide nanofiltration membrane, which comprises the following steps: coating a dispersion liquid containing graphene oxide on a base membrane, crosslinking the graphene oxide by using polyamine, and performing post-treatment on the crosslinked graphene oxide membrane by using sodium hypochlorite to obtain a graphene oxide nanofiltration membrane; wherein the polyamine is selected from organic substances containing at least two amino and/or imino groups.
In the research of the invention, the inventor creatively discovers that: the graphene oxide nanofiltration membrane after polyamine crosslinking has unique advantages in the separation of salt and dye in a high-salt environment, and specifically shows that the nanofiltration membrane has excellent retention performance on the dye in the high-salt environment and keeps a very low desalination rate. The traditional conventional nanofiltration membrane has high desalination rate and high osmotic pressure in a high-salt environment, almost has no flux, greatly reduces the retention rate of dye due to charged shielding, and cannot realize effective separation of salt and dye. The interlayer spacing of the polyamine crosslinked graphene oxide membrane prepared by the invention is fixed, and the ultralow interception of the membrane to salt can be realized by adjusting the interlayer spacing, so that the problems of high osmotic pressure and no flux can not occur during wastewater filtration; meanwhile, due to the fact that the distance between graphene oxide layers is fixed, charged shielding in a high-salt environment hardly influences the trapping of dyes, and therefore ultrahigh trapping of the dyes can be achieved in the high-salt environment, and separation of the salts and the dyes is achieved.
According to the graphene oxide nanofiltration membrane, dyes in wastewater are filtered by utilizing the distance between graphene oxide layers and charged oxygen-containing groups on the graphene oxide, and sodium hypochlorite is used as a strong oxidant to further improve the oxidation degree of the groups on the surface of the graphene oxide and increase the retention performance of the graphene oxide nanofiltration membrane on the dyes. The polyamine crosslinking can crosslink the graphene oxide lamella of two adjacent layers together to play a stabilizing role, so that the graphene oxide nanofiltration membrane can stably run in the wastewater decolorization. However, in the crosslinking process, part of polyamine is only combined with a single-layer graphene oxide sheet layer, and the part of polyamine cannot achieve the effect of stabilizing the graphene oxide nanofiltration membrane, but blocks the interlayer spacing of the graphene oxide, so that the flux of the nanofiltration membrane is greatly reduced. In addition, the graphene oxide nanofiltration membrane mainly utilizes the interlayer spacing between graphene to filter the dye, the proper sodium hypochlorite post-treatment can not damage the structure of the graphene and the interlayer spacing of the graphene oxide, and the selectivity of the graphene oxide nanofiltration membrane on the dye caused by the damage of the membrane structure is avoided. The purpose of the traditional organic membrane treatment by sodium hypochlorite is mainly to corrode polyamide with low crosslinking degree, the method destroys the fine polymer network structure of the original polyamide layer, so that the aperture or free volume of the separation membrane is increased, although the flux is increased, the selectivity of membrane separation is reduced, the desalination rate is reduced, and the service life is reduced; sodium chlorate treatment of traditional organic membranes is a compromise by destroying the bulk structure of the membrane, relying on sacrificing salt rejection and service life to increase flux.
According to a specific embodiment of the present invention, in the above production method, preferably, the polyamine is selected from one or a combination of two or more of ethylenediamine, propylenediamine, butylenediamine, pentylenediamine, hexylenediamine, octylenediamine, m-phenylenediamine, p-phenylenediamine, polyethyleneimine, diethylenetriamine, N-aminoethylpiperazine, 1, 2-bis (2-aminoethoxy) ethane, 1, 4-bis (3-aminopropyl) piperazine, and more preferably octylenediamine or 1, 4-bis (3-aminopropyl) piperazine.
According to a specific embodiment of the present invention, in the above preparation method, preferably, the crosslinking manner is selected from pre-crosslinking in which polyamine is mixed with the dispersion liquid and then coated on the base film, or post-crosslinking in which the dispersion liquid is coated on the base film and then the base film is soaked in the polyamine aqueous solution.
According to an embodiment of the present invention, in the above production method, the concentration of the polyamine in the mixed solution after mixing in the pre-crosslinking is preferably 0.005 to 0.5g/ml, more preferably 0.01 to 1g/ml.
According to a specific embodiment of the present invention, in the above production method, preferably, in the post-crosslinking, the concentration of the polyamine in the polyamine aqueous solution is 0.005 to 0.5g/ml, more preferably 0.01 to 0.2g/ml.
According to a specific embodiment of the present invention, in the above preparation method, preferably, the post-treatment manner is selected from soaking the crosslinked graphene oxide membrane in a sodium hypochlorite solution, or filtering the sodium hypochlorite solution with the crosslinked graphene oxide membrane.
According to a specific embodiment of the present invention, in the above preparation method, preferably, the sodium hypochlorite solution has an effective chlorine concentration of 0.002 to 0.5%, more preferably 0.005 to 0.05%.
According to a specific embodiment of the present invention, in the above preparation method, the post-treatment time is preferably 5min to 24 hours, more preferably 0.5 to 10 hours.
According to a specific embodiment of the present invention, in the above preparation method, preferably, the graphene oxide has a sheet diameter of 0.5 to 500 μm, and more preferably 2 to 50 μm.
According to a specific embodiment of the present invention, in the above preparation method, preferably, the concentration of the graphene oxide in the dispersion liquid is 0.5 to 10g/L, and more preferably 2 to 5g/L.
According to a specific embodiment of the present invention, in the above preparation method, preferably, the base film is made of a material selected from nylon (PA), polyvinylidene fluoride (PVDF), polysulfone (PSF), polyethersulfone (PES), polyacrylonitrile (PAN), or Cellulose Acetate (CA).
According to a specific embodiment of the present invention, in the above production method, preferably, the base film has an average pore diameter of 0.05 to 10 μm, more preferably 0.25 to 0.5 μm.
According to a specific embodiment of the present invention, in the above production method, preferably, the coating process is selected from wire bar coating or slit coating.
According to a specific embodiment of the present invention, in the above production method, preferably, the coating wet film thickness is 5 to 500. Mu.m, more preferably 50 to 100. Mu.m.
According to a specific embodiment of the present invention, in the above production method, preferably, the coating speed is 1 to 500mm/s, more preferably 20 to 100mm/s.
The invention also provides the graphene oxide nanofiltration membrane prepared by the preparation method.
Tests prove that the water flux of 2000PPM sodium sulfate solution adopting the graphene oxide nanofiltration membrane is 1-50L/(m) 2 H. Bar), the salt rejection is 20-95%.
The invention also provides an application of the graphene oxide nanofiltration membrane in wastewater decolorization.
According to a particular embodiment of the invention, in the above applications, the water flux is preferably between 1 and 50L/(m) 2 H. Bar), dyeingThe retention rate of the material is 85-99.5%. The graphene oxide nanofiltration membrane can be used for filtering dye-containing wastewater and efficiently removing dyes.
The technical scheme provided by the invention has the following beneficial effects:
according to the invention, the graphene oxide is crosslinked through the polyamine, and adjacent graphene oxide sheets are crosslinked together, so that the structural stability and the performance stability of the graphene oxide membrane are improved, the graphene oxide membrane is not easy to damage, fall off and disintegrate, and the performances are not obviously different when different solutions are tested; in addition, the invention further carries out post-treatment by sodium hypochlorite, greatly improves the flux of the graphene oxide nanofiltration membrane, and keeps higher dye retention rate, so that the graphene oxide nanofiltration membrane is successfully applied to the decolorization treatment of actual wastewater.
Drawings
Fig. 1 is a scanning electron microscope image of a graphene oxide nanofiltration membrane prepared in example 1 of the present invention;
fig. 2 is a scanning electron microscope image of the graphene oxide nanofiltration membrane prepared in example 1 of the present invention.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention should not be construed as limiting the implementable scope of the present invention.
Example 1
The embodiment provides a graphene oxide nanofiltration membrane, and a preparation method of the graphene oxide nanofiltration membrane comprises the following steps:
(1) Dropwise adding 3g of octanediamine into 89ml of deionized water to prepare an octanediamine aqueous solution, then taking 10ml of 10mg/ml graphene oxide dispersion liquid with the average lamella diameter of 5 mu m, dispersing the graphene oxide dispersion liquid into 90ml of the octanediamine aqueous solution, and repeatedly shaking to uniformly mix the graphene oxide dispersion liquid and the octanediamine aqueous solution to prepare a mixed solution containing 3g/L graphene oxide and 0.01g/ml octanediamine;
(2) Spreading a polyvinylidene fluoride micro-filtration membrane with the average pore diameter of 0.25 mu m on an automatic coating machine, uniformly coating the mixed solution prepared in the step (1) on the micro-filtration membrane by using a wire rod coating method to obtain a graphene oxide membrane, wherein the thickness of a coating wet membrane is 40 mu m, and the coating speed is 100mm/s;
(3) Placing the graphene oxide film obtained in the step (2) in a drying oven to be dried for 2h at the temperature of 80 ℃, and further improving the crosslinking degree of octanediamine and graphene oxide;
(4) And (3) soaking the graphene oxide membrane dried in the step (3) in a sodium hypochlorite solution with the effective chlorine concentration of 0.05% for post-treatment for 2h, then taking out, washing with clear water, and naturally airing to obtain the graphene oxide nanofiltration membrane, wherein the scanning electron microscope images of the graphene oxide nanofiltration membrane are shown in fig. 1 and fig. 2.
The graphene oxide nanofiltration membrane is tested for salt and dye interception performance, and when the graphene oxide nanofiltration membrane filters 2000PPM sodium sulfate solution, the water flux is 10L/(m) 2 H. Bar), the rejection rate is 85%; when 1g/L of BlueR dye solution is filtered, the water flux is 2L/(m) 2 H.bar), dye retention 99.5%.
Example 2
The embodiment provides a graphene oxide nanofiltration membrane, and a preparation method of the graphene oxide nanofiltration membrane comprises the following steps:
(1) Taking 0.2g of graphene oxide powder with the average lamella diameter of 50 mu m, adding the graphene oxide powder into 90ml of deionized water, and carrying out ultrasonic treatment for 2 hours to prepare a uniform graphene oxide dispersion liquid with the concentration of 2 mg/ml;
(2) Flatly paving a cellulose acetate microfiltration membrane with the average pore diameter of 0.3 mu m on an automatic coating machine, uniformly coating the graphene oxide dispersion liquid prepared in the step (1) on the microfiltration membrane by using a slit coating method to obtain a graphene oxide membrane, wherein the thickness of a coating wet membrane is 25 mu m, and the coating speed is 80mm/s;
(3) And (3) naturally airing the graphene oxide film obtained in the step (2), then soaking the naturally aired graphene oxide film in a 10% hexamethylene diamine water solution for 8h, taking out, and then placing in an oven to dry for 15min at 80 ℃.
(4) And (4) soaking the dried graphene oxide membrane obtained in the step (3) in a sodium hypochlorite solution with the effective chlorine concentration of 0.04%, performing aftertreatment for 2h, taking out, washing with clear water, and naturally drying to obtain the graphene oxide nanofiltration membrane.
The graphene oxide nanofiltration membrane is subjected to salt and dye rejectionTest shows that when the graphene oxide nanofiltration membrane filters 2000PPM sodium sulfate solution, the water flux is 4L/(m) 2 H · Bar), retention rate 80%; when 1g/L of BlueR dye solution is filtered, the water flux is 5L/(m) 2 H. Bar), dye retention 95%.
Example 3
The embodiment provides a graphene oxide nanofiltration membrane, and a preparation method of the graphene oxide nanofiltration membrane comprises the following steps:
(1) Taking 0.4g of graphene oxide powder with the average lamella diameter of 50 microns, adding the graphene oxide powder into 90ml of deionized water, and carrying out ultrasonic treatment for 2 hours to prepare a uniform graphene oxide dispersion liquid; then, 10ml of 1, 4-bis (3-aminopropyl) piperazine was added to 90ml of the graphene oxide dispersion liquid prepared above, and shaking was repeated to mix the graphene oxide dispersion liquid uniformly to prepare a mixed solution containing 4mg/ml of graphene oxide and 0.1g/ml of 1, 4-bis (3-aminopropyl) piperazine;
(2) Flatly spreading a nylon microfiltration membrane with the average pore diameter of 0.5 mu m on an automatic coating machine, uniformly coating the mixed solution prepared in the step (1) on the microfiltration membrane by using a slit coating method to obtain a graphene oxide membrane, wherein the thickness of a coating wet membrane is 5 mu m, and the coating speed is 60mm/s;
(3) Placing the graphene oxide film obtained in the step (2) in a drying oven, and drying for 30min at 60 ℃, so as to further improve the crosslinking degree of the graphene oxide;
(4) And (4) soaking the dried graphene oxide membrane obtained in the step (3) in a sodium hypochlorite solution with the effective chlorine concentration of 0.02% for post-treatment for 8h, then taking water, washing with clear water, and naturally airing to obtain the graphene oxide nanofiltration membrane.
The graphene oxide nanofiltration membrane is tested for salt and dye interception performance, and when the graphene oxide nanofiltration membrane filters 2000PPM sodium sulfate solution, the water flux is 25L/(m) 2 H · Bar), retention 50%; when 1g/L of BlueR dye solution is filtered, the water flux is 8L/(m) 2 H. Bar), dye retention 90%.
Comparative example 1
The present comparative example provides a graphene oxide film, which is prepared in the same manner as in example 1, except that step (4) is not included, that is, sodium hypochlorite post-treatment is not performed, and the specific steps are as follows:
(1) Dropwise adding 3g of octanediamine into 89ml of deionized water to prepare an octanediamine aqueous solution, then taking 10ml of 10mg/ml graphene oxide dispersion liquid with the average lamella diameter of 5 mu m, dispersing the graphene oxide dispersion liquid into 90ml of the octanediamine aqueous solution, and repeatedly shaking to uniformly mix the graphene oxide dispersion liquid and the octanediamine aqueous solution to prepare a mixed solution containing 3g/L graphene oxide and 0.01g/ml octanediamine;
(2) Spreading a polyvinylidene fluoride micro-filtration membrane with the average pore diameter of 0.25 mu m on an automatic coating machine, uniformly coating the mixed solution prepared in the step (1) on the micro-filtration membrane by using a wire rod coating method to obtain a graphene oxide membrane, wherein the thickness of a coating wet membrane is 40 mu m, and the coating speed is 100mm/s;
(3) And (3) drying the graphene oxide film obtained in the step (2) in an oven at the temperature of 80 ℃ for 2h, and further improving the crosslinking degree of the octanediamine and the graphene oxide to obtain the graphene oxide film.
The graphene oxide membrane of the comparative example was tested for salt and dye retention performance, and when the graphene oxide membrane filtered 2000PPM sodium sulfate solution, the water flux was 10L/(m) 2 H. Bar), the rejection rate is 85.4%; when 1g/L of BlueR dye solution is filtered, the water flux is 0.7L/(m) 2 H.bar), dye retention 99.5%. Compared with example 1, the graphene oxide of the comparative example has greatly reduced water flux when filtering the dye solution.
Claims (18)
1. A preparation method of a graphene oxide nanofiltration membrane for high-salinity wastewater decolorization comprises the following steps: coating a dispersion liquid containing graphene oxide on a base membrane, crosslinking the graphene oxide by using polyamine, and performing post-treatment on the crosslinked graphene oxide membrane by using sodium hypochlorite to obtain a graphene oxide nanofiltration membrane; wherein the polyamine is selected from organic substances containing at least two amino and/or imino groups;
the base film is made of nylon, polyvinylidene fluoride, polysulfone, polyether sulfone, polyacrylonitrile or cellulose acetate;
the post-treatment mode is selected from the step of soaking the crosslinked graphene oxide membrane in a sodium hypochlorite solution, or filtering the sodium hypochlorite solution by using the crosslinked graphene oxide membrane; the effective chlorine concentration of the sodium hypochlorite solution is 0.005-0.05%, and the post-treatment time is 0.5-10h.
2. The production method according to claim 1, wherein the polyamine is one or a combination of two or more selected from ethylenediamine, propylenediamine, butylenediamine, pentylenediamine, hexylenediamine, octylenediamine, m-phenylenediamine, p-phenylenediamine, polyethyleneimine, diethylenetriamine, N-aminoethylpiperazine, 1, 2-bis (2-aminoethoxy) ethane, and 1, 4-bis (3-aminopropyl) piperazine.
3. The production method according to claim 2, wherein the polyamine is octanediamine or 1, 4-bis (3-aminopropyl) piperazine.
4. The method according to claim 1, wherein the crosslinking is selected from the group consisting of pre-crosslinking in which the polyamine is mixed with the dispersion and then applied to the base film and post-crosslinking in which the base film is soaked in an aqueous polyamine solution after the dispersion is applied to the base film.
5. The process according to claim 4, wherein the polyamine concentration in the mixed solution after mixing in the pre-crosslinking is 0.005 to 0.5g/ml.
6. The method according to claim 5, wherein the polyamine concentration in the mixed solution after mixing in the pre-crosslinking is 0.01 to 1g/ml.
7. The process according to claim 4, wherein the polyamine concentration in the polyamine aqueous solution in the post-crosslinking is from 0.005 to 0.5g/ml.
8. The production process according to claim 7, wherein in the post-crosslinking, the concentration of the polyamine in the polyamine aqueous solution is 0.01 to 0.2g/ml.
9. The production method according to claim 1, wherein the graphene oxide has a sheet diameter of 0.5 to 500 μm.
10. The production method according to claim 9, wherein the graphene oxide has a sheet diameter of 2 to 50 μm.
11. The production method according to claim 1, wherein the concentration of the graphene oxide in the dispersion liquid is 0.5 to 10 g/L.
12. The production method according to claim 11, wherein the concentration of the graphene oxide in the dispersion liquid is 2 to 5g/L.
13. The production method according to claim 4, wherein the average pore diameter of the base film is 0.25 to 0.5 μm.
14. The method of claim 4, wherein the coating process is selected from wire bar coating or slot coating.
15. The production method according to claim 4, wherein the coating wet film thickness is 50 to 100 μm; the coating speed is 20-100mm/s.
16. A graphene oxide nanofiltration membrane obtained by the preparation method of any one of claims 1 to 15.
17. Use of a graphene oxide nanofiltration membrane according to claim 16 for wastewater decolorization.
18. Use according to claim 17, wherein the water flux is 1-50L/(m) 2 h.Bar) the retention of the dye is 85-99.5%.
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