CN114130201A - Titanium dioxide graphene oxide modified organic ultrafiltration membrane and preparation method thereof - Google Patents
Titanium dioxide graphene oxide modified organic ultrafiltration membrane and preparation method thereof Download PDFInfo
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- CN114130201A CN114130201A CN202010925597.6A CN202010925597A CN114130201A CN 114130201 A CN114130201 A CN 114130201A CN 202010925597 A CN202010925597 A CN 202010925597A CN 114130201 A CN114130201 A CN 114130201A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0048—Inorganic membrane manufacture by sol-gel transition
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
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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
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0095—Drying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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- 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
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Abstract
The invention discloses a titanium dioxide and graphene oxide modified organic ultrafiltration membrane and a preparation method thereof, and the titanium dioxide and graphene oxide modified organic ultrafiltration membrane comprises an organic ultrafiltration membrane support body and a functional layer, wherein the functional layer is formed on the surface of the organic ultrafiltration membrane support body by carrying out suction filtration and drying on a titanium dioxide and graphene oxide aqueous solution with the pH value of 3-5, the titanium dioxide and graphene oxide aqueous solution is prepared by taking a graphene oxide aqueous solution and an alcoholic solution of titanium organic salt as raw materials through a sol-gel method, the concentration of the graphene oxide aqueous solution is 2-5mg/L, and nano titanium dioxide is uniformly loaded on a graphene oxide sheet layer. According to the invention, the hydrophilic performance of the film layer can be increased and the photocatalytic effect can be improved by loading titanium dioxide on the graphene oxide.
Description
Technical Field
The invention belongs to the technical field of membrane material preparation, and particularly relates to a titanium dioxide graphene oxide modified organic ultrafiltration membrane and a preparation method thereof.
Background
In recent years, with the development of the membrane industry, the membrane technology becomes an effective means for water pollution control. In water pollution treatment, the membrane treatment sewage mainly depends on the membrane aperture to separate pollutants, so as to achieve stable and higher interception efficiency, but also consumes huge energy. Therefore, researchers are gradually focusing on the contaminant removal mechanism in membrane treatment, how to trap contaminants in water while maintaining a certain pore size. The photocatalysis technology is a novel green and environment-friendly technology with resource saving, environmental protection and great application prospect in the field of treating organic pollutants. Under the irradiation of ultraviolet light, the photocatalyst can decompose organic pollutants in water without secondary pollution. Photocatalysis has become an effective means for removing various environmental pollutants. Thus, the organic combination of photocatalytic and membrane treatment technologies can improve membrane separation performance.
Titanium dioxide is a typical semiconductor photocatalyst, and is very popular among people due to the characteristics of good photoactivity, good stability, no harm to human bodies, low cost, mild reaction conditions, no secondary pollution and the like. However, titanium dioxide has a wide band gap and a photogenerated electron-hole pair recombination rate, which limits its large-scale application.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a titanium dioxide graphene oxide modified organic ultrafiltration membrane.
The invention also aims to provide a preparation method of the titanium dioxide graphene oxide modified organic ultrafiltration membrane.
The technical scheme of the invention is as follows:
the titanium dioxide graphene oxide modified organic ultrafiltration membrane comprises an organic ultrafiltration membrane support body and a functional layer, wherein the functional layer is formed on the surface of the organic ultrafiltration membrane support body by carrying out suction filtration and drying on a titanium dioxide graphene oxide aqueous solution with the pH value of 3-5, the titanium dioxide graphene oxide aqueous solution is prepared by taking a graphene oxide aqueous solution and an alcoholic solution of titanium organic salt as raw materials through a sol-gel method, the concentration of the graphene oxide aqueous solution is 2-5mg/L, and nano titanium dioxide is uniformly loaded on a graphene oxide sheet layer.
In a preferred embodiment of the present invention, the material of the organic ultrafiltration membrane support is polyethersulfone or polycarbonate.
Further preferably, the molecular weight of the polyether sulfone or polycarbonate is 50-100 KD.
The preparation method of the titanium dioxide graphene oxide modified organic ultrafiltration membrane comprises the following steps:
(1) preparing a graphene oxide aqueous solution by using a modified Hummers method;
(2) dropwise adding the graphene oxide aqueous solution into an alcoholic solution of titanium organic salt, and then adding nitric acid or hydrochloric acid to perform dispergation to obtain the titanium dioxide graphene oxide aqueous solution;
(3) and (3) carrying out suction filtration on the titanium dioxide graphene oxide aqueous solution on the organic ultrafiltration membrane support body, standing, removing the titanium dioxide graphene oxide aqueous solution which is not adsorbed, washing with ethanol and deionized water, and drying to obtain the titanium dioxide graphene oxide modified organic ultrafiltration membrane.
In a preferred embodiment of the present invention, the concentration of the graphene oxide aqueous solution is 2 to 5 mg/L.
In a preferred embodiment of the invention, the organic salt of titanium is n-butyl titanate or isopropyl titanate.
Further preferably, the concentration of the alcoholic solution of the titanium organic salt is 0.1 to 0.3 mol/L.
In a preferred embodiment of the present invention, the dropping rate is 0.8 to 1.2 drops/s.
In a preferred embodiment of the invention, the pressure of the suction filtration is 0.1MPa, the time of the suction filtration is 1min, and the time of the standing is 15 min.
In a preferred embodiment of the present invention, the drying temperature is 30-80 ℃ and the time is 1-5 h.
The invention has the beneficial effects that: according to the invention, the titanium dioxide is loaded on the graphene oxide, so that the hydrophilic performance of the film layer can be increased, the photocatalytic effect is improved, and the film layer has higher flux and rejection rate on 1g/L bovine serum albumin under ultraviolet irradiation and under the test condition of 0.1 MPa.
Drawings
Fig. 1 is an EDS spectrum of the titanium dioxide graphene oxide modified organic ultrafiltration membrane prepared in examples 1 to 2 of the present invention (the electron microscope model is S4800, and the EDS spectrum shows that titanium dioxide is uniformly dispersed on graphene oxide sheets).
Detailed Description
The technical solution of the present invention will be further illustrated and described below with reference to the accompanying drawings by means of specific embodiments.
The modified Hummers process of the following comparative examples and examples specifically includes:
(1) 1000mL of beaker is cleaned and dried, 3g of crystalline flake graphite is added, and 360mL of concentrated sulfuric acid (98% H) is slowly added under magnetic stirring2SO4) And 40mL concentrated phosphoric acid (95% H)3PO4) Then 18g of potassium permanganate (KMBO) is slowly added in batches4) (ii) a The beaker was transferred to a 50 ℃ oil bath and stirred for 12 h. Taking out the beaker, and naturally cooling to room temperature. The reaction solution was slowly poured into 400mL of dilute hydrogen peroxide (containing 18mL of 30% H)2O2) On ice, the solution turned bright yellow;
(2) carrying out cross-flow filtration on the solution by using a tubular ceramic membrane with the aperture of 0.05 mu m to remove impurities, and obtaining an oxidized graphene solution after impurity removal; the basic principle is that the pore size screening effect of the ceramic membrane is utilized, namely the size of the filtering pore size of the ceramic tubular membrane is smaller than that of the GO sheet layer, so that the GO sheet layer cannot flow out through the tubular ceramic membrane and flows back to a material liquid barrel along with the circulation of liquid in a pipeline, membrane holes cannot be blocked, smoothness of the membrane holes is guaranteed, and the GO sheet layer with larger size is crushed and stripped; the ceramic tubular membrane filtration pore size is larger than the impurity ion size of GO solution, so that H is obtained+、K+、Mn2+The isoacid radicals and metal ions can be easily discharged through the pore diameter of the ceramic tubular membrane. The GO, the waste acid and the K are repeatedly circulated in the way+And Mn2+Separation of plasma metal ions, and collection of GO solution,washing and impurity removal of GO are completed;
(3) and diluting or concentrating according to the required concentration to obtain the graphene oxide aqueous solutions with different concentrations.
Example 1
(1) Preparing a graphene oxide aqueous solution with the concentration of 2mg/L by using a modified Hummers method;
(2) dropwise adding the graphene oxide aqueous solution into 0.2mol/L ethanol solution of n-butyl titanate at the speed of 1 drop/s, then adding 5mol/L nitric acid or hydrochloric acid for dispergation, wherein the pH of the dispergated solution is 4, in-situ covering nano titanium dioxide particles on a graphene oxide sheet layer in the graphene oxide aqueous solution by a sol-gel method, and diluting to obtain the titanium dioxide graphene oxide aqueous solution with the concentration of 2 mg/L;
(3) soaking the polyethersulfone ultrafiltration membrane with the molecular weight of 50KD in absolute ethyl alcohol and RO water, respectively soaking for 60min at room temperature, taking out, and drying in an oven at 50 ℃;
(4) pumping and filtering the titanium dioxide graphene oxide aqueous solution on the dried polyethersulfone ultrafiltration membrane for 1min under the pressure of 0.1MPa, standing for 15min, pouring out the unadsorbed titanium dioxide graphene oxide aqueous solution, washing with ethanol and RO water, and airing;
(5) placing the material obtained in the step (4) in a shade place for air drying, then placing the material in a 50 ℃ oven for heat treatment for 3h, and then cooling the material along with the oven to obtain the titanium dioxide graphene oxide modified organic ultrafiltration membrane shown in the figure 1;
the titanium dioxide graphene oxide modified organic ultrafiltration membrane prepared in the embodiment is subjected to an anti-pollution performance test: under the test conditions of 9W ultraviolet light irradiation and 0.1MPa pressure, the flux of 1g/L bovine serum albumin after running for 24 hours is 50LHM and the retention rate is 98%.
Example 2
(1) Preparing a graphene oxide aqueous solution with the concentration of 5mg/L by using a modified Hummers method;
(2) dropwise adding the graphene oxide aqueous solution into 0.2mol/L ethanol solution of n-butyl titanate at the speed of 1 drop/s, then adding 5mol/L nitric acid or hydrochloric acid to perform dispergation, wherein the pH of the dispergated solution is 4, nano titanium dioxide particles are coated on a graphene oxide sheet layer in situ in the graphene oxide aqueous solution by a sol-gel method, and the titanium dioxide graphene oxide aqueous solution with the concentration of 5mg/L is obtained by dilution;
(3) soaking a 50KD polycarbonate ultrafiltration membrane in absolute ethyl alcohol and RO water, respectively soaking for 60min at room temperature, taking out, and drying in an oven at 50 ℃;
(4) pumping and filtering the titanium dioxide graphene oxide aqueous solution on the dried polycarbonate ultrafiltration membrane for 1min under the pressure of 0.1MPa, standing for 15min, pouring out the unadsorbed titanium dioxide graphene oxide aqueous solution, washing with ethanol and RO water, and airing;
(5) placing the material obtained in the step (4) in a shade place for air drying, then placing the material in a 50 ℃ oven for heat treatment for 3h, and then cooling the material along with the oven to obtain the titanium dioxide graphene oxide modified organic ultrafiltration membrane shown in the figure 1;
the titanium dioxide graphene oxide modified organic ultrafiltration membrane prepared in the embodiment is subjected to an anti-pollution performance test: under the test conditions of 9W ultraviolet irradiation and 0.1MPa pressure, the flux of 1g/L bovine serum albumin after running for 24 hours is 55LHM and the retention rate is 97%.
Comparative example 1
The comparative example is a 50KD polyethersulfone ultrafiltration membrane, and the performance test of the membrane tube is carried out: under the test conditions of 9W ultraviolet irradiation and 0.1MPa pressure, the flux of 1g/L bovine serum albumin after running for 24 hours is 13LHM and the retention rate is 94%.
Comparative example 2
(1) Preparing a graphene oxide aqueous solution with the concentration of 1mg/L by using a modified Hummers method;
(2) soaking the polyethersulfone ultrafiltration membrane with the molecular weight of 50KD in absolute ethyl alcohol and RO water, respectively soaking for 60min at room temperature, taking out, and drying in an oven at 50 ℃;
(3) pumping and filtering the titanium dioxide graphene oxide aqueous solution on the dried polyethersulfone ultrafiltration membrane for 1min under the pressure of 0.1MPa, standing for 15min, pouring out the unadsorbed titanium dioxide graphene oxide aqueous solution, washing with ethanol and RO water, and airing;
(4) placing the material obtained in the step (3) in a shade place for air drying, then placing the material into a 50 ℃ oven for heat treatment for 3 hours, and then cooling the material along with the oven to obtain a graphene oxide modified organic ultrafiltration membrane support body;
and (3) carrying out an anti-pollution performance test on the graphene oxide modified organic ultrafiltration membrane support prepared by the comparative example: under the test conditions of 9W ultraviolet light irradiation and 0.1MPa pressure, the flux of 1g/L bovine serum albumin after running for 24 hours is 20LHM and the retention rate is 95%.
Comparative example 3
(1) Preparing a graphene oxide aqueous solution with the concentration of 2mg/L by using a modified Hummers method;
(2) dropwise adding the graphene oxide aqueous solution into 0.2mol/L ethanol solution of n-butyl titanate at the speed of 1 drop/s, then adding 5mol/L nitric acid or hydrochloric acid to perform dispergation, wherein the pH of the dispergated solution is 4, nano titanium dioxide particles are coated on a graphene oxide sheet layer in situ in the graphene oxide aqueous solution by a sol-gel method, and the titanium dioxide graphene oxide aqueous solution with the concentration of 2mg/L is obtained by dilution;
(3) soaking the polyethersulfone ultrafiltration membrane with the molecular weight of 50KD in absolute ethyl alcohol and RO water, respectively soaking for 60min at room temperature, taking out, and drying in an oven at 50 ℃;
(4) pumping and filtering the titanium dioxide graphene oxide aqueous solution on the dried polyethersulfone ultrafiltration membrane for 1min under the pressure of 0.1MPa, standing for 15min, pouring out the unadsorbed titanium dioxide graphene oxide aqueous solution, washing with ethanol and RO water, and airing;
(5) placing the material obtained in the step (4) in a shade place for air drying, then placing the material in a 50 ℃ oven for heat treatment for 3 hours, and then cooling the material along with the oven to obtain a contrast film;
the comparative film prepared in this comparative example was subjected to an anti-contamination performance test: under the test conditions of ultraviolet light and pressure of 0.1MPa, the flux of 1g/L bovine serum albumin after running for 24 hours is 52LHM and the retention rate is 82%.
Comparative example 4
(1) Preparing a graphene oxide aqueous solution with the concentration of 6mg/L by using a modified Hummers method;
(2) dropwise adding the graphene oxide aqueous solution into 0.2mol/L ethanol solution of n-butyl titanate at the speed of 1 drop/s, then adding 5mol/L nitric acid or hydrochloric acid to perform dispergation, wherein the pH of the dispergated solution is 4, nano titanium dioxide particles are coated on a graphene oxide sheet layer in situ in the graphene oxide aqueous solution by a sol-gel method, and the titanium dioxide graphene oxide aqueous solution with the concentration of 2mg/L is obtained by dilution;
(3) - (5) same as comparative example 3;
the comparative film prepared in this comparative example was subjected to an anti-contamination performance test: under the test conditions of ultraviolet light and pressure of 0.1MPa, the flux of 1g/L bovine serum albumin after running for 24 hours is 40LHM and the retention rate is 95%.
Comparative example 5
(1) Preparing a graphene oxide aqueous solution with the concentration of 2mg/L by using a modified Hummers method;
(2) dropwise adding the graphene oxide aqueous solution into 0.2mol/L ethanol solution of n-butyl titanate at the speed of 1 drop/s, then adding 5mol/L nitric acid or hydrochloric acid to perform dispergation, wherein the pH of the dispergated solution is 4, nano titanium dioxide particles are coated on a graphene oxide sheet layer in situ in the graphene oxide aqueous solution by a sol-gel method, and the titanium dioxide graphene oxide aqueous solution with the concentration of 1mg/L is obtained by dilution;
(3) - (5) same as comparative example 3;
the comparative film prepared in this comparative example was subjected to an anti-contamination performance test: under the test conditions of ultraviolet light and pressure of 0.1MPa, the flux of 1g/L bovine serum albumin after running for 24 hours is 55LHM and the retention rate is 85%.
Comparative example 6
(1) Preparing a graphene oxide aqueous solution with the concentration of 2mg/L by using a modified Hummers method;
(2) dropwise adding the graphene oxide aqueous solution into 0.2mol/L ethanol solution of n-butyl titanate at the speed of 1 drop/s, then adding 5mol/L nitric acid or hydrochloric acid to perform dispergation, wherein the pH of the dispergated solution is 4, in-situ covering nano titanium dioxide particles on a graphene oxide sheet layer in the graphene oxide aqueous solution by a sol-gel method, and concentrating to obtain the titanium dioxide graphene oxide aqueous solution with the concentration of 6 mg/L;
(3) - (5) same as comparative example 3;
the comparative film prepared in this comparative example was subjected to an anti-contamination performance test: under the test conditions of ultraviolet light and pressure of 0.1MPa, the flux of 1g/L bovine serum albumin after running for 24 hours is 25LHM and the retention rate is 95%.
Comparative example 7
(1) Preparing a graphene oxide aqueous solution with the concentration of 2mg/L by using a modified Hummers method;
(2) preparing a 2mg/L titanium dioxide/graphene oxide aqueous solution by using a hydrothermal method: adding 2g of titanium sulfate into 100mL of 2mg/L graphene oxide aqueous solution for ultrasonic dissolution, putting the solution into a reaction kettle, heating the solution at 90 ℃ for 10 hours, and diluting the solution with RO water to obtain 2mg/L titanium dioxide graphene oxide aqueous solution;
(3) - (5) same as comparative example 3;
the comparative film prepared in this comparative example was subjected to an anti-contamination performance test: under the test conditions of ultraviolet light and pressure of 0.1MPa, the flux of 1g/L bovine serum albumin after 24 hours of operation is 60LHM and the retention rate is 53 percent.
Comparative example 8
(1) Preparing a graphene oxide aqueous solution with the concentration of 2mg/L by using a modified Hummers method;
(2) dropwise adding the graphene oxide aqueous solution into 0.2mol/L ethanol solution of n-butyl titanate at the speed of 1 drop/s, then adding 5mol/L nitric acid or hydrochloric acid to perform dispergation, wherein the pH of the dispergated solution is 4, nano titanium dioxide particles are coated on a graphene oxide sheet layer in situ in the graphene oxide aqueous solution by a sol-gel method, and the titanium dioxide graphene oxide aqueous solution with the concentration of 2mg/L is obtained by dilution;
(3) the same as comparative example 3;
(4) pumping and filtering the titanium dioxide graphene oxide aqueous solution on the dried polyethersulfone ultrafiltration membrane for 2min under the pressure of 0.1MPa, standing for 15min, pouring out the unadsorbed titanium dioxide graphene oxide aqueous solution, washing with ethanol and RO water, and airing;
(5) the same as comparative example 3;
the comparative film prepared in this comparative example was subjected to an anti-contamination performance test: under the test conditions of ultraviolet light and pressure of 0.1MPa, the flux of 1g/L bovine serum albumin after 24 hours of operation is 38LHM and the retention rate is 96%.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (10)
1. A titanium dioxide graphene oxide modified organic ultrafiltration membrane is characterized in that: the functional layer is formed on the surface of the organic ultrafiltration membrane support body by filtering and drying a titanium dioxide graphene oxide aqueous solution with the pH value of 3-5, the titanium dioxide graphene oxide aqueous solution is prepared by taking the graphene oxide aqueous solution and an alcoholic solution of titanium organic salt as raw materials through a sol-gel method, the concentration of the graphene oxide aqueous solution is 2-5mg/L, and nano titanium dioxide is uniformly loaded on a graphene oxide sheet layer.
2. The titanium dioxide graphene oxide modified organic ultrafiltration membrane of claim 1, wherein: the organic ultrafiltration membrane support body is made of polyether sulfone or polycarbonate.
3. The titanium dioxide graphene oxide modified organic ultrafiltration membrane of claim 2, wherein: the molecular weight of the polyether sulfone or the polycarbonate is 50-100 KD.
4. The method for preparing the titanium dioxide and graphene oxide modified organic ultrafiltration membrane of any one of claims 1 to 3, wherein the method comprises the following steps: the method comprises the following steps:
(1) preparing a graphene oxide aqueous solution by using a modified Hummers method;
(2) dropwise adding the graphene oxide aqueous solution into an alcoholic solution of titanium organic salt, and then adding nitric acid or hydrochloric acid to perform dispergation to obtain the titanium dioxide graphene oxide aqueous solution;
(3) and (3) carrying out suction filtration on the titanium dioxide graphene oxide aqueous solution on the organic ultrafiltration membrane support body, standing, removing the titanium dioxide graphene oxide aqueous solution which is not adsorbed, washing with ethanol and deionized water, and drying to obtain the titanium dioxide graphene oxide modified organic ultrafiltration membrane.
5. The method of claim 4, wherein: the concentration of the graphene oxide aqueous solution is 2-5 mg/L.
6. The method of claim 4, wherein: the titanium organic salt is n-butyl titanate or isopropyl titanate.
7. The method of claim 6, wherein: the concentration of the alcoholic solution of the titanium organic salt is 0.1-0.3 mol/L.
8. The method of claim 4, wherein: the dropping speed is 0.8-1.2 drops/s.
9. The method of claim 4, wherein: the pressure of the suction filtration is 0.1MPa, the suction filtration time is 1min, and the standing time is 15 min.
10. The method of claim 4, wherein: the drying temperature is 30-80 ℃ and the drying time is 1-5 h.
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