CN113797769B - Dopamine modified titanium dioxide graphene oxide polyamide nanofiltration membrane and preparation method thereof - Google Patents
Dopamine modified titanium dioxide graphene oxide polyamide nanofiltration membrane and preparation method thereof Download PDFInfo
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- CN113797769B CN113797769B CN202010539611.9A CN202010539611A CN113797769B CN 113797769 B CN113797769 B CN 113797769B CN 202010539611 A CN202010539611 A CN 202010539611A CN 113797769 B CN113797769 B CN 113797769B
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- 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
- B01D71/56—Polyamides, e.g. polyester-amides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
- B01D69/105—Support pretreatment
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- 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
- B01D71/02—Inorganic material
- B01D71/024—Oxides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
Abstract
The invention discloses a dopamine modified titanium dioxide graphene oxide polyamide nanofiltration membrane and a preparation method thereof. The invention has higher retention rate (more than 96 percent) for 0.2 weight percent of magnesium sulfate solution under the test conditions of room temperature and 0.6MPa, and the pure water flux is 50-60LHM.
Description
Technical Field
The invention belongs to the technical field of membrane separation, and particularly relates to a dopamine modified titanium dioxide graphene oxide polyamide nanofiltration membrane and a preparation method thereof.
Background
Nanofiltration membranes are novel pressure driven membranes with membrane pore sizes between ultrafiltration and reverse osmosis, and can be used for separation of divalent and monovalent salts. The nanofiltration membrane has the characteristics of low operation pressure, high flux, energy conservation and the like, so the nanofiltration membrane is widely applied to the fields of bioengineering, medicine, metallurgy, water treatment, electronics and the like. The nanofiltration membrane commonly used in industry is an organic nanofiltration membrane, and has the advantages of high air permeability, low density, good film forming property, low cost, good flexibility and the like, but the organic nanofiltration membrane has the defects of low flux, poor pollution resistance and the like in industrial application, so that the organic nanofiltration membrane needs to be modified, and the flux and pollution resistance of a membrane layer are improved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a dopamine modified titanium dioxide graphene oxide polyamide nanofiltration membrane.
The invention further aims to provide a preparation method of the dopamine modified titanium dioxide graphene oxide polyamide nanofiltration membrane.
The technical scheme of the invention is as follows:
the dopamine modified titanium dioxide oxidized graphene polyamide nanofiltration membrane comprises a polyethersulfone support and an organic functional layer arranged on the polyethersulfone support, wherein the organic functional layer is formed on the polyethersulfone support by taking a water phase monomer, an organic phase monomer and an acid acceptor as raw materials through interfacial polymerization reaction;
the aqueous monomer contains dopamine modified titanium dioxide, graphene oxide and piperazine;
the organic phase monomer is trimesic acid chloride;
the acid acceptor is polyamine.
In a preferred embodiment of the invention, the polyamine is diethylamine.
In a preferred embodiment of the invention, the pore size of the polyethersulfone support is in the range of 20-50KD.
In a preferred embodiment of the invention, the dopamine-modified titanium dioxide has a mass ratio of dopamine to titanium dioxide of 1:0.6-1.5.
Further preferably, the mass ratio of the dopamine modified titanium dioxide, the graphene oxide and the piperazine is 1-2:240:320:320.
The other technical scheme of the invention is as follows:
the preparation method of the dopamine modified titanium dioxide graphene oxide polyamide nanofiltration membrane comprises the following steps: preparing titanium dioxide nano particles by a sol-gel method, and modifying dopamine to obtain dopamine modified titanium dioxide; the dopamine modified titanium dioxide, graphene oxide and piperazine mixture is used as a water phase monomer, the isophthaloyl dichloride is used as an organic monomer, the polyamine is used as an acid acceptor, and the organic functional layer is formed on the polyether sulfone support through interfacial polymerization reaction, so that the dopamine modified titanium dioxide graphene oxide polyamide nanofiltration membrane is obtained.
In a preferred embodiment of the invention, the method comprises the steps of:
(1) Preparing titanium oxide sol by a sol-gel method;
(2) Mixing titanium oxide sol with a dopamine aqueous solution, and reacting at 60-90 ℃ for 1-3 hours to obtain a dopamine modified titanium dioxide solution;
(3) Preparing an aqueous graphene oxide solution using a modified Hummers method;
(4) Stirring and mixing the dopamine modified titanium dioxide solution, the graphene oxide aqueous solution and the piperazine aqueous solution uniformly, adding PEG1000 and polyamine, and carrying out ultrasonic treatment to obtain an aqueous phase solution;
(5) Soaking the polyether sulfone support body which is washed by ethanol and water in normal hexane solution of trimesoyl chloride, carrying out water soaking and blow-drying after room temperature reaction, and then soaking in the aqueous phase solution prepared in the step (4), carrying out water soaking and blow-drying after the reaction at room temperature; repeating this step at least 1 time;
(6) And (3) drying the material obtained in the step (5) in the shade, performing heat treatment at 50-80 ℃, and cooling along with a furnace to obtain the dopamine modified titanium dioxide graphene oxide polyamide nanofiltration membrane.
Further preferably, in the step (4), the concentration of the dopamine-modified titanium dioxide solution is 0.25-0.5mg/L, the concentration of the graphene oxide aqueous solution is 0.25-0.5mg/L, and the concentration of the piperazine aqueous solution is 0.8-1.2wt%.
Still more preferably, in the step (4), the concentration of the polyamine in the mixture of the dopamine-modified titanium dioxide solution, the graphene oxide aqueous solution and the piperazine aqueous solution is 0.8 to 1.2wt%, and the concentration of the PEG1000 in the mixture of the dopamine-modified titanium dioxide solution, the graphene oxide aqueous solution and the piperazine aqueous solution is 0.8 to 1.2wt%.
Further preferably, the concentration of the n-hexane solution of trimesoyl chloride is 1.8-2.2wt%.
The beneficial effects of the invention are as follows: according to the invention, the dopamine modified titanium dioxide-graphene oxide polyamide nanofiltration membrane is prepared by adding the dopamine modified titanium dioxide-graphene oxide into a water phase monomer and performing interfacial polymerization, and has a higher rejection rate (more than 96%) for a 0.2wt% magnesium sulfate solution under the test conditions of room temperature and 0.6MPa, and the pure water flux is 50-60LHM.
Detailed Description
The technical scheme of the invention is further illustrated and described through the following specific embodiments.
The modified Hummers method in the following comparative examples and examples specifically includes:
(1) A1000 mL beaker was washed and dried, 3g of crystalline flake graphite was added, and 360mL of concentrated sulfuric acid (98% H) was slowly added under magnetic stirring 2 SO 4 ) And 40mL of concentrated phosphoric acid (95% H) 3 PO 4 ) Slowly adding 18g of potassium permanganate (KMnO) into the mixture in batches 4 ) The method comprises the steps of carrying out a first treatment on the surface of the The beaker was moved to a 50 ℃ oil bath and stirred for 12h. The beaker was taken out and naturally cooled to room temperature. The reaction solution was slowly poured into 400mL of diluted hydrogen peroxide (18 mL of 30% H) 2 O 2 ) The solution turned bright yellow on the ice cubes;
(2) Cross-flow filtering the solution by using a tubular ceramic membrane with the aperture of 0.05 mu m to remove impurities, thereby obtaining a graphene oxide solution after impurity removal; the basic principle is that the pore size screening effect of the ceramic membrane is utilized, namely, the pore size of the ceramic tubular membrane is smaller than the size of the GO sheet layer, so that the GO sheet layer cannot flow out through the tubular ceramic membrane, but flows back to the feed liquid barrel along with the circulation of liquid in the pipeline, the membrane pores are not blocked, the smoothness of the membrane pores is ensured, and the GO sheet layer with larger size is crushed and peeled; the pore size of the ceramic tubular membrane is larger than the size of the impurity ions of the GO solution, so that H + 、K + 、Mn 2+ The isoacid radical and the metal ions can be easily discharged through the aperture of the ceramic tubular membrane. Repeating the cycle to realize GO, waste acid and K + And Mn 2+ Separating plasma metal ions, collecting GO solution, and washing and impurity removing GO;
(3) And diluting or concentrating according to the required concentration to obtain graphene oxide aqueous solutions with different concentrations.
Comparative example 1
(1) Preparing an aqueous graphene oxide solution with a concentration of 0.25mg/L by using a modified Hummers method;
(2) 50ml of 0.25mg/L graphene oxide aqueous solution and 300ml of 1wt% piperazine aqueous solution are uniformly stirred, 1wt% PEG1000 and 1wt% diethylamine are added, and ultrasound is carried out for 30min, so as to prepare uniform aqueous phase solution;
(3) Soaking 20KD polyethersulfone which is washed by ethanol and water in TMC normal hexane solution with the mass fraction of 2wt%, reacting for 10min at room temperature, taking out, and drying by a water soaking and air gun; soaking the graphene oxide polyamide nanofiltration membrane in the aqueous phase solution, reacting for 10min at room temperature, taking out, blowing with water and an air gun, drying for 1 time, then placing the graphene oxide polyamide nanofiltration membrane in a drying oven at 50 ℃ after drying in the shade, heat-treating for 15min, and cooling along with the furnace.
The graphene oxide polyamide nanofiltration membrane prepared in the comparative example is tested under the conditions of room temperature and 0.6MPa, the pure water flux is 32LHM, and the retention rate of 0.2wt% magnesium sulfate solution is 94.8%.
Comparative example 2
(1) Adding 0.5wt% of dispersing agent polyethylene glycol into 0.5mol/L of n-butyl titanate solution, wherein in a sol-gel reaction, the mol ratio of the n-butyl titanate to water is 1:50, adding acid to carry out dispergation, wherein the pH value of the dispergated sol is 4, obtaining titanium dioxide sol, adding 1wt% of dispersing agent polyethylene glycol, uniformly mixing to prepare well-dispersed titanium oxide sol with the concentration of 0.5mg/L, and then diluting with water to the concentration of 0.25mg/L;
(2) Preparing an aqueous graphene oxide solution with a concentration of 0.25mg/L by using a modified Hummers method;
(3) Uniformly stirring 50ml of a titanium dioxide solution with the concentration of 0.25mg/L, 50ml of a graphene oxide aqueous solution with the concentration of 0.25mg/L and 300ml of a piperazine aqueous solution with the concentration of 1wt%, adding 1wt% PEG1000 and 1wt% diethylamine, and performing ultrasonic treatment for 30min to prepare a uniform aqueous phase solution;
(4) Soaking a 20KD polyether sulfone support body which is washed by ethanol and water in a normal hexane solution of trimesoyl chloride with the concentration of 2wt%, reacting for 10min at room temperature, then drying by a water soaking air gun, soaking in the water phase solution, reacting at room temperature, and then drying by the water soaking air gun; repeating the step 1 times;
(5) And (3) placing the material obtained in the step (4) in a shade place for air drying, then carrying out heat treatment for 15min in a 50 ℃ oven, and then cooling along with the oven to obtain the titanium dioxide-graphene oxide polyamide nanofiltration membrane.
Film tube performance test: the titanium dioxide-graphene oxide polyamide nanofiltration membrane prepared in the comparative example is tested under the conditions of room temperature and 0.6MPa, the pure water flux of the membrane is 40LHM, and the retention rate of the membrane on a 0.2wt% magnesium sulfate solution is 95%.
Example 1
(1) Adding 0.5wt% of dispersing agent polyethylene glycol into 0.5mol/L of n-butyl titanate solution, wherein in a sol-gel reaction, the mol ratio of the n-butyl titanate to water is 1:50, adding acid to carry out dispergation, wherein the pH value of the dispergated sol is 4, obtaining titanium dioxide sol, adding 1wt% of dispersing agent polyethylene glycol, uniformly mixing to prepare well-dispersed titanium oxide sol with the concentration of 0.5mg/L, and then diluting with water to the concentration of 0.2mg/L;
(2) 50ml of 1mg/L aqueous solution of dopamine is added into 150ml of 0.2mg/L titanium oxide sol, and the mixture is heated in an oil bath at 60 ℃ for reaction for 3 hours to obtain solution of dopamine modified titanium dioxide, and then the solution is concentrated to the concentration of 0.25mg/L;
(3) Preparing an aqueous graphene oxide solution with a concentration of 0.25mg/L by using a modified Hummers method;
(4) 50ml of 0.25mg/L dopamine modified titanium dioxide solution, 50ml of 0.25mg/L graphene oxide aqueous solution and 300ml of 1wt% piperazine aqueous solution are uniformly stirred, 1wt% PEG1000 and 1wt% diethylamine are added, and ultrasound is carried out for 30min, so as to prepare uniform aqueous phase solution;
(5) Soaking a 20KD polyether sulfone support body which is washed by ethanol and water in a normal hexane solution of trimesoyl chloride with the concentration of 2wt%, reacting for 10min at room temperature, then drying by a water soaking air gun, soaking in the water phase solution, reacting at room temperature, and then drying by the water soaking air gun; repeating the step 1 times;
(6) And (3) placing the material obtained in the step (5) in a shade place for air drying, then carrying out heat treatment for 15min in a 50 ℃ oven, and then cooling along with the oven to obtain the dopamine modified titanium dioxide graphene oxide polyamide nanofiltration membrane.
Film tube performance test: the dopamine modified titanium dioxide oxidized graphene polyamide nanofiltration membrane prepared in the embodiment is tested under the conditions of room temperature and 0.6MPa, the pure water flux of the membrane is 55LHM, and the retention rate of the membrane on a 0.2wt% magnesium sulfate solution is 98%.
Example 2
(1) Adding 0.5wt% of dispersing agent polyethylene glycol into 0.5mol/L of n-butyl titanate solution, wherein in a sol-gel reaction, the mol ratio of the n-butyl titanate to water is 1:50, adding acid to carry out dispergation, wherein the pH value of the dispergated sol is 4, obtaining titanium dioxide sol, adding 1wt% of dispersing agent polyethylene glycol, and uniformly mixing to obtain the titanium oxide sol with good dispersion concentration of 0.5 mg/L;
(2) 50ml of 1mg/L aqueous solution of dopamine is added into 150ml of 0.2mg/L titanium oxide sol, and the mixture is heated in an oil bath at 60 ℃ for reaction for 3 hours to obtain solution of dopamine modified titanium dioxide;
(3) Preparing an aqueous graphene oxide solution with a concentration of 0.5mg/L by using a modified Hummers method;
(4) 50ml of 0.5mg/L dopamine modified titanium dioxide solution, 50ml of 0.5mg/L graphene oxide aqueous solution and 300ml of 1wt% piperazine aqueous solution are uniformly stirred, 1wt% PEG1000 and 1wt% diethylamine are added, and ultrasound is carried out for 30min, so as to prepare uniform aqueous phase solution;
(5) Soaking a 50KD polyether sulfone support body which is washed by ethanol and water in a normal hexane solution of trimesoyl chloride with the concentration of 2wt%, reacting for 10min at room temperature, then drying by a water soaking air gun, soaking in the water phase solution, reacting at room temperature, and then drying by the water soaking air gun; repeating the step 1 times;
(6) And (3) placing the material obtained in the step (5) in a shade place for air drying, then carrying out heat treatment for 15min in a 50 ℃ oven, and then cooling along with the oven to obtain the dopamine modified titanium dioxide graphene oxide polyamide nanofiltration membrane.
Film tube performance test: the dopamine modified titanium dioxide oxidized graphene polyamide nanofiltration membrane prepared in the embodiment is tested under the conditions of room temperature and 0.6MPa, the pure water flux of the membrane is 58LHM, and the rejection rate of the membrane to a 0.2wt% magnesium sulfate solution is 96.5%.
The foregoing description is only illustrative of the preferred embodiments of the present invention and is not to be construed as limiting the scope of the invention, i.e., the invention is not to be limited to the details of the invention.
Claims (1)
1. The preparation method of the dopamine modified titanium dioxide graphene oxide polyamide nanofiltration membrane is characterized by comprising the following steps of: the method comprises the following steps:
(1) Preparing titanium oxide sol by a sol-gel method;
(2) Mixing titanium oxide sol with a dopamine aqueous solution, and reacting at 60-90 ℃ for 1-3 hours to obtain a dopamine modified titanium dioxide solution, wherein the mass ratio of dopamine to titanium dioxide in the dopamine modified titanium dioxide is 1:0.6-1.5;
(3) Preparing an aqueous graphene oxide solution using a modified Hummers method;
(4) Stirring and mixing the dopamine-modified titanium dioxide solution, the graphene oxide aqueous solution and the piperazine aqueous solution uniformly, adding PEG1000 and diethylamine, and carrying out ultrasonic treatment to obtain an aqueous phase solution, wherein the volume ratio of the dopamine-modified titanium dioxide solution to the graphene oxide aqueous solution to the piperazine aqueous solution is 50:300, the concentration of the dopamine-modified titanium dioxide solution is 0.25-0.5mg/L, the concentration of the graphene oxide aqueous solution is 0.25-0.5mg/L, the concentration of the piperazine aqueous solution is 0.8-1.2wt%, the concentration of diethylamine in the mixture of the dopamine-modified titanium dioxide solution, the graphene oxide aqueous solution and the piperazine aqueous solution is 0.8-1.2wt%, and the concentration of the PEG1000 in the mixture of the dopamine-modified titanium dioxide solution, the graphene oxide aqueous solution and the piperazine aqueous solution is 0.8-1.2wt%;
(5) Soaking a polyethersulfone support with the pore diameter of 20-50KD after ethanol and water washing in an n-hexane solution of trimesoyl chloride with the concentration of 1.8-2.2wt%, carrying out water soaking and blow-drying after room temperature reaction, and then soaking in the aqueous phase solution prepared in the step (4), carrying out water soaking and blow-drying after the room temperature reaction; repeating this step at least 1 time;
(6) And (3) drying the material obtained in the step (5) in the shade, performing heat treatment at 50-80 ℃, and cooling along with a furnace to obtain the dopamine modified titanium dioxide graphene oxide polyamide nanofiltration membrane.
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