CN115814617A - Application of phytic acid-nitrogen doped carbon quantum dot composite as aqueous phase monomer in preparation of polyamide nanofiltration membrane - Google Patents
Application of phytic acid-nitrogen doped carbon quantum dot composite as aqueous phase monomer in preparation of polyamide nanofiltration membrane Download PDFInfo
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- CN115814617A CN115814617A CN202211635904.2A CN202211635904A CN115814617A CN 115814617 A CN115814617 A CN 115814617A CN 202211635904 A CN202211635904 A CN 202211635904A CN 115814617 A CN115814617 A CN 115814617A
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Abstract
The invention discloses an application of a phytic acid-nitrogen doped carbon quantum dot compound as an aqueous phase monomer in preparation of a polyamide nanofiltration membrane, wherein the preparation method of the phytic acid-nitrogen doped carbon quantum dot compound comprises the following steps: the method comprises the steps of preparing nitrogen-doped carbon quantum dots by a hydrothermal reaction method, and preparing a phytic acid-nitrogen-doped carbon quantum dot composite by taking the nitrogen-doped carbon quantum dots and phytic acid as raw materials by a solution synthesis method. According to the preparation method, the phytic acid-doped carbon quantum dot composite is added into the water-phase monomer, the phytic acid-doped carbon quantum dot composite doped polyamide nanofiltration membrane is prepared through interfacial polymerization, the rejection rate (more than 98%) of 0.2wt% magnesium sulfate solution is high under the test conditions of room temperature and 0.6MPa, and the pure water flux is 65-75LHM.
Description
Technical Field
The invention belongs to the technical field of nanofiltration membranes, and particularly relates to application of a phytic acid-nitrogen doped carbon quantum dot compound as an aqueous phase monomer in preparation of a polyamide nanofiltration membrane.
Background
The nanofiltration membrane is a novel pressure-driven membrane, the pore size of the membrane is between that of ultrafiltration and reverse osmosis, and the nanofiltration membrane can be used for separating divalent salt and monovalent salt. The nanofiltration membrane has the characteristics of low operating 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, which 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 the organic nanofiltration membrane needs to be modified to improve the flux and pollution resistance of the membrane layer. In addition, as the thickness of the organic nanofiltration membrane increases, the flux of the membrane layer decreases, so that the preparation of defect-free and ultrathin organic nanofiltration membranes becomes a hot point of research.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides application of a phytic acid-nitrogen doped carbon quantum dot compound as an aqueous phase monomer in preparation of a polyamide nanofiltration membrane.
The invention also aims to provide a polyamide nanofiltration membrane.
The technical scheme of the invention is as follows:
the application of the phytic acid-nitrogen doped carbon quantum dot compound as an aqueous phase monomer in the preparation of a polyamide nanofiltration membrane comprises the following steps: the method comprises the steps of preparing nitrogen-doped carbon quantum dots by a hydrothermal reaction method, and preparing a phytic acid-nitrogen-doped carbon quantum dot composite by taking the nitrogen-doped carbon quantum dots and phytic acid as raw materials by a solution synthesis method.
In a preferred embodiment of the present invention, the method for preparing the phytic acid-nitrogen doped carbon quantum dot composite comprises the following steps:
(1) Dissolving urea and citric acid in deionized water, carrying out hydrothermal reaction for 2.5-3.5h at 175-185 ℃, then dialyzing for 6-8d, and freeze-drying to obtain nitrogen-doped carbon quantum dot powder, wherein the ratio of the urea to the citric acid to the deionized water is 0.8-1.2 g: 1.5-2.4 g: 20-30mL;
(2) Uniformly mixing phytic acid and the aqueous solution of the nitrogen-doped carbon quantum dots, and carrying out heating reflux reaction at 60-90 ℃ for 0.8-1.2h to obtain the solution of the phytic acid-nitrogen-doped carbon quantum dot composite.
In a preferred embodiment of the invention, the mass ratio of the phytic acid to the nitrogen-doped carbon quantum dots in the phytic acid-nitrogen-doped carbon quantum dot composite is 1-5:1.
Further preferably, the mass ratio of the phytic acid to the nitrogen-doped carbon quantum dots in the phytic acid-nitrogen-doped carbon quantum dot composite is 1-2:1.
The other technical scheme of the invention is as follows:
a polyamide nanofiltration membrane comprises a polyether sulfone ultrafiltration support layer and an organic nanofiltration membrane layer on the polyether sulfone ultrafiltration support layer through interfacial polymerization, wherein in the interfacial polymerization, a water phase monomer consists of phytic acid-nitrogen doped carbon quantum dot compound and piperazine, an acid acceptor is polyamine, an organic phase monomer is triphenyl acyl chloride, and the preparation method of the phytic acid-nitrogen doped carbon quantum dot compound comprises the following steps: the method comprises the steps of preparing nitrogen-doped carbon quantum dots by a hydrothermal reaction method, and preparing a phytic acid-nitrogen-doped carbon quantum dot composite by taking the nitrogen-doped carbon quantum dots and phytic acid as raw materials by a solution synthesis method.
In a preferred embodiment of the present invention, the method for preparing the phytic acid-nitrogen doped carbon quantum dot composite comprises the following steps:
(1) Dissolving urea and citric acid in deionized water, carrying out hydrothermal reaction for 2.5-3.5h at 175-185 ℃, then dialyzing for 6-8d, and freeze-drying to obtain nitrogen-doped carbon quantum dot powder, wherein the ratio of the urea to the citric acid to the deionized water is 0.8-1.2 g: 1.5-2.4 g: 20-30mL;
(2) Uniformly mixing phytic acid and the aqueous solution of the nitrogen-doped carbon quantum dots, and carrying out heating reflux reaction at 60-90 ℃ for 0.8-1.2h to obtain the solution of the phytic acid-nitrogen-doped carbon quantum dot composite.
In a preferred embodiment of the invention, the mass ratio of the phytic acid to the nitrogen-doped carbon quantum dots in the phytic acid-nitrogen-doped carbon quantum dot composite is 1-5:1.
Further preferably, the mass ratio of the phytic acid to the nitrogen-doped carbon quantum dots in the phytic acid-nitrogen-doped carbon quantum dot composite is 1-2:1.
In a preferred embodiment of the invention, the polyamine is diethylamine or triethylamine.
In a preferred embodiment of the present invention, the mass ratio of the phytic acid-nitrogen doped carbon quantum dot composite to the piperazine is 1-5:1.
The invention has the beneficial effects that: according to the method, the phytic acid-doped carbon quantum dot compound is added into the water-phase monomer, the ultrathin phytic acid-doped carbon quantum dot compound doped polyamide nanofiltration membrane is prepared through interfacial polymerization, the flux and the anti-pollution capacity can be remarkably improved by reducing the thickness of the nanofiltration membrane layer, the rejection rate (more than 98%) of 0.2wt% magnesium sulfate solution is high under the test conditions of room temperature and 0.6MPa, and the pure water flux is 65-75LHM.
Drawings
FIG. 1 is a scanning electron microscope photograph of an organic nanofiltration membrane layer of the phytic acid-polyamide nanofiltration membrane prepared in comparative example 2 of the present invention.
Fig. 2 is a scanning electron microscope photograph of an organic nanofiltration membrane layer of the phytic acid-nitrogen doped carbon quantum dot doped polyamide nanofiltration membrane prepared in example 2 of the present invention.
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description in conjunction with the accompanying drawings.
Comparative example 1
(1) 1g of urea and 2g of citric acid are dissolved in 25mL of deionized water and placed in a 25mL hydrothermal reaction kettle to react for 3h at 180 ℃. Taking out, dialyzing for 7 days, and freeze-drying to obtain nitrogen-doped carbon quantum dot powder;
(2) Uniformly stirring 0.1g of the aqueous solution of the nitrogen-doped carbon quantum dot powder and 100mL of a 0.1wt% piperazine aqueous solution (wherein the mass ratio of the phytic acid-nitrogen-doped carbon quantum dot composite to the piperazine is 1: 1), adding 1wt% of PEG1000 and 1wt% of diethylamine, and carrying out ultrasonic treatment for 30min to prepare a uniform aqueous solution;
(3) Soaking 20KD of polyether sulfone washed by ethanol and water in 0.2wt% of TMC n-hexane solution, reacting at room temperature for 10min, taking out, and carrying out water soaking and air gun blow-drying; and soaking in the aqueous phase solution, reacting at room temperature for 10min, taking out, soaking in water, blowing with an air gun, repeating the step for 1 time, placing in a shade, air drying, placing in a 50 ℃ oven, performing heat treatment for 15min, and cooling along with the oven to prepare the nitrogen-doped carbon quantum dot polyamide nanofiltration membrane.
The nitrogen-doped carbon quantum dot doped polyamide nanofiltration membrane prepared by the comparative example is tested under the conditions of room temperature and pressure of 0.6MPa, the pure water flux of the nanofiltration membrane is 56.8LHM, and the rejection rate of 0.2wt% magnesium sulfate solution is 97.1%.
Comparative example 2
(1) Stirring 100mg phytic acid and 100mL 0.1wt% piperazine water solution uniformly, adding 1wt% PEG1000 and 1wt% diethylamine, and subjecting to ultrasound for 30min to obtain uniform water phase solution;
(4) Soaking the polyether sulfone support layer of 20KD after ethanol and water washing in a normal hexane solution of trimesoyl chloride with the concentration of 0.2wt%, carrying out water soaking and air gun blow-drying after reacting for 10min at room temperature, soaking in the aqueous phase solution, and carrying out water soaking and air gun blow-drying after reacting at room temperature; repeating the step for 1 time;
(5) And (3) air-drying the material obtained in the step (4) in a shade place, then performing heat treatment in a 50 ℃ oven for 15min, and then cooling along with the oven to obtain the phytic acid-polyamide nanofiltration membrane, wherein the thickness of the organic nanofiltration membrane layer is 112nm, as shown in figure 1.
Testing the performance of the membrane tube: the phytic acid-polyamide nanofiltration membrane prepared by the comparative example is tested under the conditions of room temperature and 0.6MPa, the pure water flux is 56LHM, and the rejection rate of 0.2wt% of magnesium sulfate solution is 98.5%.
Example 1
(1) 1g of urea and 2g of citric acid are dissolved in 25mL of deionized water and placed in a 25mL hydrothermal reaction kettle to react for 3h at 180 ℃. Taking out, dialyzing for 7 days, and freeze-drying to obtain nitrogen-doped carbon quantum dot powder;
(2) Dissolving phytic acid and nitrogen-doped carbon quantum dot powder in 100mL of water according to the mass ratio of 5:1, uniformly mixing, and carrying out reflux reaction at 60-90 ℃ for 1h to obtain 20mg/mL phytic acid-nitrogen-doped carbon quantum dot composite solution;
(3) Uniformly stirring and mixing the 20mg/mL phytic acid-nitrogen doped carbon quantum dot complex solution and a 0.1wt% piperazine water solution (wherein the mass ratio of the phytic acid-nitrogen doped carbon quantum dot complex to the piperazine is 1: 1), adding 1wt% of PEG1000 and 1wt% of diethylamine, and performing ultrasonic treatment to obtain an aqueous solution;
(4) Soaking the polyether sulfone support layer of 20KD after ethanol and water washing in a normal hexane solution of trimesoyl chloride with the concentration of 0.2wt%, carrying out water soaking and air gun blow-drying after reacting for 10min at room temperature, soaking in the aqueous phase solution, and carrying out water soaking and air gun blow-drying after reacting at room temperature; repeating the step for 1 time;
(5) And (3) placing the material obtained in the step (5) in a shade place for air drying, then performing heat treatment in a 50 ℃ oven for 15min, and then cooling along with the oven to obtain the phytic acid-nitrogen doped carbon quantum dot doped polyamide nanofiltration membrane.
Testing the performance of the membrane tube: the phytic acid-nitrogen doped carbon quantum dot doped polyamide nanofiltration membrane prepared in the embodiment is tested under the conditions of room temperature and 0.6MPa, the pure water flux is 70LHM, and the rejection rate of 0.2wt% of magnesium sulfate solution is 98.6%.
Example 2
(1) Dissolving 1g of urea and 2g of citric acid in 25mL of deionized water, placing the mixture in a 25mL hydrothermal reaction kettle, and reacting for 3h at 180 ℃. Taking out, dialyzing for 7 days, and freeze-drying to obtain nitrogen-doped carbon quantum dot powder;
(2) Dissolving phytic acid and nitrogen-doped carbon quantum dot powder in 100mL of water according to the mass ratio of 5:1, uniformly mixing, and carrying out reflux reaction at 60-90 ℃ for 1h to obtain 20mg/mL phytic acid-nitrogen-doped carbon quantum dot composite solution;
(3) Uniformly stirring and mixing the 20mg/mL phytic acid-nitrogen-doped carbon quantum dot composite solution and a 0.1wt% piperazine water solution (wherein the mass ratio of the phytic acid-nitrogen-doped carbon quantum dot composite to the piperazine is 5: 1), adding 1wt% PEG1000 and 1wt% diethylamine, and performing ultrasonic treatment to obtain an aqueous phase solution;
(4) Soaking the polyether sulfone support layer of 20KD after ethanol and water washing in a normal hexane solution of trimesoyl chloride with the concentration of 0.2wt%, carrying out water soaking and air gun blow-drying after reacting for 10min at room temperature, soaking in the aqueous phase solution, and carrying out water soaking and air gun blow-drying after reacting at room temperature; repeating the step for 1 time;
(5) And (3) air-drying the material obtained in the step (5) in a shade place, then performing heat treatment in a 50 ℃ oven for 15min, and then cooling along with the oven to obtain the phytic acid-nitrogen doped carbon quantum dot doped polyamide nanofiltration membrane, wherein the thickness of an organic nanofiltration membrane layer is 45nm, as shown in figure 2.
Testing the performance of the membrane tube: the phytic acid-nitrogen doped carbon quantum dot doped polyamide nanofiltration membrane prepared in the embodiment is tested under the conditions of room temperature and 0.6MPa, the pure water flux is 75LHM, and the rejection rate of 0.2wt% of magnesium sulfate solution is 98%.
Example 3
(1) 1g of urea and 2g of citric acid are dissolved in 25mL of deionized water and placed in a 25mL hydrothermal reaction kettle to react for 3h at 180 ℃. Taking out, dialyzing for 7 days, and freeze-drying to obtain nitrogen-doped carbon quantum dot powder;
(2) Mixing phytic acid and nitrogen-doped carbon quantum dot powder in a ratio of 10: dissolving the mass ratio of 1 in 100mL of water, uniformly mixing, and carrying out reflux reaction at 60-90 ℃ for 1h to obtain 20mg/mL phytic acid-nitrogen doped carbon quantum dot composite solution;
(3) Uniformly stirring and mixing the 20mg/mL phytic acid-nitrogen-doped carbon quantum dot composite solution and a 0.1wt% piperazine water solution (wherein the mass ratio of the phytic acid-nitrogen-doped carbon quantum dot composite to the piperazine is 1: 1), adding 1wt% PEG1000 and 1wt% diethylamine, and performing ultrasonic treatment to obtain an aqueous phase solution;
(4) Soaking the polyether sulfone support layer of 20KD after ethanol and water washing in a normal hexane solution of trimesoyl chloride with the concentration of 0.2wt%, carrying out water soaking and air gun blow-drying after reacting for 10min at room temperature, soaking in the aqueous phase solution, and carrying out water soaking and air gun blow-drying after reacting at room temperature; repeating the step for 1 time;
(5) And (3) placing the material obtained in the step (5) in a shade place for air drying, then performing heat treatment in a 50 ℃ oven for 15min, and then cooling along with the oven to obtain the phytic acid-nitrogen doped carbon quantum dot doped polyamide nanofiltration membrane.
Testing the performance of the membrane tube: the phytic acid-nitrogen doped carbon quantum dot doped polyamide nanofiltration membrane prepared in the embodiment is tested under the conditions of room temperature and 0.6MPa, the pure water flux is 68LHM, and the rejection rate of 0.2wt% of magnesium sulfate solution is 99%.
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. The application of the phytic acid-nitrogen doped carbon quantum dot compound as an aqueous phase monomer in the preparation of a polyamide nanofiltration membrane is characterized in that: the preparation method of the phytic acid-nitrogen doped carbon quantum dot compound comprises the following steps: the method comprises the steps of preparing nitrogen-doped carbon quantum dots by a hydrothermal reaction method, and preparing a phytic acid-nitrogen-doped carbon quantum dot composite by taking the nitrogen-doped carbon quantum dots and phytic acid as raw materials by a solution synthesis method.
2. The use of claim 1, wherein: the preparation method of the phytic acid-nitrogen doped carbon quantum dot compound comprises the following steps:
(1) Dissolving urea and citric acid in deionized water, carrying out hydrothermal reaction for 2.5-3.5h at 175-185 ℃, then dialyzing for 6-8d, and freeze-drying to obtain nitrogen-doped carbon quantum dot powder, wherein the ratio of the urea to the citric acid to the deionized water is 0.8-1.2 g: 1.5-2.4 g: 20-30mL;
(2) Uniformly mixing phytic acid and the aqueous solution of the nitrogen-doped carbon quantum dots, and carrying out heating reflux reaction at 60-90 ℃ for 0.8-1.2h to obtain the solution of the phytic acid-nitrogen-doped carbon quantum dot composite.
3. Use according to claim 1 or 2, characterized in that: the mass ratio of the phytic acid to the nitrogen-doped carbon quantum dots in the phytic acid-nitrogen-doped carbon quantum dot composite is 1-5:1.
4. Use according to claim 3, characterized in that: the mass ratio of the phytic acid to the nitrogen-doped carbon quantum dots in the phytic acid-nitrogen-doped carbon quantum dot composite is 1-2:1.
5. A polyamide nanofiltration membrane, which is characterized in that: the preparation method comprises a polyether sulfone ultrafiltration supporting layer and an organic nanofiltration membrane layer on the polyether sulfone ultrafiltration supporting layer through interfacial polymerization, wherein in the interfacial polymerization, an aqueous phase monomer consists of phytic acid-nitrogen doped carbon quantum dot compound and piperazine, an acid acceptor is polyamine, an organic phase monomer is triphenyl acyl chloride, and the preparation method of the phytic acid-nitrogen doped carbon quantum dot compound comprises the following steps: the method comprises the steps of preparing nitrogen-doped carbon quantum dots by a hydrothermal reaction method, and preparing a phytic acid-nitrogen-doped carbon quantum dot composite by taking the nitrogen-doped carbon quantum dots and phytic acid as raw materials by a solution synthesis method.
6. A polyamide nanofiltration membrane according to claim 5, wherein: the preparation method of the phytic acid-nitrogen doped carbon quantum dot compound comprises the following steps:
(1) Dissolving urea and citric acid in deionized water, carrying out hydrothermal reaction for 2.5-3.5h at 175-185 ℃, then dialyzing for 6-8d, and freeze-drying to obtain nitrogen-doped carbon quantum dot powder, wherein the ratio of the urea to the citric acid to the deionized water is 0.8-1.2 g: 1.5-2.4 g: 20-30mL;
(2) Uniformly mixing phytic acid and the aqueous solution of the nitrogen-doped carbon quantum dots, and then carrying out heating reflux reaction at 60-90 ℃ for 0.8-1.2h to obtain the solution of the phytic acid-nitrogen-doped carbon quantum dot compound.
7. A polyamide nanofiltration membrane according to claim 5, wherein: the mass ratio of the phytic acid to the nitrogen-doped carbon quantum dots in the phytic acid-nitrogen-doped carbon quantum dot composite is 1-5:1.
8. The use of claim 7, wherein: the mass ratio of the phytic acid to the nitrogen-doped carbon quantum dots in the phytic acid-nitrogen-doped carbon quantum dot composite is 1-2:1.
9. a polyamide nanofiltration membrane according to claim 5, wherein: the polyamine is diethylamine or triethylamine.
10. A polyamide nanofiltration membrane according to claim 5, wherein: the mass ratio of the phytic acid-nitrogen doped carbon quantum dot compound to the piperazine is 1-5:1.
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| CN116855246A (en) * | 2023-07-03 | 2023-10-10 | 广西科学院 | Phosphorus self-doping type biomass carbon quantum dot corrosion inhibitor and preparation method and application thereof |
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| CN116855246A (en) * | 2023-07-03 | 2023-10-10 | 广西科学院 | Phosphorus self-doping type biomass carbon quantum dot corrosion inhibitor and preparation method and application thereof |
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