CN113600012A - High-flux high-rejection nanofiltration membrane modified by carbonic acid lactone and preparation method thereof - Google Patents
High-flux high-rejection nanofiltration membrane modified by carbonic acid lactone and preparation method thereof Download PDFInfo
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- CN113600012A CN113600012A CN202110834542.9A CN202110834542A CN113600012A CN 113600012 A CN113600012 A CN 113600012A CN 202110834542 A CN202110834542 A CN 202110834542A CN 113600012 A CN113600012 A CN 113600012A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0093—Chemical modification
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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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
- B01D71/06—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
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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Abstract
The invention discloses a carbonic acid lactone modified high-flux high-rejection rate nanofiltration membrane and a preparation method thereof, wherein the nanofiltration membrane is prepared from an ultrafiltration membrane supporting layer, a polyamide layer and a carbonic acid lactone modified monomer; the preparation process comprises the following steps: firstly, an interface polymerization is carried out on a support layer to form a polyamide layer, namely an initial nanofiltration membrane, and then the polyamide layer and the carbonate lactone react to prepare the modified nanofiltration membrane. The nanofiltration membrane prepared by the invention has high flux and high retention rate, the preparation method is simple and feasible, the cost is low, and the nanofiltration membrane can be applied to the fields of water softening, sewage treatment, seawater desalination, chemical material separation and the like, and has good industrial application prospect.
Description
Technical Field
The invention relates to the technical field of nanofiltration membranes, in particular to a high-flux high-rejection nanofiltration membrane modified by carbonic acid lactone and a preparation method thereof.
Background
The problems of the continuous increase of population and the shortage of water resources make global sustainable development face huge challenges. The membrane separation technology has the advantages of energy conservation, environmental protection and high efficiency, and becomes a mainstream process in the field of water treatment. Nanofiltration (NF) is a novel pressure-driven separation process between reverse osmosis and ultrafiltration. The nanofiltration membrane is a separation membrane with charge, and inorganic salts with different valence states are effectively separated through the dual functions of aperture screening and electrostatic repulsion. It has a rejection of less than 50% for monovalent salts, but greater than 90% for multivalent salts. Nanofiltration has the characteristics of low operating pressure, low cost, strong selectivity and the like, and is widely applied in the fields of seawater desalination, softened water and industrial wastewater treatment.
At present, the nanofiltration membrane material is prepared in various types, such as: aromatic polyamides, sulfonated polysulfones, and the like. However, the nanofiltration membranes prepared by the materials have respective defects to a certain extent, such as low flux and mutual limitation between flux and rejection efficiency (Trade-Off). Therefore, the modification of nanofiltration membranes has attracted increasing researchers' attention. However, the existing reports show that the modified membrane materials still have the problems of unobvious modification effect, complex preparation process, high cost, easy generation of defects of the membrane and the like. The zwitterion nanofiltration membrane prepared by directly carrying out the surface grafting modification of the carbonic acid lactone on the polyamide polysulfone nanofiltration membrane can improve the water permeability by improving the surface hydrophilicity.
Disclosure of Invention
The invention aims to overcome the defects of the existing nanofiltration membrane modification and provides a carbonate lactone modified high-flux high-rejection rate nanofiltration membrane and a preparation method thereof.
Therefore, the technical scheme of the invention is as follows: a preparation method of a carbonate lactone modified high-flux high-rejection nanofiltration membrane comprises the following steps:
1) after the ultrafiltration membrane supporting layer is cleaned by deionized water and dried in the air, pouring an aqueous phase solution containing amine monomers on the surface of the ultrafiltration supporting layer for dipping to form an aqueous phase liquid layer on the surface, and then pouring out and drying in the air;
2) contacting and dipping the membrane obtained in the step 1) with an organic phase solution containing acyl chloride monomers, forming a polyamide layer on the surface of an ultrafiltration membrane supporting layer through interfacial polymerization reaction, then pouring off and carrying out heat treatment to obtain an initial nanofiltration membrane;
3) cleaning the membrane obtained in the step 2) with deionized water, then modifying with a solution containing carbonic acid lactone, and obtaining the high-flux high-retention modified nanofiltration membrane after cleaning.
Preferably, the ultrafiltration membrane support layer in the step 1) is prepared from one or more of polysulfone, polyethersulfone, polyetherketone, polyarylsulfone, polyacrylonitrile and polyvinylidene fluoride.
Preferably, the aqueous amine monomer in step 1) may comprise one or more of piperazine, m-phenylenediamine, o-phenylenediamine, p-phenylenediamine, ethylenediamine, hexamethylenediamine, 1, 4-butanediamine, 4-diaminodiphenyl ether, 4, -diaminodiphenylmethane, o-biphenylmethylamine, 1, 2-propanediamine, 1, 3-propanediamine, 2, 4-diaminotoluene, 1, 2-cyclohexanediamine, 4, 5-dichlorophthalenediamine, diethylenetriamine, trimesamine and derivatives thereof.
Preferably, the mass fraction of the aqueous phase monomer in step 1) is 0.2 wt%; pH of the aqueous solution is 10; the soaking time was 4 min.
Preferably, the acyl chloride monomer in step 2) may comprise one or more of isophthaloyl dichloride, terephthaloyl dichloride, phthaloyl dichloride, poly aromatic sulfonyl chloride and derivatives thereof.
Preferably, the organic phase solvent in step 2) is one or a mixture of n-hexane, cyclohexane, toluene, benzene and ethyl acetate.
Preferably, the mass fraction of the organic phase acyl chloride monomer in the step 2) is 0.1 wt%; the soaking time is 1 min; the heat treatment temperature is 60 deg.C, and the time is 15 min.
Preferably, the carbonic acid lactone monomer in step 3) may comprise one or more of β -propiolactone, β -butyrolactone, γ -valerolactone, δ -valerolactone, γ -caprolactone, δ -caprolactone, ε -caprolactone, 4-heptalactone, 5-octalactone, γ -octalactone, 5-nonalactone, γ -nonalactone, δ -decalactone, δ -undecalactone, γ -dodecalactone, butyldodecalactone, δ -tridecanolactone, δ -tetradecanolide, and cyclopentadecanolide.
Preferably, the concentration of the solution of the carbonic acid lactone monomer in the step (3) is 0.08-0.8 mol/L, and the solvent is ethanol; the area of the polyamide nanofiltration membrane is a circle with the diameter of 6 cm; the modification temperature is 25-60 ℃, and the modification time is 8 h.
The other technical scheme of the invention is as follows: the nanofiltration membrane modified by carbonic acid lactone and having high flux and high rejection rate is prepared by the method.
The carbonate lactone modified high-flux high-rejection nanofiltration membrane obtained by the invention not only keeps Na2SO4And Mg2SO4High interception rate of 96-99%, and water flux of 6-7.3 Lm-2h-1bar-1Is more than 2 times of the unmodified nanofiltration membrane.
The nanofiltration membrane prepared by the invention has high flux and high retention rate, the preparation method is simple and feasible, the cost is low, and the nanofiltration membrane can be applied to the fields of water softening, sewage treatment, seawater desalination, chemical material separation and the like, and has good industrial application prospect.
Drawings
The following detailed description is made with reference to the accompanying drawings and embodiments of the present invention
FIG. 1 is a graph of the separation performance of nanofiltration membranes (water flux and Na)2SO4Rejection rate);
figure 2 is a surface topography of the initial nanofiltration membrane of example 1;
figure 3 is a surface topography of the modified nanofiltration membrane-1 in example 2;
figure 4 is a surface topography of the modified nanofiltration membrane-2 in example 3;
figure 5 is a surface topography of the modified nanofiltration membrane-3 in example 4.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be more fully described in connection with the following examples. The invention may, however, be embodied in many different forms and the scope of protection is not limited to the embodiments described herein.
The preparation environment of all the initial nanofiltration membranes in the examples was: the temperature is 25 ℃, the humidity is 40%, and the pressure is normal.
A high-flux high-rejection modified nano-filter membrane is composed of a polysulfone ultra-filter membrane as a supporting layer and a modified polyamide layer as a functional layer. The preparation method comprises the following specific steps:
(1) soaking the polysulfone ultrafiltration membrane support membrane in an aqueous phase monomer solution to form an aqueous phase liquid layer on the surface of the polysulfone ultrafiltration membrane support membrane; wherein the water phase monomer is piperazine;
(2) contacting the membrane obtained in the step (1) with an organic phase solution containing acyl chloride monomers, and forming a polyamide layer on the surface of a polysulfone ultrafiltration support layer through interfacial polymerization reaction to obtain an initial nanofiltration membrane; wherein the monomer is trimesoyl chloride;
(3) and (3) cleaning the membrane obtained in the step (2) by using deionized water, then modifying the membrane by using a solution containing carbonic lactone at 40 ℃ for 8 hours, and cleaning the membrane by using deionized water to obtain the high-flux high-rejection modified nanofiltration membrane.
The mass fraction of the water phase monomer in the step (1) is 0.2 wt%. The pH of the aqueous phase solution of step (1) was 10. The step (1) further comprises: before the polysulfone ultrafiltration membrane supporting layer is immersed, the polysulfone ultrafiltration membrane supporting layer is cleaned by deionized water, after air drying, the water phase solution is poured on the surface of the polysulfone ultrafiltration supporting layer for 4min, and then the water phase solution is poured out and air drying is carried out. The mass fraction of the organic phase active monomer in the step (2) is 0.1 wt%. The organic phase solvent in the step (2) is n-hexane. The step (2) further comprises the following steps: covering a layer of organic phase solution on the polysulfone ultrafiltration membrane support layer obtained in the step (1) for 1min, then pouring off, and carrying out heat treatment at 60 ℃ for 15 min. The carbonic acid lactone monomers in the step (3) are gamma-butyrolactone, delta-valerolactone and epsilon-caprolactone. The concentration of the solution of the carbonic acid lactone monomer in the step (3) is 0.16 mol/L. The solvent used in the solution in the step (3) is ethanol. The polyamide nanofiltration membrane in the step (3) is a circle with the diameter of 6 cm. In the step (3), the temperature is 40 ℃, and the modification time is 8 h.
Example 1:
(1) immersing a polysulfone ultrafiltration nanofiltration membrane supporting layer in 0.2 wt% piperazine aqueous solution with the pH value of 10 for 4min, pouring out the aqueous solution, and airing the membrane to form an aqueous phase liquid layer on the surface of the membrane;
(2) and (3) carrying out interfacial polymerization on the obtained membrane and 0.1 wt% of trimesoyl chloride n-hexane solution for 1min to form a polyamide layer on the surface of the polysulfone ultrafiltration membrane supporting layer, thus obtaining the initial nanofiltration membrane.
Analytical testing of the nanofiltration membranes obtained in example 1:
the nanofiltration membrane prepared by the embodiment is loaded into a membrane performance evaluation device, and the experimental conditions are as follows: at normal temperature, 0.6MPa, pre-pressing for 1h, 1g/L of Na2SO4、MgSO4、MgCl2A salt solution; the experimental results are as follows: water flux: 3.4Lm-2h-1bar-1,Na2SO4Retention rate: 97.7%, MgSO4Retention rate: 97% of MgCl2Retention rate: 79 percent.
In addition, the anti-pollution performance of the membrane is tested by Bovine Serum Albumin (BSA) simulation solution (0.5g/L) for 7h, and then the membrane is washed by alkali liquor with pH being 9, and the flux recovery rate is measured; the experimental results are as follows: the flux recovery rate is 100 percent
Example 2:
(1) immersing a polysulfone ultrafiltration nanofiltration membrane supporting layer in 0.2 wt% piperazine aqueous solution with the pH value of 10 for 4min, pouring out the aqueous solution, and airing the membrane to form an aqueous phase liquid layer on the surface of the membrane;
(2) and (3) carrying out interfacial polymerization on the aqueous phase liquid layer and 0.1 wt% of trimesoyl chloride n-hexane solution for 1min to form a polyamide layer on the surface of the polysulfone ultrafiltration membrane supporting layer, thus obtaining the initial nanofiltration membrane.
(3) And cleaning the initial nanofiltration membrane by using deionized water, then modifying the initial nanofiltration membrane at 40 ℃ for 8 hours by using a solution only containing gamma-butyrolactone with the concentration of 0.16mol/L, and obtaining the high-flux high-rejection modified nanofiltration membrane-1 after cleaning the initial nanofiltration membrane by using the deionized water.
The membrane performance test method is the same as that of example 1, and the experimental result is as follows: water flux: 7.3Lm-2h-1bar-1,Na2SO4Retention rate: 98.6%, MgSO4Retention rate: 97.5% of MgCl2Retention rate: 76.2 percent and 100 percent of flux recovery rate.
Example 3:
the method comprises the following specific steps:
(1) immersing a polysulfone ultrafiltration nanofiltration membrane supporting layer in 0.2 wt% piperazine aqueous solution with the pH value of 10 for 4min, pouring out the aqueous solution, and airing the membrane to form an aqueous phase liquid layer on the surface of the membrane;
(2) and (3) carrying out interfacial polymerization on the aqueous phase liquid layer and 0.1 wt% of trimesoyl chloride n-hexane solution for 1min to form a polyamide layer on the surface of the polysulfone ultrafiltration membrane supporting layer, thus obtaining the initial nanofiltration membrane.
(3) And cleaning the initial nanofiltration membrane by using deionized water, then modifying the initial nanofiltration membrane at 40 ℃ for 8 hours by using a solution only containing delta-valerolactone with the concentration of 0.16mol/L, and obtaining the high-flux high-retention modified nanofiltration membrane-2 after cleaning the initial nanofiltration membrane by using the deionized water.
The membrane performance test method is the same as that of example 1, and the experimental result is as follows: water flux: 6.7Lm-2h-1bar-1,Na2SO4Retention rate: 98.8%, MgSO4Retention rate: 96.6% of MgCl2Retention rate: 72.8 percent and the flux recovery rate is 100 percent.
Example 4:
the method comprises the following specific steps:
(1) immersing a polysulfone ultrafiltration nanofiltration membrane supporting layer in 0.2 wt% piperazine aqueous solution with the pH value of 10 for 4min, pouring out the aqueous solution, and airing the membrane to form an aqueous phase liquid layer on the surface of the membrane;
(2) and (3) carrying out interfacial polymerization on the aqueous phase liquid layer and 0.1 wt% of trimesoyl chloride n-hexane solution for 1min to form a polyamide layer on the surface of the polysulfone ultrafiltration membrane supporting layer, thus obtaining the initial nanofiltration membrane.
(3) And (2) cleaning the initial nanofiltration membrane by using deionized water, then modifying the initial nanofiltration membrane at 40 ℃ for 8 hours by using a solution only containing epsilon-caprolactone with the concentration of 0.16mol/L, and obtaining the high-flux high-rejection modified nanofiltration membrane-3 after the initial nanofiltration membrane is cleaned by using the deionized water.
The membrane performance test method is the same as that of example 1, and the experimental result is as follows: water flux: 6.0Lm-2h-1bar-1,Na2SO4Retention rate: 98.3%, MgSO4Retention rate: 96.3% of MgCl2Retention rate: 71 percent and the flux recovery rate is 100 percent.
Table 1 separation performance of nanofiltration membrane examples
Claims (10)
1. A preparation method of a carbonate lactone modified high-flux high-rejection nanofiltration membrane is characterized by comprising the following steps: the method comprises the following steps:
1) after the ultrafiltration membrane supporting layer is cleaned by deionized water and dried in the air, pouring an aqueous phase solution containing amine monomers on the surface of the ultrafiltration supporting layer for dipping to form an aqueous phase liquid layer on the surface, and then pouring out and drying in the air;
2) contacting and dipping the membrane obtained in the step 1) with an organic phase solution containing acyl chloride monomers, forming a polyamide layer on the surface of an ultrafiltration membrane supporting layer through interfacial polymerization reaction, then pouring off and carrying out heat treatment to obtain an initial nanofiltration membrane;
3) cleaning the membrane obtained in the step 2) with deionized water, then modifying with a solution containing carbonic acid lactone, and obtaining the high-flux high-retention modified nanofiltration membrane after cleaning.
2. The method for preparing the nanofiltration membrane modified by the carbonic acid lactone with high flux and high rejection rate as claimed in claim 1, wherein the method comprises the following steps: the ultrafiltration membrane support layer in the step 1) is prepared from one or more of polysulfone, polyethersulfone, polyetherketone, polyarylsulfone, polyacrylonitrile and polyvinylidene fluoride.
3. The method for preparing the nanofiltration membrane modified by the carbonic acid lactone with high flux and high rejection rate as claimed in claim 1, wherein the method comprises the following steps: the aqueous amine monomer in step 1) may comprise one or more of piperazine, m-phenylenediamine, o-phenylenediamine, p-phenylenediamine, ethylenediamine, hexamethylenediamine, 1, 4-butanediamine, 4-diaminodiphenyl ether, 4, -diaminodiphenylmethane, o-biphenylmethylamine, 1, 2-propanediamine, 1, 3-propanediamine, 2, 4-diaminotoluene, 1, 2-cyclohexanediamine, 4, 5-dichlorophthalenediamine, diethylenetriamine, trimesamine, and derivatives thereof.
4. The method for preparing the nanofiltration membrane modified by the carbonic acid lactone with high flux and high rejection rate as claimed in claim 1, wherein the method comprises the following steps: the mass fraction of the water phase monomer in the step 1) is 0.2 wt%; pH of the aqueous solution is 10; the soaking time was 4 min.
5. The method for preparing the nanofiltration membrane modified by the carbonic acid lactone with high flux and high rejection rate as claimed in claim 1, wherein the method comprises the following steps: the acyl chloride monomer in the step 2) can comprise one or more of isophthaloyl dichloride, terephthaloyl dichloride, phthaloyl dichloride, poly-aromatic sulfonyl chloride and derivatives thereof.
6. The method for preparing the nanofiltration membrane modified by the carbonic acid lactone with high flux and high rejection rate as claimed in claim 1, wherein the method comprises the following steps: the organic phase solvent in the step 2) is one or a mixture of more of n-hexane, cyclohexane, toluene, benzene and ethyl acetate.
7. The method for preparing the nanofiltration membrane modified by the carbonic acid lactone with high flux and high rejection rate as claimed in claim 1, wherein the method comprises the following steps: the mass fraction of the organic phase acyl chloride monomer in the step 2) is 0.1 wt%; the soaking time is 1 min; the heat treatment temperature is 60 deg.C, and the time is 15 min.
8. The method for preparing the nanofiltration membrane modified by the carbonic acid lactone with high flux and high rejection rate as claimed in claim 1, wherein the method comprises the following steps: the carbonic acid lactone monomer in the step 3) can comprise one or more of beta-propiolactone, beta-butyrolactone, gamma-valerolactone, delta-valerolactone, gamma-caprolactone, delta-caprolactone, epsilon-caprolactone, 4-heptalactone, 5-octalactone, gamma-octalactone, 5-nonalactone, gamma-nonalactone, delta-decalactone, delta-undecalactone, gamma-dodecalactone, delta-tridecanolactone, delta-tetradecanolide and cyclopentadecanolide.
9. The method for preparing the nanofiltration membrane modified by the carbonic acid lactone with high flux and high rejection rate as claimed in claim 1, wherein the method comprises the following steps: the concentration of the solution of the carbonic acid lactone monomer in the step (3) is 0.08-0.8 mol/L, and the solvent is ethanol; the area of the polyamide nanofiltration membrane is a circle with the diameter of 6 cm; the modification temperature is 25-60 ℃, and the modification time is 8 h.
10. A carbonic acid lactone modified high-flux high-rejection nanofiltration membrane prepared by the preparation method of any one of claims 1 to 9.
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| CN114950165A (en) * | 2022-05-23 | 2022-08-30 | 天津工业大学 | Preparation method of high-pressure reverse osmosis membrane based on gamma-valerolactone interface auxiliary polymerization |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114950165A (en) * | 2022-05-23 | 2022-08-30 | 天津工业大学 | Preparation method of high-pressure reverse osmosis membrane based on gamma-valerolactone interface auxiliary polymerization |
| CN114950165B (en) * | 2022-05-23 | 2023-10-13 | 天津工业大学 | Preparation method of high-pressure reverse osmosis membrane based on gamma-valerolactone interface assisted polymerization |
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