CN113244781A - Anti-yellowing composite reverse osmosis membrane and preparation method thereof - Google Patents
Anti-yellowing composite reverse osmosis membrane and preparation method thereof Download PDFInfo
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- CN113244781A CN113244781A CN202110533266.2A CN202110533266A CN113244781A CN 113244781 A CN113244781 A CN 113244781A CN 202110533266 A CN202110533266 A CN 202110533266A CN 113244781 A CN113244781 A CN 113244781A
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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
- B01D69/02—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
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0006—Organic membrane manufacture by chemical reactions
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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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- 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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic 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
- 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 relates to a preparation method and application of an anti-yellowing composite reverse osmosis membrane, wherein poly (ethylene glycol dimethacrylate (EGMA)/isobutoxy acrylamide (IBMA)/Acrylamide (AM)) ternary anti-yellowing copolymer particles are synthesized, the ternary anti-yellowing copolymer particles are fixed in an ultrafiltration membrane, IBMA is added in an interfacial polymerization process to form two anti-yellowing layers, and the IBMA can be crosslinked with polybasic acyl chloride or self to form a flexible network in the interfacial polymerization process to improve the stability of a desalting layer. The test result shows that compared with the existing reverse osmosis membrane, the anti-yellowing composite reverse osmosis membrane prepared by the invention has the advantages of excellent anti-yellowing performance, longer service life, higher flux and higher desalting performance.
Description
Technical Field
The invention relates to the technical field of separation membranes, in particular to a preparation method and application of an anti-yellowing composite reverse osmosis membrane.
Background
Membrane separation techniques are currently widely used in a variety of water treatment problems. According to requirements, the method is divided into microfiltration, ultrafiltration, nanofiltration and reverse osmosis. Reverse osmosis membranes (RO membranes) are currently the most widely and promising Membrane products in the field of Membrane separation.
The reverse osmosis membrane is formed by an interfacial polymerization process on the surface of an ultrafiltration membrane, the membrane surface of a reverse osmosis membrane product can be yellowed due to the excessive amino and acyl chloride in interfacial polymerization, the deeper the color is along with the prolonging of the service time, the service life of the membrane is shortened, the appearance of the membrane is influenced, and the application and the popularization of the reverse osmosis membrane in different fields are limited.
Therefore, there is a strong need for anti-yellowing reverse osmosis membranes and techniques for making the same.
Disclosure of Invention
In order to solve the problem of yellowing in the preparation and use processes of the reverse osmosis membrane, in the manufacturing process of the composite reverse osmosis membrane, anti-yellowing particles (IBMA) are introduced into an ultrafiltration layer and an interfacial polymerization layer simultaneously. By synthesizing a hydrophilic anti-yellowing copolymer, in particular to a poly (ethylene glycol dimethacrylate (EGMA)/isobutoxy acrylamide (IBMA)/Acrylamide (AM)) terpolymer, the synthesized terpolymer is added into a polysulfone ultrafiltration layer, and IBMA is added in the interfacial polymerization process to form a two-layer anti-yellowing system, so that the anti-yellowing and hydrophilic properties of the reverse osmosis membrane are greatly improved.
An anti-yellowing composite reverse osmosis membrane and a preparation method thereof comprise the following steps:
(1) adding IBMA, EGMA and AM into xylene solvent, ultrasonically stirring and uniformly stirring at 25 ℃, adding an initiator, vacuumizing, stirring and reacting at 80 ℃ for 8 hours, and centrifugally separating after reaction to obtain anti-yellowing copolymer particles poly (IBMA-EGMA-AM);
the IBMA, the EGMA, the AM and the initiator are in the mass ratio of: (1-3): (0.5-2): (1-2): (0.005: 0.008);
the initiator is one of Azobisisobutyronitrile (AIBN), Azobisisoheptonitrile (ABVN) and dibenzoyl peroxide (BPO).
(2) Sequentially adding resin, a pore-forming agent, an additive and the anti-yellowing copolymer particles prepared in the step (1) into a solvent, mixing and stirring uniformly at 65 ℃, and defoaming to obtain a casting solution;
the casting solution comprises the following components in percentage by mass; anti-yellowing copolymer particles (0-3%), resin (11-20%), pore-forming agent (0.5-2.5%), additive (0.3-1.5%) and solvent (75-88%);
the resin is one of polyvinylidene fluoride (PVDF), Polysulfone (PSF) and polyvinyl chloride (PVC);
the pore-foaming agent is one of PVPK30, PVPK60, PVPK90, PEG200, PEG400, PEG600, PEG800 and triethyl phosphate;
the additive is one of tween 85, sodium dodecyl benzene sulfonate, cetyl trimethyl ammonium bromide and sorbitan fatty acid.
The solvent is dimethyl acetamide (DMAc), dimethyl formamide (DMF) and N-methyl pyrrolidone.
(3) And (3) uniformly inverting the casting solution prepared in the step (2) on a non-woven fabric, scraping the membrane by using a scraper, placing the membrane in ultrapure water for phase separation, and obtaining the functional ultrafiltration membrane after the phase separation.
(4) Immersing the functional ultrafiltration membrane prepared in the step (3) into the water phase solution for 15s-60s, draining the solution by using a rubber roller, immersing the solution into the oil phase solution for 15s-60s, taking out the solution, and performing heat treatment to obtain the anti-yellowing composite reverse osmosis membrane;
the aqueous phase solution comprises the following components in percentage by mass; IBMA (0-3%), monomer (2.5%), triethylamine (0.15%), camphorsulfonic acid (0.25%);
the monomer in the aqueous phase solution is one of p-phenylenediamine, m-phenylenediamine and o-phenylenediamine;
the oil phase solution comprises the following raw material components in percentage by mass; 0.08% terephthaloyl chloride in ISOPAR G.
The heat treatment temperature is 75 ℃, and the time is 5min-10 min.
The technical scheme adopted by the invention has the following beneficial effects:
firstly, compared with the common reverse osmosis membrane, the anti-yellowing composite reverse osmosis membrane prepared by the invention has longer service life, can not be yellowed after being used for a long time, and the synthesized anti-yellowing copolymer particles also have higher hydrophilicity, thereby improving the hydrophilicity of the membrane. And secondly, the anti-yellowing particles IBMA introduced by the invention can form a flexible network by self-crosslinking in interfacial polymerization, so that the polyamide desalting layer is protected, and the risk of skin layer falling off in the use process is reduced.
Drawings
FIG. 1 shows the anti-yellowing composite reverse osmosis membrane surface prepared by the present invention
FIG. 2 shows the surface of a reverse osmosis membrane prepared in comparative example
Detailed Description
The following provides a specific embodiment of an anti-yellowing composite reverse osmosis membrane of the present invention.
Example 1
Adding IBMA, EGMA and AM with the mass ratio of 2:1:1 into a solvent xylene, ultrasonically stirring and uniformly stirring at 25 ℃, adding an initiator AIBN with the mass ratio of 0.005, vacuumizing, stirring and reacting at 80 ℃ for 8 hours, and centrifugally separating after reaction to obtain the anti-yellowing copolymer particles.
Adding 2% of anti-yellowing copolymer particles, 15% of PVDF, 1% of PVP K30 and 0.5% of Tween 85 into 81.5% of DMAc solution, mixing and stirring uniformly at 65 ℃, and defoaming to obtain the casting solution.
And uniformly inverting the membrane casting solution on a non-woven fabric, scraping the membrane by using a scraper, placing the membrane in ultrapure water for phase separation, and obtaining the functional ultrafiltration membrane after the phase separation.
Immersing the functional ultrafiltration membrane into the water phase solution for 30s, wherein the mass percent of each component is 2% of IBMA, 2.5% of m-phenylenediamine, 0.15% of triethylamine and 0.25% of camphorsulfonic acid, draining by using a rubber roller, immersing into the ISOPAR G oil phase solution of 0.08% of terephthaloyl chloride for 30s, taking out, and carrying out heat treatment at 75 ℃ for 5min to obtain the anti-yellowing composite reverse osmosis membrane.
Example 2
An anti-yellowing composite reverse osmosis membrane was obtained in the same manner as in example 1, except that the mass ratio of IBMA, EGMA and AM was adjusted to 3:2: 1.
Example 3
An anti-yellowing composite reverse osmosis membrane was obtained in the same manner as in example 1, except that the mass ratio of IBMA, EGMA and AM was adjusted to 1:2: 2.
Example 4
The anti-yellowing copolymer particles were prepared as in example 1.
Adding 3% of anti-yellowing copolymer particles, 17% of PSF, 1.5% of PVP K60 and 0.5% of Tween 85 into 81.5% of DMAc solution, mixing and stirring uniformly at 65 ℃, and defoaming to obtain the casting solution.
And uniformly inverting the membrane casting solution on a non-woven fabric, scraping the membrane by using a scraper, placing the membrane in ultrapure water for phase separation, and obtaining the functional ultrafiltration membrane after the phase separation.
The procedure of preparing the anti-yellowing composite reverse osmosis membrane was the same as in example 1.
Example 5
The anti-yellowing copolymer particles were prepared as in example 1.
0.5 percent of anti-yellowing copolymer particles, 19 percent of PSF, 1.5 percent of PVP K60 and 0.5 percent of sodium dodecyl benzene sulfonate are added into 78.5 percent of DMAc solution, and the mixture is mixed and stirred uniformly at 65 ℃ and defoamed to obtain casting solution.
And uniformly inverting the membrane casting solution on a non-woven fabric, scraping the membrane by using a scraper, placing the membrane in ultrapure water for phase separation, and obtaining the functional ultrafiltration membrane after the phase separation.
The procedure of preparing the anti-yellowing composite reverse osmosis membrane was the same as in example 1.
Example 6
The anti-yellowing copolymer particles and the functional ultrafiltration membrane were prepared in the same manner as in example 1.
Immersing the functional ultrafiltration membrane into the water phase solution for 20s, wherein the mass percent of each component is 3 percent of IBMA, 2.5 percent of p-phenylenediamine, 0.15 percent of triethylamine and 0.25 percent of camphorsulfonic acid, draining the components by using a rubber roller, immersing the components into the ISOPAR G oil phase solution of 0.08 percent of p-trichloro chloride for 30s, taking out the components, and carrying out heat treatment at 75 ℃ for 8min to obtain the anti-yellowing composite reverse osmosis membrane.
Example 7
The anti-yellowing copolymer particles and the functional ultrafiltration membrane were prepared in the same manner as in example 1.
Immersing the functional ultrafiltration membrane into the water phase solution for 20s, wherein the mass percent of each component is 1 percent of IBMA, 2.5 percent of p-phenylenediamine, 0.15 percent of triethylamine and 0.25 percent of camphorsulfonic acid, draining the components by using a rubber roller, immersing the components into the ISOPAR G oil phase solution of 0.08 percent of p-trichloro chloride for 30s, taking out the components, and carrying out heat treatment at 75 ℃ for 10min to obtain the anti-yellowing composite reverse osmosis membrane.
Comparative example 1
Adding 15% of PVDF, 1% of PVP K30 and 0.5% of Tween 85 into 83.5% of DMAc solution, mixing and stirring uniformly at 65 ℃, and defoaming to obtain the casting solution.
And uniformly inverting the membrane casting solution on a non-woven fabric, scraping the membrane by using a scraper, placing the membrane in ultrapure water for phase separation, and obtaining the ultrafiltration membrane after the phase separation.
Immersing an ultrafiltration membrane into the water phase solution for 30s, wherein the mass percent of each component is 2% of IBMA, 2.5% of m-phenylenediamine, 0.15% of triethylamine and 0.25% of camphorsulfonic acid, draining by using a rubber roller, immersing into the ISOPAR G oil phase solution of 0.08% of terephthaloyl chloride for 30s, taking out, and carrying out heat treatment at 75 ℃ for 5min to obtain the reverse osmosis membrane.
Comparative example 2
Adding 15% of PVDF, 1% of PVP K30 and 0.5% of Tween 85 into 83.5% of DMAc solution, mixing and stirring uniformly at 65 ℃, and defoaming to obtain the casting solution.
And uniformly inverting the membrane casting solution on a non-woven fabric, scraping the membrane by using a scraper, placing the membrane in ultrapure water for phase separation, and obtaining the ultrafiltration membrane after the phase separation.
Immersing an ultrafiltration membrane into the water phase solution for 30s, wherein the components comprise 2.5 percent of m-phenylenediamine, 0.15 percent of triethylamine and 0.25 percent of camphorsulfonic acid in percentage by mass, draining the components by using a rubber roller, immersing the components into the ISOPAR G oil phase solution of 0.08 percent of terephthaloyl chloride for 30s, taking out the components, and carrying out heat treatment at 75 ℃ for 5min to obtain the reverse osmosis membrane.
The membrane performance test in the examples and comparative examples was carried out under the conditions of pH 7 to 8, concentration of NaCl aqueous solution 2000ppm, pressure 1.55mpa, temperature 25 ℃ and degree of yellowing as measured by the membrane service time.
TABLE 1 flux, salt rejection and degree of yellowing of example and comparative reverse osmosis membranes
As can be seen from table 1: the anti-yellowing composite reverse osmosis membrane prepared by the method has excellent anti-yellowing performance in the use process, performance reduction and yellowing cannot occur after long-time use, and the hydrophilic performance of the copolymer particles and the self-crosslinking of IBMA also improve the flux, the desalting performance and the stability of a desalting layer.
The foregoing is illustrative of the preferred embodiments of the present invention, and it is to be understood that the invention is not limited thereto, and that various modifications and enhancements which fall within the spirit and scope of the invention are possible.
Claims (12)
1. A preparation method and application of an anti-yellowing composite reverse osmosis membrane are characterized in that: the method comprises the following steps:
(1) adding isobutoxy acrylamide (IBMA), ethylene glycol dimethacrylate (EGMA) and Acrylamide (AM) monomers into a solvent xylene, ultrasonically stirring and uniformly stirring at 25 ℃, adding an initiator, vacuumizing, stirring and reacting at 80 ℃ for 8 hours, and centrifugally separating after reaction to obtain anti-yellowing copolymer particles poly (IBMA-EGMA-AM);
(2) sequentially adding resin, a pore-forming agent, an additive and the anti-yellowing copolymer particles prepared in the step (1) into a solvent, mixing and stirring uniformly at 65 ℃, and defoaming to obtain a casting solution;
(3) uniformly inverting the casting film liquid prepared in the step (2) on a non-woven fabric, scraping the film by using a scraper, and then placing the film in ultrapure water for phase separation to obtain a functional ultrafiltration membrane;
(4) immersing the functional ultrafiltration membrane prepared in the step (3) into the water phase solution for 15s-60s, draining the solution by using a rubber roller, immersing the membrane into the oil phase solution for 15s-60s, taking out the membrane, and performing heat treatment to obtain the anti-yellowing composite reverse osmosis membrane.
2. The method of claim 1, wherein: in the step (1), the IBMA, the EGMA, the AM and the initiator are in the mass ratio of: (1-3): (0.5-2): (1-2): (0.005:0.008).
3. The method of claim 1, wherein: the components in the casting solution in the step (1) are in percentage by mass; anti-yellowing copolymer particles (0-3%), resin (11-20%), pore-forming agent (0.5-2.5%), additive (0.3-1.5%) and solvent (75-88%).
4. The method of claim 1, wherein: in the step (1), the initiator is one of Azobisisobutyronitrile (AIBN), Azobisisoheptonitrile (ABVN) and dibenzoyl peroxide (BPO).
5. The method of claim 1, wherein: in the step (2), the resin is one of polyvinylidene fluoride (PVDF), Polysulfone (PSF) and polyvinyl chloride (PVC).
6. The method of claim 1, wherein: in the step (2), the pore-foaming agent is one of PVPK30, PVPK60, PVPK90, PEG200, PEG400, PEG600, PEG800 and triethyl phosphate.
7. The method of claim 1, wherein: in the step (2), the additive is one of tween 85, sodium dodecyl benzene sulfonate, cetyl trimethyl ammonium bromide and sorbitan fatty acid.
8. The method of claim 1, wherein: in the step (2), the solvent is dimethyl acetamide (DMAc), dimethyl formamide (DMF) or N-methyl pyrrolidone.
9. The method of claim 1, wherein: the composition of the aqueous phase solution in the step (4) comprises the components according to mass percentage; IBMA (0-3%), monomer (2.5%), triethylamine (0.15%), camphorsulfonic acid (0.25%).
10. The method of claim 1, wherein: in the step (4), the monomer in the aqueous phase solution is one of p-phenylenediamine, m-phenylenediamine and o-phenylenediamine.
11. The method of claim 1, wherein: in the step (4), the oil phase solution comprises the following raw material components in percentage by mass; 0.08% terephthaloyl chloride in ISOPAR G.
12. The method of claim 1, wherein: in the step (4), the heat treatment temperature is 75 ℃ and the time is 5-10 min.
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