CN108392991B - Polyamide composite forward osmosis membrane for wastewater desalination - Google Patents
Polyamide composite forward osmosis membrane for wastewater desalination Download PDFInfo
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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
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
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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
- B01D69/10—Supported membranes; Membrane supports
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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
- C02F1/445—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by forward osmosis
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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 provides a high-flux polyamide forward osmosis membrane for wastewater desalination, which is characterized in that a composite polyamide forward osmosis membrane with a sandwich structure and an asymmetric structure is designed, namely a high-flux polyamide separation layer and a high-selectivity polyamide separation layer are respectively designed on two sides of a polysulfone supporting layer, and then polydopamine modification is carried out on a polysulfone surface of an interfacial polymerization high-selectivity polyamide membrane, so that the water flux of the membrane is remarkably improved on the basis of ensuring that solutes in a raw material liquid do not enter the supporting layer, and the types of water phase monomers and oil phase monomers of a double-layer polyamide separation layer are selected to ensure the optimal membrane performance.
Description
Technical Field
The application relates to a forward osmosis membrane, in particular to a forward osmosis membrane for wastewater desalination.
Background
In 2015 8 months, 2040 years of national water resource pressure ranking was released by the world resource institute, and China is expected to change from a medium water resource pressure country to a very high water resource pressure country.
As an important support technology in the field of water treatment, membrane-process water treatment technologies such as Microfiltration (MF), Ultrafiltration (UF), Nanofiltration (NF), Reverse Osmosis (RO) and the like have more commercial applications through long-term development, and play a role of great importance in the field of water treatment. The forward osmosis technology, as a key technology of a novel 'zero emission' technology, is widely concerned by domestic and foreign scholars because of the advantages of low energy consumption, small membrane pollution, high water recovery rate and the like.
Forward osmosis refers to the process by which water flows from the lower osmotic pressure side through a perm-selective membrane to the higher osmotic pressure side. Compared with the nanofiltration and reverse osmosis membrane materials commonly used for desalination, the forward osmosis technology has the advantages of low energy consumption, difficult membrane pollution, easy cleaning and long service life, and is continuously concerned by domestic and foreign scholars in recent years. An ideal forward osmosis membrane should have a denser separation layer and a transporting support layer to reduce concentration polarization phenomena inside the membrane. While the internal concentration polarization occurring inside the support layer reduces the membrane permeation driving force. In order to solve this problem, it is common to reduce the thickness of the membrane so as to expect the maximum reduction of concentration polarization limitation, but the reduction of the thickness of the support layer brings about the reduction of the membrane strength, and the reduction of the thickness of the separation layer brings about the reduction of the selectivity. There have also been studies to propose a symmetrical sandwich structure using double layers which can reduce the degree of concentration polarization in the membrane by blocking the solute in the feed solution from entering the support, but the flux is not optimistic because it has one more separation layer than the conventional forward osmosis membrane.
Disclosure of Invention
Aiming at the problem of concentration polarization in the membrane, the invention provides a forward osmosis membrane, which is designed by a special membrane layer to reduce the concentration polarization phenomenon and ensure the flux of the membrane to the maximum extent.
The invention provides a polyamide forward osmosis membrane for desalting high-flux wastewater, which is characterized in that: the forward osmosis membrane comprises a polysulfone support layer and polyamide separation layers on both sides of the polysulfone support layer, the polyamide separation layers comprising a high flux polyamide separation layer facing the feed side and a high selectivity polyamide separation layer facing the permeate side during application. Wherein the high flux polyamide separation layer has a higher water flux than the high selectivity polyamide separation layer, and the high selectivity polyamide separation layer has a higher selectivity than the high flux polyamide separation layer. Preferably, the high selectivity polyamide separation layer is formed by modifying the polysulfone support layer side to be bonded to the high selectivity polyamide separation layer with polydopamine and then interfacially polymerizing the modified polydopamine.
Preferably, the high-throughput polyamide separation layer and the high-selectivity polyamide separation layer are prepared by an interfacial polymerization method.
Preferably, the high-flux polyamide membrane is prepared by interfacial polymerization of pyromellitic chloride and piperazine.
Preferably, the high-selectivity polyamide separation layer is prepared by interfacial polymerization of trimesoyl chloride and m-phenylenediamine.
The invention also provides a method for synthesizing the polyamide composite forward osmosis membrane for wastewater desalination, which is characterized by comprising the following steps:
(1) dissolving 15-20wt% of polysulfone in N, N-dimethylacetamide, adding 4-12wt% of polyethylene glycol-400, heating and stirring to completely dissolve the polysulfone, standing and defoaming at room temperature for 24 hours to obtain a casting solution, casting the casting solution on a clean glass plate by using a scraper, standing in air for 12 hours, rapidly and horizontally placing in a coagulating bath for gelling for 1 hour, and taking out to obtain a polysulfone supporting layer;
(2) dissolving polydopamine (0.01-0.05 wt%) in tris-HCl solution to form polydopamine modified solution, and soaking the B side of the polysulfone supporting layer in the polydopamine modified solution for 3-6h to modify the B side of the polysulfone supporting layer;
(3) dissolving a certain amount of piperazine, m-phenylenediamine, sodium hydroxide and sodium dodecyl sulfate in deionized water, and uniformly stirring to form a first water phase monomer; dissolving a certain amount of pyromellitic dianhydride and isophthaloyl dichloride in an alkane solvent, and uniformly stirring to form a first oil phase monomer; dissolving a certain amount of m-phenylenediamine, sodium hydroxide and sodium dodecyl sulfate in deionized water, and uniformly stirring to form a second water phase monomer; dissolving a certain amount of trimesoyl chloride in an alkane solvent, and uniformly stirring to form a second oil phase monomer;
(4) immersing the side A of the polysulfone supporting layer into a first water phase monomer for 2-5s, then taking out, removing the redundant solution on the surface, then continuously immersing the side A into a first oil phase monomer, taking out after 2-5s, and drying to generate a high-flux polyamide layer;
(5) and (3) immersing the side B of the polysulfone supporting layer into a second water phase monomer for 5-10s, then taking out, removing the redundant solution on the surface, then continuously immersing the side B into a second oil phase monomer, taking out after 5-10s, and drying to generate the high-selectivity polyamide layer.
Preferably, the first aqueous phase monomer contains 1-2wt% of piperazine, 0.5-1wt% of m-phenylenediamine, 0.3-1wt% of sodium hydroxide and 0.1-0.5% of sodium dodecyl sulfate; the first oil phase monomer contains 2-3wt% of pyromellitic chloride and 1-2wt% of isophthaloyl dichloride.
Preferably, the second aqueous phase monomer contains 1-4wt% of m-phenylenediamine, 0.3-1wt% of sodium hydroxide and 0.1-0.5% of sodium dodecyl sulfate; the monomer of the second oil phase contains 1-3wt% of trimesoyl chloride.
Technical effects
1. A polyamide membrane layer is polymerized on the interfaces of both sides of the polysulfone supporting layer, so that solute in the raw material liquid is effectively prevented from entering the supporting layer, and the concentration polarization degree in the supporting layer is reduced.
2. In order to reduce the flux reduction problem brought by the double-layer separation layer, the invention designs a high-flux polyamide separation layer on the raw material facing side and a high-selectivity polyamide separation layer on the permeation facing side. The polyamide layers on both sides of the support layer have different permeability properties, compared to the high flux polyamide separation layer, which has higher flux and poorer selectivity, while the high selectivity polyamide layer has higher selectivity and lower flux. Therefore, compared with a double-skin layer with a symmetrical structure, the invention can also block solute in the raw material liquid from entering the supporting layer by replacing a compact separation layer with a high-flux separation layer, and also obviously improves the flux of the membrane. It is noted that the presence of a high flux polyamide layer results in a significant increase in flux, relative to a single polyamide separation layer, while the total thickness of the separation layer remains constant.
3. In the design of the high-flux polyamide layer and the high-selectivity polyamide layer, the monomer types for synthesizing the high-flux polyamide layer and the high-selectivity polyamide layer are optimally selected, the conventionally adopted water-phase monomers of piperazine, m-phenylenediamine, ethylenediamine, p-phenylenediamine, polyethyleneimine, polyvinyl alcohol, bisphenol A and oil-phase monomers of isophthaloyl dichloride, terephthaloyl dichloride, trimesoyl chloride and pyromellitic tetrachloryl chloride are respectively considered in a specific cross experiment, and the optimal oil-phase monomer and water-phase monomer adopted by the double-layer polyamide separation layer are selected on the basis of comprehensively considering the permeation selectivity, the flux and the stability.
4. The invention also carries out polydopamine modification on one side of the polysulfone supporting layer polymerized high-selectivity permeable membrane, which improves the hydrophilicity of the membrane on one hand, and the polydopamine and aqueous monomer amine react to improve the binding force between the membrane and the polysulfone supporting layer. On the other hand, when five parts, namely the modified end face, namely the surface of the high-flux polyamide separation layer, the surface A of the polysulfone supporting layer (one surface of the polymerized high-flux polyamide separation layer), the surface B of the polysulfone supporting layer (one surface of the polymerized high-selectivity polyamide separation layer), the surface of the high-selectivity polyamide separation layer and the whole polysulfone supporting layer are examined, the water flux of the membrane can be improved only when the surface B of the polysulfone supporting layer is modified, but the water flux is not increased reversely when the surfaces of the high-flux polyamide separation layer and the polysulfone supporting layer are modified, and the flux is not obviously improved after the whole polysulfone supporting layer is modified, so that the transmission of water in the polysulfone supporting layer is inhibited when the surface of the high-flux polyamide separation layer, the surface A of the polysulfone supporting layer and the whole polysulfone supporting layer are subjected to hydrophilic modification, and the modified water flux of the high-selectivity polyamide separation, aggravate the concentration polarization degree outside the permeation side and reduce the power source for water to pass through.
Detailed Description
In order to make the technical means, innovative features, objectives and functions realized by the present invention easy to understand, the present invention is further described below.
Example 1
(1) Dissolving 20wt% of polysulfone in N, N-dimethylacetamide, adding 8wt% of polyethylene glycol-400, heating and stirring to completely dissolve the polysulfone, standing and defoaming at room temperature for 24 hours to obtain a casting solution, casting the casting solution on a clean glass plate by using a scraper, standing in air for 12 hours, rapidly and horizontally placing in a coagulating bath for gelling for 1 hour, and taking out to obtain a polysulfone supporting layer;
(2) dissolving 2wt% of piperazine, 0.5wt% of m-phenylenediamine, 0.5wt% of sodium hydroxide and 0.2wt% of sodium dodecyl sulfate in deionized water, and uniformly stirring to form a first water phase monomer; dissolving 2wt% of pyromellitic dianhydride and 2wt% of isophthaloyl dichloride in an alkane solvent, and uniformly stirring to form a first oil phase monomer; dissolving 4wt% of m-phenylenediamine, 0.5wt% of sodium hydroxide and 0.2wt% of sodium dodecyl sulfate in deionized water, and uniformly stirring to form a second water phase monomer; dissolving a certain amount of trimesoyl chloride in an alkane solvent, and uniformly stirring to form a second oil phase monomer;
(3) immersing the side A of the polysulfone supporting layer into a first water phase monomer for 2s, then taking out, removing the redundant solution on the surface, then continuously immersing the side A into a first oil phase monomer, and taking out and drying after 2s to generate a high-flux polyamide layer;
(4) immersing the side B of the polysulfone supporting layer into a second water phase monomer for 5s, then taking out, removing the surface redundant solution, then continuously immersing the side B into a second oil phase monomer, and taking out and drying after 5s to generate a high-selectivity polyamide layer so as to prepare the forward osmosis membrane;
(5) and washing unreacted materials in the forward osmosis membrane by deionized water, and carrying out performance characterization after continuing soaking for 24 hours.
The prepared forward osmosis membrane takes 0.1mol/L sodium chloride as raw material liquid and 4mol/L glucose solution as drawing liquid, and the flux measured at room temperature is 15 L.m2Per hour, the rejection rate of sodium chloride is 99.4%.
Comparative example 1
This comparative example was prepared in a manner substantially similar to that of example 1, except that the first aqueous phase monomer and the second aqueous phase monomer were each 4wt% of m-phenylenediamine, 0.5wt% of sodium hydroxide and 0.2wt% of sodium dodecylsulfate dissolved in deionized water and stirred uniformly; the first oil phase monomer and the second oil phase monomer are both formed by dissolving a certain amount of trimesoyl chloride in an alkane solvent and uniformly stirring.
The prepared forward osmosis membrane takes 0.1mol/L sodium chloride as raw material liquid and 4mol/L glucose solution as drawing liquid, and the flux measured at room temperature is 9.8 L.m2Per hour, the rejection rate of sodium chloride is 99.5%.
Example 2
(1) Dissolving 20wt% of polysulfone in N, N-dimethylacetamide, adding 8wt% of polyethylene glycol-400, heating and stirring to completely dissolve the polysulfone, standing and defoaming at room temperature for 24 hours to obtain a casting solution, casting the casting solution on a clean glass plate by using a scraper, standing in air for 12 hours, rapidly and horizontally placing in a coagulating bath for gelling for 1 hour, and taking out to obtain a polysulfone supporting layer;
(2) dissolving polydopamine in a tris-HCl solution to form polydopamine modified liquid, and soaking the side B of a polysulfone supporting layer in the polydopamine modified liquid for 3 hours to modify the side B of the polysulfone supporting layer, wherein the pH of the tris-HCl solution is 8.5, and the mass concentration of the polydopamine is 0.04 wt%;
(3) dissolving 2wt% of piperazine, 0.5wt% of m-phenylenediamine, 0.5wt% of sodium hydroxide and 0.2wt% of sodium dodecyl sulfate in deionized water, and uniformly stirring to form a first water phase monomer; dissolving 2wt% of pyromellitic dianhydride and 2wt% of isophthaloyl dichloride in an alkane solvent, and uniformly stirring to form a first oil phase monomer; dissolving 4wt% of m-phenylenediamine, 0.5wt% of sodium hydroxide and 0.2wt% of sodium dodecyl sulfate in deionized water, and uniformly stirring to form a second water phase monomer; dissolving a certain amount of trimesoyl chloride in an alkane solvent, and uniformly stirring to form a second oil phase monomer;
(4) immersing the side A of the polysulfone supporting layer into a first water phase monomer for 2s, then taking out, removing the redundant solution on the surface, then continuously immersing the side A into a first oil phase monomer, and taking out and drying after 2s to generate a high-flux polyamide layer;
(5) immersing the side B of the polysulfone supporting layer into a second water phase monomer for 5s, then taking out, removing the surface redundant solution, then continuously immersing the side B into a second oil phase monomer, and taking out and drying after 5s to generate a high-selectivity polyamide layer so as to prepare the forward osmosis membrane;
(6) and washing unreacted materials in the forward osmosis membrane by deionized water, and carrying out performance characterization after continuing soaking for 24 hours.
The flux measured at room temperature of the prepared forward osmosis membrane by using 0.1mol/L sodium chloride as a raw material solution and 4mol/L glucose solution as an absorption solution is 26.9 L.m2Per hour, the rejection rate of sodium chloride is 99.3%.
Comparative example 2
This comparative example was prepared substantially similarly to example 2, except that the polydopamine modification in step (2) was performed on the a-side of the polysulfone support layer.
The prepared forward osmosis membrane takes 0.1mol/L sodium chloride as raw material liquid and 4mol/L glucose solution as drawing liquid, and the flux measured at room temperature is 11.2 L.m2Per hour, the rejection rate of sodium chloride is 99.3%.
Comparative example 3
This comparative example was prepared in a substantially similar manner to example 2, except that the polydopamine modification in step (2) was performed on both sides of the polysulfone support layer.
Taking 0.1mol/L sodium chloride as raw material liquid and 4mol/L glucose solution as drawing liquid for the prepared forward osmosis membraneA flux measured at room temperature of 16.1 L.m2Per hour, the rejection rate of sodium chloride is 99.4%.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (4)
1. A polyamide composite forward osmosis membrane for wastewater desalination is characterized in that: the forward osmosis membrane comprises a polysulfone supporting layer and polyamide separation layers positioned on two sides of the polysulfone supporting layer, wherein the polyamide separation layers comprise a high-flux polyamide separation layer facing a raw material side and a high-selectivity polyamide separation layer facing a permeation side in an application process, and one side of the polysulfone supporting layer attached to the high-selectivity polyamide separation layer is subjected to polydopamine modification and then is subjected to interfacial polymerization to form the high-selectivity polyamide separation layer; the high-flux polyamide separation layer and the high-selectivity polyamide separation layer are prepared by an interfacial polymerization method; the high-flux polyamide membrane is formed by interfacial polymerization of a mixed oil phase monomer of pyromellitic dianhydride and isophthaloyl dichloride and a mixed water phase monomer of piperazine and m-phenylenediamine; the high-selectivity polyamide separation layer is formed by interfacial polymerization of trimesoyl chloride and m-phenylenediamine.
2. A method for synthesizing the polyamide composite forward osmosis membrane for wastewater desalination according to claim 1, characterized by comprising the steps of:
(1) dissolving 15-20wt% of polysulfone in N, N-dimethylacetamide, adding 4-12wt% of polyethylene glycol-400, heating and stirring to completely dissolve the polysulfone, standing and defoaming at room temperature for 24 hours to obtain a casting solution, casting the casting solution on a clean glass plate by using a scraper, standing in air for 12 hours, rapidly and horizontally placing in a coagulating bath for gelling for 1 hour, and taking out to obtain a polysulfone supporting layer;
(2) dissolving polydopamine in a tris-HCl solution to form polydopamine modified liquid, and soaking the side B of the polysulfone supporting layer in the polydopamine modified liquid for 3-6 hours to modify the side B of the polysulfone supporting layer;
(3) dissolving a certain amount of piperazine, m-phenylenediamine, sodium hydroxide and sodium dodecyl sulfate in deionized water, and uniformly stirring to form a first water phase monomer; dissolving a certain amount of pyromellitic dianhydride and isophthaloyl dichloride in an alkane solvent, and uniformly stirring to form a first oil phase monomer; dissolving a certain amount of m-phenylenediamine, sodium hydroxide and sodium dodecyl sulfate in deionized water, and uniformly stirring to form a second water phase monomer; dissolving a certain amount of trimesoyl chloride in an alkane solvent, and uniformly stirring to form a second oil phase monomer;
(4) immersing the side A of the polysulfone supporting layer into a first water phase monomer for 2-5s, then taking out, removing the redundant solution on the surface, then continuously immersing the side A into a first oil phase monomer, taking out after 2-5s, and drying to generate a high-flux polyamide layer;
(5) and (3) immersing the side B of the polysulfone supporting layer into a second water phase monomer for 5-10s, then taking out, removing the redundant solution on the surface, then continuously immersing the side B into a second oil phase monomer, taking out after 5-10s, and drying to generate the high-selectivity polyamide layer.
3. The method according to claim 2, wherein the first aqueous phase monomer comprises 1-2wt% of piperazine and 0.5-1wt% of m-phenylenediamine, 0.3-1wt% of sodium hydroxide and 0.1-0.5% of sodium dodecyl sulfonate; the first oil phase monomer contains 2-3wt% of pyromellitic chloride and 1-2wt% of isophthaloyl dichloride.
4. The method according to claim 2, wherein the second aqueous phase monomer comprises 1 to 4wt% of m-phenylenediamine, 0.3 to 1wt% of sodium hydroxide, and 0.1 to 0.5wt% of sodium dodecylsulfate; the monomer of the second oil phase contains 1-3wt% of trimesoyl chloride.
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| CN109603577B (en) * | 2018-12-25 | 2021-03-19 | 大连海事大学 | Method for preparing forward osmosis membrane with reserved draw solute and double active layers |
| CN112516821B (en) * | 2020-11-18 | 2022-07-22 | 西安科技大学 | Dopamine and polyvinyl alcohol composite modified polysulfone forward osmosis membrane, preparation method and application |
| CN112808020B (en) * | 2020-12-31 | 2022-08-02 | 华中科技大学 | Forward osmosis base membrane with optimized surface charge on side of drawing solution and preparation method thereof |
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| CN103432913B (en) * | 2013-08-05 | 2015-08-19 | 株洲时代新材料科技股份有限公司 | High temperature resistant pair of positive osmosis composite membrane of cortex and preparation method thereof |
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