CN111249925A - Low-pressure high-flux hydrophilic ultrafiltration membrane and preparation method thereof - Google Patents
Low-pressure high-flux hydrophilic ultrafiltration membrane and preparation method thereof Download PDFInfo
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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
- B01D71/58—Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
- B01D71/62—Polycondensates having nitrogen-containing heterocyclic rings in the main chain
- B01D71/64—Polyimides; Polyamide-imides; Polyester-imides; Polyamide acids or similar polyimide precursors
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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
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
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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
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
Abstract
The invention discloses a low-pressure high-flux hydrophilic ultrafiltration membrane and a preparation method thereof, and the low-pressure high-flux hydrophilic ultrafiltration membrane comprises the following components: a base film material, an organic solvent, a monomer A and a monomer B; dissolving a base membrane material in an organic solvent, mechanically heating, stirring and fully and uniformly mixing to obtain a primary membrane casting solution; and adding the monomer A into the preliminary membrane casting solution, mechanically stirring and fully mixing the monomer A and the monomer B uniformly, adding the monomer B, mechanically stirring the monomer A and the monomer B to react in the preliminary membrane casting solution, standing the solution in a vacuum to defoam the solution to obtain a clear transparent solution, and then placing the clear transparent solution on a glass plate or a non-woven fabric to scrape the membrane. The monomer A and the monomer B are subjected to polycondensation reaction in the primary membrane casting solution to generate gel-state polyamic acid, and the gel-state polyamic acid is scraped to prepare the ultrafiltration membrane, so that the ultrafiltration membrane has good hydrophilicity, temperature resistance and toughness, is stable in membrane performance, and is not easy to lose hydrophilic substances.
Description
Technical Field
The invention belongs to the technical field of membrane separation, and relates to a low-pressure high-flux hydrophilic ultrafiltration membrane and a preparation method thereof.
Background
The membrane separation technology is a new technology which appears in the early stage of the 20 th century and rises rapidly after the 60 th century, is a new and promising industrial process, and can replace some disadvantages of the traditional separation technology in competition due to the advantages of good selectivity, simple equipment, low energy consumption, high efficiency, flexibility, easy operation, low investment and the like. The ultrafiltration is one of membrane separation technologies, the pressure difference between two sides of a membrane is used as a driving force, the ultrafiltration membrane is used as a filter medium, macromolecular substances larger than micropores on the surface of the membrane can be selectively intercepted under certain pressure, and small molecular substances smaller than the pores of the membrane are allowed to pass through, so that the separation and purification effects are achieved. The ultrafiltration membrane separation technology is widely applied to separation of macromolecular components and low-molecular-mass substances, and comprises the fields of water treatment, food industry, medicine, chemical industry and the like, but at present, membrane pollution is still a more prominent and urgent problem to be solved by ultrafiltration membranes, and particularly, adsorption of proteins on the surfaces of the membranes and high operation pressure are added, so that the degree of pollution of the membranes in the operation process is increased, and the separation performance and the service life of the ultrafiltration membranes are seriously influenced.
Many researchers have made a lot of researches on solving the problem of membrane pollution, and the researches show that the ultrafiltration membrane with hydrophilicity has better anti-pollution performance, so that the hydrophilization modification of the membrane is the main method for preparing the anti-pollution ultrafiltration membrane. Currently, the methods for hydrophilization modification of membranes are mainly surface coating, surface grafting and blending modification. The surface coating is to directly coat a hydrophilic material on the surface of the membrane through physical adsorption so as to improve the hydrophilicity of the membrane surface, a coating layer of the membrane modified by the method is easy to fall off in the long-term use and cleaning processes, and a plurality of researchers often adopt methods such as sulfonation, crosslinking and the like in order to enhance the stability of the coating layer. The surface grafting modification is to induce and graft hydrophilic monomer or group onto the surface of the membrane by plasma, electron beam, free radical, irradiation, ultraviolet light and other methods, so as to improve the hydrophilic performance of the membrane surface. The blending modification refers to the preparation of a blending membrane by physically blending a base membrane material and a hydrophilic material such as an organic high molecular polymer, inorganic nano particles or an amphiphilic copolymer to prepare a membrane casting solution.
As can be seen from the above, the preparation of ultrafiltration membranes by using the existing techniques still has certain defects, and is difficult to meet the requirements of various performances. Therefore, the way to research the performance of ultrafiltration membranes and the preparation method thereof is to go on to prepare more multifunctional ultrafiltration membranes and obtain better and excellent water quality. The researchers provide a new idea for the low-pressure high-flux hydrophilic ultrafiltration membrane and the preparation method thereof through exploration.
The polyamic acid (PAA) contains a large amount of carboxyl and secondary amino groups in molecules, and the tail end of the molecule also contains a primary amino group, so that the polyamic acid (PAA) has strong hydrophilicity and can promote the transmission of water. The PAA is in a gel state at normal temperature, and by utilizing the characteristic and the hydrophilicity, the water flux can be improved, and the operating pressure of the membrane can be reduced, so that the anti-pollution performance of the membrane is improved. The problems of the compatibility and the dispersibility of the polymer in the membrane casting solution are solved to a great extent by synthesizing the polyamic acid in situ in the base membrane material, and the common blending method for preparing the ultrafiltration membrane usually adopts a method of directly adding the hydrophilic material into the membrane casting solution, which limits the amount of additives in the membrane casting solution. Therefore, the selection of hydrophilic materials and the construction of good compatibility and dispersibility between polymers are problems to be solved urgently for preparing low-pressure high-flux hydrophilic ultrafiltration membranes by physical blending.
Disclosure of Invention
The invention aims to provide a low-pressure high-flux hydrophilic ultrafiltration membrane and a preparation method thereof, wherein the membrane has good hydrophilicity and pure water flux. The method has simple process, easy operation and easy amplification.
The invention is realized by the following technical scheme:
a low-pressure high-flux hydrophilic ultrafiltration membrane is characterized in that: the raw materials comprise, by mass, 10-25 parts of a base film material, 70-85 parts of an organic solvent, 0.2-5 parts of a monomer A and 0.2-5 parts of a monomer B; the base membrane material is any one of Polysulfone (PSF) and polyether sulfone (PES); the organic solvent is any one of N-methylpyrrolidone (NMP), N-Dimethylformamide (DMF) and N, N-dimethylacetamide (DMAc); the monomer A is any one of 4,4 '-diaminodiphenyl ether (ODA), 4' -diaminodiphenyl sulfone (DDS), p-Phenylenediamine (PDA), 4 '-diaminodiphenyl Methane (MDA), 3' -dimethyl-4, 4 '-diaminodiphenyl methane (DMMDA), 2-bis [4- (4-aminophenoxy) phenyl ] propane (BAPP) and 4,4' -diaminobiphenyl; the monomer B is any one of pyromellitic dianhydride (PMDA), diphenyl ether dianhydride (ODPA), 3', 4,4' -biphenyl tetracarboxylic dianhydride (BPDA) and 3,3', 4,4' -triphenyl diether tetracarboxylic dianhydride (HQDPA).
A preparation method of a low-pressure high-flux hydrophilic ultrafiltration membrane comprises the following steps:
(1) dissolving a base membrane material in the organic solvent according to the mass part, heating and uniformly stirring the base membrane material by using a stirrer to obtain a primary membrane casting solution, cooling the primary membrane casting solution to room temperature, adding the monomer A in the mass part, continuously stirring the mixture by using the stirrer to dissolve the monomer A and uniformly mix the monomer A and the monomer B, continuously stirring the mixture by using the stirrer for a certain time to react the monomer A and the monomer B, and then carrying out vacuum defoaming on the mixed solution to obtain a clear transparent solution;
(2) and (2) placing the clear transparent solution obtained in the step (1) on a glass plate or non-woven fabric for membrane scraping, and then placing the clear transparent solution in a coagulating bath at 15-30 ℃ for coagulation, so as to finally obtain the ultrafiltration membrane.
Preferably, the stirrer is a mechanical stirrer, and the stirring speed is 200-500 r/min.
Preferably, in the mass part of the monomer A and the monomer B, the molar ratio is 1:1-1.02, and the stirring time of the stirrer is 4-24 h; the monomer A and the monomer B react in the primary casting solution to carry out polycondensation reaction to generate polyamic acid.
Formula I, formula II and formula III are reaction formulas of one of monomer A and monomer B:
preferably, the vacuum degree required by the vacuum defoaming is 0.03-0.09MPa, and the defoaming time is 6-24 h.
Preferably, the coagulation bath is water or an organic solvent or a composite solution of water and an organic solvent.
The invention has the following advantages and technical effects:
1) the monomer A and the monomer B are subjected to polycondensation reaction in a casting solution of a base film material, a clear transparent solution with good compatibility is obtained through mechanical stirring, and the prepared film has good hydrophilicity, and high pure water flux and good durability are obtained at low pressure.
2) Through serial discussion of the mass ratio of the raw materials and the process of preparing the ultrafiltration membrane, the hydrophilic substance has better compatibility and dispersibility in the base membrane material, the prepared membrane has better water flux under lower pressure, the application cost of the membrane technology is reduced, and the technical development in the membrane preparation field is promoted to a certain extent.
Detailed Description
The following examples give tests of hydrophilicity of hydrophilic ultrafiltration membranes under some conditions, Bovine Serum Albumin (BSA) rejection and pure water flux at low pressure. It is stated that these examples are provided only as a partial illustration and are not intended to limit the invention.
The test procedure was as follows: prepressing for 30min under a certain pressure, then measuring the pure water flux of the ultrafiltration membrane, and carrying out retention performance test on Bovine Serum Albumin (BSA) of 500mg/L on the basis of the pressure. The change in static contact angle before and after the film addition of monomer A and monomer B was measured using a video optical contact angle tester (OCA50AF, Germany, Dataphysics). 5 points were measured for each film and the average was taken. The retention rate of the membrane is measured by adopting an ultraviolet visible spectrophotometer (TU-1810, Beijing Pujingyu Instrument, Ltd.), the absorbance values of the stock solution and the permeate of the BSA solution are respectively measured under the ultraviolet wavelength of 278nm, and the concentration of the BSA solution corresponding to the absorbance values can be known by a corresponding standard curve, so that the retention rate of the membrane to the BSA is obtained.
Examples 1 to 5
Hydrophilicity of modified membrane, Bovine Serum Albumin (BSA) retention performance test
Stirring and dissolving 15 parts by mass of polyether sulfone in N, N-Dimethylformamide (DMF) by using a mechanical device at 80 ℃ to obtain a primary casting solution, cooling to room temperature, adding 0-1.0 part by mass of monomer 4,4' -diaminodiphenyl sulfone (DDS), continuously stirring by using a stirrer to dissolve and mix the monomers uniformly, adding monomer pyromellitic dianhydride (PMDA) corresponding to the DDS in a molar ratio of 1:1.02, continuously stirring by using the stirrer for 4 hours to react the two monomers to obtain a mixed solution, standing and defoaming for 12 hours under the vacuum degree of 0.05MPa, and finally obtaining a clear transparent solution; and placing the clear transparent solution on a glass plate for membrane scraping, and then placing the clear transparent solution in deionized water at the temperature of 20 ℃ for solidification to prepare the ultrafiltration membrane.
The test is carried out by adopting a contact angle tester, and the hydrophilicity and Bovine Serum Albumin (BSA) retention performance test is carried out on the hydrophilic membrane at the operation pressure of 0.1MPa in 500mg/L BSA solution, as shown in Table 1:
TABLE 1
Examples 6 to 10
Low-pressure, high-flux testing of modified membranes with pure water
As with the above example, at 80 ℃, 15 parts by mass of polyethersulfone is dissolved in N, N-Dimethylformamide (DMF) with a mechanical stirrer under stirring to obtain a preliminary casting solution, then cooled to room temperature, 0.8 part by mass of monomeric 4,4' -diaminodiphenylsulfone (DDS) is added, the mixture is stirred with a stirrer continuously to be dissolved and mixed uniformly, then monomeric pyromellitic dianhydride (PMDA) corresponding to DDS (molar ratio 1:1.02) is added, the mixture is stirred with a stirrer continuously for 4 hours to react the two monomers to obtain a mixed solution, and then the mixed solution is allowed to stand and defoamed for 12 hours under a vacuum degree of 0.05MPa, and finally a clear transparent solution is obtained; and placing the clear transparent solution on a glass plate for membrane scraping, and then placing the clear transparent solution in deionized water at the temperature of 20 ℃ for solidification to prepare the ultrafiltration membrane.
Pure water was flux tested at an operating pressure of 0.01-0.05MPa as shown in table 2:
TABLE 2
| Examples | Operating pressure/MPa | Pure water flux/(L/(m)2·h)) |
| 6 | 0.01 | 304.73 |
| 7 | 0.02 | 498.40 |
| 8 | 0.03 | 494.09 |
| 9 | 0.04 | 472.65 |
| 10 | 0.05 | 467.99 |
Comparative example 1
Test for hydrophilicity and Bovine Serum Albumin (BSA) retention performance of control membrane
Stirring and dissolving 15 parts by mass of polyether sulfone in N, N-Dimethylformamide (DMF) by using a mechanical device at 80 ℃ to obtain a primary membrane casting solution, standing and defoaming for 12 hours under the vacuum degree of 0.05MPa, and finally obtaining a clear transparent solution; and placing the clear transparent solution on a glass plate for membrane scraping, and then placing the clear transparent solution in deionized water at the temperature of 20 ℃ for solidification to prepare the ultrafiltration membrane.
The hydrophilic membrane was tested for hydrophilicity and Bovine Serum Albumin (BSA) retention performance using a contact angle tester at 500mg/L BSA solution at an operating pressure of 0.1MPa, as shown in Table 3:
TABLE 3
| Comparative example | Contact angle | Pure water flux/(L/(m)2·h)) | BSA retention/%) |
| 1 | 64.22 | 238.44 | 98.42 |
As seen from examples 1 to 5 and comparative example 1, the hydrophilic ultrafiltration membrane obtained had better hydrophilicity.
Comparative examples 2 to 6
Low-pressure, high-flux testing of pure water for comparative membranes
Stirring and dissolving 15 parts by mass of polyether sulfone in N, N-Dimethylformamide (DMF) by using a mechanical device at 80 ℃ to obtain a primary membrane casting solution, standing and defoaming for 12 hours under the vacuum degree of 0.05MPa, and finally obtaining a clear transparent solution; and placing the clear transparent solution on a glass plate for membrane scraping, and then placing the clear transparent solution in deionized water at the temperature of 20 ℃ for solidification to prepare the ultrafiltration membrane.
Pure water was subjected to flux testing at an operating pressure of 0.01-0.05MPa, as shown in Table 4:
TABLE 4
| Comparative example | Operating pressure/MPa | Pure water flux/(L/(m)2·h)) |
| 2 | 0.01 | 100.33 |
| 3 | 0.02 | 204.57 |
| 4 | 0.03 | 240.26 |
| 5 | 0.04 | 265.30 |
| 6 | 0.05 | 283.00 |
As seen from examples 6 to 10 and comparative examples 2 to 6, the hydrophilic ultrafiltration membrane obtained had a high pure water flux at low pressure, and had a remarkable effect.
Claims (6)
1. A low-pressure high-flux hydrophilic ultrafiltration membrane is characterized in that: the raw materials comprise, by mass, 10-25 parts of a base film material, 70-85 parts of an organic solvent, 0.2-5 parts of a monomer A and 0.2-5 parts of a monomer B; the base membrane material is any one of Polysulfone (PSF) and polyether sulfone (PES); the organic solvent is any one of N-methylpyrrolidone (NMP), N-Dimethylformamide (DMF) and N, N-dimethylacetamide (DMAc); the monomer A is any one of 4,4 '-diaminodiphenyl ether (ODA), 4' -diaminodiphenyl sulfone (DDS), p-Phenylenediamine (PDA), 4 '-diaminodiphenyl Methane (MDA), 3' -dimethyl-4, 4 '-diaminodiphenyl methane (DMMDA), 2-bis [4- (4-aminophenoxy) phenyl ] propane (BAPP) and 4,4' -diaminobiphenyl; the monomer B is any one of pyromellitic dianhydride (PMDA), diphenyl ether dianhydride (ODPA), 3', 4,4' -biphenyl tetracarboxylic dianhydride (BPDA) and 3,3', 4,4' -triphenyl diether tetracarboxylic dianhydride (HQDPA).
2. The method of preparing a low pressure high flux hydrophilic ultrafiltration membrane of claim 1, wherein: the method comprises the following steps:
(1) dissolving a base membrane material in the organic solvent according to the mass part, heating and uniformly stirring the base membrane material by using a stirrer to obtain a primary membrane casting solution, cooling the primary membrane casting solution to room temperature, adding the monomer A in the mass part, continuously stirring the mixture by using the stirrer to dissolve the monomer A and uniformly mix the monomer A and the monomer B, continuously stirring the mixture by using the stirrer for a certain time to react the monomer A and the monomer B, and then carrying out vacuum defoaming on the mixed solution to obtain a clear transparent solution;
(2) and (2) placing the clear transparent solution obtained in the step (1) on a glass plate or non-woven fabric for membrane scraping, and then placing the clear transparent solution in a coagulating bath at 15-30 ℃ for coagulation, so as to finally obtain the ultrafiltration membrane.
3. The method of preparing a low pressure high flux hydrophilic ultrafiltration membrane of claim 2, wherein: the stirrer is mechanically stirred, and the stirring speed is 200-500 r/min.
4. The method of preparing a low pressure high flux hydrophilic ultrafiltration membrane of claim 3, wherein: in the mass part of the monomer A and the monomer B, the molar ratio is 1:1-1.02, and the stirring time of a stirrer is 4-24 h; the monomer A and the monomer B react in the primary casting solution to carry out polycondensation reaction to generate polyamic acid.
5. The method of preparing a low pressure high flux hydrophilic ultrafiltration membrane of claim 2, wherein: the vacuum degree required by the vacuum defoaming is 0.03-0.09MPa, and the defoaming time is 6-24 h.
6. The method of preparing a low pressure high flux hydrophilic ultrafiltration membrane of claim 2, wherein: the coagulating bath is water or organic solvent or composite solution of water and organic solvent.
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