CN115350598A - Method for preparing nanofiltration membrane by using 1-methylimidazole as water phase additive - Google Patents
Method for preparing nanofiltration membrane by using 1-methylimidazole as water phase additive Download PDFInfo
- Publication number
- CN115350598A CN115350598A CN202210782911.9A CN202210782911A CN115350598A CN 115350598 A CN115350598 A CN 115350598A CN 202210782911 A CN202210782911 A CN 202210782911A CN 115350598 A CN115350598 A CN 115350598A
- Authority
- CN
- China
- Prior art keywords
- methylimidazole
- membrane
- nanofiltration membrane
- piperazine
- preparing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000012528 membrane Substances 0.000 title claims abstract description 114
- 238000001728 nano-filtration Methods 0.000 title claims abstract description 67
- MCTWTZJPVLRJOU-UHFFFAOYSA-N 1-methyl-1H-imidazole Chemical compound CN1C=CN=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-N 0.000 title claims abstract description 55
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000000654 additive Substances 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 18
- 230000000996 additive effect Effects 0.000 title claims abstract description 16
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000004952 Polyamide Substances 0.000 claims abstract description 43
- 229920002647 polyamide Polymers 0.000 claims abstract description 43
- 239000002131 composite material Substances 0.000 claims abstract description 32
- 238000000926 separation method Methods 0.000 claims abstract description 14
- UWCPYKQBIPYOLX-UHFFFAOYSA-N benzene-1,3,5-tricarbonyl chloride Chemical compound ClC(=O)C1=CC(C(Cl)=O)=CC(C(Cl)=O)=C1 UWCPYKQBIPYOLX-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000012071 phase Substances 0.000 claims description 37
- 239000008346 aqueous phase Substances 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 7
- 238000012695 Interfacial polymerization Methods 0.000 claims description 6
- 238000007605 air drying Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000000178 monomer Substances 0.000 abstract description 7
- 238000004132 cross linking Methods 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 36
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 32
- 239000011780 sodium chloride Substances 0.000 description 16
- 239000007864 aqueous solution Substances 0.000 description 14
- 230000004907 flux Effects 0.000 description 14
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 13
- 150000003839 salts Chemical class 0.000 description 13
- 229910052938 sodium sulfate Inorganic materials 0.000 description 13
- 235000011152 sodium sulphate Nutrition 0.000 description 13
- 238000012360 testing method Methods 0.000 description 9
- PASDCCFISLVPSO-UHFFFAOYSA-N benzoyl chloride Chemical compound ClC(=O)C1=CC=CC=C1 PASDCCFISLVPSO-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 230000014759 maintenance of location Effects 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 3
- 239000006184 cosolvent Substances 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001368 micro-extraction in a packed syringe Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- -1 2- ((4-aminophenyl) amino) ethyl Chemical group 0.000 description 1
- 206010041277 Sodium retention Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 150000002391 heterocyclic compounds Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000010841 municipal wastewater Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- KCXFHTAICRTXLI-UHFFFAOYSA-M propane-1-sulfonate Chemical compound CCCS([O-])(=O)=O KCXFHTAICRTXLI-UHFFFAOYSA-M 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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 discloses a method for preparing a nanofiltration membrane by using 1-methylimidazole as a water phase additive, which comprises the steps of preparing a water phase solution of 1-methylimidazole and piperazine, infiltrating a supporting membrane, forming a polyamide separation layer, preparing a polyamide composite nanofiltration membrane and the like, wherein hydrogen bonds formed by the 1-methylimidazole and the piperazine inhibit the piperazine from diffusing deeper into a reaction zone, so that the surface of the generated membrane is smoother, the pollution resistance of the membrane is favorably improved, and the 1-methylimidazole can react with an oil phase monomer trimesoyl chloride. The introduction of the reaction competes with the reaction of piperazine and trimesoyl chloride, the main body crosslinking degree of a polyamide separation layer is reduced, the pore diameter of the membrane is enlarged, and the membrane is loosened.
Description
Technical Field
The invention relates to the field of composite nanofiltration membrane preparation, and in particular relates to a method for preparing a nanofiltration membrane by using 1-methylimidazole as an aqueous phase additive.
Background
At present, nanofiltration membranes are widely used in the fields of seawater desalination pretreatment, drinking water purification, municipal/industrial wastewater treatment, resource recovery, material separation and concentration and the like. The nanofiltration membrane has obvious difference on the rejection performance of monovalent salt and divalent salt or multivalent salt, generally has lower rejection rate on monovalent salt and higher rejection rate on divalent or multivalent salt, and therefore, the separation of monovalent/divalent or multivalent salt can be realized. The nanofiltration membrane technology is an important means for relieving the crisis of water resources, and the high-permeability nanofiltration membrane can reduce the process energy consumption and equipment investment and improve the recovery rate; the high-selectivity nanofiltration membrane can improve the process efficiency and the quality of produced water and reduce the post-treatment cost.
In the prior art, an interfacial polymerization method is usually adopted, piperazine (PIP) and trimesoyl chloride (TMC) are respectively used as water/oil phase monomers to prepare a polyamide composite membrane, and the nanofiltration membrane has the problems of low water-contacting flux, high rejection rate of monovalent salt such as NaCl and low monovalent/divalent salt selectivity; in the water/oil phase, introduction of additives is a common method for optimizing the structure of the separation layer to improve the performance of the nanofiltration membrane, and the common additives are reactive additives, co-solvents and the like. Li and the like synthesize a novel reactive additive 3- (4- (2- ((4-aminophenyl) amino) ethyl) morpholino-4-onium) propane-1-sulfonate (PPD-MEPS), the PPD-MEPS is mixed with a water-phase monomer PIP, and then the mixture and an oil-phase monomer TMC are subjected to interfacial polymerization reaction to prepare the nanofiltration membrane. The membrane has a loose separating layer with more negative charge, the water flux of the membrane is all improved, the NaCl retention rate is reduced, and Na is maintained 2 SO 4 Retention rate of (ACS Applied Materials)&Interfaces,2019,11 (45): 42846-42855), however, synthesizing the reactive additive adds an additional film-making step and a film-making cost.
Liu et al prepared nanofiltration membranes using Dioxane (DOX) as a co-solvent. The water permeability of the modified Membrane is significantly improved because the addition of DOX improves the miscibility of the two-phase solution and promotes the diffusion of the aqueous monomer PIP into the oil phase, so that the PIP reacts more strongly with the oil phase monomer TMC, increasing the roughness of the Membrane surface and further increasing the water molecule permeation area (Journal of Membrane Science,2015, 478). In addition, the commonly used cosolvent is usually an organic solvent and has the defects of low lightning, high volatility, flammability, explosiveness and the like.
Disclosure of Invention
The invention discloses a method for preparing a nanofiltration membrane by using 1-methylimidazole as an aqueous phase additive, aiming at the problems in the prior art, the 1-methylimidazole has the characteristics of high boiling point, high flash point, non-flammability, non-explosion and the like relative to a cosolvent, the 1-methylimidazole is used as the aqueous phase additive to prepare the polyamide composite nanofiltration membrane, and the prepared nanofiltration membrane has high flux, low monovalent salt rejection rate and high divalent salt rejection rate.
The technical scheme adopted for realizing the invention is as follows: a method for preparing a nanofiltration membrane by using 1-methylimidazole as an aqueous phase additive is characterized by comprising the following steps:
1) According to the mass percentage, the volume mass fraction of 1-methylimidazole is 0.05-0.3%, the volume mass fraction of piperazine is 0.25-1.0%, and the volume fraction of water is 98.7-99.7%, adding the piperazine and 1-methylimidazole into water in sequence, and stirring uniformly to prepare an aqueous phase solution of 1-methylimidazole and piperazine;
2) Soaking a support membrane in the aqueous phase solution of 1-methylimidazole and piperazine in the step 1) for 20-40 seconds to fully soak the support membrane;
3) Soaking the support membrane soaked in the step 2) in the oil phase solution of trimesoyl chloride again, and forming a polyamide separation layer after the interfacial polymerization reaction is carried out for 20-40 s;
4) And (3) placing the support membrane forming the polyamide separation layer in the step 3) in a forced air drying oven at the temperature of 70-90 ℃, and carrying out heat treatment for 4-6 min to obtain the polyamide composite nanofiltration membrane.
Preferably, in the step 1), the mass percentage of the 1-methylimidazole is 0.1%, the mass percentage of the piperazine is 0.5%, and the mass percentage of the water is 99.4%.
Preferably, in step 3), the support membrane soaked in step 2) is soaked in the oil phase solution of trimesoyl chloride again, and after 30 seconds of interfacial polymerization, a polyamide separation layer is formed.
Preferably, in the step 4), the support membrane forming the polyamide separation layer in the step 3) is placed in a forced air drying oven at 80 ℃, and after heat treatment is carried out for 5min, the polyamide composite nanofiltration membrane is prepared.
Preferably, the polyamide composite nanofiltration membrane prepared in the step 4) is washed by deionized water.
The method for preparing the nanofiltration membrane by using the 1-methylimidazole as the water phase additive has the following beneficial effects:
1. a method for preparing nanofiltration membrane by using 1-methylimidazole as water phase additive, hydrogen bond formed by 1-methylimidazole and piperazine inhibits piperazine from diffusing deeper into a reaction zone, so that the surface of the generated membrane is smoother, the anti-pollution performance of the membrane is improved, 1-methylimidazole endows the nanofiltration membrane with loose polyamide structure and more carboxylic acid groups on the surface of the membrane, and the prepared polyamide composite nanofiltration membrane has the characteristics of high flux, high divalent salt rejection rate and low monovalent salt rejection rate;
2. a method for preparing nanofiltration membrane by using 1-methylimidazole as water phase additive, wherein 1-methylimidazole can react with oil phase monomer trimesoyl chloride. The introduction of the reaction competes with the reaction of piperazine and trimesoyl chloride, reduces the main body crosslinking degree of the polyamide separation layer, enlarges the membrane aperture, and loosens the membrane.
Drawings
FIG. 1 is a scanning electron microscope image of the surface structure of the polyamide composite nanofiltration membrane prepared by adding 1-methylimidazole in example 2;
FIG. 2 is a scanning electron microscope image of the surface structure of the polyamide composite nanofiltration membrane prepared in the comparative example 2 without adding 1-methylimidazole.
Detailed Description
The present invention will be described in further detail with reference to the accompanying fig. 1-2 and the specific embodiments described herein, which are provided for illustration only and are not intended to limit the invention.
The 1-methylimidazole is a heterocyclic compound containing tertiary amine, is liquid at normal temperature and is miscible with water, and the structural formula of the compound is as follows:
the equation for the reaction of 1-methylimidazole with trimesoyl chloride and the hydrolysis of the reaction product is shown below:
example 1
Preparing an aqueous phase solution containing 1-methylimidazole in a mass percentage of 0.05 percent and 0.25 percent of piperazine, pouring the prepared aqueous phase solution on the surface of a support membrane, fully soaking, removing the redundant aqueous phase solution, pouring an oil phase solution containing the benzoyl chloride after the membrane surface is dried, reacting for 20s, removing the redundant oil phase solution to obtain a nanofiltration membrane, and finally, carrying out heat treatment on the membrane at 70 ℃ for 4min to obtain the 1-methylimidazole-added polyamide composite nanofiltration membrane.
The flux and the sodium sulfate retention rate of the polyamide composite nanofiltration membrane added with the 1-methylimidazole are respectively 28.0L/(m) by testing with 2000mg/L sodium sulfate aqueous solution at 25 ℃ under 0.6MPa 2 H.bar) and 70%; the test of 2000mg/L sodium chloride aqueous solution shows that the sodium chloride rejection rate of the polyamide composite nanofiltration membrane added with 1-methylimidazole is 4.00%.
Example 2
Preparing an aqueous phase solution containing 0.1 percent by mass of 1-methylimidazole and 0.5 percent by mass of piperazine, pouring the prepared aqueous phase solution on the surface of a support membrane, removing the redundant aqueous phase solution after the support membrane is fully soaked, pouring an oil phase solution containing benzoyl chloride after the membrane surface is dried, reacting for 30s, and removing the redundant oil phase solution to obtain the nanofiltration membrane; and finally, carrying out heat treatment on the membrane at 80 ℃ for 5min to obtain the polyamide composite nanofiltration membrane added with 1-methylimidazole. The scanning electron microscope image of the polyamide composite nanofiltration membrane prepared in the example shows that the surface of the prepared nanofiltration membrane is very smooth, as shown in figure 1.
The flux and the sodium sulfate retention rate of the polyamide composite nanofiltration membrane added with 1-methylimidazole are respectively 16.6L/(m) by testing with 2000mg/L sodium sulfate aqueous solution at 25 ℃ under 0.6MPa 2 H.bar) and 94.9%, the polyamide composite nanofiltration membrane added with 1-methylimidazole has a sodium chloride rejection rate of 11.58% by utilizing a 2000mg/L sodium chloride aqueous solution test.
Example 3
Preparing an aqueous phase solution containing 1-methylimidazole in a mass percentage of 0.3 percent and 1.0 percent of piperazine in a mass percentage, pouring the prepared aqueous phase solution on the surface of a support membrane, fully soaking, removing the redundant aqueous phase solution, pouring an oil phase solution containing the benzoyl chloride after the surface of the membrane is dried, reacting for 40s, removing the redundant oil phase solution to obtain a nanofiltration membrane, and finally, carrying out heat treatment on the membrane at 90 ℃ for 6min to obtain the 1-methylimidazole added polyamide composite nanofiltration membrane.
The flux and the sodium sulfate retention rate of the polyamide composite nanofiltration membrane added with the 1-methylimidazole are respectively 7.4L/(m) by utilizing a 2000mg/L sodium sulfate aqueous solution test at the temperature of 25 ℃ and under the pressure of 0.6MPa 2 H.bar) and 97.65%, the sodium chloride rejection of the polyamide composite nanofiltration membrane added with 1-methylimidazole is 17.34% as tested by 2000mg/L of sodium chloride aqueous solution.
Comparative example 1
Unlike example 1, the aqueous solution was prepared without 1-methylimidazole. Preparing a water phase solution of 0.25 mass percent of piperazine, pouring the prepared water phase solution on the surface of a support membrane, removing the redundant water phase solution after full infiltration, pouring an oil phase solution containing benzoyl chloride after the membrane surface is dried, reacting for 20s, and removing the redundant oil phase solution to obtain the nanofiltration membrane. And finally, carrying out heat treatment on the membrane at 70 ℃ for 4min to obtain the polyamide composite nanofiltration membrane without adding 1-methylimidazole.
The flux and sodium sulfate rejection rate of the polyamide composite nanofiltration membrane without 1-methylimidazole are respectively 16.7L/(m) by testing with 2000mg/L sodium sulfate aqueous solution at 25 ℃ under 0.6MPa 2 H.bar) and 92.89%, the sodium chloride rejection of the polyamide composite nanofiltration membrane is 15.23% by using 2000mg/L sodium chloride aqueous solution.
Comparative example 2
Unlike example 2, the aqueous solution was prepared without 1-methylimidazole. Preparing a water phase solution of 0.5% by mass of piperazine, pouring the prepared water phase solution on the surface of a support membrane, removing the redundant water phase solution after full infiltration, pouring an oil phase solution containing benzoyl chloride after the membrane surface is dried, reacting for 30s, and removing the redundant oil phase solution to obtain the nanofiltration membrane. And finally, carrying out heat treatment on the membrane at 80 ℃ for 5min to obtain the polyamide composite nanofiltration membrane without 1-methylimidazole, wherein an electron microscope picture is shown as an attached figure 2.
The flux and sodium sulfate rejection rate of the polyamide composite nanofiltration membrane without 1-methylimidazole are respectively 7.8L/(m) by testing with 2000mg/L sodium sulfate aqueous solution at 25 ℃ under 0.6MPa 2 H.bar) and 96.14%, the sodium chloride rejection of the polyamide composite nanofiltration membrane is 29.74% by testing with 2000mg/L sodium chloride aqueous solution.
Comparative example 3
Unlike example 3, the aqueous solution was prepared without 1-methylimidazole. Preparing a water phase solution of 1.0 mass percent of piperazine, pouring the prepared water phase solution on the surface of a support membrane, fully soaking, removing the redundant water phase solution, pouring an oil phase solution containing the benzoyl chloride after the membrane surface is dried, reacting for 40s, and removing the redundant oil phase solution to obtain the nanofiltration membrane. And finally, carrying out heat treatment on the membrane at 90 ℃ for 6min to obtain the polyamide composite nanofiltration membrane without 1-methylimidazole.
The flux and the sulfuric acid of the polyamide composite nanofiltration membrane without 1-methylimidazole are obtained by testing the flux and the sulfuric acid by using 2000mg/L sodium sulfate aqueous solution at the temperature of 25 ℃ and under the pressure of 0.6MPaThe sodium retention rate is respectively 6.3L/(m) 2 H.bar) and 97.62%, the sodium chloride rejection of the polyamide composite nanofiltration membrane was 28.59% as measured with 2000mg/L aqueous sodium chloride solution.
The nanofiltration membrane performance of comparative example 2 and example 2 is shown in table 1. As can be seen from the table, the water flux of the nanofiltration membrane prepared by using 1-methylimidazole as an additive is remarkably improved (improved by 113%) compared with that of the nanofiltration membrane prepared by using 1-methylimidazole as an additive, the sodium chloride rejection rate is remarkably reduced from 29.74% to 11.58%, and the sodium sulfate rejection rate is maintained. In conclusion, in the aspect of preparing the nanofiltration membrane with high water flux and low monovalent salt rejection rate, the 1-methylimidazole used as the additive has obvious advantages.
| Film | Flux (L/(m) 2 ·h·bar)) | Sodium sulfate rejection (%) | Sodium chloride rejection (%) |
| Comparative example 2 | 7.8 | 96.14 | 29.74 |
| Example 2 | 16.6 | 94.90 | 11.58 |
TABLE 1
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and improvements can be made without departing from the principle of the present invention, and these modifications and improvements should also be considered as the protection scope of the present invention.
Claims (5)
1. A method for preparing a nanofiltration membrane by using 1-methylimidazole as an aqueous phase additive is characterized by comprising the following steps:
1) According to the mass percentage, the volume mass fraction of 1-methylimidazole is 0.05-0.3%, the volume mass fraction of piperazine is 0.25-1.0%, and the volume fraction of water is 98.7-99.7%, adding the piperazine and 1-methylimidazole into water in sequence, and stirring uniformly to prepare an aqueous phase solution of 1-methylimidazole and piperazine;
2) Soaking a support membrane in the aqueous phase solution of 1-methylimidazole and piperazine in the step 1) for 20-40 s to fully soak the support membrane;
3) Soaking the support membrane soaked in the step 2) in the oil phase solution of trimesoyl chloride again, and forming a polyamide separation layer after the interfacial polymerization reaction is carried out for 20-40 s;
4) And (3) placing the support membrane for forming the polyamide separation layer in the step 3) in a forced air drying oven at the temperature of 70-90 ℃, and performing heat treatment for 4-6 min to obtain the polyamide composite nanofiltration membrane.
2. The method for preparing nanofiltration membrane according to claim 1, wherein in the step 1), the mass percentage of 1-methylimidazole, the mass percentage of piperazine and the mass percentage of water are respectively 0.1%, 0.5% and 99.4%.
3. The method for preparing nanofiltration membrane according to claim 1, wherein the support membrane impregnated in the step 2) is further impregnated in the oil-phase solution of trimesoyl chloride in the step 3), and the polyamide separation layer is formed after the interfacial polymerization reaction is performed for 30 s.
4. The method for preparing nanofiltration membrane according to claim 1, wherein the supported membrane forming the polyamide separation layer in the step 3) is placed in a forced air drying oven at 80 ℃ in the step 4), and is subjected to heat treatment for 5min to obtain the polyamide composite nanofiltration membrane.
5. The method for preparing nanofiltration membrane according to claim 1, 2, 3 or 4, wherein the polyamide composite nanofiltration membrane prepared in the step 4) is washed with deionized water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210782911.9A CN115350598A (en) | 2022-07-05 | 2022-07-05 | Method for preparing nanofiltration membrane by using 1-methylimidazole as water phase additive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210782911.9A CN115350598A (en) | 2022-07-05 | 2022-07-05 | Method for preparing nanofiltration membrane by using 1-methylimidazole as water phase additive |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115350598A true CN115350598A (en) | 2022-11-18 |
Family
ID=84030774
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210782911.9A Pending CN115350598A (en) | 2022-07-05 | 2022-07-05 | Method for preparing nanofiltration membrane by using 1-methylimidazole as water phase additive |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115350598A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110284454A1 (en) * | 2010-05-24 | 2011-11-24 | Mickols William E | Composite membrane with coating comprising polyalkylene oxide and imidazol compounds |
| EP3215258A1 (en) * | 2014-11-04 | 2017-09-13 | Katholieke Universiteit Leuven KU Leuven Research & Development | Improved method for synthesis of polyamide composite membranes |
| CN110787654A (en) * | 2019-10-21 | 2020-02-14 | 天津大学 | Method for preparing reverse osmosis membrane by using 1-methylimidazole as water phase additive |
| CN112892249A (en) * | 2019-12-04 | 2021-06-04 | 时代沃顿科技有限公司 | Polyamide reverse osmosis membrane and preparation method thereof |
| CN113893711A (en) * | 2021-10-15 | 2022-01-07 | 中国石油大学(华东) | High-flux reverse osmosis composite membrane and preparation method thereof |
-
2022
- 2022-07-05 CN CN202210782911.9A patent/CN115350598A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110284454A1 (en) * | 2010-05-24 | 2011-11-24 | Mickols William E | Composite membrane with coating comprising polyalkylene oxide and imidazol compounds |
| EP3215258A1 (en) * | 2014-11-04 | 2017-09-13 | Katholieke Universiteit Leuven KU Leuven Research & Development | Improved method for synthesis of polyamide composite membranes |
| CN110787654A (en) * | 2019-10-21 | 2020-02-14 | 天津大学 | Method for preparing reverse osmosis membrane by using 1-methylimidazole as water phase additive |
| CN112892249A (en) * | 2019-12-04 | 2021-06-04 | 时代沃顿科技有限公司 | Polyamide reverse osmosis membrane and preparation method thereof |
| CN113893711A (en) * | 2021-10-15 | 2022-01-07 | 中国石油大学(华东) | High-flux reverse osmosis composite membrane and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| YINGYING LIU,ET.AL: "1-methylimidazole as a novel additive for reverse osmosis membrane with high flux-rejection combinations and good stability", JOURNAL OF MEMBRANE SCIENCE, vol. 599, pages 1 - 10 * |
| 杨静等: "界面聚合法制备聚哌嗪酰胺复合纳滤膜", 化学研究与应用, vol. 22, no. 4, pages 456 - 460 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Xu et al. | Network cross-linking of polyimide membranes for pervaporation dehydration | |
| CN104841288B (en) | One kind is used for CO2/N2Detached microgel composite membrane of gas and preparation method thereof | |
| CN110801736B (en) | Preparation method of organic solvent-resistant and difficult-to-peel nanofiltration membrane | |
| CN1608720A (en) | Composite semipermeable membrane, and production process thereof | |
| CN113769593B (en) | Nanofiltration membrane for extracting lithium from salt lake and preparation method thereof | |
| CN110066415B (en) | Preparation method of porous membrane with functionalized surface | |
| CN110585931B (en) | High-flux organic solvent-resistant composite nanofiltration membrane containing metal skeleton compound intermediate layer and preparation method thereof | |
| CN112675716A (en) | UIO-66-NH2Method for preparing high-flux defect-free polyamide membrane by using derivative | |
| CN115121128A (en) | Preparation method of composite membrane and composite membrane | |
| CN111151137B (en) | High-flux high-salt-rejection reverse osmosis composite membrane and preparation method thereof | |
| JPH06210145A (en) | Hydrous gelatinous gas separating membrane | |
| EP2626127A2 (en) | Polyazole membrane for water purification | |
| CN113893711A (en) | High-flux reverse osmosis composite membrane and preparation method thereof | |
| CN111921378B (en) | Polyamide membrane for separating dye and salt and preparation method thereof | |
| CN115350598A (en) | Method for preparing nanofiltration membrane by using 1-methylimidazole as water phase additive | |
| CN107626217A (en) | A kind of complex reverse osmosis membrane and preparation method thereof | |
| CN111282453B (en) | Preparation method of high-performance seawater desalination membrane and prepared seawater desalination membrane | |
| CN107362700B (en) | A kind of nanofiltration separation method of dyestuff intermediate | |
| CN112337318B (en) | Polyphenylene sulfide/porous carbon nanofiber composite membrane and preparation method thereof | |
| CN110787654B (en) | Method for preparing reverse osmosis membrane by using 1-methylimidazole as water phase additive | |
| US11628410B2 (en) | Modified porous membrane material and preparation method thereof, and liquid membrane separation method of carbon dioxide | |
| CN115920679B (en) | Preparation method and application of MOFs transition layer modified solvent-resistant nanofiltration membrane | |
| CN111569675A (en) | Reverse osmosis membrane based on dimethyl carbonate and preparation method thereof | |
| CN113828165B (en) | Preparation method of polyvinyl alcohol ultrathin selective layer nanofiltration membrane | |
| CN113441020B (en) | Composite nanofiltration membrane and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20221118 |