CN112316753B - Preparation method of high-flux loose hollow fiber nanofiltration membrane - Google Patents
Preparation method of high-flux loose hollow fiber nanofiltration membrane Download PDFInfo
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
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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
- B01D71/30—Polyalkenyl halides
Abstract
A preparation method of a high-flux loose hollow fiber nanofiltration membrane is characterized by comprising the following steps: dissolving a metal silver salt in water to prepare a metal silver salt solution, then adding ethylenediamine into the metal silver salt solution, and stirring to obtain a uniform water phase solution; soaking the hollow fiber ultrafiltration membrane into the prepared water phase solution, taking out after soaking, and removing residual solution on the surface of the hollow fiber ultrafiltration membrane; soaking the hollow fiber ultrafiltration membrane obtained in the step two into the prepared oil phase solution, and carrying out interfacial polymerization reaction on the surface of the hollow fiber membrane; and fourthly, taking the hollow fiber ultrafiltration membrane obtained in the third step out of the oil phase, drying, soaking in a salt solution, taking out, and then washing with pure water to obtain the hollow fiber nanofiltration membrane. The silver chloride nano particles can be uniformly distributed in the ultrathin separating layer in an in-situ production mode, and cavities formed after the nano particles are dissolved can greatly improve the flux while ensuring the interception performance of the nanofiltration membrane.
Description
Technical Field
The invention relates to a filtering membrane, in particular to a preparation method of a nanofiltration membrane. Belongs to the technical field of filtering membranes.
Background
The interface polymerization method is the most common method for preparing the nanofiltration membrane at present, and the basic principle is that a layer of ultrathin separation layer with nano-scale aperture is formed on the surface of an ultrafiltration base membrane to form a thin-layer composite nanofiltration membrane, wherein the performance of the nanofiltration membrane is mainly determined by the pore structure and the surface property of the ultrathin separation layer. The related documents refer to chinese patent application publication No. 201310026899.X, a method for preparing a composite nanofiltration membrane by an interfacial polymerization method (application publication No. CN103933881A), chinese patent application publication No. 201610479377.9, a graphene oxide modified polyamide composite nanofiltration membrane and a preparation method thereof (application publication No. CN106076132A), and chinese patent application publication No. 201910891874.3, a method for preparing a polyamide nanofiltration membrane by an interfacial polymerization method (application publication No. CN 110756056A). At present, the nanofiltration membrane prepared by the conventional interfacial polymerization method has the problem of low flux.
Research in recent years finds that the performance of the nanofiltration membrane can be remarkably improved by introducing the nano particles into the ultrathin separation layer, and the flux is greatly improved. The literature can refer to the disclosure of Chinese patent application with application number 201410168497.8, namely a composite nanofiltration membrane containing composite nanoparticles and a preparation method (application publication number: CN105080367A), in which attapulgite-nano silica composite nanoparticles are added into an organic phase, and then interfacial polymerization is carried out, so that the nanoparticles are uniformly dispersed in a functional layer.
The chinese patent application No. 201910609824.1 discloses a method for preparing a loose nanofiltration membrane based on interfacial polymerization (application publication No. CN110180402A), and hydrophilic nano materials are introduced into the aqueous phase, so that the hydrophilicity of the membrane surface can be improved; on the other hand, the sandwich structure can be formed by introducing the nanomaterial into the polycondensation process of the interfacial polymerization process, and the polyamide grows around the nanomaterial simultaneously in the direction perpendicular to the nanomaterial.
The traditional nano particle filling method has the problems of insufficient dispersibility, poor organic/inorganic interface compatibility and the like, so that the ultrathin separation layer is easy to have defects and the interception performance is reduced. Because the existence of the nano particles causes certain resistance to the permeation of water molecules, the improvement of the nano-filtration membrane permeability by the filling of the nano particles is limited.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing a high-flux loose hollow fiber nanofiltration membrane with uniformly dispersed nano particles aiming at the technical current situation.
The technical scheme adopted by the invention for solving the technical problems is as follows: 1. a preparation method of a high-flux loose hollow fiber nanofiltration membrane is characterized by comprising the following steps:
dissolving a metal silver salt in water to prepare a metal silver salt solution with the concentration of 0.01-0.5 wt%, adding ethylenediamine into the metal silver salt solution according to the mass ratio of silver ions to ethylenediamine of 1: 20-1: 100, and stirring to obtain a uniform water phase solution;
soaking the hollow fiber ultrafiltration membrane into the prepared water phase solution, taking out after soaking, and removing residual solution on the surface of the hollow fiber ultrafiltration membrane;
soaking the hollow fiber ultrafiltration membrane obtained in the step two into the prepared oil phase solution, and carrying out interfacial polymerization reaction on the surface of the hollow fiber membrane;
and fourthly, taking the hollow fiber ultrafiltration membrane obtained in the third step out of the oil phase, drying, soaking in a salt solution, taking out, and then washing with pure water to obtain the hollow fiber nanofiltration membrane.
Preferably, the metal silver salt in step (r) is at least one selected from silver nitrate, silver perchlorate and silver tetrafluoroborate.
Preferably, the hollow fiber ultrafiltration membrane in the second step is at least one of a polysulfone hollow fiber ultrafiltration membrane, a polyethersulfone hollow fiber ultrafiltration membrane or a polyvinyl chloride hollow fiber ultrafiltration membrane.
Preferably, the soaking time in the step II is 1-10 min.
Preferably, the oil phase solution in the step (c) is an organic solution of aromatic polybasic acyl chloride.
Preferably, the concentration of the aromatic polybasic acyl chloride is 0.01-1 wt%.
Preferably, the aromatic polybasic acyl chloride is at least one of trimesoyl chloride, terephthaloyl chloride or isophthaloyl chloride, and the organic solvent of the organic solution is at least one of n-hexane, n-heptane or cyclohexane.
Preferably, the time of the interfacial polymerization reaction in the step (c) is 5 to 120 s.
Preferably, the salt solution in the step (iv) is at least one of an ammonium carbonate solution, a sodium thiosulfate solution and a potassium thiocyanate solution, and the concentration of the salt solution is 1-10 wt%.
Preferably, the drying conditions in the step (iv) are as follows: putting the mixture into an oven, and carrying out heat treatment for 10-120 s at 50-120 ℃.
Compared with the prior art, the invention has the advantages that:
1. the AgCl nanoparticles are formed by in-situ growth by utilizing hydrogen chloride generated in the interfacial polymerization process and are uniformly dispersed in the ultrathin separating layer, so that the defects of the nanofiltration membrane are reduced.
2. In the polymerization process, Ag + and a water phase monomer exist in a complexing mode, so that the problem of poor interface compatibility between the nano particles and the ultrathin separation layer is solved, the dispersibility of the nano particles is further enhanced, and the interception performance is ensured while the flux of the nanofiltration membrane is improved.
3. The prepared nanofiltration membrane is cleaned by using the salt solution, AgCl nano particles are dissolved on the premise of not influencing the structure and the property of the nanofiltration membrane, and cavities are formed in the ultrathin separation layer, so that the flux is greatly improved while the interception performance of the nanofiltration membrane is ensured.
4. The metal silver salt can react with the hydrogen chloride which is a byproduct of the interface polymer, so that the content of the hydrogen chloride in a water phase is reduced, and the metal silver salt can be used as an acid-absorbing agent (hydrogen chloride) to accelerate the process of the interface polymer, so that the formed ultrathin separation layer is compact and uniform.
Drawings
FIG. 1 is a scanning electron microscope image of the hollow fiber nanofiltration membrane prepared in example 1.
FIG. 2 is a scanning electron microscope image of the hollow fiber nanofiltration membrane prepared in example 2.
FIG. 3 is a scanning electron microscope image of the hollow fiber nanofiltration membrane prepared in example 3.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
Example 1
Film-making environmental conditions: the temperature is 25 +/-3 ℃, and the humidity is 45% +/-5.
(1) Weighing 0.0169g of silver nitrate, dissolving the silver nitrate in 100ml of deionized water, then dropwise adding 0.6g of ethylenediamine into the silver nitrate solution, and stirring to obtain an aqueous phase solution;
(2) soaking a polysulfone hollow fiber ultrafiltration membrane into the prepared water phase solution, soaking for 1min, taking out, and wiping residual solution on the surface of the ultrafiltration membrane by using filter paper;
(3) weighing 0.01g of trimesoyl chloride, dissolving in 100ml of n-hexane to obtain an oil phase solution, soaking the hollow fiber ultrafiltration membrane obtained in the step (2) in the oil phase solution, reacting for 15s, taking out, placing in a drying oven, and treating for 10s at 50 ℃;
(4) weighing 1g of ammonium carbonate to dissolve in 100ml of deionized water, soaking the membrane obtained in the step (3) in an ammonium carbonate solution for 1min, taking out, finally soaking in pure water to obtain a nanofiltration membrane, cleaning, and soaking in pure water if stored.
The hollow fiber nanofiltration membrane obtained in example 1 was analyzed:
the membrane structure was observed under an electron microscope, and as a result, as shown in fig. 1, the micro-protrusions were uniformly distributed on the surface of the nanofiltration membrane: the hollow fiber nanofiltration membrane prepared by the embodiment is loaded into membrane testing equipment for testing, and the experimental result is as follows: the water flux is 12.35L/m 2 h.bar, the Na2SO4 rejection rate is 99.2%, and the MgSO4 rejection rate is 97.9%.
Example 2
Film-making environmental conditions: the temperature is 25 +/-3 ℃, and the humidity is 45% +/-5.
(1) Weighing 0.204g of silver perchlorate, dissolving the silver perchlorate in 100ml of deionized water, then dropwise adding 3g of ethylenediamine into the silver perchlorate solution, and stirring to obtain an aqueous phase solution;
(2) soaking the polyether sulfone hollow fiber ultrafiltration membrane into the prepared water phase solution, soaking for 5min, taking out, and wiping the residual solution on the surface of the ultrafiltration membrane by using filter paper;
(3) weighing 0.1g of terephthaloyl chloride, dissolving in 100ml of n-heptane to obtain an oil phase solution, soaking the hollow fiber ultrafiltration membrane obtained in the step (2) in the oil phase solution, reacting for 60s, taking out, placing in an oven, and treating for 50s at 80 ℃;
(4) weighing 5g of sodium thiosulfate and dissolving the sodium thiosulfate in 100ml of deionized water, soaking the membrane obtained in the step (3) in a sodium thiosulfate solution for 10min, taking out the membrane, and finally soaking the membrane in pure water to obtain the nanofiltration membrane.
The hollow fiber nanofiltration membrane obtained in example 2 was analyzed:
the film structure was observed under an electron microscope, and the results are shown in FIG. 2: spherical protrusions are uniformly distributed on the surface of the nanofiltration membrane, and the roughness is obviously increased; the hollow fiber nanofiltration membrane prepared by the embodiment is loaded into membrane testing equipment for testing, and the experimental result is as follows: the water flux is 25.62L/m2 h.bar, the Na2SO4 retention rate is 98.3%, and the MgSO4 retention rate is 96.8%.
Example 3
Film-making environmental conditions: the temperature is 25 +/-3 ℃, and the humidity is 45% +/-5.
(1) Weighing 0.485g of silver perchlorate, dissolving the silver perchlorate in 100ml of deionized water, then dropwise adding 3g of ethylenediamine into the silver perchlorate solution, and stirring to obtain an aqueous phase solution;
(2) soaking a polyvinyl chloride hollow fiber ultrafiltration membrane into the prepared water phase solution, soaking for 10min, taking out, and wiping residual solution on the surface of the ultrafiltration membrane by using filter paper;
(3) weighing 1g of isophthaloyl dichloride, dissolving in 100ml of cyclohexane to obtain an oil phase solution, soaking the hollow fiber ultrafiltration membrane obtained in the step (2) in the oil phase solution, reacting for 120s, taking out, placing in an oven, and treating for 120s at 120 ℃;
(4) weighing 10g of potassium thiocyanate, dissolving the potassium thiocyanate in 100ml of deionized water, soaking the membrane obtained in the step (3) in a potassium thiocyanate solution for 30min, taking out the membrane, and finally soaking the membrane in pure water to obtain the nanofiltration membrane.
Analysis of the hollow fiber nanofiltration membrane obtained in example 3:
the film structure was observed under an electron microscope, and the results are shown in FIG. 3: large granular protrusions are uniformly distributed on the surface of the nanofiltration membrane, and the roughness is greatly increased; the hollow fiber nanofiltration membrane prepared by the embodiment is loaded into membrane testing equipment for testing, and the experimental result is as follows: the water flux is 20.58L/m2 h.bar, the Na2SO4 rejection rate is 97.5%, and the MgSO4 rejection rate is 95.1%.
Claims (9)
1. A preparation method of a high-flux loose hollow fiber nanofiltration membrane is characterized by comprising the following steps:
dissolving a metal silver salt in water to prepare a metal silver salt solution with the concentration of 0.01-0.5 wt%, adding ethylenediamine into the metal silver salt solution according to the mass ratio of silver ions to ethylenediamine of 1: 20-1: 100, and stirring to obtain a uniform water phase solution;
soaking the hollow fiber ultrafiltration membrane into the prepared water phase solution, taking out after soaking, and removing residual solution on the surface of the hollow fiber ultrafiltration membrane;
soaking the hollow fiber ultrafiltration membrane obtained in the step two into the prepared oil phase solution, and carrying out interfacial polymerization reaction on the surface of the hollow fiber membrane;
fourthly, taking the hollow fiber ultrafiltration membrane obtained in the third step out of the oil phase, drying, soaking in a salt solution, taking out, and then washing with pure water to obtain a hollow fiber nanofiltration membrane;
in the step (iv), the salt solution is at least one of an ammonium carbonate solution, a sodium thiosulfate solution or a potassium thiocyanate solution, and the concentration of the salt solution is 1-10 wt%.
2. The method according to claim 1, wherein the silver salt of a metal in step (i) is at least one selected from the group consisting of silver nitrate, silver perchlorate and silver tetrafluoroborate.
3. The preparation method according to claim 1, wherein the hollow fiber ultrafiltration membrane in the step (II) is at least one of a polysulfone hollow fiber ultrafiltration membrane, a polyethersulfone hollow fiber ultrafiltration membrane or a polyvinyl chloride hollow fiber ultrafiltration membrane.
4. The preparation method according to claim 1, wherein the soaking time in the step (II) is 1-10 min.
5. The method according to claim 1, wherein the oil phase solution in step (c) is an organic solution of an aromatic polybasic acid chloride.
6. The method according to claim 5, wherein the aromatic polybasic acid chloride has a concentration of 0.01 to 1 wt%.
7. The method according to claim 5, wherein the aromatic poly-acid chloride is at least one of trimesoyl chloride, terephthaloyl chloride and isophthaloyl chloride, and the organic solvent of the organic solution is at least one of n-hexane, n-heptane or cyclohexane.
8. The method according to claim 1, wherein the time for the interfacial polymerization reaction in step (c) is 5 to 120 seconds.
9. The method according to claim 1, wherein the drying conditions in the step (iv) are as follows: putting the mixture into an oven, and carrying out heat treatment for 10-120 s at 50-120 ℃.
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