CN118577149A - A high-throughput hollow fiber nanofiltration membrane and preparation method thereof - Google Patents
A high-throughput hollow fiber nanofiltration membrane and preparation method thereof Download PDFInfo
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- C02F1/00—Treatment of water, waste water, or sewage
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Abstract
本申请涉及一种高通量中空纤维纳滤膜及其制备方法，该方案包括S00、将料液和芯液从纺丝设备的纺丝喷丝头中挤出，使得喷出的膜丝暴露在空气间隙中；S10、膜丝经过空气间隙后接触到纯水水槽，以使得膜丝与纯水接触发生相变，形成中空纤维基膜；S20、将中空纤维基膜收集并进行纺丝和干燥，得到中空纤维纳滤膜；S30、通过交联溶液一和交联溶液二对中空纤维纳滤膜进行分别浸泡干燥，得到高通量中空纤维纳滤膜。本申请的纳滤膜可适用于各类水处理，具有通量高和透水性好的优点。
The present application relates to a high-flux hollow fiber nanofiltration membrane and a preparation method thereof, which includes S00, extruding a feed liquid and a core liquid from a spinning spinneret of a spinning device so that the ejected membrane filaments are exposed to an air gap; S10, the membrane filaments are contacted with a pure water tank after passing through the air gap so that the membrane filaments and the pure water contact a phase change to form a hollow fiber base membrane; S20, collecting the hollow fiber base membrane and spinning and drying it to obtain a hollow fiber nanofiltration membrane; S30, soaking and drying the hollow fiber nanofiltration membrane with a cross-linking solution 1 and a cross-linking solution 2, respectively, to obtain a high-flux hollow fiber nanofiltration membrane. The nanofiltration membrane of the present application can be applied to various types of water treatment, and has the advantages of high flux and good water permeability.
Description
Technical Field
The application relates to the technical field of water treatment, in particular to a high-flux hollow fiber nanofiltration membrane and a preparation method thereof, aiming at improving the water flux of the nanofiltration membrane and reducing the operating pressure so as to optimize the efficiency and the economy of water resource treatment.
Background
With the increasing shortage of global water resources and the exacerbation of water pollution problems, efficient and economical water treatment technologies are becoming a hotspot for research. Nanofiltration membrane technology has been attracting attention as a leading water treatment technology because of its ability to remove harmful substances in water while retaining beneficial minerals. Among them, the roll nanofiltration membrane becomes a mainstream product in the water treatment industry due to its mature technology and wide market application. However, the roll nanofiltration membranes have inherent limitations including high operating pressure requirements, complex pretreatment requirements, and relatively low water flux, which not only increase the operating costs and energy consumption of the water treatment system, but also increase the complexity of operation.
In recent years, hollow fiber nanofiltration membranes have attracted attention in the industry due to their unique structural advantages. The design of hollow fiber membranes provides a larger effective surface area and an open channel structure, which allows them to exhibit lower flow resistance while maintaining comparable retention properties to the roll nanofiltration membranes. In theory, these characteristics should help significantly reduce operating pressure and simplify pretreatment steps, thereby reducing overall energy consumption and maintenance costs.
Nevertheless, the water flux of existing hollow fiber nanofiltration membrane products is generally low, typically below 10L/m 2 hr bar, which limits to some extent their efficiency and applicability in large-scale water treatment applications.
In addition, in order to fully play the advantages of the hollow fiber nanofiltration membrane, the challenges are overcome, and further technical innovation and process optimization are particularly urgent. In view of the above, the invention aims to provide a new hollow fiber nanofiltration membrane solution to break through the bottleneck of the prior art, realize higher water flux and wider application scenes, and make contribution to effective management and sustainable utilization of water resources.
Disclosure of Invention
The application aims at solving the problems in the prior art and provides a high-flux hollow fiber nanofiltration membrane and a preparation method thereof.
In order to achieve the purpose of the application, the application adopts the following technical scheme: the preparation method of the high-flux hollow fiber nanofiltration membrane comprises the following steps:
S00, extruding feed liquid and core liquid from a spinning spinneret of a spinning device, so that the sprayed film yarn is exposed in an air gap;
wherein the feed liquid is a mixture of macromolecular polyethersulfone, polyethylene glycol and dimethylacetamide; the core liquid is pure water;
S10, the membrane wires contact a pure water tank after passing through an air gap, so that the membrane wires contact pure water to generate phase change, and a hollow fiber base membrane is formed;
s20, collecting the hollow fiber base membrane, spinning and drying to obtain a hollow fiber nanofiltration membrane;
S30, respectively soaking and drying the hollow fiber nanofiltration membrane through a first crosslinking solution and a second crosslinking solution to obtain a high-flux hollow fiber nanofiltration membrane;
Wherein, the first crosslinking solution and the second crosslinking solution comprise a crosslinking agent, an additive and a solvent.
Further, the core liquid is obtained by mixing dimethylacetamide, macromolecular polyethersulfone with the molecular weight of 80000-100000g/mol and polyethylene glycol with the molecular weight of 200-1000g/mol and then vacuum defoaming.
Further, the size of the air gap is 20-50cm.
Further, the crosslinking solution I takes 1-methylpiperazine as a crosslinking agent, sodium hydroxide and camphorsulfonate as additives, and pure water as a solvent; the crosslinking solution II takes isophthaloyl dichloride as a crosslinking agent, acetone as an additive and n-hexane as a solvent.
Further, the preparation step of the crosslinking solution I is as follows:
2%1-methylpiperazine, 0.2% sodium hydroxide, 1% sodium camphorsulfonate and 96.8% pure water were mixed to obtain a crosslinked solution I.
Further, the preparation step of the crosslinking solution II is as follows:
0.1 to 0.3 percent of isophthaloyl dichloride, 0.5 to 2 percent of acetone and 97.7 to 99.4 percent of normal hexane are mixed to obtain a crosslinking solution II.
Further, the preparation step of the crosslinking solution I is as follows:
placing 20% of high polymer polyethersulfone, 30% of polyethylene glycol and 30% of dimethylacetamide in a stirring tank;
Uniformly stirring the feed liquid components for 24 hours at the constant temperature of 70 ℃ until the polyethersulfone is completely dissolved in the solvent;
And vacuumizing for defoaming for more than 7 hours, and cooling to room temperature to obtain a crosslinking solution I.
Further, the specific steps of S30 are:
Soaking the dried hollow fiber nanofiltration membrane in a cross-linking solution I and drying;
And soaking the dried hollow fiber nanofiltration membrane in a crosslinking solution II, and then airing to obtain the high-flux hollow fiber nanofiltration membrane.
The high-flux hollow fiber nanofiltration membrane is prepared by the preparation method of the high-flux hollow fiber nanofiltration membrane.
Further, the molecular weight cutoff of the high-flux hollow fiber nanofiltration membrane is 400-1000Da, and the pure water flux is 20-25L/m 2. H.bar.
Compared with the prior art, the application has the following beneficial effects:
1. The water flux is obviously improved: by controlling the degree of the crosslinking reaction, the hollow fiber nanofiltration membrane prepared by the method realizes water flux as high as 25L/m 2.h.bar, which is far higher than the average flux level (< 10L/m 2.h.bar) of the nanofiltration membrane in the prior art. The remarkable improvement effectively improves the efficiency of water treatment and reduces the cost of unit water treatment.
2. Maintains excellent separation performance: the nanofiltration membrane of the invention still maintains good separation performance while greatly improving water flux, can effectively remove harmful substances in water, and simultaneously retains minerals beneficial to human bodies, thereby meeting the high standard requirements of water purification treatment and industrial sewage treatment.
3. The optimized preparation process comprises the following steps: the membrane preparation method adopted by the invention comprises spinning and crosslinking post-treatment of the hollow fiber base membrane, and the process flow is simple and efficient. The pore size distribution of the membrane and the density of the crosslinked layer can be precisely controlled by finely adjusting the proportion of spinning feed liquid components and the crosslinked solution, thereby realizing customized adjustment of the membrane performance.
4. Wide applicability: the high-flux hollow fiber nanofiltration membrane is suitable for various water treatment application scenes, can perform excellent both drinking water purification and industrial wastewater treatment, and has extremely high practical value and market potential.
In conclusion, the high-flux hollow fiber nanofiltration membrane solves the problems of high operating pressure, complex pretreatment and the like in the prior art, greatly improves the water flux, optimizes the separation performance, and opens up a new path for technical innovation and sustainable development of the water treatment industry. The preparation method can produce the high-performance nanofiltration membrane with the molecular weight cut-off (MWCO) of 400-1000Da and the pure water flux of 20-25L/m 2 & h & bar, and provides powerful technical support for solving the global water resource crisis.
Drawings
FIG. 1 is a schematic diagram of the structure of a high-flux hollow fiber nanofiltration membrane wire prepared by the application;
FIG. 2 is a schematic diagram II of the structure of the high-flux hollow fiber nanofiltration membrane wire prepared by the application.
Detailed Description
The following description of the embodiments of the present application will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present application, but not all embodiments. All other embodiments, which are derived by a person skilled in the art based on the embodiments of the application, fall within the scope of protection of the application.
It will be appreciated by those skilled in the art that in the present disclosure, the terms "longitudinal," "transverse," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," etc. refer to an orientation or positional relationship based on that shown in the drawings, which is merely for convenience of description and to simplify the description, and do not refer to or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus the above terms should not be construed as limiting the present application.
Example 1: preparation of high flux hollow fiber based membranes
Preparing spinning feed liquid:
The polymer polyethersulfone (molecular weight about 90,000 g/mol) was mixed at 20% mass fraction, the polyethylene glycol (molecular weight about 600 g/mol) at 30% mass fraction and the dimethylacetamide at 30% mass fraction.
Stirring was carried out at a constant temperature of 70℃for 24 hours, ensuring adequate dissolution of the polyethersulfone.
Then, the mixture is vacuumized and defoamed for at least 7 hours, and cooled to room temperature for standby.
Spinning core solution: 100% pure water was used.
Spinning:
a gear pump is used to deliver spinning feed and core liquor to the spinneret, respectively.
The film filaments extruded from the spinneret were formed in an air gap of 20-50cm (height) and immediately immersed in a pure water tank. Therefore, the outer layer of the membrane can form a loose enough structure, which is beneficial to the water permeability of the membrane wires.
In the water tank, the membrane filaments rapidly undergo phase transition to form a stable hollow fiber-based membrane.
The formed hollow fiber base membrane is collected by a wire collecting wheel and is dried naturally or dried for standby.
The gear pump and the spinneret are all part of the structure of the existing spinning equipment, and the spinning equipment mainly comprises a material liquid tank, a core liquid tank, a gear pump, the spinneret, a gel tank and a filament collecting wheel and is used for preparing the central control fiber membrane filaments.
Example 2: crosslinking post-treatment of high-flux hollow fiber nanofiltration membranes
Preparation of a crosslinking solution:
2% by mass of 1-methylpiperazine, 0.2% by mass of sodium hydroxide, 1% by mass of sodium camphorsulfonate and 96.8% by mass of pure water were mixed.
Stirring uniformly for 2 hours to obtain a stable and uniform solution.
Preparing a crosslinking solution II:
0.2% by mass of isophthaloyl dichloride, 1% by mass of acetone and 98.8% by mass of n-hexane were mixed.
Likewise, stirring was carried out uniformly for 2 hours, ensuring uniformity of the solution.
Crosslinking post-treatment process:
and soaking the dried hollow fiber base membrane in the first crosslinking solution for 1-10 minutes, taking out, removing the redundant solution and drying.
And soaking the membrane filaments in the crosslinking solution II for 1-10 minutes, taking out, removing the redundant solution, and naturally airing.
After the steps are finished, the high-flux hollow fiber nanofiltration membrane with a loose polyamide desalting layer with a firm structure can be obtained.
The post-treatment of the hollow fiber nanofiltration membrane is mainly carried out by forming a loose polyamide desalination layer with firm structure on the hollow fiber base membrane, as shown in fig. 1 and 2, wherein the inner layer is of a loose and firm desalination layer structure, and the outer layer is of a porous base membrane structure. The reaction mechanism is that 1-methylpiperazine is firstly coated on the surface of a base film uniformly, and then the base film and isophthaloyl dichloride are subjected to crosslinking reaction. The crosslinking reaction degree can be controlled by adjusting the crosslinking agent and additive components in the crosslinking solution, so that the high-flux hollow fiber nanofiltration membrane with the molecular weight cut-off (MWCO) of 400-1000Da is obtained. The pure water flux is 20-25L/m 2. H.bar.
Example 3: comparative test
The following table shows the two components of the cross-linked solution for preparing the high flux hollow fiber nanofiltration membranes. According to the preparation methods of the hollow fiber nanofiltration membranes in example 1 and example 2, the inner diameter and the outer diameter of the obtained hollow fiber nanofiltration membranes were 0.7/1.2mm, namely, the membrane preparation cases 1 to 3.
The control group was spun by the same film-forming step, but the crosslinking solution was composed of piperazine and trimesoyl chloride as crosslinking agents, and the composition thereof was as follows:
-crosslinking solution one: 2% piperazine, 0.2% sodium hydroxide, 1% sodium camphorsulfonate and 96.8% pure water;
-crosslinking solution two: 0.15% isophthaloyl dichloride and 99.85% n-hexane.
Then, the high flux hollow fiber nanofiltration membrane wires in the membrane preparation case are assembled into a membrane assembly, and the following nanofiltration membrane performance test is carried out:
1. Pure water flux (P pw): reverse osmosis water was used as the test feed water and was run at 3bar and 25℃and the permeate flow (Q p) was recorded and calculated using equation 1.
Equation 1: p pw＝Qp/(A.DELTA.P)
Wherein P pw is pure water flux (L/m 2.h.bar)、Qp is permeate flux (L/h), A is effective membrane filtration area (m 2), and ΔP is transmembrane pressure (bar).
2. Molecular weight cut-off (MWCO) test: the polyethylene glycol solution is used as a test solution, the molecular weight distribution is 200-1500, the analysis is carried out under the running condition of 1bar and 25 ℃, and the analysis is carried out by comparing polyethylene glycol components in the original solution and the permeate (equation 2) so as to intercept MWCO with the molecular weight of polyethylene glycol of >90 percent as a middle fiber nanofiltration membrane.
Equation 2: r= (1-C p/Cf). Times.100%
Where R is the rejection, C p is the solute concentration in the permeate, and C f is the solute concentration in the original solution.
3. Divalent ion entrapment test: the magnesium sulfate solution was used as a divalent ion representative as a test solution, and was carried out under an operating condition of 3bar and 25 c, and analyzed by comparing the magnesium sulfate component test in the original solution and the permeate (equation 2).
The test results are as follows:
| Membrane filament | Pure water flux (L/m 2. H.bar) | Molecular weight cut-off (Da) | Magnesium sulfate retention rate |
| Film forming case 1 | 23 | 630 | 86％ |
| Film forming case 2 | 25 | 930 | 82％ |
| Film forming case 3 | 22 | 500 | 88％ |
| Control group | 13 | 750 | 84％ |
Therefore, the pure water flux of the control group is greatly behind the membrane preparation cases 1-3 of the application, and the pure water flux is not ensured to be more than 20L/m 2. H.bar while the molecular weight cut-off rate is ensured to be between 400 and 1000 Da. The data of the membrane preparation case 2 are the most excellent, and the crosslinking reaction degree can be adjusted by adjusting the proportion of the crosslinking agent and the additive in the crosslinking solution II, so that the high-flux hollow fiber nanofiltration membrane with the molecular weight cut-off (MWCO) of 400-1000Da is obtained, and the pure water flux of the high-flux hollow fiber nanofiltration membrane is 20-25L/m 2. H.bar.
Example 4: dye removal test
The hollow fiber nanofiltration membrane prepared by the membrane preparation case 1 is assembled into a membrane assembly, 100mg/L of Reactive Blue 19 dye solution is prepared as water inlet stock solution, the test pressure is 3bar, the test temperature is 25 ℃, the stock solution is conveyed from a stock solution barrel to the membrane assembly through a water pump, produced water is collected in a water production barrel, and concentrated water flows back into the stock solution barrel. The test result shows that the average flux of the hollow fiber nanofiltration membrane is 21.9L/m 2. H.bar, and the dye removal can reach 88.5%.
Example 5: leather factory waste water color removal test
The hollow fiber nanofiltration membrane prepared by the membrane preparation case 3 is assembled into a membrane assembly, waste water of a certain leather production enterprise is taken as raw water inlet liquid, the test pressure is 4bar, the test temperature is 25 ℃, the raw liquid is conveyed from a raw liquid barrel to the membrane assembly through a water pump, produced water is collected in a produced water barrel, and concentrated water flows back into the raw liquid barrel. The test result shows that the average flux of the hollow fiber nanofiltration membrane is 20L/m 2. H.bar, and the color removal effect of >99% and turbidity removal of >99% can be achieved.
The application is not described in detail in the prior art, and therefore, the application is not described in detail.
It will be understood that the terms "a" and "an" should be interpreted as referring to "at least one" or "one or more," i.e., in one embodiment, the number of elements may be one, while in another embodiment, the number of elements may be plural, and the term "a" should not be interpreted as limiting the number.
Although specific terms are used more herein, the use of other terms is not precluded. These terms are used merely for convenience in describing and explaining the nature of the application; they are to be interpreted as any additional limitation that is not inconsistent with the spirit of the present application.
The present application is not limited to the above-mentioned preferred embodiments, and any person can obtain various other products without departing from the scope of the present application, but any changes in shape or structure of the present application are within the scope of the present application.
Claims (10)
1. The preparation method of the high-flux hollow fiber nanofiltration membrane is characterized by comprising the following steps of:
S00, extruding feed liquid and core liquid from a spinning spinneret of a spinning device, so that the sprayed film yarn is exposed in an air gap;
Wherein the feed liquid is a mixture of high molecular polyether sulfone, polyethylene glycol and dimethylacetamide; the core liquid is pure water;
S10, the membrane wires contact a pure water tank after passing through an air gap, so that the membrane wires contact pure water to generate phase change, and a hollow fiber base membrane is formed;
S20, collecting the hollow fiber base membrane, spinning and drying to obtain a hollow fiber nanofiltration membrane;
s30, respectively soaking and drying the hollow fiber nanofiltration membrane through a crosslinking solution I and a crosslinking solution II to obtain a high-flux hollow fiber nanofiltration membrane;
wherein the first crosslinking solution and the second crosslinking solution comprise a crosslinking agent, an additive and a solvent.
2. The method for preparing the high-flux hollow fiber nanofiltration membrane according to claim 1, wherein the core liquid is obtained by mixing dimethylacetamide, high molecular polyether sulfone with molecular weight of 80000-100000g/mol and polyethylene glycol with molecular weight of 200-1000g/mol and then vacuum defoaming.
3. The method for preparing a high-flux hollow fiber nanofiltration membrane according to claim 1, wherein the size of the air gap is 20-50cm.
4. The method for preparing the high-flux hollow fiber nanofiltration membrane according to claim 1, wherein the cross-linking solution I takes 1-methylpiperazine as a cross-linking agent, sodium hydroxide and camphorsulfonate as additives, and pure water as a solvent; the crosslinking solution II takes isophthaloyl dichloride as a crosslinking agent, acetone as an additive and n-hexane as a solvent.
5. The method for preparing a high-flux hollow fiber nanofiltration membrane according to claim 4, wherein the preparation step of the first crosslinking solution is as follows:
2%1-methylpiperazine, 0.2% sodium hydroxide, 1% sodium camphorsulfonate and 96.8% pure water were mixed to obtain a crosslinked solution I.
6. The method for preparing a high-flux hollow fiber nanofiltration membrane according to claim 4, wherein the preparation step of the crosslinking solution II comprises the following steps:
0.1 to 0.3 percent of isophthaloyl dichloride, 0.5 to 2 percent of acetone and 97.7 to 99.4 percent of normal hexane are mixed to obtain a crosslinking solution II.
7. The method for preparing a high-flux hollow fiber nanofiltration membrane according to claim 5, wherein the preparation step of the first crosslinking solution is as follows:
placing 20% of high polymer polyethersulfone, 30% of polyethylene glycol and 30% of dimethylacetamide in a stirring tank;
Uniformly stirring the feed liquid components for 24 hours at the constant temperature of 70 ℃ until the polyethersulfone is completely dissolved in the solvent;
And vacuumizing for defoaming for more than 7 hours, and cooling to room temperature to obtain a crosslinking solution I.
8. The method for preparing a high-flux hollow fiber nanofiltration membrane according to any one of claims 1 to 7, wherein the specific step of S30 is:
Soaking the dried hollow fiber nanofiltration membrane in a cross-linking solution I and drying;
And soaking the dried hollow fiber nanofiltration membrane in a crosslinking solution II, and then airing to obtain the high-flux hollow fiber nanofiltration membrane.
9. A high-flux hollow fiber nanofiltration membrane, characterized in that the high-flux hollow fiber nanofiltration membrane is prepared by the preparation method of any one of claims 1 to 8.
10. The high flux hollow fiber nanofiltration membrane of claim 9, wherein the molecular weight cutoff of the high flux hollow fiber nanofiltration membrane is 400-1000Da and the pure water flux is 20-25L/m 2. H.bar.
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| CN118949721A (en) * | 2024-09-27 | 2024-11-15 | 南京惟益环保中心(有限合伙) | Hollow fiber nanofiltration membrane and preparation method thereof |
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