CN111437734A - Super-hydrophobic solvent-resistant composite nanofiltration membrane and preparation method thereof - Google Patents
Super-hydrophobic solvent-resistant composite nanofiltration membrane and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a super-hydrophobic solvent-resistant composite nanofiltration membrane and a preparation method thereof. The method for preparing the super-hydrophobic solvent-resistant composite nanofiltration membrane comprises the following steps: (1) providing a base film; (2) forming an aqueous coating on at least a portion of a surface of the base film using an aqueous solution comprising: piperazine, proton absorbent, surfactant and water; (3) forming an oil phase coating on at least part of the surface of the water phase coating far away from the base film by using the oil phase solution, and carrying out interfacial polymerization reaction on the oil phase coating and the water phase coating to form a composite layer; the oil phase solution comprises trimesoyl chloride, a hydrophobic end-capping reagent and n-hexane; (4) and (4) carrying out heat treatment on the product obtained in the step (3) to obtain the super-hydrophobic solvent-resistant composite nanofiltration membrane. The method has the advantages of simple process and mild conditions, and the prepared nanofiltration membrane has strong super-hydrophobicity and solvent resistance and has good application prospect in the field of organic solvent system separation.
Description
Technical Field
The invention relates to the technical field of membrane separation, in particular to a method for preparing a super-hydrophobic solvent-resistant composite nanofiltration membrane and the super-hydrophobic solvent-resistant composite nanofiltration membrane prepared by the method.
Background
Nanofiltration membrane separation is a novel membrane separation technology between ultrafiltration membrane separation and reverse osmosis membrane separation, and is widely applied to a plurality of industrial fields such as hard water softening, removal of a small amount of organic matters in water, dye purification and desalination, separation and purification of organic matters with different molecular weights, and the like. Most of the existing nanofiltration membranes are aqueous and mainly aim at a system using water as a solvent, but in practical industrial application, a large amount of substance separation needs of a non-aqueous solution system exist, so that the nanofiltration membranes are required to have good solvent resistance.
Patent CN106902651A reports a composite film with hydrophilic-hydrophobic gradient change and a preparation method thereof, wherein a silicon dioxide sol and a titanium dioxide sol are positioned and infiltrated on an organic or inorganic base film for multiple times along a specific direction, and the surface roughness of the base film is changed by regulating and controlling inorganic nanoparticles to obtain the composite film with hydrophilic-hydrophobic gradient change.
In patent CN102953105A, an electrochemical deposition technology is adopted to deposit long-chain alkyl siloxane hydrolysate on the surface of a solid, so that the superhydrophobicity of the nanofiltration membrane is realized.
Patent CN103993423A adopts an electrostatic spinning technology, SiO2 nano particles modified by epoxy modified silicone oil are respectively mixed with polystyrene solution and polyacrylonitrile solution to obtain two spinning solutions, and the two spinning solutions are subjected to double-nozzle electrospinning and drying to obtain the super-hydrophobic fiber membrane.
At present, the method for improving the hydrophobicity and the solvent resistance of the nanofiltration membrane is generally to add some hydrophobic inorganic nano particles, however, the existing method for improving the hydrophobicity and the solvent resistance of the nanofiltration membrane still needs to be improved.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, the invention aims to provide a method for preparing a super-hydrophobic solvent-resistant composite nanofiltration membrane and the super-hydrophobic solvent-resistant composite nanofiltration membrane prepared by the method. The method has the advantages of simple process and mild conditions, and the prepared nanofiltration membrane has strong super-hydrophobicity and solvent resistance and has good application prospect in the field of organic solvent system separation.
In one aspect of the invention, the invention provides a method for preparing a super-hydrophobic solvent-resistant composite nanofiltration membrane. According to an embodiment of the invention, the method comprises: (1) providing a base film; (2) forming an aqueous coating on at least a portion of a surface of the base film using an aqueous solution comprising: piperazine, proton absorbent, surfactant and water; (3) forming an oil phase coating on at least part of the surface of the water phase coating far away from the base film by using an oil phase solution, and carrying out interfacial polymerization reaction on the oil phase coating and the water phase coating to form a composite layer; the oil phase solution comprises trimesoyl chloride, a hydrophobic end-capping agent and n-hexane; (4) and (4) carrying out heat treatment on the product obtained in the step (3) to obtain the super-hydrophobic solvent-resistant composite nanofiltration membrane.
According to the method for preparing the super-hydrophobic solvent-resistant composite nanofiltration membrane, the water phase coating and the oil phase coating are sequentially formed on the surface of the base membrane, and the oil phase coating and the water phase coating are subjected to interfacial polymerization reaction to obtain the high-performance composite functional layer. According to the method, the hydrophobic end-capping agent is mixed in the oil phase solution, the structure of the polymer in the composite functional layer is changed through interfacial polymerization, and the prepared super-hydrophobic solvent-resistant composite nanofiltration membrane is more stable in performance. And the hydrophobic end-capping agent is used in a controlled amount, so that the hydrophobicity of the nanofiltration membrane can be adjusted within a certain range to meet the application requirements of the nanofiltration membrane on different occasions. Meanwhile, the method has simple process and mild conditions, and the prepared nanofiltration membrane has strong super-hydrophobicity and solvent resistance and has good application prospect in the field of organic solvent system separation.
In addition, the method for preparing the superhydrophobic solvent-resistant composite nanofiltration membrane according to the embodiment of the invention can also have the following additional technical characteristics:
in some embodiments of the invention, the base membrane is a polysulfone ultrafiltration membrane.
In some embodiments of the invention, the proton absorbent is selected from at least one of sodium carbonate, sodium bicarbonate, sodium phosphate, sodium hydrogen phosphate, sodium hydroxide, potassium hydroxide, triethylamine.
In some embodiments of the invention, the surfactant is selected from at least one of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate.
In some embodiments of the present invention, the aqueous solution comprises 0.1 to 5 wt% of piperazine, 0.1 to 1 wt% of a proton absorbent, 0.05 to 0.3 wt% of a surfactant, and the balance water. Preferably, the aqueous phase solution comprises 1-3 wt% of piperazine, 0.3-0.5 wt% of proton absorbent, 0.1-0.15 wt% of surfactant and the balance of water.
In some embodiments of the invention, the hydrophobic capping agent is selected from at least one of naphthoyl chloride, anthracoyl chloride, anthracenesulfonyl chloride.
In some embodiments of the present invention, the content of the trimesoyl chloride in the oil phase solution is 0.05 to 0.5 wt%, and the ratio of the hydrophobic end-capping agent to the trimesoyl chloride is (1:9) to (4: 1). Preferably, in the oil phase solution, the content of trimesoyl chloride is 0.1-0.2 wt%, and the usage ratio of the hydrophobic end-capping reagent to the trimesoyl chloride is 1: 1.
In some embodiments of the invention, the first coating layer and the second coating layer are formed by dip coating.
In some embodiments of the invention, the heat treatment is performed at 40-80 ℃ for 30 s-5 min.
In some embodiments of the invention, the superhydrophobic solvent-resistant composite nanofiltration membrane product prepared by the method is stored in deionized water.
In another aspect of the invention, the invention provides a super-hydrophobic solvent-resistant composite nanofiltration membrane. According to the embodiment of the invention, the superhydrophobic solvent-resistant composite nanofiltration membrane is prepared by the method for preparing the superhydrophobic solvent-resistant composite nanofiltration membrane. Therefore, the nanofiltration membrane has strong super-hydrophobicity and solvent resistance, has good application prospect in the field of organic solvent system separation, and has the advantages of simple preparation method and mild conditions.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
fig. 1 is a schematic flow chart of a method for preparing a superhydrophobic solvent-resistant composite nanofiltration membrane according to one embodiment of the invention.
Detailed Description
The following describes embodiments of the present invention in detail. The following examples are illustrative only and are not to be construed as limiting the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
In one aspect of the invention, the invention provides a method for preparing a super-hydrophobic solvent-resistant composite nanofiltration membrane. According to an embodiment of the invention, the method comprises: (1) providing a base film; (2) forming an aqueous coating on at least a portion of a surface of the base film using an aqueous solution comprising: piperazine, proton absorbent, surfactant and water; (3) forming an oil phase coating on at least part of the surface of the water phase coating far away from the base film by using the oil phase solution, and carrying out interfacial polymerization reaction on the oil phase coating and the water phase coating to form a composite layer; the oil phase solution comprises trimesoyl chloride, a hydrophobic end-capping reagent and n-hexane; (4) and (4) carrying out heat treatment on the product obtained in the step (3) to obtain the super-hydrophobic solvent-resistant composite nanofiltration membrane.
According to the method for preparing the super-hydrophobic solvent-resistant composite nanofiltration membrane, the water phase coating and the oil phase coating are sequentially formed on the surface of the base membrane, and the oil phase coating and the water phase coating are subjected to interfacial polymerization reaction to obtain the high-performance composite functional layer. According to the method, the hydrophobic end-capping agent is mixed in the oil phase solution, the structure of the polymer in the composite functional layer is changed through interfacial polymerization, and the prepared super-hydrophobic solvent-resistant composite nanofiltration membrane is more stable in performance. And the hydrophobic end-capping agent is used in a controlled amount, so that the hydrophobicity of the nanofiltration membrane can be adjusted within a certain range to meet the application requirements of the nanofiltration membrane on different occasions. Meanwhile, the method has simple process and mild conditions, and the prepared nanofiltration membrane has strong super-hydrophobicity and solvent resistance and has good application prospect in the field of organic solvent system separation.
The method for preparing the superhydrophobic solvent-resistant composite nanofiltration membrane according to the embodiment of the invention is further described in detail below. Referring to fig. 1, according to an embodiment of the invention, the method comprises:
s100: providing a base film
The specific kind of the above-mentioned base film is not particularly limited, and those skilled in the art can select a base film commonly used in the art according to actual needs. According to some embodiments of the invention, the base membrane is a polysulfone ultrafiltration membrane. Therefore, the prepared super-hydrophobic solvent-resistant composite nanofiltration membrane product has better performance.
S200: forming an aqueous coating
In this step, an aqueous coating layer is formed on at least a part of the surface of the base film by an aqueous solution comprising: piperazine (anhydrous piperazine), a proton absorber, a surfactant, and water. According to some embodiments of the present invention, the oil phase coating layer may be formed by dip coating the base film with an oil phase solution.
The proton absorbent has the main function of absorbing acid (such as hydrochloric acid) generated in the interfacial polymerization reaction of the water phase coating and the oil phase coating, and promoting the forward progress of the interfacial polymerization reaction. According to some embodiments of the present invention, the proton absorbent may be at least one selected from the group consisting of sodium carbonate, sodium bicarbonate, sodium phosphate, sodium hydrogen phosphate, sodium hydroxide, potassium hydroxide, and triethylamine. By using the proton absorbent, the forward progress of the interfacial polymerization reaction can be further facilitated.
The primary function of the surfactant is to promote the diffusion of the water phase into the oil phase, thereby increasing the interfacial polymerization rate. According to some embodiments of the present invention, the surfactant may be selected from at least one of sodium dodecyl sulfate, and sodium dodecyl benzene sulfonate. By using the above surfactant, the rate of polymerization can be further increased.
According to some embodiments of the present invention, the aqueous solution comprises 0.1 to 5 wt% of piperazine, 0.1 to 1 wt% of proton absorbent, 0.05 to 0.3 wt% of surfactant, and the balance of water. Specifically, the content of piperazine (anhydrous piperazine) may be 0.1 wt%, 0.5 wt%, 0.8 wt%, 1 wt%, 1.5 wt%, 2 wt%, 2.5 wt%, 3 wt%, 4 wt%, 4.5 wt%, 5 wt%, or the like; the proton absorber may be present in an amount of 0.1 wt%, 0.2 wt%, 0.3 wt%, 0.4 wt%, 0.5 wt%, 0.8 wt%, 1 wt%, etc.; the content of the surfactant may be 0.05 wt%, 0.08 wt%, 0.1 wt%, 0.12 wt%, 0.15 wt%, 0.2 wt%, 0.25 wt%, 0.3 wt%, etc. Preferably, the aqueous solution comprises 1-3 wt% of piperazine, 0.3-0.5 wt% of proton absorbent, 0.1-0.15 wt% of surfactant and the balance of water. The inventor finds in research that if the amount of the anhydrous piperazine is less than 0.1 wt%, the concentration of the aqueous phase monomer is too low, and a complete functional layer is not easily formed; if the content of the anhydrous piperazine is higher than 5 wt%, the water phase concentration is too high during interfacial polymerization, long-chain macromolecules are not easy to form through polymerization, the formed functional layer is loose, and the retention rate is low. If the dosage of the proton absorbent is less than 0.1 wt%, the proton absorbent is not easy to play a role in proton absorption, the normal operation of polymerization reaction cannot be fully ensured, and a compact functional layer is difficult to form; if the proton absorber is used in an amount of more than 0.5 wt%, the basicity is too high, and the formed polyamide functional layer is very susceptible to hydrolysis. If the amount of the surfactant is less than 0.05 wt%, the effect of increasing the reaction speed is not achieved; if the amount of the surfactant is more than 0.3 wt%, the aqueous monomer molecules are easily emulsified to affect the polymerization reaction.
S300: forming an oily coating and undergoing interfacial polymerization
In the step, an oil phase coating is formed on at least part of the surface of the water phase coating far away from the base film by using an oil phase solution, and the oil phase coating and the water phase coating are subjected to interfacial polymerization reaction to form a composite layer; the oil phase solution comprises trimesoyl chloride, a hydrophobic end-capping agent and n-hexane. According to some embodiments of the present invention, the oil phase coating may be formed by dip coating the resulting product of S200 with an oil phase solution.
According to some embodiments of the present invention, the hydrophobic capping agent may be at least one selected from the group consisting of naphthoyl chloride, anthracoyl chloride, and anthracenesulfonyl chloride. The hydrophobic end-capping agent has strong hydrophobicity of a plurality of benzene rings and contains monofunctional acyl chloride. Therefore, the hydrophobic property and the solvent resistance of the super-hydrophobic solvent-resistant composite nanofiltration membrane can be further improved.
According to some embodiments of the present invention, in the oil phase solution, the content of trimesoyl chloride may be 0.05 to 0.5 wt%, and the ratio of the hydrophobic end-capping agent to the trimesoyl chloride may be (1:9) to (4: 1). The trimesoyl chloride may be contained in an amount of 0.05 wt%, 0.08 wt%, 0.1 wt%, 0.15 wt%, 0.2 wt%, 0.25 wt%, 0.3 wt%, 0.5 wt%, etc. The dosage ratio of the hydrophobic end-capping reagent to the trimesoyl chloride can be 1:9, 1:6, 1:2, 1:1, 2:1, 4:1 and the like. Preferably, in the oil phase solution, the content of trimesoyl chloride is 0.1-0.2 wt%, and the ratio of the hydrophobic end-capping agent to the trimesoyl chloride is 1: 1. The inventor finds in research that if the amount of trimesoyl chloride is less than 0.05 wt%, the reaction is insufficient and a complete functional layer cannot be formed; if it exceeds 0.5 wt%, the resulting membrane is too dense and the flux is seriously decreased. If the dosage ratio of the hydrophobic end capping agent to the trimesoyl chloride is too low, the hydrophobic end capping effect cannot be achieved; if the dosage ratio of the hydrophobic end-capping reagent to trimesoyl chloride is too high, a long-chain polymer cannot be formed, the functional layer is not compact, and even the functional layer cannot be formed.
S400: thermal treatment
In the step, the product obtained in the step S300 is subjected to heat treatment to obtain the super-hydrophobic solvent-resistant composite nanofiltration membrane.
According to some embodiments of the invention, the heat treatment is performed at 40-80 ℃ for 30 s-5 min. Specifically, the heat treatment temperature may be 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃ and the like, and the heat treatment time may be 30s, 1min, 2min, 3min, 4min, 5min and the like. The inventor finds that the short heat treatment time or the low heat treatment temperature can cause the heat treatment effect to be not obvious, the polymerization degree is not enough, and the product interception is low; and if the heat treatment time is too long or the heat treatment temperature is too high, the base film is shrunk, and the product flux is reduced.
In another aspect of the invention, the invention provides a super-hydrophobic solvent-resistant composite nanofiltration membrane. According to the embodiment of the invention, the superhydrophobic solvent-resistant composite nanofiltration membrane is prepared by the method for preparing the superhydrophobic solvent-resistant composite nanofiltration membrane. Therefore, the nanofiltration membrane has strong super-hydrophobicity and solvent resistance, has good application prospect in the field of organic solvent system separation, and has the advantages of simple preparation method and mild conditions.
In addition, it should be noted that all the features and advantages described above for the method for preparing the superhydrophobic solvent-resistant composite nanofiltration membrane are also applicable to the superhydrophobic solvent-resistant composite nanofiltration membrane. And will not be described in detail herein.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way.
Example 1
2 wt% of anhydrous piperazine, 0.1 wt% of sodium hydroxide and 0.1 wt% of sodium dodecyl sulfate are dissolved in water to prepare an aqueous solution. 0.1 wt% of trimesoyl chloride and 0.1 wt% of hydrophobic end-capping agent 2-naphthalenesulfonyl chloride are dissolved in n-hexane to prepare an oil phase solution. Soaking the cleaned polysulfone ultrafiltration base membrane in the water phase solution for 40s, taking out the polysulfone ultrafiltration base membrane, drying the redundant water on the surface by using an air knife, soaking the polysulfone ultrafiltration base membrane in the oil phase solution for 1min, taking out the polysulfone ultrafiltration base membrane, placing the polysulfone ultrafiltration base membrane in an oven at 60 ℃ for drying for 2min to finally obtain a finished nanofiltration membrane, and placing the nanofiltration membrane in deionized water to be detected.
Example 2
3 wt% of anhydrous piperazine, 0.1 wt% of sodium carbonate and 0.1 wt% of sodium dodecyl sulfate are dissolved in water to prepare an aqueous solution. 0.2 wt% of trimesoyl chloride and 0.05 wt% of hydrophobic end-capping agent 2-naphthalenesulfonyl chloride are dissolved in n-hexane to prepare an oil phase solution. Soaking the cleaned polysulfone ultrafiltration base membrane in the water phase solution for 40s, taking out the polysulfone ultrafiltration base membrane, drying the redundant water on the surface by using an air knife, soaking the polysulfone ultrafiltration base membrane in the oil phase solution for 1min, taking out the polysulfone ultrafiltration base membrane, placing the polysulfone ultrafiltration base membrane in an oven at 80 ℃ for drying for 1min, and finally obtaining a finished nanofiltration membrane to be detected, and placing the nanofiltration membrane in deionized water.
Example 3
2 wt% of anhydrous piperazine, 0.1 wt% of potassium hydroxide and 0.1 wt% of sodium dodecyl sulfate are dissolved in water to prepare an aqueous solution. 0.15 wt% of trimesoyl chloride and 0.05 wt% of hydrophobic end-capping agent 1-anthracene formyl chloride are dissolved in normal hexane to prepare an oil phase solution. Soaking the cleaned polysulfone ultrafiltration base membrane in the water phase solution for 40s, taking out the polysulfone ultrafiltration base membrane, drying the redundant water on the surface by using an air knife, soaking the polysulfone ultrafiltration base membrane in the oil phase solution for 1min, taking out the polysulfone ultrafiltration base membrane, placing the polysulfone ultrafiltration base membrane in an oven at 60 ℃ for drying for 1min, and finally obtaining a finished nanofiltration membrane to be detected, and placing the nanofiltration membrane in deionized water.
Example 4
2 wt% of anhydrous piperazine, 0.1 wt% of sodium hydroxide and 0.1 wt% of sodium dodecyl sulfate are dissolved in water to prepare an aqueous solution. 0.2 wt% of trimesoyl chloride and 0.1 wt% of hydrophobic end-capping agent 1-naphthoyl chloride are dissolved in n-hexane to prepare an oil phase solution. Soaking the cleaned polysulfone ultrafiltration base membrane in the water phase solution for 40s, taking out the polysulfone ultrafiltration base membrane, drying the redundant water on the surface by using an air knife, soaking the polysulfone ultrafiltration base membrane in the oil phase solution for 1min, taking out the polysulfone ultrafiltration base membrane, placing the polysulfone ultrafiltration base membrane in an oven at 80 ℃ for drying for 1min, and finally obtaining a finished nanofiltration membrane to be detected, and placing the nanofiltration membrane in deionized water.
Comparative example
2 wt% of anhydrous piperazine, 0.1 wt% of sodium hydroxide and 0.1 wt% of sodium dodecyl sulfate are dissolved in water to prepare an aqueous solution. 0.2 wt% of trimesoyl chloride is dissolved in normal hexane to prepare an oil phase solution. Soaking the cleaned polysulfone ultrafiltration base membrane in the water phase solution for 40s, taking out the polysulfone ultrafiltration base membrane, drying the redundant water on the surface by using an air knife, soaking the polysulfone ultrafiltration base membrane in the oil phase solution for 1min, taking out the polysulfone ultrafiltration base membrane, placing the polysulfone ultrafiltration base membrane in an oven at 60 ℃ for drying for 2min to finally obtain a finished nanofiltration membrane, and placing the nanofiltration membrane in deionized water to be detected.
Test example
The nanofiltration membranes prepared in examples 1-4 and comparative examples were compared in separation performance and solvent resistance under the conditions of 25 ℃ and 1.0MPa, 100 mg-L-1And (3) measuring the rejection rate and the corresponding solvent flux of the prepared nanofiltration membrane by using the rhodamine B (479Da) -ethanol solution. The results are shown in Table 1.
TABLE 1 comparison of nanofiltration Membrane separation Performance between comparative and example
| Retention (%) | Water flux (L MH) | |
| Example 1 | 97.43 | 81.4 |
| Example 2 | 98.57 | 75.2 |
| Example 3 | 97.75 | 77.2 |
| Example 4 | 98.29 | 71.9 |
| Comparative example | 75.22 | 123.4 |
Test results show that the nanofiltration membrane prepared by the comparative example is easy to swell in ethanol, so that the rejection rate is reduced, and the water flux is increased. The nanofiltration membrane prepared in the embodiment 1-4 has good and stable separation performance and water flux performance in ethanol through hydrophobic end capping, which indicates that the nanofiltration membrane has good solvent resistance.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. A method for preparing a super-hydrophobic solvent-resistant composite nanofiltration membrane is characterized by comprising the following steps:
(1) providing a base film;
(2) forming an aqueous coating on at least a portion of a surface of the base film using an aqueous solution comprising: piperazine, proton absorbent, surfactant and water;
(3) forming an oil phase coating on at least part of the surface of the water phase coating far away from the base film by using an oil phase solution, and carrying out interfacial polymerization reaction on the oil phase coating and the water phase coating to form a composite layer; the oil phase solution comprises trimesoyl chloride, a hydrophobic end-capping agent and n-hexane;
(4) and (4) carrying out heat treatment on the product obtained in the step (3) to obtain the super-hydrophobic solvent-resistant composite nanofiltration membrane.
2. The method of claim 1, wherein the base membrane is a polysulfone ultrafiltration membrane.
3. The method according to claim 1, wherein the proton absorbent is selected from at least one of sodium carbonate, sodium bicarbonate, sodium phosphate, sodium hydrogen phosphate, sodium hydroxide, potassium hydroxide, and triethylamine.
4. The method of claim 1, wherein the surfactant is selected from at least one of sodium dodecyl sulfate, and sodium dodecyl benzene sulfonate.
5. The method according to claim 1, wherein the aqueous solution comprises 0.1 to 5 wt% of piperazine, 0.1 to 1 wt% of a proton absorbent, 0.05 to 0.3 wt% of a surfactant, and the balance of water.
6. The method of claim 1, wherein the hydrophobic capping agent is selected from at least one of naphthoyl chloride, anthracoyl chloride, anthracenesulfonyl chloride.
7. The method according to claim 1, wherein the content of the trimesoyl chloride in the oil phase solution is 0.05-0.5 wt%, and the usage ratio of the hydrophobic end-capping agent to the trimesoyl chloride is (1:9) - (4: 1).
8. The method of claim 1, wherein the first coating and the second coating are formed by dip coating.
9. The method according to claim 1, wherein the heat treatment is performed at 40 to 80 ℃ for 30s to 5 min.
10. A super-hydrophobic solvent-resistant composite nanofiltration membrane, which is prepared by the method for preparing the super-hydrophobic solvent-resistant composite nanofiltration membrane according to any one of claims 1 to 9.
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| CN113694727A (en) * | 2021-09-24 | 2021-11-26 | 中国农业大学 | Surfactant modified high-flux polyamide nanofiltration membrane and preparation method thereof |
| CN115253717A (en) * | 2022-07-21 | 2022-11-01 | 中国科学院过程工程研究所 | Hydrophilic and hydrophobic composite membrane and preparation method and application thereof |
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| CN115253717A (en) * | 2022-07-21 | 2022-11-01 | 中国科学院过程工程研究所 | Hydrophilic and hydrophobic composite membrane and preparation method and application thereof |
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