CN113289500A - Preparation method of high-flux reverse osmosis membrane and high-flux reverse osmosis membrane obtained by preparation method - Google Patents
Preparation method of high-flux reverse osmosis membrane and high-flux reverse osmosis membrane obtained by preparation method Download PDFInfo
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Abstract
The invention provides a preparation method of a high-flux reverse osmosis membrane, which comprises the following steps: step one, manufacturing a supporting structure; depositing a nano calcium carbonate layer on the supporting structure; and step three, performing interfacial polymerization reaction on the support structure deposited with the nano calcium carbonate layer to form the reverse osmosis membrane containing the polyamide functional layer. According to the invention, the nano calcium carbonate is deposited on the surface of the supporting structure in situ, so that the surface roughness of the supporting layer is improved, the adsorption of a water phase solution is facilitated, and meanwhile, the nano calcium carbonate is used as a barrier layer, so that the growth of polyamide in the interfacial polymerization reaction process is reasonably limited, the depth of the polyamide in the holes of the supporting structure is reduced, the water conduction resistance is reduced, and the flux of the reverse osmosis membrane is improved. The invention also provides a high-flux reverse osmosis membrane, the water flux of the high-flux reverse osmosis membrane is 79-123LMH, and the salt rejection rate of the high-flux reverse osmosis membrane is 95.74-99.39%.
Description
Technical Field
The invention relates to the technical field of reverse osmosis membrane preparation, in particular to a preparation method of a high-flux reverse osmosis membrane and the high-flux reverse osmosis membrane.
Background
The reverse osmosis technology is one of the most important and effective water purification technologies, has the advantages of high separation efficiency, low cost and the like, and is widely applied to the fields of seawater desalination, brackish water desalination, reclaimed water recycling, ultrapure water preparation and the like.
In the application process of the reverse osmosis membrane, flux and salt rejection are used as two parameters for evaluating the core performance of the reverse osmosis membrane, and the higher the flux is, the more purified water is under the same condition, and the lower the energy consumption is. However, the traditional reverse osmosis membrane preparation method tends to decrease the desalination rate while increasing the flux, and thus the quality of water is also decreased, and therefore, how to break through the trade-off problem (trade-off phenomenon) between the flux and the desalination rate of the reverse osmosis membrane, and preparing the reverse osmosis membrane with high flux while maintaining a high desalination rate becomes a hot spot of current research.
Currently, the most commercially available reverse osmosis membrane is a polyamide composite reverse osmosis membrane, which is mainly composed of a non-woven fabric layer, a polysulfone layer, and a polyamide functional layer, wherein the polyamide functional layer often determines the performance of the reverse osmosis membrane. In the prior art:
for example, patent application CN111790277A discloses a method for preparing a high performance reverse osmosis membrane for promoting growth of polyamide nanovesicles, which is to introduce potassium perfluorobutylsulfonate into a water phase to promote growth of polyamide nanovesicles, increase surface roughness of the membrane, and further improve permeation flux of the membrane. The technical scheme has the disadvantage that the flux increasing capacity of the reverse osmosis membrane prepared by the additive similar to the water phase or the oil phase is limited.
For example, patent CN109847586A discloses a high flux reverse osmosis membrane, a preparation method and an application thereof, which is to prepare a basement membrane from a polymer solution dispersed with inorganic silicate nano-materials, then invade the basement membrane into a dopamine/ZIF-8 suspension to obtain a basement membrane with a dopamine/ZIF-8 intermediate nano-layer, and then perform interfacial polymerization to obtain the high flux reverse osmosis membrane. The technical scheme has the defects that the preparation method is complicated, the cost is high, and industrial production is difficult to realize.
Therefore, it is important to develop a method for preparing a reverse osmosis membrane that can achieve both desalination rate and flux.
Disclosure of Invention
The invention provides a preparation method of a high-flux reverse osmosis membrane, which greatly improves the flux of the reverse osmosis membrane on the basis of maintaining high desalination rate, solves the problem of long-term elimination of flux and desalination rate of the reverse osmosis membrane, and is simple and efficient, and easy for industrial production. The specific technical scheme is as follows:
a preparation method of a high-flux reverse osmosis membrane comprises the following steps:
step one, manufacturing a supporting structure;
step two, depositing a nano calcium carbonate layer on the support structure obtained in the step one;
and step three, performing interfacial polymerization reaction on the support structure deposited with the nano calcium carbonate layer to form the reverse osmosis membrane containing the polyamide functional layer.
Preferably, the second step is specifically: soaking the support structure obtained in the step one in CaCl2After the aqueous solution is used for a period of time, transferring the aqueous solution into a carbonate aqueous solution with the same concentration to obtain a support structure with a nano calcium carbonate layer deposited in situ; wherein: CaCl2The concentration of the aqueous solution is 0.05-1mol/L, and the soaking time is 1-5 min; the aqueous carbonate solution is K2CO3、Na2CO3、(NH4)2CO3At least one of aqueous solutions.
Preferably, in the interfacial polymerization reaction of the third step: the aqueous phase solution is m-phenylenediamine solution; the oil phase solution is trimesoyl chloride solution.
Preferably, the aqueous phase solution is an aqueous solution of 1-5 wt% of m-phenylenediamine and 0.05-0.2 wt% of sodium dodecyl benzene sulfonate; the oil phase solution is 0.1-0.2 wt% trimesoyl chloride solution, and the solvent of the oil phase solution is at least one of n-hexane, cyclohexane, heptane, octane, and ISOPAR-G (such as Ixon Mobil chemical production).
Preferably, the step one of manufacturing the support structure specifically comprises: uniformly coating the polymer solution on non-woven fabrics by using a scraper after the polymer solution is subjected to vacuum degassing, then placing the non-woven fabrics in a pure water coagulating bath to be converted into a film, and cleaning the film to obtain a supporting structure; wherein: the polymer solution is at least one of polysulfone solution, polyether sulfone solution and polyphenylsulfone solution; the concentration of the polymer solution is 15 wt% to 20 wt%.
Preferably, the method further comprises a fourth step, wherein the fourth step specifically comprises the following steps: and (3) putting the reverse osmosis membrane containing the polyamide functional layer prepared in the step three into an oxidant solution with the concentration of 1-5 wt% for cleaning, and then cleaning with pure water to obtain the high-flux reverse osmosis membrane.
Preferably, the oxidant solution is a citric acid solution and/or an acetic acid solution.
The high-flux reverse osmosis membrane obtained by the preparation method comprises a supporting structure and a polyamide functional layer arranged on the supporting structure, has the water flux of 79-123LMH, and has the salt rejection rate of 95.74-99.39%.
The technical scheme of the invention has the following beneficial effects:
1. the preparation method of the invention firstly manufactures the supporting structure, then deposits the nano calcium carbonate layer on the supporting structure, and finally carries out interfacial polymerization reaction to form the reverse osmosis membrane containing the polyamide functional layer. The optimization of the structure of the polyamide functional layer is the most effective way for improving the selective permeability of the reverse osmosis membrane, and the scheme of the invention is specifically represented in three aspects: firstly, the nano calcium carbonate is deposited on the surface of the supporting structure in situ, so that the surface roughness of the supporting layer is improved, the adsorption of a water phase solution is facilitated, and meanwhile, the nano calcium carbonate is used as a barrier layer, so that the boundary is reasonably limitedThe polyamide grows in the surface polymerization reaction process, so that the depth of the polyamide in the holes of the supporting structure is reduced, the water conduction resistance is reduced, and the flux of the reverse osmosis membrane is improved; secondly, the polyamide functional layer obtained by the preparation method contains a large number of nano holes which determine the performance of the reverse osmosis membrane, and the nano holes are mainly formed by the release of dissolved gases caused by the heat release of interfacial polymerization reaction, and the mechanism is as follows: the interfacial polymerization reaction in the present invention mainly includes a main reaction between m-phenylenediamine and trimesoyl chloride and a side reaction between one of the by-products of the main reaction (e.g., HCl) and nano calcium carbonate on the supporting structure, which consumes the nano calcium carbonate and further reduces the water conduction resistance, and the side reaction product includes CO2，CO2The presence of (A) can influence the structure of the polyamide functional layer, i.e. CO2Due to the existence and the non-directional characteristic of the polyamide functional layer, a large number of nano holes appear in the forming process of the polyamide functional layer, so that the flux of the reverse osmosis membrane is improved; thirdly, the consumption of the side reaction HCl can promote the main reaction, and the crosslinking degree of the polyamide is improved, so that the high salt rejection rate of the reverse osmosis membrane is maintained.
2. The in-situ deposition of the nano calcium carbonate is specifically as follows: soaking the support structure in CaCl2After the aqueous solution is used for a period of time, transferring the aqueous solution into a carbonate aqueous solution with the same concentration to obtain a support structure with a nano calcium carbonate layer deposited in situ; wherein: CaCl2The concentration of the aqueous solution is 0.05-1mol/L, and the soaking time is 1-5 min; the aqueous carbonate solution is K2CO3、Na2CO3、(NH4)2CO3At least one of aqueous solutions. The calcium chloride and the carbonate and the proper condition parameters are adopted, so that the generation of the nano calcium carbonate can be ensured, and the nano calcium carbonate can be ensured to be deposited on the supporting structure.
3. In the interfacial polymerization reaction of the present invention: the aqueous phase solution is m-phenylenediamine solution; the oil phase solution is trimesoyl chloride solution. Preferably: the aqueous phase solution is an aqueous solution of m-phenylenediamine with the concentration of 1 to 5 weight percent and sodium dodecyl benzene sulfonate with the concentration of 0.05 to 0.2 weight percent; the oil phase solution is 0.1-0.2 wt% trimesoyl chloride solution, and the solvent of the oil phase solution is n-hexane. Not only can ensure the formation of the polyamide layer, but also can ensure the generation of byproducts such as HCL and the like which can effectively react with nano calcium carbonate in the formation process of the polyamide layer, and ensure the high desalination rate and high flux of the reverse osmosis membrane.
4. The support structure manufactured in the invention specifically comprises the following steps: uniformly coating the polymer solution on non-woven fabrics by using a scraper after the polymer solution is subjected to vacuum degassing, then placing the non-woven fabrics in a pure water coagulating bath to be converted into a film, and cleaning the film to obtain a supporting structure; wherein: the polymer solution is at least one of polysulfone solution, polyether sulfone solution and polyphenylsulfone solution; the concentration of the polymer solution is 15 wt% to 20 wt%. The surface of the supporting structure is of a film structure, which is beneficial to the effective deposition of the nano calcium carbonate.
5. The invention also comprises a post-treatment step, which specifically comprises the following steps: and (3) putting the reverse osmosis membrane containing the polyamide functional layer prepared in the step three into an oxidant solution with the concentration of 1-5 wt% for cleaning, and then cleaning with pure water to obtain the high-flux reverse osmosis membrane. And the post-treatment step is used for removing redundant nano calcium carbonate and improving the performance of the reverse osmosis membrane.
The invention also provides a high-energy reverse osmosis membrane obtained by the preparation method, which comprises a supporting structure and a polyamide functional layer arranged on the supporting structure, wherein the water flux of the high-energy reverse osmosis membrane is 79-123LMH, and the salt rejection rate of the high-energy reverse osmosis membrane is 95.74-99.39%. The high-flux reverse osmosis membrane prepared by the method has thinner polyamide functional layer, the polyamide separation layer is of a large-blade structure containing a large number of nano holes, the relative effective permeation area is larger, the water conduction resistance is smaller, meanwhile, the crosslinking degree of the polyamide functional layer is improved, and the high desalination rate is maintained while the flux of the reverse osmosis membrane is improved.
Drawings
FIG. 1 is a schematic diagram of reverse osmosis membrane preparation, wherein: (a) is a preparation schematic diagram of comparative example 1; (b) comparative example 2 is a schematic diagram of the preparation of less precipitated nano calcium carbonate; (c) a schematic diagram was prepared for example 1; (d) comparative example 3 preparation schematic diagram of in-situ deposition of more nano calcium carbonate;
FIG. 2 is a scanning electron microscope image of the surface of the reverse osmosis membrane in comparative example 1;
FIG. 3 is a scanning electron microscope image of the surface of the high flux reverse osmosis membrane in example 1.
Detailed Description
The embodiments of the invention are described in detail below with reference to examples, but the invention can be implemented in many different ways as defined and covered by the claims.
Example 1:
a preparation method of a reverse osmosis membrane, which is a high-flux reverse osmosis membrane, comprises the following steps:
step one, preparing a support structure: preparing 18 wt% of polysulfone solution, filtering to remove undissolved impurities, uniformly coating the polymer solution on non-woven fabric by using a scraper after vacuum degassing, then placing the non-woven fabric in a pure water coagulating bath at 15 ℃ for 1min, converting the non-woven fabric into a membrane, and cleaning to obtain the porous support membrane;
step two, in-situ deposition of nano calcium carbonate: soaking the support structure prepared in the step 1 in CaCl with the concentration of 0.1mol/L2After a period of time (specifically 3min) in the aqueous solution, it was transferred to 0.1mo/L Na2CO3In the water solution, the supporting structure with the nano calcium carbonate deposited in situ is obtained after being washed for three times by pure water;
step three, preparation of aqueous phase solution: preparing m-phenylenediamine with the concentration of 3 wt% and a sodium dodecyl benzene sulfonate aqueous solution with the concentration of 0.1 wt%, wherein the m-phenylenediamine is a water phase reaction monomer, and the sodium dodecyl benzene sulfonate is a surfactant;
step four, preparation of oil phase solution: preparing 0.12 wt% of trimesoyl chloride, wherein the solvent of the oil phase solution is n-hexane;
step five, interfacial polymerization: soaking the prepared porous support membrane in an aqueous phase solution for 30s, taking out, removing excessive water on the surface, soaking in an oil phase solution for 20s, and carrying out interfacial polymerization to obtain a reverse osmosis membrane containing a polyamide functional layer; the main reaction formula of the interfacial polymerization is as follows:
step six, cleaning: and (4) putting the reverse osmosis membrane prepared in the step five into a 2 wt% citric acid solution for 30s for cleaning, mainly removing redundant in-situ deposited nano calcium carbonate particles, and then cleaning with pure water for 30s to obtain the high-flux reverse osmosis membrane.
The preparation principle of the high-flux reverse osmosis membrane is shown in figure 1 (c). The surface scanning electron microscope image of the high-flux reverse osmosis membrane is shown in figure 3.
Example 2-example 6:
example 2 differs from example 1 in that: CaCl in the second step2And Na2CO3The concentration of the aqueous solution was 0.05mol/L, and the others were unchanged.
Example 3 differs from example 1 in that: CaCl in the second step2And Na2CO3The concentration of the aqueous solution was 0.6mol/L, and the others were unchanged.
Example 4 differs from example 1 in that: CaCl in the second step2And Na2CO3The concentration of the aqueous solution is 1mol/L, and the others are unchanged.
Example 5 differs from example 2 in that: in the second step, Na2CO3The aqueous solution is K2CO3Aqueous solution, otherwise unchanged.
Example 6 differs from example 2 in that: in the second step, Na2CO3The aqueous solution is (NH)4)2CO3Aqueous solution, otherwise unchanged.
Comparative example 1:
step one, preparing a support structure: preparing 18 wt% of polysulfone solution, filtering to remove undissolved impurities, uniformly coating the polymer solution on non-woven fabric by using a scraper after vacuum degassing, then placing the non-woven fabric in a pure water coagulating bath at 15 ℃ for 1min, converting the non-woven fabric into a membrane, and cleaning to obtain the porous support membrane;
step two, preparation of aqueous phase solution: preparing m-phenylenediamine with the concentration of 3 wt% and sodium dodecyl benzene sulfonate aqueous solution with the concentration of 0.1 wt%, wherein the m-phenylenediamine is a water phase reaction monomer, and the sodium dodecyl benzene sulfonate is a surfactant.
Step three, preparation of oil phase solution: 0.12 wt% of trimesoyl chloride is prepared, and the oil phase solvent is normal hexane.
Step four, interfacial polymerization: and soaking the prepared porous support membrane in the water phase solution for 30s, taking out, removing excessive water on the surface, soaking in the oil phase solution for 20s, and carrying out interfacial polymerization to obtain the reverse osmosis membrane.
The preparation principle of the high-flux reverse osmosis membrane is shown in detail in figure 1(a), and the surface scanning electron micrograph thereof is shown in figure 2.
Comparative example 2:
the difference from example 1 is: CaCl in the second step2And Na2CO3The concentration of the aqueous solution was 0.04mol/L, and the others were unchanged.
The manufacturing principle of the reverse osmosis membrane is shown in fig. 1 (b).
Comparative example 3:
the difference from example 1 is: CaCl in the second step2And Na2CO3The concentration of the aqueous solution was 1.2mol/L, and the others were unchanged.
The manufacturing principle of the reverse osmosis membrane is shown in fig. 1 (d).
And (3) testing the performance of the membrane:
the antibacterial polyamide reverse osmosis membranes prepared in examples 1 to 6 and the polyamide reverse osmosis composite membranes produced in comparative examples 1 to 3 were placed on a cross-flow type membrane test bed, and a test was performed under conditions of an operating pressure of 150 psi, raw water of 1500ppm NaCl aqueous solution at a temperature of 25 c and a pH of 6.5 to 7.5, and the water flux (J) and the salt rejection (R) of the polyamide reverse osmosis membranes were calculated according to the formulas P1 and P2, respectively, as detailed in table 1.
Calculating formula P1: j ═ V/(sxt);
wherein the water flux (J) is the volume (V) of water passing through a unit membrane area (S) per unit time (t) under a certain operation condition, and the unit of the water flux (J) is L.m-2·h-1(ii) a V is permeate volume (in L); s is the effective surface area (in m) of the polyamide reverse osmosis membrane2) (ii) a t is the water permeation time (in h).
Calculating formula P2: r ═ 1-Cp/Cf)×100％；
Wherein R represents the rejection rate of the polyamide reverse osmosis membrane to the solute, namely the salt rejection rate (%), Cp、CfRespectively showing the concentration of a penetrating fluid and the concentration of raw water after the raw water passes through a polyamide reverse osmosis membrane.
TABLE 1 comparison of Performance of high flux Polyamide composite membranes according to examples 1-6 of the present invention and comparative examples 1-3
By combining the surface scanning electron micrographs of example 1 and comparative example 1, it can be seen that: the surface of the reverse osmosis membrane prepared in the example 1 is in a nodular structure, while the surface of the reverse osmosis membrane prepared in the comparative example 1 is obviously in a large-blade structure, and the morphological structures of the two are obviously different.
As can be seen from table 1:
1. as can be seen from examples 1 to 6 of the invention, the high-flux reverse osmosis membrane obtained by the invention has the water flux of 79 to 123LMH, the desalination rate of 95.74 to 99.39 percent, and compared with comparative example 1, the flux is greatly improved (improved by 119 to 241 percent) on the basis of keeping the high desalination rate. Therefore, the method utilizes the support structure to carry out in-situ deposition of nano calcium carbonate particles for interfacial polymerization, utilizes the reaction of byproduct HCl generated by the reaction of aniline and acyl chloride and nano calcium carbonate to generate carbon dioxide gas, adjusts the structure of the polyamide functional layer, prepares a large-blade structure and improves the flux; meanwhile, the consumption of the product promotes the forward reaction, the crosslinking degree of the polyamide functional layer is improved, and the high desalting rate is still maintained.
2. Combining examples 1-6 and comparative examples 2-3 of the present invention, it can be seen that the nano calcium carbonate layer has a great influence on the overall performance of the reverse osmosis membrane, and from fig. 1(c), the amount of the nano calcium carbonate layer is appropriate, which can not only generate sufficient gas, but also ensure the cross-linking of the polyamide layer, and can effectively take into account the flux and salt rejection rate of the reverse osmosis membrane. When the nano calcium carbonate is too little, the gas is not generated enough, the influence on the polyamide layer is not clear, and the flux is not obviously improved; when the amount of the nano calcium carbonate is too large, as shown in fig. 1(d), the produced nano calcium carbonate is agglomerated or has a large size, which affects interfacial polymerization, and simultaneously generates excessive gas, increases pressure, breaks through a nano cavity structure, causes defects in the produced polyamide functional layer, and thus the salt rejection rate is reduced.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A preparation method of a high-flux reverse osmosis membrane is characterized by comprising the following steps:
step one, manufacturing a supporting structure;
step two, depositing a nano calcium carbonate layer on the support structure obtained in the step one;
and step three, performing interfacial polymerization reaction on the support structure deposited with the nano calcium carbonate layer to form the reverse osmosis membrane containing the polyamide functional layer.
2. The preparation method according to claim 1, wherein the second step is specifically: soaking the support structure obtained in the step one in CaCl2After the aqueous solution is used for a period of time, transferring the aqueous solution into a carbonate aqueous solution with the same concentration to obtain a support structure with a nano calcium carbonate layer deposited in situ; wherein: CaCl2The concentration of the aqueous solution is 0.05-1mol/L, and the soaking time is 1-5 min; the aqueous carbonate solution is K2CO3、Na2CO3、(NH4)2CO3At least one of aqueous solutions.
3. The method according to claim 1, wherein in the interfacial polymerization reaction of step three: the aqueous phase solution is m-phenylenediamine solution; the oil phase solution is trimesoyl chloride solution.
4. The production method according to claim 3, wherein the aqueous phase solution is an aqueous solution of 1 to 5% by weight of m-phenylenediamine and 0.05 to 0.2% by weight of sodium dodecylbenzenesulfonate; the oil phase solution is 0.1-0.2 wt% trimesoyl chloride solution, and the solvent of the oil phase solution is at least one of n-hexane, cyclohexane, heptane, octane, and ISOPAR-G.
5. The method according to claim 1, wherein the step one of fabricating the support structure comprises: uniformly coating the polymer solution on non-woven fabrics by using a scraper after the polymer solution is subjected to vacuum degassing, then placing the non-woven fabrics in a pure water coagulating bath to be converted into a film, and cleaning the film to obtain a supporting structure; wherein: the polymer solution is at least one of polysulfone solution, polyether sulfone solution and polyphenylsulfone solution; the concentration of the polymer solution is 15 wt% to 20 wt%.
6. The method according to any one of claims 1 to 5, further comprising a fourth step, wherein the fourth step is specifically: and (3) putting the reverse osmosis membrane containing the polyamide functional layer prepared in the step three into an oxidant solution with the concentration of 1-5 wt% for cleaning, and then cleaning with pure water to obtain the high-flux reverse osmosis membrane.
7. The method according to claim 6, wherein the oxidizing agent solution is a citric acid solution and/or an acetic acid solution.
8. A high flux reverse osmosis membrane having a water flux of 79 to 123LMH and a salt rejection of 95.74 to 99.39% obtained by the production method according to any one of claims 1 to 7, comprising a support structure and a polyamide functional layer provided on the support structure.
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