CN112657353A - Preparation method of electrically neutral polyamide composite reverse osmosis membrane material - Google Patents
Preparation method of electrically neutral polyamide composite reverse osmosis membrane material Download PDFInfo
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- CN112657353A CN112657353A CN202110279041.9A CN202110279041A CN112657353A CN 112657353 A CN112657353 A CN 112657353A CN 202110279041 A CN202110279041 A CN 202110279041A CN 112657353 A CN112657353 A CN 112657353A
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Abstract
The invention discloses a preparation method of an electrically neutral polyamide composite reverse osmosis membrane material, which specifically comprises the following steps: step one, interfacial polymerization is carried out to form a polyamide composite reverse osmosis membrane A; step two, cleaning a monomer of the polyamide composite reverse osmosis membrane A to obtain a polyamide composite reverse osmosis membrane B; step three, treating the polyamide composite reverse osmosis membrane B by a cleaning activating agent to obtain a polyamide composite reverse osmosis membrane C; the wash activator comprises a functional agent; and step four, carrying out post-treatment on the polyamide composite reverse osmosis membrane C to obtain the neutral polyamide composite reverse osmosis membrane. The preparation method of the electrically neutral polyamide composite reverse osmosis membrane material has the characteristics that: the charge state of the surface of the membrane can be effectively changed; the prepared membrane material keeps higher desalination rate, and the water yield is greatly improved; the anti-pollution performance of the membrane material can be improved; the preparation method is simple and easy to operate, the process is controllable, and industrial scale production can be realized.
Description
Technical Field
The invention relates to the technical field of reverse osmosis membranes, in particular to a preparation method of an electrically neutral polyamide composite reverse osmosis membrane material.
Background
The reverse osmosis membrane is the core of reverse osmosis technology, and the most widely used membrane material at present is a polyamide composite reverse osmosis membrane. The surface of the existing polyamide reverse osmosis membrane usually has more negative charges, and when sewage is treated, the surface of the membrane can easily adsorb a cationic surfactant to cause the fouling of the membrane material, so that the water yield of the membrane is greatly reduced, and the recovery by chemical cleaning is difficult.
In the prior art, there are some methods for post-treating reverse osmosis membrane materials:
CN102974221B discloses a method for controlling surface potential of a reverse osmosis membrane, which adopts NaClO solution to oxidize the reverse osmosis membrane so as to reduce zeta potential value of the membrane surface; the treatment method can change the charge state of the membrane surface, but active chlorine is also a main substance for destroying amide bonds, so that defects are generated in a functional layer to reduce the separation performance of the membrane.
CN106345299A discloses a method for improving performance of reverse osmosis membrane, which comprises subjecting reverse osmosis membrane to acid washing and then to chemical surface treatment with chemical surface treatment agent, so as to remove active substances on the membrane surface, improve the performance of the membrane surface, remove residual monomers on the membrane surface in advance, and improve the chemical composition of the membrane surface. The treatment method can remove residual functional monomers on the surface of the reverse osmosis membrane, but the charge state on the functional layer on the surface of the membrane is not changed.
Therefore, it is important to develop a reverse osmosis membrane which can effectively reduce the electronegativity of the membrane and has excellent membrane performance.
Disclosure of Invention
The invention provides a preparation method of an electrically neutral polyamide composite reverse osmosis membrane material, which is characterized in that: the charge state of the surface of the membrane can be effectively changed; the prepared membrane material keeps higher desalination rate, and the water yield is greatly improved; the anti-pollution performance of the membrane material can be improved; the preparation method is simple and easy to operate, the process is controllable, and industrial scale production can be realized. The specific technical scheme is as follows:
a preparation method of an electrically neutral polyamide composite reverse osmosis membrane material comprises the following steps:
the method comprises the following steps: interfacial polymerization to form a polyamide composite reverse osmosis membrane A;
step two: cleaning a monomer of the polyamide composite reverse osmosis membrane A obtained in the step one to obtain a polyamide composite reverse osmosis membrane B;
step three: treating the polyamide composite reverse osmosis membrane B obtained in the step two by using a cleaning activating agent to obtain a polyamide composite reverse osmosis membrane C; the cleaning activator comprises a functional reagent or a mixed solution of the functional reagent and water, wherein the functional reagent is at least one of p-hydroxybenzoic acid, phenol, toluene, xylene, pyridine, tetrahydrofuran and aminopropanediol;
step four: and (4) carrying out aftertreatment on the polyamide composite reverse osmosis membrane C obtained in the step three to obtain the neutral polyamide composite reverse osmosis membrane.
Preferably, the cleaning activator in the third step is used for dissolving and removing linear chain oligomers (linear chain structures) on the surface of the film, and enabling the crosslinked polyamide molecular chains to migrate due to swelling under the action of a solvent, so that the positions originally occupied by the oligomers are filled with the crosslinked polyamide molecular chains again.
Preferably, the mass concentration of the functional reagent is 6-12%; in the cleaning activator treatment: the temperature for cleaning the activating agent is 40-65 ℃; the treatment time is 10 seconds to 10 minutes. The dosage of the cleaning activator and the treatment temperature play an important role in clearing linear chain structures and swelling crosslinked polyamide molecular chains, so that the reasonable selection of the dosage and the range of the treatment temperature are of great importance. Combining the cost and the action effect of the reagent, preferably, the mass concentration of the functional reagent is 6-10%; the temperature for cleaning the activating agent is 50-55 ℃; the cleaning activator treatment time is 2-8 minutes.
Preferably, in the first step, the polyamide composite reverse osmosis membrane A is obtained by performing interfacial polymerization reaction on m-phenylenediamine and trimesoyl chloride.
Preferably, the monomer washing in the second step is specifically: cleaning the polyamide composite reverse osmosis membrane A obtained in the step one by adopting a cleaning agent at the temperature of 50-85 ℃; the cleaning agent is at least one of water, sodium dodecyl benzene sulfonate aqueous solution, citric acid aqueous solution, oxalic acid aqueous solution, lactic acid aqueous solution, hydrochloric acid aqueous solution and sodium ethylene diamine tetracetate aqueous solution. Preferably, the temperature of monomer washing is 65-75 ℃; the cleaning agent is an oxalic acid aqueous solution, wherein the mass concentration of oxalic acid is 5-10%; the cleaning time is 30 seconds to 5 minutes. Can effectively clean the monomer on the surface of the membrane.
Preferably, the post-treatment in the fourth step comprises the steps of water washing, moisturizing and drying.
Drawings
FIG. 1 is a scanning electron microscope image of the surface of the polyamide composite reverse osmosis membrane prepared in comparative example 1;
FIG. 2 is a scanning electron microscope image of the surface of the electrically neutral polyamide composite reverse osmosis membrane prepared in example 1.
Detailed Description
The embodiments of the present invention will be described in detail with reference to the accompanying drawings so that the advantages and features of the invention can be more easily understood by those skilled in the art, and the scope of the invention will be clearly and clearly defined.
Comparative example 1:
a polyamide reverse osmosis membrane is prepared by the following steps:
1. the reverse osmosis membrane was prepared by interfacial polymerization as follows:
repeatedly washing the surface of the polysulfone membrane by using deionized water, and then purging the membrane surface by using nitrogen until no liquid drops exist; preparing an aqueous solution containing 3.5 mass percent of m-phenylenediamine, 2.5 mass percent of triethylamine, 2 mass percent of camphorsulfonic acid and 1 mass percent of sodium dodecyl sulfate, contacting the surface of a polysulfone membrane with the aqueous solution for 20s, and purging the membrane surface by nitrogen until no liquid drops exist; preparing an oil phase solution, specifically preparing a normal hexane solution containing 0.2% of trimesoyl chloride by mass concentration, contacting the surface of a polysulfone membrane soaked with the water phase solution with the oil phase solution for 15s, and purging the membrane surface by nitrogen until no liquid drops exist to obtain a reverse osmosis membrane;
2. the post-treatment specifically comprises the following steps:
soaking the prepared reverse osmosis membrane in 8% oxalic acid water solution, cleaning at 75 deg.C for 2min, purging to remove water drops on the surface, soaking in 8% glycerol water solution for 1min, and oven drying at 65 deg.C to obtain reverse osmosis membrane material, wherein the membrane material is shown in figure 1 in detail by electron microscope.
The reverse osmosis membrane material is subjected to basic performance and anti-pollution performance tests, and specifically comprises the following steps:
the membrane is taken to be tested on a cross-flow membrane detection table, the initial flux and the salt rejection rate of the membrane are tested under the test conditions of 2000ppm NaCl and 50ppm hexadecyl trimethyl ammonium bromide aqueous solution, 225psi operating pressure, 25 ℃ temperature and 6.5-7.5 pH value, the water flux is tested after 4 hours of operation, and the obtained result is shown in table 2.
Example 1:
the preparation method of the electrically neutral polyamide composite reverse osmosis membrane specifically comprises the following steps:
the method comprises the following steps: the polyamide composite reverse osmosis membrane A is obtained by carrying out interfacial polymerization reaction on m-phenylenediamine and trimesoyl chloride, and specifically comprises the following steps: repeatedly washing the surface of the polysulfone membrane by using deionized water, and then purging the membrane surface by using nitrogen until no liquid drops exist; preparing an aqueous solution containing 3.5 mass percent of m-phenylenediamine, 2.5 mass percent of triethylamine, 2 mass percent of camphorsulfonic acid and 1 mass percent of sodium dodecyl sulfate, contacting the surface of a polysulfone membrane with the aqueous solution for 20s, and purging the membrane surface by nitrogen until no liquid drops exist; preparing a normal hexane solution (namely an oil phase solution) containing 0.2% of trimesoyl chloride by mass concentration, contacting the surface of a polysulfone membrane soaked in the water phase solution with the oil phase solution for 15s, and then purging the membrane surface by nitrogen until no liquid drops exist to obtain a polyamide composite reverse osmosis membrane A;
step two: and (2) carrying out monomer cleaning on the polyamide composite reverse osmosis membrane A obtained in the step one to obtain a polyamide composite reverse osmosis membrane B, which specifically comprises the following steps:
cleaning the polyamide composite reverse osmosis membrane A obtained in the step one for 2 minutes by adopting a cleaning agent at the temperature of 75 ℃; the cleaning agent is an oxalic acid aqueous solution, and the mass concentration of oxalic acid is 8%; blowing dry surface water drops;
step three: treating the polyamide composite reverse osmosis membrane B obtained in the step two by using a cleaning activating agent to obtain a polyamide composite reverse osmosis membrane C; the cleaning activator is a mixed solution of a functional reagent and water, the functional reagent is tetrahydrofuran, and the mass concentration of the functional reagent is 7%; the temperature for cleaning the activating agent is 50 ℃; the treatment time of the cleaning activating agent is 2.5 minutes;
step four: and (4) carrying out aftertreatment on the polyamide composite reverse osmosis membrane C obtained in the step three to obtain the neutral polyamide composite reverse osmosis membrane. The post-treatment here is specifically: firstly, soaking in clean water for cleaning for 2min (water cleaning); then blowing the water drops on the dry surface, and soaking in a glycerol aqueous solution with the mass fraction of 8% for 1min (moisture preservation treatment); and finally drying at 65 ℃ (drying step).
The detail of the electrically neutral polyamide composite reverse osmosis membrane obtained in the example is shown in fig. 2, and as is apparent from comparing fig. 1 and fig. 2, the surface of the membrane material in the comparative example 1 is in a peak-valley shape, while the surface leaf-shaped structure of the membrane in the example 1 is converted into more compact spherical particles after the membrane is cleaned and activated.
The neutral polyamide composite reverse osmosis membrane obtained in the example was subjected to the basic performance and anti-pollution performance test in the manner of comparative example 1, and is detailed in table 2.
Examples 2 to 7 and comparative examples 2 to 4:
the statistical details of the parameters of examples 1-7 and comparative examples 1-4 are given in Table 1 (examples 2-7 and comparative examples 2-3 are otherwise identical to example 1):
TABLE 1 statistical tables of parameters for examples 1-7 and comparative examples 1-4
Wherein:
example 2 compared with example 1, the procedure was otherwise the same as example 1 except that the mass fraction and temperature of tetrahydrofuran in step three were different (6% for tetrahydrofuran and 55 ℃ for temperature).
Examples 3-4 were compared with example 1, except that the mass fraction of tetrahydrofuran in step three was different, and the other examples were the same as example 1.
Example 5 in comparison with example 1, only the cleaning activator in step three was p-hydroxybenzoic acid, and the other examples were the same as example 1.
Example 6 compared to example 1, the same procedure as in example 1 was followed except that aminopropanediol was used as the cleaning activator in step three.
Example 7 is compared to example 1 with the difference that only step three: soaking the polyamide composite reverse osmosis membrane A into oxalic acid water solution with the mass fraction of 8% and cleaning for 2min at 75 ℃ to obtain a polyamide composite reverse osmosis membrane B; after blowing the water drops on the dry surface, immersing the water drops into an aqueous solution containing 3 mass percent of phenol and 5 mass percent of tetrahydrofuran, and immersing the water solution at the temperature of 45 ℃ for 2.5min to obtain a polyamide composite reverse osmosis membrane C; and (3) immersing the membrane in water bath for cleaning for 2min, immersing the membrane in glycerol aqueous solution with the mass fraction of 8% for soaking for 1min after blowing off water drops on the dry surface, and drying the membrane in a drying oven at the temperature of 65 ℃ to obtain the neutral polyamide composite reverse osmosis membrane.
Example 8 compares with example 1, except that step three: soaking the polyamide composite reverse osmosis membrane A into oxalic acid water solution with the mass fraction of 8% and cleaning for 2min at 75 ℃ to obtain a polyamide composite reverse osmosis membrane B; after blowing the water drops on the surface, immersing the membrane into an aqueous solution containing 2 mass percent of p-hydroxybenzoic acid and 8 mass percent of pyridine, and soaking the membrane for 3.5min at the temperature of 55 ℃ to obtain a polyamide composite reverse osmosis membrane C; and (3) immersing the membrane in water bath for cleaning for 3min, immersing the membrane in glycerol aqueous solution with the mass fraction of 8% after blowing off water drops on the dry surface for soaking for 1min, and drying the membrane in a drying oven at the temperature of 65 ℃ to obtain the neutral polyamide composite reverse osmosis membrane.
Comparative example 2 differs from example 1 in the amount of tetrahydrofuran (5%) and otherwise the same as example 1.
Comparative examples 3 to 4 differ from example 1 in the temperature in step three (35 ℃ for comparative example 3 and 70 ℃ for comparative example 4) and are otherwise the same as example 1.
Examples 2-8 and comparative examples 2-4 the basic and anti-pollution performance tests were carried out in the manner of comparative example 1, see table 2.
TABLE 2 comparative examples 1 to 4 and comparative examples 1 to 7
As can be seen from table 2:
1. the zeta potential values of the membrane surfaces of examples 1 to 8 are obviously improved compared with those of comparative examples 1 to 3, which shows that the electronegativity of the membrane material is reduced.
2. The salt rejection rates of examples 1-8 were substantially identical to those of comparative example 1, indicating that the surface treatment did not increase the defect sites of the functional layer; the water flux of examples 1-8 was slightly increased compared to comparative example 1; and after running for 4 hours after the cationic surfactant contamination, the flux decay rate of the membranes in examples 1-8 was much smaller than that of the membranes in the comparative examples.
3. As can be seen from comparison between examples 1-4 and comparative example 2, the amount of the cleaning activator is very important, and is too low (as in comparative example 2), the amount of the linear chain structure to be removed is limited, and the linear chain structure still exists, although the zeta potential value of the membrane surface is improved compared with comparative example 1, the zeta potential value is still lower (-21.2 mV), and the flux attenuation rate is larger; too high (as in example 4), excess rinse activator is wasted because the linear chain structure of the membrane surface has been substantially cleared and the extent to which the crosslinked polyamide layer is activated has reached a limit. Therefore, the dosage of the cleaning activator is reasonably selected by adopting the scope of the invention in combination with two aspects of cost and action effect.
4. By combining the example 1 and the comparative examples 3 to 4, the temperature control is very critical in the process of treating the cleaning activator, the temperature is too low (comparative example 3), the effect of the cleaning activator is not obvious, the linear chain structure still exists, and the zeta potential value of the membrane surface is not effectively improved (still lower, here is-23.6 mV); the temperature was too high (comparative example 4), and although the zeta potential value of the membrane surface was increased (here, to-9.4 mV), the separation performance of the membrane was also greatly decreased, the salt rejection rate was decreased due to the poor flux stability caused by the excessively porous membrane surface functional layer, and the flux attenuation rate was also large.
In conclusion, the electronegativity of the surface of the membrane can be reduced, the basic performance of the membrane can be improved, and the pollution resistance to cationic pollutants can be greatly improved by adopting the electrically neutral polyamide composite reverse osmosis membrane prepared by the method disclosed by the invention, and the mechanism is as follows:
the functional layer of the polyamide composite reverse osmosis membrane is obtained by performing interfacial polymerization reaction on m-phenylenediamine and trimesoyl chloride, because the trimesoyl chloride has three functionality degrees and is difficult to completely perform chemical reaction, one or two acyl chloride groups are not reacted finally, carboxyl is formed after hydrolysis to enable the surface of the membrane to have stronger negative charges, and the polyamide formed by only one or two acyl chloride groups participating in the polymerization reaction generally has smaller molecular weight, lower crosslinking degree and even linear chain structure. According to the method, the polyamide composite membrane is subjected to two steps of monomer cleaning and cleaning activator treatment, so that linear chain oligomers on the surface of the membrane can be removed, and the carboxyl content on the surface of the membrane is reduced; meanwhile, the cleaning activator can activate the crosslinked polyamide layer, namely, crosslinked polyamide molecular chains can swell under the action of a solvent, and the molecular chains migrate, so that the positions originally occupied by the oligomer are filled with the crosslinked polyamide molecular chains again, and thus, the membrane material cannot generate defects to reduce the desalination rate. Therefore, the surface of the membrane material of the polyamide reverse osmosis membrane modified by the method of the invention tends to be electrically neutral (from about-40 mV which is not cleaned and activated in the prior art to about-10 mV), the pollution resistance to positively charged substances is greatly improved, and the water yield is improved under the condition of keeping the desalination rate of the membrane material not reduced.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (8)
1. The preparation method of the electrically neutral polyamide composite reverse osmosis membrane material is characterized by comprising the following steps of:
the method comprises the following steps: interfacial polymerization to form a polyamide composite reverse osmosis membrane A;
step two: cleaning a monomer of the polyamide composite reverse osmosis membrane A obtained in the step one to obtain a polyamide composite reverse osmosis membrane B;
step three: treating the polyamide composite reverse osmosis membrane B obtained in the step two by using a cleaning activating agent to obtain a polyamide composite reverse osmosis membrane C; the cleaning activator comprises a functional reagent or a mixed solution of the functional reagent and water, wherein the functional reagent is at least one of p-hydroxybenzoic acid, phenol, toluene, xylene, pyridine, tetrahydrofuran and aminopropanediol;
step four: and (4) carrying out aftertreatment on the polyamide composite reverse osmosis membrane C obtained in the step three to obtain the neutral polyamide composite reverse osmosis membrane.
2. The method for preparing the electrically neutral polyamide composite reverse osmosis membrane material of claim 1, wherein the cleaning activator in the third step is used for dissolving and removing linear chain oligomers on the surface of the membrane, and the crosslinked polyamide molecular chains are swelled under the action of the solvent to cause the molecular chains to migrate, so that the positions originally occupied by the oligomers are filled with the crosslinked polyamide molecular chains again.
3. The preparation method of the electrically neutral polyamide composite reverse osmosis membrane material of claim 1, wherein the mass concentration of the functional reagent is 6-12%; in the cleaning activator treatment: the temperature for cleaning the activating agent is 40-65 ℃; the treatment time is 10 seconds to 10 minutes.
4. The preparation method of the electrically neutral polyamide composite reverse osmosis membrane material of claim 3, wherein the mass concentration of the functional reagent is 6-10%; the temperature for cleaning the activating agent is 50-55 ℃; the cleaning activator treatment time is 2-8 minutes.
5. The method for preparing the electrically neutral polyamide composite reverse osmosis membrane material as claimed in claim 1, wherein in the first step, the polyamide composite reverse osmosis membrane A is prepared by performing interfacial polymerization reaction on m-phenylenediamine and trimesoyl chloride.
6. The preparation method of the electrically neutral polyamide composite reverse osmosis membrane material according to any one of claims 1 to 5, wherein the monomer washing in the second step is specifically: cleaning the polyamide composite reverse osmosis membrane A obtained in the step one by adopting a cleaning agent at the temperature of 50-85 ℃; the cleaning agent is at least one of water, sodium dodecyl benzene sulfonate aqueous solution, citric acid aqueous solution, oxalic acid aqueous solution, lactic acid aqueous solution, hydrochloric acid aqueous solution and sodium ethylene diamine tetracetate aqueous solution.
7. The preparation method of the electrically neutral polyamide composite reverse osmosis membrane material of claim 6, wherein the temperature for monomer cleaning is 65-75 ℃; the cleaning agent is an oxalic acid aqueous solution, wherein the mass concentration of oxalic acid is 5-10%; the cleaning time is 30 seconds to 5 minutes.
8. The preparation method of the electrically neutral polyamide composite reverse osmosis membrane material as claimed in claim 1, wherein the post-treatment in the fourth step comprises the steps of water cleaning, moisturizing and drying.
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