CN114984782B - Anti-pollution polyamide reverse osmosis membrane with high flux and high desalination rate and preparation method thereof - Google Patents
Anti-pollution polyamide reverse osmosis membrane with high flux and high desalination rate and preparation method thereof Download PDFInfo
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- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D2323/38—Graft polymerization
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
The invention provides a preparation method of an anti-pollution polyamide reverse osmosis membrane with high flux and high salt rejection rate, which adopts double-end amino polyethylene glycol to react with carboxyl on the surface of a polyamide layer so as to improve the salt rejection rate of the composite polyamide reverse osmosis membrane, and meanwhile, the flux is not basically lost, and the polyethylene glycol is an electrically neutral water-soluble long-chain polymer, has flexible and flexible molecular chains, and can prevent hydrophobic substances and macromolecules from being adsorbed through the volume exclusion effect and the unique compatibility with water molecules so as to improve the anti-pollution performance of the composite polyamide reverse osmosis membrane.
Description
Technical Field
The invention belongs to the technical field of reverse osmosis membranes, and particularly relates to an anti-pollution polyamide reverse osmosis membrane with high flux and high desalination rate and a preparation method thereof.
Background
Reverse osmosis is an advanced and energy efficient separation technology today. The principle is to separate the solute from the solvent in solution by selective interception by means of a semi-permeable membrane that allows only water to permeate but not other substances, under the action of a pressure higher than the osmotic pressure of the solution. By utilizing the separation characteristic of the reverse osmosis membrane, impurities such as dissolved salt, colloid, organic matters, bacteria, microorganisms and the like in water can be effectively removed. Has the advantages of low energy consumption, no pollution, advanced process, simple and convenient operation and maintenance, and the like. The reverse osmosis membrane is the core of reverse osmosis technology, and the research and application of the reverse osmosis membrane are always the most popular research direction in the field of reverse osmosis technology.
Chinese patent CN 109847597A provides a method for preparing a high flux high desalination reverse osmosis membrane, which can increase the flux of the reverse osmosis membrane by adding one or a mixture of any of chloroform, dichloroethane, trichloroethane, chloroform, tetrahydrofuran and ethyl acetate in an oil phase reaction solution, on the premise of keeping the desalination rate of the reverse osmosis membrane unchanged, but it does not mention the improvement of the anti-pollution capability.
Xun et al (Xurong, liyan, guo fieng, etc.. PA/PEG cross-linked copolymerized reverse osmosis membrane preparation and fouling resistance [ J ] chemical engineering progress, 2021, 40 (12): 8.) polyethylene glycol (PEG) is introduced in the interface polymerization reaction process of trimesoyl chloride (TMC) and m-phenylenediamine (MPD) to prepare a Polyamide (PA)/PEG reverse osmosis composite membrane, so that the fouling resistance is greatly improved, but the method cannot simultaneously improve the flux and desalination rate of the reverse osmosis membrane.
Disclosure of Invention
In view of this, the present invention provides an anti-pollution polyamide reverse osmosis membrane with high flux and high salt rejection and a preparation method thereof, wherein the reverse osmosis membrane prepared by the method has greatly improved salt rejection and improved anti-pollution capability.
The invention provides a preparation method of an anti-pollution polyamide reverse osmosis membrane with high flux and high salt rejection rate, which comprises the following steps:
coating a water phase solution on the polysulfone supporting layer, then coating an oil phase solution, and drying to obtain the nascent state aromatic polyamide reverse osmosis membrane;
the aqueous phase solution comprises 0.5 to 5 percent of polyfunctional amine, 0.05 to 2 percent of surfactant, 3 to 10 percent of polar solvent and the balance of water; the multifunctional amine is selected from one or more of aromatic amine, aliphatic amine and alicyclic amine;
the pH value of the aqueous phase solution is 7 to 9; the pH value is preferably adjusted by using a sodium hydroxide solution.
The multifunctional amine is selected from one or more of m-phenylenediamine, ethylenediamine, propylenediamine, butylenediamine, hexylenediamine, N- (2-hydroxyethyl) ethylenediamine, 1, 2-diaminocyclohexane, 1, 3-diaminocyclohexane, 1, 4-diaminocyclohexane, diethylenetriamine, m-phenylenediamine, p-phenylenediamine, o-phenylenediamine, pyromellitic triamine, piperazine and 4-aminomethylpiperazine;
the surfactant is selected from sodium dodecyl benzene sulfonate or sodium lauryl sulfate;
the polar solvent is selected from dimethyl sulfoxide and/or N-methyl pyrrolidone. The invention uses polar solvent with higher concentration to carry out interfacial polymerization reaction in water phase to form a nascent polyamide reverse osmosis membrane with higher flux;
the oil phase solution comprises 0.05 to 0.3 percent of polyfunctional acyl halide, and the balance is oil phase solvent; the oil phase solvent is selected from one or more of C4-C12 aliphatic hydrocarbon, cycloaliphatic hydrocarbon and aromatic hydrocarbon, and is preferably isoparaffin solvent oil; in a specific embodiment, the oil phase solvent is Isopar G.
After the polysulfone supporting layer is coated with the water phase solution, the redundant solution on the surface is removed, and then the polysulfone membrane absorbed with the water phase solution passes through a closed space with a heat supply and air exhaust system. In the invention, the aqueous phase solution is coated, then the aqueous phase solution is volatilized at the temperature of 20 to 30 ℃ and the relative humidity of 40 to 80 percent until the water content is 28 to 31 percent, and then the oil phase solution is coated.
After the oil phase solution is coated, the polyamide reverse osmosis membrane is dried in an oven at the temperature of 60-80 ℃, water on the surface of the membrane and a solvent of the oil phase solution volatilize in the drying process, and simultaneously unreacted monomers can further react, so that the desalination rate of the polyamide reverse osmosis membrane can be improved. The drying time is generally 1 to 3min, the drying is carried out until no oil printing exists on the surface of the film, and the temperature of the surface of the film is generally controlled to be 25 to 40 ℃.
Rinsing the nascent state aromatic polyamide reverse osmosis membrane, soaking in the grafted treatment solution, and air-drying to obtain the anti-pollution polyamide reverse osmosis membrane with high flux and high desalination rate.
In the present invention, the rinsing specifically includes:
and rinsing the nascent state aromatic polyamide reverse osmosis membrane by deionized water, an isopropanol aqueous solution, a citric acid aqueous solution, deionized water and a glycerol aqueous solution in sequence.
In the present invention, the mass concentration of the isopropyl alcohol (IPA) aqueous solution is 5 to 25%, preferably 10 to 20%; the invention adopts IPA solution with higher concentration to rinse and then remove residual reactant, and can further improve the flux of the nascent polyamide reverse osmosis membrane through the swelling action;
the concentration of the citric acid aqueous solution is 1 to 5 percent, preferably 1 to 2 percent;
the concentration of the aqueous glycerol solution is 0.5 to 10%, preferably 5 to 9%.
The invention adopts the treatment solution after grafting for soaking, and mainly aims to fully wash away unreacted residues and other impurities. In the invention, the post-grafting treatment fluid is of the molecular formula H 2 NCH 2 CH 2 （CH 2 CH 2 O） n CH 2 CH 2 NH 2 The molecular weight of the aqueous solution of amino-terminated polyethylene glycol is 400 to 5000; the mass fraction is 0.01 to 0.08 percent, and the mass fraction is preferably 0.01 to 0.05 percent. The molecular weight of the amino-terminated polyethylene glycol is 400 to 2000. In a specific embodiment, the amino-terminated polyethylene glycol is amino-terminated polyethylene glycol with a molecular weight of 400, amino-terminated polyethylene glycol with a molecular weight of 1000, amino-terminated polyethylene glycol with a molecular weight of 2000, or amino-terminated polyethylene glycol with a molecular weight of 400. According to the invention, the polyethylene glycol with double amino groups is used as a cross-linking agent to improve the cross-linking degree of the polyamide layer on the surface of the reverse osmosis membrane, so that the anti-pollution capability of the reverse osmosis membrane is further improved, and the anti-pollution polyamide reverse osmosis membrane with high flux and high desalination rate is obtained.
In the present invention, the polyfunctional acyl halide is trimesoyl chloride.
The present invention is preferably blow dried with dry air until the film surface is free of visible moisture.
The performance of the reverse osmosis membrane is tested by adopting the following test method:
and (3) filtering a 1500ppm sodium chloride aqueous solution at 1.03MPa, 25 ℃ and the membrane surface flow rate of 1.1GPM/min, flushing for 30min, and testing to obtain the initial flux and the desalination rate of the polyamide reverse osmosis membrane with high flux, high desalination rate and pollution resistance.
And under the same operation condition, the test aqueous solution is changed into a mixed solution of an electronegative lauryl sodium sulfate solution (50 g/L), electropositive lauryl trimethyl ammonium bromide (50 g/L) and electroneutral bovine serum albumin (100 g/L) for dissolving and washing for 30min, the flux of the anti-pollution polyamide reverse osmosis membrane with high flux and high desalination rate after pollution is obtained through testing, all test results are shown in table 2, pressure is relieved after pollution testing is finished, the polluted membrane is cleaned by using deionized water as a feeding solution, then 1500ppm of sodium chloride aqueous solution is filtered for 30min at 1.03MPa and 25 ℃ at the membrane surface flow rate of 1.1GPM/min, and the flux and the desalination rate of the polyamide reverse osmosis membrane with high flux and high desalination rate and anti-pollution after pollution treatment are obtained through testing.
The invention provides a preparation method of an anti-pollution polyamide reverse osmosis membrane with high flux and high salt rejection rate, which adopts double-end amino polyethylene glycol to react with carboxyl on the surface of a polyamide layer so as to improve the salt rejection rate of the composite polyamide reverse osmosis membrane, and meanwhile, the flux is not basically lost, and the polyethylene glycol is an electrically neutral water-soluble long-chain polymer, has flexible and flexible molecular chains, and can prevent hydrophobic substances and macromolecules from being adsorbed through the volume exclusion effect and the unique compatibility with water molecules so as to improve the anti-pollution performance of the composite polyamide reverse osmosis membrane.
Detailed Description
To further illustrate the present invention, the following examples are provided to describe in detail the anti-fouling polyamide reverse osmosis membrane with high flux and high salt rejection and the preparation method thereof, but they should not be construed as limiting the scope of the present invention.
Comparative example:
the production method of the anti-pollution polyamide reverse osmosis membrane with high flux and high desalination rate comprises the following steps:
1. preparing an aqueous phase liquid: 25g of m-phenylenediamine, 1g of sodium dodecyl sulfate and 80g of N-methylpyrrolidone are added and dissolved in 894g of water, the pH value is adjusted to 8.5-9 by adopting sodium hydroxide, and the mixture is uniformly stirred to obtain an aqueous phase solution.
2. Preparing an oil phase solution: 2.5G of trimesoyl chloride was dissolved in 997.5G of Isopar G, and stirred uniformly to obtain an oil phase solution.
3. Firstly, coating a water phase solution on a polysulfone support layer, removing the redundant solution on the surface, then leading the polysulfone basement membrane adsorbed with the water phase solution to pass through a closed space with a heat supply and air exhaust system, controlling the internal temperature to be 20-30 ℃ and the relative humidity to be 40-80%, and further volatilizing the water on the membrane surface. And then coating an oil phase solution on the surface of the polyamide reverse osmosis membrane, removing a part of the oil phase solution on the surface, and then drying in an oven at the temperature of 60-80 ℃ to form a polyamide ultrathin separation layer, thereby obtaining the nascent polyamide reverse osmosis membrane.
4. And (3) filtering a 1500ppm sodium chloride aqueous solution at 1.03MPa, 25 ℃ and the membrane surface flow rate of 1.1GPM/min, flushing for 30min, and testing to obtain the initial flux and the desalination rate of the polyamide reverse osmosis membrane with high flux, high desalination rate and pollution resistance, wherein all test results are shown in Table 1. And under the same operation condition, the test aqueous solution is changed into a mixed solution of an electronegative lauryl sodium sulfate solution (50 g/L), electropositive lauryl trimethyl ammonium bromide (50 g/L) and electroneutral bovine serum albumin (100 g/L) for dissolving and washing for 30min, the flux of the anti-pollution polyamide reverse osmosis membrane with high flux and high desalination rate after pollution is obtained through testing, all test results are shown in table 2, pressure is relieved after the pollution test is finished, the polluted membrane is cleaned by using deionized water as a feeding solution, then 1500ppm of sodium chloride aqueous solution is filtered for 30min at 1.03MPa and 25 ℃ at the membrane surface flow rate of 1.1GPM/min, the flux and the desalination rate of the polyamide reverse osmosis membrane after pollution treatment and cleaning are obtained through testing, and all test results are shown in table 2.
Example 1
The production method of the anti-pollution polyamide reverse osmosis membrane with high flux and high desalination rate comprises the following steps:
1. the same as the comparative example.
2. The same as the comparative example.
3. Preparation of rinsing liquid 1: 1200g IPA was dissolved in 8800g water to give rinse 1;
4. preparation of rinsing liquid 2: dissolving 200g of citric acid in 9800g of water to obtain a rinsing solution 2;
5. preparation of rinsing liquid 3: dissolving 800g of glycerol in 9200g of water to obtain a rinsing liquid 3;
6. preparation of a graft post-treatment solution: 1g of double-end amino polyethylene glycol with the molecular weight of 400 is dissolved in 9999g of water to obtain a grafted post-treatment solution;
7. firstly, coating a water phase solution on a polysulfone support layer, removing the redundant solution on the surface, then leading the polysulfone basement membrane adsorbed with the water phase solution to pass through a closed space with a heat supply and air exhaust system, controlling the internal temperature to be 20-30 ℃ and the relative humidity to be 40-80%, and further volatilizing the water on the membrane surface. And then coating an oil phase solution on the surface of the polyamide ultra-thin separation layer, removing a part of the oil phase solution on the surface of the polyamide ultra-thin separation layer, drying the polyamide ultra-thin separation layer in a drying oven at 60-80 ℃ to form a nascent polyamide reverse osmosis membrane, soaking and rinsing the nascent polyamide reverse osmosis membrane by using deionized water, a rinsing solution 1, a rinsing solution 2, deionized water and a rinsing solution 3 in sequence, soaking and rinsing the nascent polyamide reverse osmosis membrane, then soaking and grafting a post-treatment solution, and air-drying the solution to obtain the anti-pollution polyamide reverse osmosis membrane with high flux and high desalination rate.
8. The same as the comparative example.
Example 2:
the production method of the anti-pollution polyamide reverse osmosis membrane with high flux and high salt rejection rate comprises the following steps:
1. the same as the comparative example.
2. The same as the comparative example.
3. The same as example 1;
4. the same as example 1;
5. the same as example 1;
6. preparation of a grafting post-treatment solution: 1g of double-end amino polyethylene glycol with the molecular weight of 1000 is dissolved in 9999g of water to obtain a grafted post-treatment solution;
7. the same as in example 1.
8. The same as the comparative example.
Example 3:
the production method of the anti-pollution polyamide reverse osmosis membrane with high flux and high desalination rate comprises the following steps:
1. the same as the comparative example.
2. The same as the comparative example.
3. The same as example 1;
4. the same as example 1;
5. the same as example 1;
6. preparation of a graft post-treatment solution: 1g of double-end amino polyethylene glycol with molecular weight of 2000 is dissolved in 9999g of water to obtain a grafted post-treatment solution;
7. the same as in example 1.
8. The same as the comparative example.
Example 4:
the production method of the anti-pollution polyamide reverse osmosis membrane with high flux and high desalination rate comprises the following steps:
1. the same as the comparative example.
2. The same as the comparative example.
3. The same as example 1;
4. the same as example 1;
5. the same as example 1;
6. preparation of a graft post-treatment solution: selecting 3g of double-end amino polyethylene glycol with molecular weight of 400 to be dissolved in 9997g of water to obtain a grafted post-treatment solution;
7. the same as in example 1.
8. The same as the comparative example.
Example 5:
the production method of the anti-pollution polyamide reverse osmosis membrane with high flux and high desalination rate comprises the following steps:
1. the same as the comparative example.
2. The same as the comparative example.
3. The same as example 1;
4. the same as example 1;
5. the same as example 1;
6. preparation of a graft post-treatment solution: selecting 6g of double-end amino polyethylene glycol with molecular weight of 400 to be dissolved in 9994g of water to obtain a grafting post-treatment solution;
7. the same as in example 1.
8. The same as the comparative example.
TABLE 1 initial flux and salt rejection of polyamide composite reverse osmosis membranes
TABLE 2 flux of polyamide composite reverse osmosis membrane after fouling
Post-contamination flux decay rate = (1-post-contamination flux/initial flux) × 100%; post-wash flux recovery = (post-wash flux/initial flux) × 100%.
From the above examples, it can be seen that in the method provided by the present invention, the polyamide separation layer is formed and then subjected to a crosslinking reaction with the amino group-terminated polyethylene glycol, such that the degree of crosslinking of the polyamide separation layer can be increased, and the salt rejection of the polyamide reverse osmosis membrane can be increased. The experimental results show that: the method provided by the invention can improve the flux of the obtained polyamide reverse osmosis membrane by 12%; (2) the salt rejection is improved by 0.7-1.5%; and (3) the flux recovery rate of the membrane after pollution cleaning can reach 90-92%.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. A preparation method of an anti-pollution polyamide reverse osmosis membrane with high flux and high salt rejection rate comprises the following steps:
coating a water phase solution on a polysulfone support layer, volatilizing at 20-30 ℃ and relative humidity of 40-80% until the water mass content is 28-31%, coating an oil phase solution, and drying to obtain a nascent-state aromatic polyamide reverse osmosis membrane;
the aqueous phase solution comprises 0.5 to 5 percent of polyfunctional amine, 0.05 to 2 percent of surfactant, 3 to 10 percent of polar solvent and the balance of water; the multifunctional amine is selected from one or more of aromatic amine, aliphatic amine and alicyclic amine; the pH value of the aqueous phase solution is 7 to 9;
the oil phase solution comprises 0.05 to 0.3 percent of polyfunctional acyl halide, and the balance is oil phase solvent; the oil phase solvent is selected from one of C4-C12 aliphatic hydrocarbon, cycloaliphatic hydrocarbon and aromatic hydrocarbon;
rinsing the nascent state aromatic polyamide reverse osmosis membrane, soaking in the grafted treatment solution, and air-drying to obtain the anti-pollution polyamide reverse osmosis membrane with high flux and high desalination rate;
the grafting post-treatment solution has a molecular formula H 2 NCH 2 CH 2 （CH 2 CH 2 O） n CH 2 CH 2 NH 2 An aqueous solution of amino-terminated polyethylene glycol having a molecular weight of 400 to 2000; the mass fraction is 0.01 to 0.05 percent;
the rinsing specifically comprises:
rinsing the nascent state aromatic polyamide reverse osmosis membrane by deionized water, an isopropanol aqueous solution, a citric acid aqueous solution, deionized water and a glycerol aqueous solution in sequence;
the mass concentration of the isopropanol aqueous solution is 5 to 25 percent;
the concentration of the citric acid aqueous solution is 1 to 5 percent;
the concentration of the glycerol aqueous solution is 0.5 to 10 percent.
2. The method according to claim 1, wherein the polyfunctional amine is selected from one or more of m-phenylenediamine, ethylenediamine, propylenediamine, butylenediamine, hexylenediamine, N- (2-hydroxyethyl) ethylenediamine, 1, 2-diaminocyclohexane, 1, 3-diaminocyclohexane, 1, 4-diaminocyclohexane, diethylenetriamine, m-phenylenediamine, p-phenylenediamine, o-phenylenediamine, sym-benzenetriamine, piperazine, and 4-aminomethylpiperazine;
the surfactant is selected from sodium dodecyl benzene sulfonate or sodium lauryl sulfate;
the polar solvent is selected from dimethyl sulfoxide and/or N-methyl pyrrolidone.
3. The method of claim 1, wherein the polyfunctional acyl halide is trimesoyl chloride.
4. The method according to claim 1, wherein the amino-terminated polyethylene glycol is specifically an amino-terminated polyethylene glycol having a molecular weight of 1000, an amino-terminated polyethylene glycol having a molecular weight of 2000, or an amino-terminated polyethylene glycol having a molecular weight of 400.
5. An anti-pollution polyamide reverse osmosis membrane with high flux and high salt rejection rate, which is prepared by the preparation method of any one of claims 1 to 4.
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