CN109603577B - Method for preparing forward osmosis membrane with reserved draw solute and double active layers - Google Patents
Method for preparing forward osmosis membrane with reserved draw solute and double active layers Download PDFInfo
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Abstract
The invention belongs to the field of membrane separation, and relates to a method for preparing a forward osmosis membrane with a reserved draw solute double active layers. The porous membrane is used as a supporting layer, the active layers are prepared on the two sides of the supporting layer by adopting an interfacial polymerization method, a certain amount of draw solute is reserved in the supporting layer, and the double-active-layer forward osmosis membrane with the reserved draw solute has higher flux than a conventional double-active-layer forward osmosis membrane, has more excellent pollution resistance than a single-active-layer forward osmosis membrane in an AL-DS mode, and has the advantages of simple preparation process and easiness in large-scale production.
Description
Technical Field
The invention belongs to the field of membrane separation, and relates to a method for preparing a double-active-layer forward osmosis membrane.
Background
Nowadays, the development of society is seriously influenced by the deterioration of water quality and the shortage of water resources. The membrane separation technology is taken as the most promising water treatment process in the 21 st century, and because no chemical reagent is needed to be added in the separation process, the operation is simple and convenient, and the membrane separation technology is widely concerned and popularized in recent years. The core of the membrane separation technology is a permeable membrane which can be divided into a microfiltration Membrane (MF), an ultrafiltration membrane (UF), a nanofiltration membrane (NF), a reverse osmosis membrane (RO) and a forward osmosis membrane (FO) according to the pore size of the membrane, wherein the forward osmosis membrane has the advantages of high separation efficiency, low membrane pollution tendency, capability of running under the conditions of low pressure or even no pressure and the like in the separation process, and has good separation performance in the field of water treatment. The traditional forward osmosis membrane is an asymmetric membrane and consists of a loose supporting layer and a compact active layer, wherein to a certain extent, the active layer determines the retention rate of the membrane to ions, and the supporting layer determines the water flux. Two modes of operation, AL-FS and AL-DS, can be distinguished during treatment depending on the orientation of the active layer, with the active layer being referred to as the AL-FS mode when it is in direct contact with the influent stock solution and the active layer being referred to as the AL-DS mode when it is in direct contact with the draw solution. However, the orientation of the membrane has a large impact on membrane fouling, water flux and rejection. In the AL-FS mode, the flux of water is lowered due to the problem of internal concentration polarization, and the treatment efficiency is influenced; in the AL-DS mode, although the flux problem of water is improved, the membrane has low anti-fouling performance because the solute in the treated water sample enters the support layer to block the pores of the membrane and even scale.
In order to solve the above problems, an innovative concept of a double-active layer film is proposed, the film material forms a compact active layer on both sides of a supporting layer, and the active layer on the raw material side can protect the supporting layer from pollution. Such a membrane design can achieve a similar effect as the AL-DS mode, i.e. minimal internal concentration polarization without the membrane fouling concerns. However, the double active layer will result in a lower water flux than the single active layer due to the entrapment of solutes. Therefore, the development of a high-flux and high-pollution-resistant double-active-layer forward osmosis membrane is urgently needed.
Disclosure of Invention
The invention aims to provide a method for preparing a high-flux and high-pollution-resistance forward osmosis membrane with reserved draw solute and double active layers aiming at the defects and market demands of the prior art.
Aiming at the problems of internal concentration polarization and membrane pollution, the invention provides a method for drawing solute in the reserved part of the supporting layer, and the drawing solute reserved in the supporting layer can effectively slow down the problem of internal concentration polarization in the supporting layer while protecting the supporting layer from being polluted, thereby improving the flux of water.
The technical scheme of the invention is as follows:
a double-active-layer forward osmosis membrane comprises a supporting layer and dense active layers positioned on the upper surface and the lower surface of the supporting layer; a porous membrane is used as a support layer, and the porous membrane contains a draw solute.
The draw solute is present in the porous membrane in an amount of 10-80% of the added concentration.
The porous membrane is an organic polymer membrane. Either as a commercially available organic film, or as a laboratory preparation by phase inversion or electrospinning.
The property of the active layer can be regulated and controlled by the concentration of reactants and the reaction time in the interfacial polymerization process.
The porous membrane is made of nylon, polyether sulfone, polyacrylonitrile, polyvinylidene fluoride, cellulose triacetate or cellulose acetate organic microporous filter membrane.
The pore size range of the porous membrane is as follows: 50-1000nm, and the porosity is 20-98%.
The porous membrane is a flat membrane, a tubular membrane, a capillary membrane or a hollow fiber membrane.
The drawing solute is an organic matter, an inorganic salt or a synthetic material; the organic matter is glucose, fructose, sucrose, ethanol, sodium formate, sodium acetate, magnesium acetate or sodium propionate; the inorganic salt is sulfate, nitrate, chloride or carbonate;
the synthetic material can be polyacrylic acid magnetic nanoparticles, monovalent or divalent dimethyl organic imidazole compounds, sodium polyacrylate, polymer gel and acyl-TAEA (triacyl triaminoethylamine derivatives).
The sulfate is potassium sulfate, sodium sulfate, magnesium sulfate or copper sulfate; the nitrate is potassium nitrate, sodium nitrate or calcium nitrate; the chloride is potassium chloride, sodium chloride, calcium chloride or ammonium chloride; the carbonate is sodium bicarbonate or potassium bicarbonate.
According to the preparation method of the double-active-layer forward osmosis membrane, the active layer generates the polyamide active layer through an interfacial polymerization method. The polyamide active layer is usually formed by polymerization of polyamine and polyacyl chloride monomer at the interface of two mutually incompatible solvents, so as to form an ultrathin compact polyamide layer on the support.
The polyamide active layer and the draw solute have no specific corresponding relation and can correspond to any draw solute.
The amine monomer is triethylene tetramine, diethylenetriamine, ethylenediamine, p-phenylenediamine, m-phenylenediamine, 1, 2-phenylenediamine, 1, 4-phenylenediamine, piperazine, polyethyleneimine, triethanolamine or methyldiethanolamine; the acyl chloride monomer is isophthaloyl dichloride, paraphthaloyl chloride, trimesoyl chloride, pyromellitic dianhydride or 5-isocyanate-isopeptide acyl chloride.
The preparation method comprises the following steps:
step A, washing the porous membrane with deionized water, and drying at 40-60 ℃ for 1-60 min for later use;
b, dissolving polyamine in deionized water to form 1-7 wt% of polyamine solution;
step C, adding a drawing solute into the polyamine solution obtained in the step B, wherein the concentration of the drawing solute is 0-15 wt%, and preparing a mixed solution;
d, dissolving polyacyl chloride in the n-hexane solution to form 0.01-1 wt% of polyacyl chloride solution;
step E, soaking the porous membrane treated in the step A in the mixed solution obtained in the step C for 1-30 min to enable the draw solute to be remained in the supporting layer; taking out, drying the residual solution on the surface of the support layer by using filter paper, and placing the solution in a suction filtration device;
step F, soaking one single side of the porous membrane in the polybasic acyl chloride solution obtained in the step D for 10-120s to obtain a polyamide active layer;
g, repeating the step F to prepare a polyamide active layer on the other side of the porous membrane;
and H, putting the membrane into deionized water, and then putting the membrane into an oven at 80-100 ℃ for treatment for 1-20 min.
The invention has the following characteristics:
1. the forward osmosis membrane with the reserved draw solute and the double active layers has high flux and pollution resistance;
2. the draw solute reserved between the two active layers (namely in the support layer) can improve the permeation flux of the forward osmosis membrane;
3. the permeation flux improvement degree of the forward osmosis membrane can be regulated and controlled by regulating the amount of reserved draw solute;
drawings
FIG. 1 is a photograph of a polyacrylonitrile fiber membrane with a double active layer reserved for draw solute in example 1;
FIG. 2 is a scanning electron micrograph of a polyacrylonitrile fiber support layer in example 1;
FIG. 3 is a scanning electron micrograph of the double active layer forward osmosis membrane with the solute reserved in example 1.
FIG. 4 is a graph showing the results of the film contamination resistance performance in example 1;
FIG. 5 is a graph showing the results of the anti-film-fouling performance in example 2;
FIG. 6 is a graph showing the results of the film contamination resistance performance in example 3.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way. The test methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
A double-active-layer forward osmosis membrane reserved for drawing solute can be divided into an active layer and a supporting layer. And preparing the active layer by an interfacial polymerization method by using a porous substrate reserved with part of the draw solute as a supporting layer. The amount of the draw solute reserved in the supporting layer can be regulated and controlled according to the osmotic pressure difference between the driving liquid and the raw material inlet water in the operation process.
The preparation method of the forward osmosis membrane with the reserved draw solute double active layers comprises the following steps:
step A, washing the supporting layer with the aperture range of 50-1000nm and the porosity range of 20-98% by deionized water, and drying for 1-60 min at 40-60 ℃ for later use;
b, dissolving polyamine in deionized water to form 1-7 wt% of polyamine solution;
step C, adding a drawing solute into the polyamine solution obtained in the step B, wherein the concentration of the drawing solute is 0-15 wt%, and preparing a mixed solution;
d, dissolving polyacyl chloride in the n-hexane solution to form 0.01-1 wt% of polyacyl chloride solution;
step E, soaking the supporting layer in the solution obtained in the step C for 1-30 min to enable the draw solute to be remained in the supporting layer;
step F, taking out the support layer, drying the residual solution on the surface of the support layer by using filter paper, putting the support layer in a suction filtration device, soaking the single-side support layer in the solution obtained in the step D for 10-120s to obtain a polyamide active layer, and repeating the process to prepare the polyamide active layer on the other side of the support layer;
and G, taking out the double-active-layer forward osmosis membrane reserved with the draw solute, putting the forward osmosis membrane into deionized water, and then putting the forward osmosis membrane into an oven at the temperature of 80-100 ℃ for treatment for 1-20 min to increase the crosslinking degree.
Example 1
(1) Washing the polyacrylonitrile fiber supporting layer substrate with the pore diameter of 200nm and the porosity of 90% with deionized water, and drying at 40 ℃ for 10min for later use;
(2) dissolving m-phenylenediamine in deionized water to prepare a 2 wt% m-phenylenediamine solution;
(3) adding sodium chloride into a 2 wt% m-phenylenediamine solution, wherein the concentration of the sodium chloride is 3 wt%, and preparing a mixed solution;
(4) dissolving trimesoyl chloride in n-hexane solution to form 0.2 wt% of trimesoyl chloride solution;
(5) soaking a polyacrylonitrile fiber support layer in a solution containing 2 wt% of m-phenylenediamine (containing 3 wt% of NaCl) for 2 min;
(6) taking out the polyacrylonitrile fiber supporting layer reserved with a draw solute (NaCl), sucking excess water by using filter paper, putting the polyacrylonitrile fiber supporting layer in a suction filtration device, soaking a single layer in 0.2 wt% of trimesoyl chloride/n-hexane for 30s to obtain a polyamide active layer, and repeating the step to prepare the polyamide active layer on the other surface of the supporting layer;
(7) and taking out the double-active-layer forward osmosis membrane reserved with the draw solute and placing the membrane in deionized water at 80 ℃ for treatment for 10 min.
The performance test of the polyacrylonitrile fiber membrane prepared by the method is carried out, 0.5mol/L sodium chloride solution is used as an extraction solution, deionized water is used as a feeding solution, the flux and the salt removal rate of double activities of the extraction solute which are not reserved and reserved are respectively calculated, and the test result at room temperature is as follows:
the double-active-layer forward osmosis membrane is prepared by the method, and the single-active-layer polyacrylonitrile fiber membrane without reserved draw solute is prepared by the same method. And (3) continuously running for 6 hours by using 0.5mol/L sodium chloride solution as a drawing solution and 100ppm sodium alginate as a feeding solution, washing for 1 hour by using deionized water, and continuously running for 6 hours.
The test results at room temperature were: the water flux of the double active layers reserved for drawing the solute is gradually reduced from 24.0LMH to 23.1LMH, and the water flux is almost recovered by one hundred percent after the deionized water is washed; the water flux of the single-active-layer forward osmosis membrane is reduced from 15.2LMH to 7.6LMH in the AL-DS mode, and the water flux is recovered eighty percent after being washed by deionized water.
Example 2
(1) Washing the polyvinylidene fluoride supporting layer with the aperture of 100nm and the porosity of 80% with deionized water, and drying at 50 ℃ for later use;
(2) dissolving m-phenylenediamine in deionized water to prepare a 3 wt% m-phenylenediamine solution;
(3) adding sodium chloride into a 3 wt% m-phenylenediamine solution, wherein the concentration of the sodium chloride is 3.5 wt%, and preparing a mixed solution;
(4) dissolving trimesoyl chloride in n-hexane solution to form 0.2 wt% of trimesoyl chloride solution;
(5) soaking a polyvinylidene fluoride support layer in a solution containing 3 wt% of m-phenylenediamine (containing 3.5 wt% of NaCl) for 2 min;
(6) taking out the polyvinylidene fluoride supporting layer reserved with a draw solute (NaCl), sucking excess water by using filter paper, placing the polyvinylidene fluoride supporting layer in a suction filtration device, soaking a single layer in 0.2 wt% of trimesoyl chloride/normal hexane for 30s to obtain a polyamide active layer, and repeating the step to prepare the polyamide active layer on the other surface of the supporting layer;
(7) and taking out the double-active-layer forward osmosis membrane reserved with the draw solute and placing the membrane in deionized water at 80 ℃ for treatment for 10 min.
The polyvinylidene fluoride membrane prepared by the method is subjected to performance test, 0.5mol/L sodium chloride solution is used as an extraction solution, deionized water is used as a feeding solution, the flux and the salt removal rate of double activities of the extraction solute which are not reserved and reserved are respectively calculated, and the test result at room temperature is as follows:
the double-active-layer forward osmosis membrane is prepared by the method, and the single-active-layer polyvinylidene fluoride membrane without reserved draw solute is prepared by the same method. And (3) continuously running for 6 hours by using 0.5mol/L sodium chloride solution as a drawing solution and 100ppm sodium alginate as a feeding solution, washing for 1 hour by using deionized water, and continuously running for 6 hours.
The test results at room temperature were: the water flux of the double active layers reserved for drawing solute is gradually reduced from 22.3LMH to 21.0LMH, and the water flux is almost recovered by one hundred percent after the deionized water is washed; the water flux of the single-active-layer forward osmosis membrane is reduced from 16.4LMH to 7.8LMH in the AL-DS mode, and the water flux is recovered eighty percent after being washed by deionized water.
Example 3
(1) Washing the polyethersulfone hollow fiber supporting layer with the aperture of 300nm and the porosity of 90% by using deionized water, and drying at 40 ℃ for later use;
(2) dissolving m-phenylenediamine in deionized water to prepare a 4 wt% m-phenylenediamine solution;
(3) adding glucose into a 4 wt% m-phenylenediamine solution, wherein the concentration of the glucose is 3.5 wt%, and preparing a mixed solution;
(4) dissolving trimesoyl chloride in n-hexane solution to form 0.15 wt% of trimesoyl chloride solution;
(5) injecting a solution containing 4 wt% of m-phenylenediamine (containing 3.5 wt% of glucose) into a pipe of the polyether sulfone hollow fiber membrane at a flow rate of 1m/s, and the process lasts for 2 min;
(6) purging with high pressure gas such as inert gas such as air, nitrogen, argon, etc. at flow rate of 1m/s for 1min to remove residual solution on the surface, injecting 0.15 wt% trimesoyl chloride/n-hexane solution into the tube at flow rate of 1m/s for 60s to obtain polyamide active layer in the tube, sealing two ends of the hollow fiber membrane with glue, and repeating the same steps to obtain the outer polyamide active layer.
(7) And taking out the double-active-layer forward osmosis membrane reserved with the draw solute and placing the membrane in deionized water at 90 ℃ for treatment for 15 min.
The polyethersulfone hollow fiber membrane prepared by the method is subjected to performance test, 0.5mol/L sodium chloride solution is used as an extraction solution, deionized water is used as a feeding solution, the flux and the salt removal rate of double activities of the extraction solute which are not reserved and reserved are respectively calculated, and the test result at room temperature is as follows:
the double-active-layer forward osmosis membrane is prepared by the method, and the single-active-layer polyether sulfone hollow fiber membrane without reserved draw solute is prepared by the same method. And (3) continuously running for 6 hours by using 0.5mol/L sodium chloride solution as a drawing solution and 100ppm sodium alginate as a feeding solution, washing for 1 hour by using deionized water, and continuously running for 6 hours.
The test results at room temperature were: the water flux of the double active layers reserved for drawing solute is gradually reduced from 23.0LMH to 20.6LMH, and the water flux is almost recovered by one hundred percent after the deionized water is washed; the water flux of the single-active-layer forward osmosis membrane is reduced from 14.6LMH to 6.9LMH in the AL-DS mode, and the water flux is recovered eighty percent after being washed by deionized water.
The above-mentioned embodiments are only exemplary embodiments of the present invention, and should not be construed as limiting the invention, so that the obvious modifications and other modifications without departing from the spirit of the present invention, which are described in the claims of the present invention, are all included in the protection scope of the present invention.
Claims (10)
1. A double-active-layer forward osmosis membrane comprises a supporting layer and dense active layers positioned on the upper surface and the lower surface of the supporting layer; characterized in that a porous membrane is used as a support layer, and the porous membrane contains a draw solute.
2. The double active layer forward osmosis membrane according to claim 1, wherein the draw solute is present in the porous membrane in an amount of 10-80% of the added concentration.
3. The double active layer forward osmosis membrane according to claim 1, wherein the porous membrane is an organic polymer membrane.
4. The double-active-layer forward osmosis membrane according to claim 1, wherein the porous membrane is made of nylon, polyethersulfone, polyacrylonitrile, polyvinylidene fluoride, cellulose triacetate, or cellulose acetate organic microporous membrane.
5. The double active layer forward osmosis membrane according to claim 1 or 2, wherein the porous membrane has a pore size in the range of: 50-1000nm, and the porosity is 20-98%.
6. The double active layer forward osmosis membrane according to claim 1,2 or 3, wherein the porous membrane is a flat sheet membrane, a tubular, a capillary or a hollow fiber membrane.
7. The double active layer forward osmosis membrane according to claim 1, wherein the draw solute is an organic substance, an inorganic salt, or a synthetic material; the organic matter is glucose, fructose, sucrose, ethanol, sodium formate, sodium acetate, magnesium acetate or sodium propionate; the inorganic salt is sulfate, nitrate, chloride or carbonate; the synthetic material is polyacrylic acid magnetic nano particles, monovalent or divalent dimethyl imidazole compounds, sodium polyacrylate, polymer gel or acyl-TAEA.
8. The double active layer forward osmosis membrane according to claim 7,
the sulfate is potassium sulfate, sodium sulfate, magnesium sulfate or copper sulfate,
the nitrate is potassium nitrate, sodium nitrate or calcium nitrate,
the chloride is potassium chloride, sodium chloride, calcium chloride or ammonium chloride,
the carbonate is sodium bicarbonate or potassium bicarbonate.
9. The method for preparing a double active layer forward osmosis membrane according to any one of claims 1 to 4, wherein the active layer is formed into a polyamide active layer by interfacial polymerization.
10. The method of claim 9, comprising the steps of:
step A, washing the porous membrane with deionized water, and drying at 40-60 ℃ for 1-60 min;
b, dissolving polyamine in deionized water to form 1-7 wt% of polyamine solution;
step C, adding a drawing solute into the polyamine solution obtained in the step B, wherein the concentration of the drawing solute is 3-15 wt%, and preparing a mixed solution;
d, dissolving polyacyl chloride in the n-hexane solution to form 0.01-1 wt% of polyacyl chloride solution;
step E, soaking the porous membrane treated in the step A in the mixed solution obtained in the step C for 1-30 min;
step F, soaking one single side of the porous membrane in the polybasic acyl chloride solution obtained in the step D for 10-120s to obtain a polyamide active layer;
g, repeating the step F to prepare a polyamide active layer on the other side of the porous membrane;
and H, putting the membrane into deionized water, and then putting the membrane into an oven at 80-100 ℃ for treatment for 1-20 min.
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