CN109110878B - Method for improving water flux of composite forward osmosis membrane - Google Patents
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Abstract
The invention discloses a method for improving water flux of a composite forward osmosis membrane, which comprises the following steps: (1) soaking the base membrane of the forward osmosis membrane in an aqueous solution of an organic solvent; (2) taking out the base membrane after soaking treatment, and cleaning the base membrane with water; (3) and preparing a separation layer on the base membrane through interfacial polymerization, thereby obtaining the high-flux polyamide composite forward osmosis membrane. According to the invention, the hole wall of the base membrane is thinned by soaking in the organic solvent, the pore structure is changed, the tortuosity of the membrane hole is reduced, the porosity of the base membrane is improved, and the number of large finger-shaped holes is increased, so that the structural parameters of the membrane are reduced, the internal concentration polarization phenomenon of the forward osmosis membrane is reduced, and the water flux of the composite forward osmosis membrane is finally improved. The method of the invention is simple, the operation is easy to realize, and the method is particularly suitable for large-scale industrial production.
Description
Technical Field
The invention relates to a preparation method of a Forward Osmosis (FO) membrane, in particular to a method for improving the water flux of a composite forward osmosis membrane, belonging to the technical field of membrane separation.
Background
The Forward Osmosis (FO) process is a process in which water automatically diffuses from a raw water side with high electrochemical potential to a draw solution side with low electrochemical potential through a selectively permeable membrane, using an osmotic pressure difference between the draw solution and the raw material solution as a driving force, and no additional pressure or energy is required in the process. Therefore, compared with Reverse Osmosis (RO) and other processes, the forward osmosis process has the advantages of low energy consumption, high water recovery rate, difficult membrane pollution, normal-temperature and normal-pressure operation and the like, has many successful attempts in the fields of food, pharmacy, energy and the like, particularly in the fields of water purification and desalination, and shows potential application value. However, the water flux of forward osmosis membranes is still generally low, so that forward osmosis technology is expected to be widely applied, and it is critical to further develop forward osmosis membranes with high water flux and high salt rejection.
The thickness and the porous structure of the separation membrane cause the concentration of two sides of the membrane and the concentration of the solution body to generate difference in the separation process, and the osmotic pressure difference in the separation process is influenced, so that the concentration polarization phenomenon is generated, and the actual forward osmosis water flux is far smaller than an ideal value. The concentration polarization phenomenon can be classified into an internal concentration polarization phenomenon and an external concentration polarization phenomenon. Wherein, the external concentration polarization phenomenon generated on the membrane surface can be eliminated by improving the flow velocity of the membrane surface, and the internal concentration polarization phenomenon generated in the porous support layer is not easy to weaken. The internal concentration polarization has a greater influence on the membrane performance, and therefore, the improvement of the forward permeability of the membrane needs to be started from the reduction of the internal concentration polarization phenomenon. In order to reduce the internal concentration polarization phenomenon of the composite membrane in the forward osmosis process, Tang and the like enable the supporting layer to be easier to form a finger-shaped pore structure by adding nano particles, thus being beneficial to increasing the porosity and improving the forward osmosis performance. In recent years, researches on composite forward osmosis membranes are increasing, researchers optimize a support layer of a membrane by improving the hydrophilicity of the membrane, reducing the thickness of the support layer, preparing a double-skin layer composite membrane and the like, and reduce the internal concentration polarization phenomenon by changing the pore structure of the support layer, but the water flux of the forward osmosis composite membrane is not greatly improved on the whole.
The internal concentration polarization phenomenon mainly occurs in the support layer of the composite membrane, so that the optimization of the structure of the base membrane (namely the support layer of the forward osmosis membrane) has an important influence on the improvement of the forward osmosis water flux of the membrane. The base membrane of the existing composite forward osmosis membrane is generally prepared by a phase inversion method, and the base membrane has more spongy pores formed in the phase inversion process, lacks a large finger-shaped pore structure, or has larger tortuosity, so that the water flux of the prepared forward osmosis membrane is lower.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a method for improving water flux of a composite forward osmosis membrane, which is simple and easy to operate, and the method increases the porosity of the membrane by treating a base membrane of the forward osmosis membrane to form more and larger finger-shaped pore structures, thereby reducing the structural parameters of the membrane, reducing the internal concentration polarization, and effectively improving the water flux of the composite forward osmosis membrane.
The purpose of the invention is realized by the following technical scheme:
a method for improving water flux of a composite forward osmosis membrane, comprising the steps of: (1) soaking the base membrane of the forward osmosis membrane in an aqueous solution of an organic solvent; (2) taking out the base membrane after soaking treatment, and cleaning the base membrane with water; (3) and preparing a separation layer on the base membrane through interfacial polymerization, thereby obtaining the high-flux polyamide composite forward osmosis membrane.
The base membrane is made of polysulfone (PSf), polyether sulfone (PES), polyvinylidene fluoride (PVDF), Polyacrylonitrile (PAN) or the like.
The basement membrane is prepared by a lyotropic phase inversion method.
The base film may also include a support material such as a polyester screen or a non-woven fabric.
The organic solvent is one or a mixture of N, N Dimethylformamide (DMF), N dimethylacetamide (DMAc), dimethyl sulfoxide (DMSO) and N-methylpyrrolidone (NMP).
The volume percentage of the organic solvent in the organic solvent aqueous solution is 30-80%. The concentration of the solvent is the key of the invention, and if the concentration is too low, the influence on the structure of the basement membrane is small, so that the effect of improving the water flux cannot be achieved; too high may cause the base membrane material to be dissolved too much and collapse the porous structure, thereby failing to improve water flux.
The soaking time in the step (1) is 10min-10 hr.
The water used for cleaning in the step (2) is pure water or tap water.
The base film and the support layer refer to the same structure in the present invention, and are generally referred to as a base film before the upper separation layer is compounded by interfacial polymerization, and a support layer after the upper separation layer is compounded by interfacial polymerization.
Testing method of membrane performance:
(1) pure water flux of basal membrane
The pure water flux (PWP) of the basement membrane is measured by an ultrafiltration membrane performance evaluation device, deionized water is used as a raw material liquid, a cross flow method is adopted, and the water yield of a certain time is measured to calculate:
in the formula (1), Δ V is the volume of pure water passing through the base film for a certain period of time, and Δ P is the applied pressure.
(2) Porosity of the base film
Porosity (ξ) of the membrane was determined by weighing the membrane wet weight (m)wetG) and mass after drying at room temperature for 12h (m)dryG) and density of water ρwAnd density of polysulfone ρpTo calculate:
(3) performance testing of composite membranes
The structural parameter (S) of the composite membrane is an important parameter for measuring the concentration polarization phenomenon in the forward osmosis membrane, and theoretically, the smaller the structural parameter of the membrane is, the weaker the internal concentration polarization phenomenon is:
where t, ε, and τ represent the thickness, porosity, and pore tortuosity, respectively, of the membrane.
And respectively taking 1M NaCl and deionized water as an extraction solution and a raw material solution, and carrying out performance test on the prepared composite forward osmosis membrane at the test temperature of (19 +/-2) DEG C. The membrane is oriented to active layer facing to raw material liquid (AL-FS), the volume of pure water permeating from the raw material liquid side to the draw liquid side is recorded through the reading of an electronic balance, the mass of solute reversely permeating to the raw material liquid side is recorded through the reading of a conductivity meter, after the membrane performance tends to be stable, data is recorded every 3min, and the test is carried out for 45 min.
Water flux (J)w，L▪m-2 ▪h-1) Is a measure of the water permeability of the membrane, calculated using the volume of pure water passing through the membrane per unit area per unit time.
Reverse salt flux (J)s，g▪m-2 ▪h-1) Is used to measure the retention performance of the membrane, corresponding to the water flux, the reverse salt flux is obtained by calculating the mass of salt per unit membrane area permeated per unit time.
Salt water ratio (J)s/Jw，g ▪L-1) Is referred to asThe ratio of the mass of solute passing through the membrane to the volume of water within the same time can be more intuitively reflected as the overall performance of the membrane.
In formula (4), Δ v (l) is the volume of water permeated during Δ t (h) in the forward osmosis process; a. thes（m2) Is the effective area of the membrane. In the formula (5), Ct(g/L) and Vt(L) represents the concentration and volume of the raw material liquid at time t, respectively.
The invention has the advantages that the hole wall of the base membrane is thinned by adopting the organic solvent for soaking, the hole structure is changed, the tortuosity of the membrane hole is reduced, the porosity is improved, and the number of large finger-shaped holes is increased, thereby reducing the structural parameters of the membrane, reducing the internal concentration polarization phenomenon of the forward osmosis membrane and finally improving the water flux of the composite forward osmosis membrane. The method of the invention is simple, the operation is easy to realize, and the method is particularly suitable for large-scale industrial production.
Drawings
FIG. 1 is a graph comparing the pure water flux of the basement membrane after treatment by soaking in DMAc solutions of different concentrations.
FIG. 2 is a water flux comparison graph of forward osmosis membranes prepared by soaking base membranes treated with different concentrations of DMAc solutions.
FIG. 3 is a graph comparing reverse salt flux for forward osmosis membranes prepared by soaking base membranes treated with different concentrations of DMAc solutions.
FIG. 4 is a comparison of brine ratios for forward osmosis membranes prepared by soaking the base membrane in DMAc solutions of different concentrations.
Fig. 5 is an SEM image of a cross-section of a forward osmosis membrane prepared by soaking the membrane in various DMAc solutions.
Wherein 1, 2 and 3 are respectively base membrane without soaking in DMAc solution, base membrane with soaking in 80% DMAc solution for 30min and base membrane with soaking in 80% DMAc solution for 1hr to prepare SEM images of sections of the forward osmosis membrane.
Detailed Description
The invention is further illustrated by the following comparative examples and specific examples in conjunction with the accompanying drawings.
Comparative example 1: the basement membrane is not soaked in organic solvent
(1) Mixing polysulfone, an additive and N, N-dimethylacetamide according to a mass ratio of 16:7.3:76.7, stirring and dissolving at 50 ℃ for 3 days to obtain a uniform membrane casting solution, and standing and defoaming at room temperature.
(2) 2.0wt% m-phenylenediamine aqueous solution and 0.20w/v% trimesoyl chloride n-hexane solution were prepared respectively as the aqueous phase and the oil phase in the interfacial polymerization stage.
(3) Placing a polyester screen mesh as a supporting material on a clean glass plate, pouring a proper amount of casting solution on the polyester screen mesh, manually scraping the film by controlling a certain scraper gap, immersing the film into deionized water for gel to obtain a polysulfone base film, and fully cleaning the polysulfone base film and placing the polysulfone base film in the deionized water for later use.
(4) Immersing the front surface of the basement membrane soaked in the organic solvent into a m-phenylenediamine aqueous solution, reacting for 2min, and removing the redundant solution; then soaking the membrane into a trimesoyl chloride normal hexane solution, reacting for 30s, and carrying out interfacial polymerization reaction with a water phase on the polysulfone base membrane to generate a compact separation layer; then treating the membrane in an oven at 90 ℃ for 10min, and finally fully cleaning the prepared membrane with deionized water and then preserving the membrane in a 1% sodium bisulfite solution.
Performance: 1M NaCl and deionized water are used as an extraction liquid and a raw material liquid, the water flux of a forward osmosis membrane is 10.02 +/-0.83 LMH, the reverse salt flux is 3.06 +/-0.86 gMH, and the salt water ratio is 0.31 g/L.
The structure is as follows: the membrane consists of a porous supporting layer and a compact separating layer, wherein the membrane supporting layer is provided with a thicker sponge-shaped structure, and the large finger-shaped pore structure is less.
Comparative example 2: soaking basement membrane in 10% DMAc for 2hr
The preparation method comprises the following steps: soaking the base membrane prepared in the step (3) of the comparative example 1 in a DMAc aqueous solution with the volume ratio of 10% for 2 hours, taking out, fully cleaning in deionized water, and fully cleaning the composite forward osmosis membrane prepared in the rest steps in the same way as the comparative example 1 by using the deionized water, and then storing in a 1% sodium bisulfite solution.
Performance: 1M NaCl and deionized water are used as a drawing liquid and a raw material liquid, the water flux of a forward osmosis membrane is 10.21 +/-0.60 LMH, the reverse salt flux is 3.02 +/-0.41 gMH, and the salt water ratio is 0.30 g/L.
The structure is as follows: the membrane consists of a porous supporting layer and a compact separating layer, wherein a sponge layer on the upper layer of the supporting layer is thicker, and large finger-shaped pore structures below the sponge layer are fewer.
Example 1: soaking basement membrane in 30% DMAc for 1hr
The preparation method comprises the following steps: soaking the base membrane prepared in the step (3) of the comparative example 1 in a DMAc aqueous solution with the volume ratio of 30% for 1hr, taking out, fully cleaning in deionized water, and fully cleaning the composite forward osmosis membrane prepared in the rest steps in the same way as the comparative example 1 by using the deionized water, and then storing in a 1% sodium bisulfite solution.
Performance: 1M NaCl and deionized water are used as a drawing liquid and a raw material liquid, the water flux of a forward osmosis membrane is 12.60 +/-0.50 LMH, the reverse salt flux is 3.21 +/-0.50 gML, and the salt water ratio is 0.25 g/L.
The structure is as follows: the membrane consists of two parts, a porous support layer and a dense separation layer, and the thickness of a sponge layer on the upper layer of the support layer is reduced but not greatly changed.
Example 2: soaking the basement membrane in 50% DMF for 30min
The preparation method comprises the following steps: and (3) soaking the base membrane prepared in the step (3) in a 50% DMF aqueous solution for 30min in the comparative example 1, taking out, fully cleaning in deionized water, and fully cleaning the prepared high-performance composite forward osmosis membrane in the same step as the comparative example 1 by using the deionized water and then storing in a 1% sodium bisulfite solution.
Performance: 1M NaCl and deionized water are used as a drawing liquid and a raw material liquid, the water flux of a forward osmosis membrane is 14.90 +/-0.61 LMH, the reverse salt flux is 3.61 +/-1.01 gMH, and the salt water ratio is 0.24 g/L.
The structure is as follows: the membrane consists of a porous support layer and a dense separation layer, the large finger-shaped pore structure in the membrane is increased, and the thickness of a spongy layer in the support layer is reduced.
Example 3: soaking basement membrane in 50% DMAc for 1hr
The preparation method comprises the following steps: soaking the base membrane prepared in the step (3) in the aqueous solution of 50% DMAc in the comparative example 1 for 1hr, taking out, fully cleaning in deionized water, and fully cleaning the prepared high-performance composite forward osmosis membrane in the same step as the comparative example 1 by using the deionized water and then storing in a 1% sodium bisulfite solution.
Performance: 1M NaCl and deionized water are used as a drawing liquid and a raw material liquid, the water flux of a forward osmosis membrane is 16.20 +/-0.72 LMH, the reverse salt flux is 3.69 +/-1.01 gMH, and the salt water ratio is 0.23 g/L.
The structure is as follows: the membrane is composed of a porous support layer and a dense separation layer, the thickness of the sponge layer in the support layer is reduced, and the large finger-shaped pore structure in the membrane is increased.
Example 4: soaking basement membrane in 80% DMAc for 30min
The preparation method comprises the following steps: and (3) soaking the base membrane prepared in the step (3) in an aqueous solution of 80% DMAc in the comparative example 1 for 30min, taking out, fully cleaning in deionized water, and fully cleaning the prepared high-performance composite forward osmosis membrane in the same step as the comparative example 1 by using the deionized water and then storing in a 1% sodium bisulfite solution.
Performance: 1M NaCl and deionized water are used as a drawing liquid and a raw material liquid, the water flux of a forward osmosis membrane is 17.91 +/-0.32 LMH, the reverse salt flux is 3.40 +/-1.20 gMH, and the salt water ratio is 0.19 g/L.
The structure is as follows: the membrane consists of a porous support layer and a dense separation layer, the large finger-shaped pore structure in the membrane is increased, and the thickness of a spongy layer in the support layer is reduced.
Example 5: soaking basement membrane in 80% DMAc for 1hr
The preparation method comprises the following steps: soaking the base membrane prepared in the step (3) in the aqueous solution of 80% DMAc in the comparative example 1 for 1hr, taking out, fully cleaning in deionized water, and fully cleaning the prepared high-performance composite forward osmosis membrane in the same step as the comparative example 1 by using the deionized water and then storing in a 1% sodium bisulfite solution.
Performance: 1M NaCl and deionized water are used as a drawing liquid and a raw material liquid, the water flux of a forward osmosis membrane is 20.40 +/-1.02 LMH, the reverse salt flux is 3.58 +/-0.50 gMH, and the salt water ratio is 0.18 g/L.
The structure is as follows: the membrane consists of a porous supporting layer and a compact separating layer, wherein a spongy layer in the supporting layer becomes thin, the macropores of the finger-shaped holes are obviously increased, and the tortuosity of the holes is reduced.
Example 6: soaking basement membrane in 80% NMP for 1hr
The preparation method comprises the following steps: soaking the base membrane prepared in the step (3) in the 80% NMP solution in the comparative example 1 for 1hr, taking out, fully cleaning in deionized water, and fully cleaning the prepared high-performance composite forward osmosis membrane in the same steps as the comparative example 1 by using the deionized water and then storing in a 1% sodium bisulfite solution.
Performance: 1M NaCl and deionized water are used as a drawing liquid and a raw material liquid, the water flux of a forward osmosis membrane is 18.10 +/-0.94 LMH, the reverse salt flux is 4.03 +/-0.45 gMH, and the salt water ratio is 0.22 g/L.
The structure is as follows: the membrane consists of a porous supporting layer and a compact separating layer, wherein a spongy layer in the supporting layer is thinner, large finger-shaped pore structures are more, pores are straighter, and the tortuosity is reduced.
TABLE 1 Effect of different soaking concentrations and times on film Performance
As can be seen from the comparison of the data in fig. 1-4 and table 1, the performance of the membrane is affected after the base membrane is soaked in the aqueous solution of the organic solvent. When the DMAc concentration is too low (less than 30%), the porosity of the base membrane is not greatly changed, and the water flux is not obviously increased; when the volume percentage concentration of DMAc is 30-80%, the porosity and water flux of the basement membrane are obviously changed, and the water flux of the forward osmosis membrane is obviously improved. As can be seen from the comparison of the SEM images of fig. 5, the composite membrane in which the base membrane is soaked in the aqueous solution of the organic solvent is more likely to form a large finger-shaped pore structure than the membrane in which the base membrane is not soaked, and at the same time, the sponge layer in the support layer becomes thinner and the porosity increases, thereby reducing the structural parameters of the composite membrane. Compared with the composite forward osmosis membrane prepared by the traditional method, the water flux of the composite forward osmosis membrane prepared by the method is improved by about 10-11 LMH, the reverse salt flux is basically kept unchanged, and the salt water ratio is reduced by about 0.13 g/L. The forward osmosis membrane treated by the method weakens the phenomenon of internal concentration polarization in the forward osmosis process, and the forward osmosis performance of the composite membrane is greatly improved.
Claims (6)
1. A method for improving water flux of a composite forward osmosis membrane is characterized by comprising the following steps: (1) soaking the base membrane of the forward osmosis membrane in an aqueous solution of an organic solvent; the organic solvent is one or a mixed solvent of more of N, N dimethylformamide, N dimethylacetamide, dimethyl sulfoxide and N-methylpyrrolidone; the volume percentage of the organic solvent in the organic solvent aqueous solution is 30-80%, and the soaking time is 10min-10 hr; (2) taking out the base membrane after soaking treatment, and cleaning the base membrane with water; (3) and preparing a separation layer on the base membrane through interfacial polymerization, thereby obtaining the high-flux polyamide composite forward osmosis membrane.
2. The method according to claim 1, wherein the base film is made of one of polysulfone, polyethersulfone, polyvinylidene fluoride, or polyacrylonitrile.
3. The method according to claim 1, characterized in that said base film is prepared by a phase inversion process.
4. The method of claim 1, wherein the base film further comprises a support material.
5. The method of claim 4, wherein the support material is a polyester mesh or nonwoven.
6. The method according to claim 1, wherein the water used for washing in the step (2) is pure water or tap water.
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| CN114588776A (en) * | 2022-04-15 | 2022-06-07 | 启成（江苏）净化科技有限公司 | Method for preparing reverse osmosis membrane by segmented interface polymerization |
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