CN113491957A - Preparation method of gaseous fiber membrane with three-dimensional welding structure for high-salt water concentration - Google Patents
Preparation method of gaseous fiber membrane with three-dimensional welding structure for high-salt water concentration Download PDFInfo
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- CN113491957A CN113491957A CN202110803635.5A CN202110803635A CN113491957A CN 113491957 A CN113491957 A CN 113491957A CN 202110803635 A CN202110803635 A CN 202110803635A CN 113491957 A CN113491957 A CN 113491957A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/36—Pervaporation; Membrane distillation; Liquid permeation
- B01D61/364—Membrane distillation
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/447—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by membrane distillation
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- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
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Abstract
The invention discloses a preparation method of a gaseous fiber membrane for high-salt water concentration with a three-dimensional welded structure, which comprises the following steps: dissolving a skeleton type polymer into a solvent with weak volatility to form a solution A, dissolving a bonding type polymer into a nonpolar solvent with strong volatility to form a solution B, and magnetically stirring and mixing the solution A and the solution B to obtain a uniform emulsion; step two: carrying out high-voltage electrostatic spinning on the emulsion prepared in the step one, and finally taking down the spun gaseous fiber membrane from a receiving carrier of the electrostatic spinning; step three: and (5) placing the gaseous fiber membrane obtained in the step two in a drying box for drying to obtain the gaseous fiber membrane with a three-dimensional welding structure. The gaseous fiber membrane with three-dimensional structure stability prepared by the invention has good stability and high water recovery rate in the concentration process of membrane distillation high-salt water, so that the gaseous fiber membrane has wide application prospect in the field of membrane distillation.
Description
Technical Field
The invention relates to a preparation method of a water treatment membrane, in particular to a preparation method of a gaseous fiber membrane with a three-dimensional welding structure for concentrating high-salt water.
Background
Membrane distillation technology is gaining increasing attention in the field of desalination of high-salinity water because it can process high-concentration brine using low-grade energy. Flux and stability are two major key parameters of membrane distillation technology. The electrostatic spinning fiber membrane technology has higher permeability in the membrane distillation process due to the unique three-dimensional interconnected pore structure and lower tortuosity, and is more and more concerned in the field. However, the electrospun fiber membrane is a membrane formed by physical stacking, and the fibers in the membrane are independent from each other. Under hydraulic agitation, fibers slide easily between them, causing membrane pores to deform and thereby causing membrane wetting. Electrospun fiber membranes therefore tend to be less stable in membrane distillation applications, which greatly limits the development of electrospinning technology in this area.
Under the condition of maintaining the advantage of high flux of the electrostatic spinning fiber membrane, the improvement of the structural stability of the electrostatic spinning fiber membrane has very important significance for the development of the electrostatic spinning fiber membrane in the field of membrane distillation. The traditional method for enhancing the structural stability of the electrostatic spinning fiber membrane comprises a steam welding method, a polydimethylsiloxane soaking welding method and a physical hot-pressing welding method. Although these welding methods can weld the surface of the film well, the welding degree is not uniform on the inner part of the film, and the result that the fibers close to the outer side are welded excessively but the fibers in the inner part are not welded completely often occurs. This may cause the steam transfer process to form condensed water inside the membrane due to loose deformation of the internal fibers, thereby causing internal wetting, which greatly increases heat loss of the system and thus severely reduces water production. The three-dimensional welding method can realize the equal welding degree of the membrane in the three-dimensional space, thus not only relieving the membrane wetting from the outside caused by the deformation of external fibers, but also relieving the internal wetting caused by the deformation of internal fibers, and realizing the high stability of the membrane distillation process. Therefore, the preparation of the gaseous fiber membrane with stable three-dimensional structure has great practical significance in the field of membrane distillation desalination.
Disclosure of Invention
In order to solve the problem that the membrane pores of the traditional electrostatic spinning fiber membrane are easy to deform under the hydraulic disturbance and the technical defect that the welding degree of the traditional fiber welding method is not uniform in space, the invention provides a preparation method of a gaseous fiber membrane for concentrating high-salt water, which has a three-dimensional welding structure. The method prepares the gaseous fiber membrane with the same welding degree in the three-dimensional space by means of a high-voltage electrostatic spinning method, the preparation process is simple, the large-scale production is easy to realize, and the obtained gaseous fiber membrane with the three-dimensional welding structure has good stability in the concentration process of membrane distillation high-salt water.
The purpose of the invention is realized by the following technical scheme:
a method for preparing a gaseous fiber membrane for high brine concentration with a three-dimensional welded structure comprises the following steps:
step one, preparing spinning emulsion: the emulsion contains two macromolecules and two mutually insoluble solvents, wherein: the two polymers are respectively skeleton type polymer and bonding type polymer, and the two solvents are solvents with different volatility; the preparation method comprises the following steps: dissolving a skeleton type polymer into a solvent with weak volatility to form a solution A, dissolving a bonding type polymer into a nonpolar solvent with strong volatility to form a solution B, and mixing the solution A and the solution B through magnetic stirring to obtain a uniform emulsion, wherein: the mass ratio of the bonding type polymer to the framework type polymer is 10: 1-10: 5; the adhesive polymer is polydimethylsiloxane; the skeleton type polymer is one of hydrophobic polymer poly (vinylidene fluoride-co-hexafluoropropylene) which is easy to spin, polyurethane, polyvinylidene fluoride, polysulfonamide, polyether sulfone and polystyrene; the nonpolar solvent with strong volatility for dissolving the bonding type macromolecule is one or more of n-hexane, cyclohexane, isooctane and heptane; the solvent with low volatility for dissolving the skeleton type polymer is one or more of N, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone; the mass concentration of the emulsion is 12-24%;
step two: carrying out high-voltage electrostatic spinning on the emulsion prepared in the step one, and finally taking down the spun gaseous fiber membrane from a receiving carrier of electrostatic spinning, wherein: the high-voltage electrostatic spinning is carried out under the conditions that the relative humidity is 40-60% and the temperature is 20-30 ℃; the voltage of electrostatic spinning is 10-50 kV, the distance of electrostatic spinning is 10-40 cm, and the injection speed is 0.1-4 mL/h; the receiving carrier of the electrostatic spinning is one of aluminum foil, non-woven fabric and copper mesh;
step three: and (3) placing the gaseous fiber membrane obtained in the step (II) in a drying oven for drying to obtain a gaseous fiber membrane with a three-dimensional welding structure, wherein the gaseous fiber membrane can be applied to the field of membrane distillation, and the method comprises the following steps: the drying temperature is 60-120 ℃, and the drying time is 1-5 h.
Compared with the prior art, the invention has the following advantages:
1. the invention provides a method for preparing a hydrophobic gaseous fiber membrane with a three-dimensional welded structure, which utilizes the solubility difference of polymers, the volatility difference of solvents and the caking property of polydimethylsiloxane to weld membrane fibers in an electrostatic spinning process in a mode of welding the membrane on a three-dimensional space to the same extent, and endows the membrane with three-dimensional hydrophobic stability.
2. The gaseous fiber membrane with three-dimensional structure stability is prepared by a high-voltage electrostatic spinning method, the preparation process is simple, the cost is low, and the large-scale production can be realized.
3. The gaseous fiber membrane with three-dimensional structure stability prepared by the invention has good stability and high water recovery rate in the concentration process of membrane distillation high-salt water, so that the gaseous fiber membrane has wide application prospect in the field of membrane distillation.
Drawings
FIG. 1 is a scanning electron microscope image of the film surface of a gaseous fiber film for high brine concentration having a three-dimensional welded structure prepared in example 1;
fig. 2 is a water contact angle photograph of a gaseous fiber membrane for high brine concentration having a three-dimensional welded structure prepared in example 1;
FIG. 3 is a pore size distribution diagram of a gaseous fiber membrane for high brine concentration having a three-dimensional welded structure prepared in example 1;
FIG. 4 is a stress-strain graph of a gaseous fiber membrane for high brine concentration having a three-dimensional welded structure prepared in example 1;
fig. 5 is a photograph of the gaseous fiber membrane for high brine concentration having a three-dimensional welded structure prepared in example 1 after being subjected to an abrasion test.
Detailed Description
The technical solutions of the present invention are further described below with reference to the following examples, but the present invention is not limited thereto, and any modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Example 1:
the embodiment provides a method for preparing a gaseous fiber membrane for high brine concentration, which has a three-dimensional welded structure, and the method is specifically carried out according to the following steps:
adding 4g of polydimethylsiloxane polymer into 10g of n-hexane, and uniformly stirring at room temperature by magnetic force to obtain a polydimethylsiloxane solution; adding 8g of poly (vinylidene fluoride-co-hexafluoropropylene) into 32g N, N-dimethylformamide, and magnetically stirring for 8 hours at 80 ℃ to obtain a poly (vinylidene fluoride-co-hexafluoropropylene) solution; and uniformly mixing the polydimethylsiloxane solution and the poly (vinylidene fluoride-co-hexafluoropropylene) solution by magnetic stirring to obtain uniform emulsion.
Secondly, under the conditions that the relative humidity is 45% and the temperature is 23 ℃, performing high-voltage electrostatic spinning on the emulsion prepared in the step one, controlling the voltage of the electrostatic spinning to be 15kV, the distance of the electrostatic spinning to be 15cm, the injection speed to be 1mL/h, and using aluminum foil as a receiving carrier of the electrostatic spinning.
And thirdly, drying the gaseous fiber membrane obtained in the second step in a forced air drying oven, wherein the temperature is controlled to be 100 ℃, and the drying time is 2 hours.
In the gaseous fiber membrane prepared in this example, the mass ratio of poly (vinylidene fluoride-co-hexafluoropropylene) to polydimethylsiloxane is 8:4, the pore diameter is 1.37 μm, the water contact angle is 143 °, the liquid admission pressure is 103kPa, and the elongation is 58%, and the textile wear resistance test is performed on the gaseous fiber membrane with a three-dimensional welding structure by using a martindale method, and after 50 times of reciprocating, the surface of the membrane is not damaged.
As can be seen from the test analysis of fig. 1 to 5, the gaseous fiber membrane for high brine concentration having a three-dimensional welded structure prepared in this example has the same degree of welding in three-dimensional space, so that the membrane has good resistance to membrane pore deformation and three-dimensional hydrophobic stability.
Example 2:
the embodiment provides a method for preparing a gaseous fiber membrane for high brine concentration, which has a three-dimensional welded structure, and the method is specifically carried out according to the following steps:
firstly, adding 3g of polydimethylsiloxane polymer into 10g of cyclohexane, and uniformly stirring at room temperature by magnetic force to obtain a polydimethylsiloxane solution; adding 8g of poly (vinylidene fluoride-co-hexafluoropropylene) into 32g N, N-dimethylformamide, and magnetically stirring for 8 hours at 80 ℃ to obtain a poly (vinylidene fluoride-co-hexafluoropropylene) solution; and uniformly mixing the polydimethylsiloxane solution and the poly (vinylidene fluoride-co-hexafluoropropylene) solution by magnetic stirring to obtain uniform emulsion.
Secondly, under the conditions that the relative humidity is 40% and the temperature is 24 ℃, performing high-voltage electrostatic spinning on the emulsion prepared in the step one, controlling the voltage of the electrostatic spinning to be 18kV, the distance of the electrostatic spinning to be 20cm, the injection speed to be 1.5mL/h, and using a copper mesh as a receiving carrier of the electrostatic spinning.
And thirdly, drying the porous fiber membrane obtained in the second step in a forced air drying oven, wherein the temperature is controlled to be 100 ℃, and the drying time is 1 h.
In the gaseous fiber membrane prepared in this example, the mass ratio of poly (vinylidene fluoride-co-hexafluoropropylene) to polydimethylsiloxane is 8:3, the pore size is 1.24 μm, the water contact angle is 142 °, the liquid admission pressure is 101kPa, the elongation is 54%, the textile wear resistance test is performed on the gaseous fiber membrane with a three-dimensional welding structure by using the martindale method, and after 40 times of reciprocating, the surface of the membrane is not damaged.
Example 3:
the embodiment provides a method for preparing a gaseous fiber membrane for high brine concentration, which has a three-dimensional welded structure, and the method is specifically carried out according to the following steps:
adding 2g of polydimethylsiloxane polymer into 10g of mixed solution of isooctane and heptane, controlling the mass ratio of isooctane to heptane to be 1:1, and magnetically stirring uniformly at room temperature to obtain polydimethylsiloxane solution; adding 6g of polyvinylidene fluoride into 34g of N, N-dimethylacetamide, and magnetically stirring at 80 ℃ for 8 hours to obtain a polyvinylidene fluoride solution; and (3) uniformly stirring and mixing the polydimethylsiloxane solution and the polyvinylidene fluoride solution by magnetic force to obtain uniform emulsion.
Secondly, under the conditions that the relative humidity is 60% and the temperature is 25 ℃, performing high-voltage electrostatic spinning on the emulsion prepared in the step one, controlling the voltage of the electrostatic spinning to be 30kV, the distance of the electrostatic spinning to be 18cm, the injection speed to be 2mL/h, and using aluminum foil as a receiving carrier of the electrostatic spinning.
And thirdly, drying the gaseous fiber membrane obtained in the second step in a forced air drying oven, wherein the temperature is controlled to be 110 ℃, and the drying time is 3 hours.
In the gaseous fiber membrane prepared in this example, the mass ratio of polyvinylidene fluoride to polydimethylsiloxane is 3:1, the pore diameter is 1.43 μm, the water contact angle is 141 °, the liquid admission pressure is 100kPa, the elongation is 52%, the textile wear resistance test is performed on the gaseous fiber membrane with a three-dimensional welding structure by the martindale method, and after 35 cycles, the surface of the membrane is not damaged.
Example 4:
the embodiment provides a method for preparing a gaseous fiber membrane for high brine concentration, which has a three-dimensional welded structure, and the method is specifically carried out according to the following steps:
firstly, adding 1g of polydimethylsiloxane polymer into 10g of heptane, and uniformly stirring at room temperature by magnetic force to obtain a polydimethylsiloxane solution; adding 9g of polystyrene into 31g N, N-dimethylformamide, and magnetically stirring for 8 hours at 80 ℃ to obtain a polystyrene solution; and (3) uniformly mixing the polydimethylsiloxane solution and the polystyrene solution by magnetic stirring to obtain uniform emulsion.
Secondly, under the conditions that the relative humidity is 40% and the temperature is 26 ℃, carrying out high-voltage electrostatic spinning on the emulsion prepared in the first step, controlling the voltage of the electrostatic spinning to be 25kV, the distance of the electrostatic spinning to be 18cm, the injection speed to be 1.8mL/h, and taking a non-woven fabric as a receiving carrier of the electrostatic spinning.
And thirdly, drying the gaseous fiber membrane obtained in the second step in a forced air drying oven, wherein the temperature is controlled to be 90 ℃, and the drying time is 4 hours.
In the gaseous fiber membrane prepared in this example, the mass ratio of poly (vinylidene fluoride-co-hexafluoropropylene) to polydimethylsiloxane is 9:1, the pore diameter is 1.94 μm, the water contact angle is 138 °, the liquid admission pressure is 97kPa, and the elongation is 44%, the textile wear resistance test is performed on the gaseous fiber membrane with a three-dimensional welding structure by using the martindale method, and after 20 times of reciprocating, the surface of the membrane is not damaged.
Claims (10)
1. A method for preparing a gaseous fiber membrane for high brine concentration with a three-dimensional welded structure is characterized by comprising the following steps:
dissolving a skeleton type polymer into a solvent with weak volatility to form a solution A, dissolving a bonding type polymer into a nonpolar solvent with strong volatility to form a solution B, magnetically stirring and mixing the solution A and the solution B to obtain a uniform emulsion, and controlling the mass ratio of the bonding type polymer to the skeleton type polymer to be 10: 1-10: 5;
step two: carrying out high-voltage electrostatic spinning on the emulsion prepared in the step one, and finally taking down the spun gaseous fiber membrane from a receiving carrier of the electrostatic spinning;
step three: and (5) placing the gaseous fiber membrane obtained in the step two in a drying box for drying to obtain the gaseous fiber membrane with a three-dimensional welding structure.
2. The method for preparing the gaseous fiber membrane for high brine concentration with the three-dimensional welded structure according to claim 1, wherein the skeleton-type polymer is one of poly (vinylidene fluoride-co-hexafluoropropylene), polyurethane, polyvinylidene fluoride, polysulfonamide, polyether sulfone and polystyrene, and the bonding-type polymer is polydimethylsiloxane.
3. The method for preparing a gaseous fiber membrane for high brine concentration having a three-dimensional welded structure according to claim 1, wherein the nonpolar solvent having high volatility is a mixed solvent of one or more of n-hexane, cyclohexane, isooctane, and heptane.
4. The method for preparing a gaseous fiber membrane for high brine concentration having a three-dimensional welded structure according to claim 1, wherein the solvent having low volatility is a mixed solvent of one or more of N, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
5. The method for preparing a gaseous fiber membrane for high brine concentration having a three-dimensional welded structure according to claim 1, wherein the mass concentration of the emulsion is 12-24%.
6. The method for preparing a gaseous fiber membrane for high brine concentration having a three-dimensional welded structure according to claim 1, wherein the high-voltage electrospinning is performed at a relative humidity of 40 to 60% and a temperature of 20 to 30 ℃.
7. The method for preparing a gaseous fiber membrane for high brine concentration having a three-dimensional welded structure according to claim 1, wherein the voltage of electrospinning is 10 to 50kV, the distance of electrospinning is 10 to 40cm, and the injection speed is 0.1 to 4 mL/h.
8. The method for preparing a gaseous fiber membrane for high brine concentration having a three-dimensional welded structure according to claim 1, wherein the receiving carrier for electrospinning is one of aluminum foil, non-woven fabric and copper mesh.
9. The method for preparing a gaseous fiber membrane for high brine concentration having a three-dimensional welded structure according to claim 1, wherein the drying temperature is 60 to 120 ℃ and the drying time is 1 to 5 hours.
10. Use of a gaseous fiber membrane for high brine concentration having a three-dimensional welded structure prepared by the method of any one of claims 1 to 9 in the field of membrane distillation.
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