CN113308799A - Double-layer nanofiber membrane for water-oil separation and preparation method thereof - Google Patents
Double-layer nanofiber membrane for water-oil separation and preparation method thereof Download PDFInfo
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- CN113308799A CN113308799A CN202110059297.9A CN202110059297A CN113308799A CN 113308799 A CN113308799 A CN 113308799A CN 202110059297 A CN202110059297 A CN 202110059297A CN 113308799 A CN113308799 A CN 113308799A
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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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
- B01D67/0006—Organic membrane manufacture by chemical reactions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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- C—CHEMISTRY; METALLURGY
- 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
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
- D01D5/0084—Coating by electro-spinning, i.e. the electro-spun fibres are not removed from the collecting device but remain integral with it, e.g. coating of prostheses
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/38—Hydrophobic membranes
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Abstract
The invention discloses a double-layer nanofiber membrane for water-oil separation and a preparation method thereof, and relates to the technical field of water-oil separation. The method takes polyvinyl alcohol and chitosan as raw materials, and mixes the two solutions after the polyvinyl alcohol and the chitosan are respectively dissolved to prepare a first layer of film by an electrostatic spinning technology; dissolving polyvinylidene fluoride into N-N dimethylacetamide, and adding fluorinated graphene into the N-N dimethylacetamide and uniformly stirring the mixture to obtain a second layer of spinning solution; and performing electrostatic spinning on the basis of the first layer to obtain the double-layer electrostatic spinning membrane for water-oil separation. The membrane has super-hydrophobicity and a porous structure, and can realize high-efficiency water-oil separation.
Description
Technical Field
The invention relates to a water-oil separation material, in particular to a water-oil separation membrane with a double-layer structure and a preparation method thereof, and belongs to the technical field of new materials.
Background
In recent decades, oil-containing wastewater generated by various industrial processes such as frequent oil leakage accidents, leather, food, textile, metal finishing and the like has been increasing, and poses a long-term threat to the ecological environment. Therefore, in order to protect human health and ecological environment, purification of petroleum-contaminated wastewater has become an indispensable task. Conventional methods for separating oil-containing wastewater include gravity separation, centrifugal separation, electric separation, adsorption separation, air flotation separation, etc., but these techniques are often limited, including high cost, low separation efficiency, and secondary contaminants. In recent years, nanofiber materials such as adsorbents, membranes and aerogels applied to water-oil separation have been rapidly developed. Among water-oil separation techniques, membrane separation techniques are considered to be one of the best methods for oil-water separation because of membrane-inherent properties such as high porosity, high productivity, cost-effectiveness, simple operation, and no need for additional chemicals. The device can effectively filter solid particles, remove protein and separate oily sewage, has the advantages of low energy consumption, high separation efficiency, stable separation performance and the like, and can filter substances by selectively regulating and controlling the surface wettability of the membrane. The nanofiber membrane prepared by the electrostatic spinning technology has the advantages of high flux, high separation efficiency, good thermal stability and the like in the field of water-oil separation.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the defects in the prior art, the invention aims to provide a preparation method of a double-layer nanofiber membrane with simple process and mild conditions. The membrane is realized by an electrostatic spinning technology, and has super-hydrophobic performance and high-efficiency water-oil separation performance.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
1) dissolving chitosan into an acetic acid solution, dissolving polyvinyl alcohol into ionized water, and uniformly mixing the two solutions to obtain a first layer of electrostatic spinning solution. And spinning the solution into a first layer of nanofiber membrane by an electrostatic spinning technology, and crosslinking by adopting an ethanol solution of glutaraldehyde.
2) Dissolving polyvinylidene fluoride into N-N dimethylacetamide, adding fluorinated graphene, and uniformly stirring to obtain a second layer of electrostatic spinning solution. And (3) spinning the solution into a second layer of nanofiber membrane on the first layer of membrane through an electrostatic spinning technology to obtain the double-layer electrostatic spinning membrane.
The concentration of the acetic acid is 1-3%, and the concentration of the chitosan is 2-6%.
The concentration of the polyvinyl alcohol is 5% -8%, and the dissolving temperature is 60-90 ℃.
The mass ratio of the chitosan solution to the polyvinyl alcohol solution is 1: 3-3: 1, and the total volume is 2.5-8 mL.
The parameters of the electrostatic spinning of the first layer are as follows: the used needle head is 16-20G, the liquid supply speed is 1-5 mL/h, the voltage is 25-35 kV, the rotation speed of the receiver is 25-35 rpm, and the distance between polar plates is 10-15 cm.
The concentration of the ethanol solution of the glutaraldehyde is 1.5-5%, and the crosslinking time is 2-10 hours.
The concentration of the polyvinylidene fluoride is 8-12%.
The concentration of the fluorinated graphene is 2.5% -6%.
The total volume of the electrostatic spinning solution is 2-5 mL.
The parameters of the second layer electrostatic spinning are as follows: the used needle head is 18-22G, the flow rate is 2-6 mL/h, the voltage is 20-30 kV, the rotation speed of the receiver is 20-40 rpm, and the distance between polar plates is 8-16 cm.
Has the advantages that: compared with the prior art, the invention has the following advantages:
1) the method has the advantages of simple process and mild conditions;
2) the double-layer nanofiber membrane prepared by the method has super-hydrophobic performance;
3) the double-layer nanofiber membrane prepared by the method has high-efficiency water-oil separation performance, and has high separation efficiency and high flux for various oils.
Drawings
Fig. 1 is a surface water contact angle picture of a double-layered nanofiber membrane prepared in example 1 of the present invention.
Fig. 2 is a photograph of an oil separation process of the two-layered nanofiber membrane prepared in example 1 of the present invention.
Fig. 3 is a graph of the separation flux of the two-layer nanofiber membrane prepared in example 1 of the present invention for different types of oils.
Detailed Description
Example 1
1) 0.3g of chitosan is dissolved in 10mL of 3% acetic acid solution, 0.6g of polyvinyl alcohol is dissolved in 10mL of ionized water at 80 ℃, and the two solutions are uniformly mixed according to the ratio of 1: 1 to obtain a first layer of electrostatic spinning solution. By using an electrostatic spinning technology, 5mL of the solution is spun into a first layer of nanofiber membrane by using an 18G needle, the liquid supply speed is 3mL/h, the voltage is 30kV, the rotation speed of a receiver is 30rpm, and the distance between polar plates is 13 cm. Crosslinking was carried out for 6 hours using a 4% glutaraldehyde solution in ethanol.
2) Dissolving 1g of polyvinylidene fluoride into 10mL of N-N dimethylacetamide, and adding 0.3g of fluorinated graphene into the mixture, and uniformly stirring the mixture to obtain a second-layer electrostatic spinning solution. And (3) spinning 5mL of the solution into a second layer of nanofiber membrane by using an 18G needle on the first layer of membrane through an electrostatic spinning technology, wherein the liquid supply speed is 3mL/h, the voltage is 30kV, the rotation speed of a receiver is 30rpm, and the distance between polar plates is 13cm, so as to obtain the double-layer nanofiber membrane.
The performance test of the double-layer nanofiber membrane prepared in example 1 was carried out as follows:
1) water contact Angle test
Fig. 1 is a photograph of water contact angle of a two-layer nanofiber membrane. As shown, the water contact angle of the surface of the double-layer nanofiber membrane is 154.7 °, showing superhydrophobic performance.
2) Process for the separation of trichloromethane
Fig. 2 is a photograph of a chloroform separation process using a two-layer nanofiber membrane. As shown, the double-layered nanofiber membrane was able to effectively separate oil red O-dyed chloroform from methylene blue-dyed water.
3) Separation flux test
Fig. 3 is a graph of the separation flux of a two-layer nanofiber membrane for different types of oil. As shown, the double layer nanofiberThe vitamin membrane has high-efficiency separation effect on different types of oil. Wherein the separation flux of the dichloromethane is 11043L/m2H; the separation flux of the trichloromethane is highest, and the flux value reaches 12012L/m2H; the separation flux of n-hexane is 10802L/m2H; the separation flux of the petroleum ether is 9927L/m2H; the separation flux to the vegetable oil is 8122L/m2H; the separation flux of the vacuum pump oil is 8217L/m2·h。
Example 2
1) 0.2g of chitosan is dissolved in 8mL of 1% acetic acid solution, 0.6g of polyvinyl alcohol is dissolved in 8mL of ionized water at 90 ℃, and the two solutions are uniformly mixed according to the ratio of 1: 3 to obtain a first layer of electrostatic spinning solution. 6mL of the solution is spun into a first layer of nanofiber membrane by an electrostatic spinning technology, a 20G needle is used, the liquid supply speed is 4mL/h, the voltage is 35kV, the rotation speed of a receiver is 25rpm, and the distance between polar plates is 10 cm. Crosslinking was carried out for 10 hours with 2% glutaraldehyde in ethanol.
2) And (3) dissolving 7.5g of polyvinylidene fluoride into 8mL of N-N dimethylacetamide, and adding 0.4g of fluorinated graphene into the mixture, and uniformly stirring the mixture to obtain a second-layer electrostatic spinning solution. And (3) spinning 3mL of the solution into a second layer of nanofiber membrane by using a 22G needle on the first layer of membrane through an electrostatic spinning technology, wherein the liquid supply speed is 5.5mL/h, the voltage is 25kV, the rotation speed of a receiver is 35rpm, and the distance between polar plates is 10cm, so as to obtain the double-layer nanofiber membrane.
Example 3
1) 0.7g of chitosan was dissolved in 15mL of 2.5% acetic acid solution, 0.7g of polyvinyl alcohol was dissolved in 12mL of ionized water at 85 ℃, and the two solutions were mixed uniformly in a ratio of 1: 2 to obtain a first layer of electrospinning solution. By using an electrostatic spinning technology, 4mL of the solution is spun into a first layer of nanofiber membrane by using a 19G needle, the liquid supply speed is 2.5mL/h, the voltage is 25kV, the rotation speed of a receiver is 35rpm, and the distance between polar plates is 12 cm. Cross-linking was carried out for 8 hours using 2.5% glutaraldehyde in ethanol.
2) Dissolving 1.1g of polyvinylidene fluoride into 12mL of N-N dimethylacetamide, and adding 0.36g of fluorinated graphene into the mixture and uniformly stirring the mixture to obtain a second-layer electrostatic spinning solution. And (3) spinning 4mL of the solution into a second layer of nanofiber membrane by using a 20G needle on the first layer of membrane through an electrostatic spinning technology, wherein the liquid supply speed is 3.5mL/h, the voltage is 20kV, the rotation speed of a receiver is 20rpm, and the distance between polar plates is 8cm, so as to obtain the double-layer nanofiber membrane.
Example 4
1) 0.75g of chitosan is dissolved in 15mL of 2% acetic acid solution, 0.3g of polyvinyl alcohol is dissolved in 5mL of ionic water at 75 ℃, and the two solutions are uniformly mixed according to the ratio of 2: 1 to obtain a first layer of electrostatic spinning solution. Spinning 4.5mL of the solution into a first layer of nanofiber membrane by using an electrostatic spinning technology and a 16G needle, wherein the liquid supply speed is 5mL/h, the voltage is 28kV, the rotation speed of a receiver is 32rpm, and the distance between polar plates is 15 cm. Cross-linking was carried out for 7 hours using a 3.5% glutaraldehyde in ethanol.
2) Dissolving 1.2g of polyvinylidene fluoride into 15mL of N-N dimethylacetamide, and adding 0.5g of fluorinated graphene into the mixture and uniformly stirring the mixture to obtain a second-layer electrostatic spinning solution. And (3.5 mL) of the solution is spun into a second layer of nanofiber membrane by using a 19G needle on the first layer of membrane through an electrostatic spinning technology, wherein the liquid supply speed is 5mL/h, the voltage is 30kV, the rotation speed of a receiver is 40rpm, and the distance between polar plates is 12cm, so that the double-layer nanofiber membrane is obtained.
Several embodiments of the present invention have been described. It is to be noted that the present invention is not limited to the above-mentioned several embodiments, and various changes can be made without departing from the essence of the present invention.
Claims (10)
1. A double-layer nanofiber membrane for water-oil separation and a preparation method thereof are characterized by comprising the following steps:
1) dissolving chitosan into an acetic acid solution, dissolving polyvinyl alcohol into ionized water, and uniformly mixing the two solutions to obtain a first layer of electrostatic spinning solution. And spinning the solution into a first layer of nanofiber membrane by an electrostatic spinning technology, and crosslinking by adopting an ethanol solution of glutaraldehyde.
2) Dissolving polyvinylidene fluoride into N-N dimethylacetamide, adding fluorinated graphene, and uniformly stirring to obtain a second layer of electrostatic spinning solution. And (3) spinning the solution into a second layer of nanofiber membrane on the first layer of membrane through an electrostatic spinning technology to obtain the double-layer electrostatic spinning membrane for water-oil separation.
2. The method of claim 1, wherein: in the step 1), the concentration of acetic acid is 1-3%, and the concentration of chitosan is 2-6%.
3. The method of claim 1, wherein: in the step 1), the concentration of the polyvinyl alcohol is 5-8%, and the dissolving temperature is 60-90 ℃.
4. The method of claim 1, wherein: in the step 1), the mass ratio of the chitosan solution to the polyvinyl alcohol solution is 1: 3-3: 1, and the total volume is 2.5-8 mL.
5. The method of claim 1, wherein: the parameters of electrostatic spinning in the step 1) are as follows: the used needle head is 16-20G, the liquid supply speed is 1-5 mL/h, the voltage is 25-35 kV, the rotation speed of the receiver is 25-35 rpm, and the distance between polar plates is 10-15 cm.
6. The method of claim 1, wherein: in the step 1), the concentration of the ethanol solution of the glutaraldehyde is 1.5-5%, and the crosslinking time is 2-10 hours.
7. The method of claim 1, wherein: the concentration of the polyvinylidene fluoride in the step 2) is 8-12%.
8. The method of claim 1, wherein: the concentration of the fluorinated graphene in the step 2) is 2.5-6%.
9. The method of claim 1, wherein: the total volume of the electrostatic spinning solution in the step 2) is 2-5 mL.
10. The method of claim 1, wherein: the parameters of electrostatic spinning in the step 2) are as follows: the used needle head is 18-22G, the flow rate is 2-6 mL/h, the voltage is 20-30 kV, the rotation speed of the receiver is 20-40 rpm, and the distance between polar plates is 8-16 cm.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104480636A (en) * | 2014-11-28 | 2015-04-01 | 江南大学 | Polyvinylidene fluoride nano-fiber membrane material and preparation method and application thereof |
| CN106894165A (en) * | 2017-04-25 | 2017-06-27 | 浙江大学 | A kind of modifying super hydrophobicity static spinning membrane and its preparation method and application |
| CN108998892A (en) * | 2017-06-07 | 2018-12-14 | 南京理工大学 | A kind of preparation method of chitosan-graphene oxide/polyacrylonitrile double-layer nanometer tunica fibrosa |
| CN109126484A (en) * | 2018-09-28 | 2019-01-04 | 成都其其小数科技有限公司 | A kind of method that 3D printing prepares the super hydrophobic porous film of polycarbonate/graphene |
| CN110053334A (en) * | 2018-01-19 | 2019-07-26 | 中国石油化工股份有限公司 | A kind of nano-fiber composite film and its preparation method and application |
| CN110872741A (en) * | 2019-09-12 | 2020-03-10 | 武汉工程大学 | Composite nanofiber membrane simultaneously used for emulsion separation and dye adsorption and preparation method thereof |
| CN111992058A (en) * | 2020-07-22 | 2020-11-27 | 苏州大学 | Composite fiber membrane for oil-water emulsion separation and preparation method thereof |
-
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- 2021-01-15 CN CN202110059297.9A patent/CN113308799A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104480636A (en) * | 2014-11-28 | 2015-04-01 | 江南大学 | Polyvinylidene fluoride nano-fiber membrane material and preparation method and application thereof |
| CN106894165A (en) * | 2017-04-25 | 2017-06-27 | 浙江大学 | A kind of modifying super hydrophobicity static spinning membrane and its preparation method and application |
| CN108998892A (en) * | 2017-06-07 | 2018-12-14 | 南京理工大学 | A kind of preparation method of chitosan-graphene oxide/polyacrylonitrile double-layer nanometer tunica fibrosa |
| CN110053334A (en) * | 2018-01-19 | 2019-07-26 | 中国石油化工股份有限公司 | A kind of nano-fiber composite film and its preparation method and application |
| CN109126484A (en) * | 2018-09-28 | 2019-01-04 | 成都其其小数科技有限公司 | A kind of method that 3D printing prepares the super hydrophobic porous film of polycarbonate/graphene |
| CN110872741A (en) * | 2019-09-12 | 2020-03-10 | 武汉工程大学 | Composite nanofiber membrane simultaneously used for emulsion separation and dye adsorption and preparation method thereof |
| CN111992058A (en) * | 2020-07-22 | 2020-11-27 | 苏州大学 | Composite fiber membrane for oil-water emulsion separation and preparation method thereof |
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