CN115364678A - High-pollutant-receiving high-strength nanofiber composite nylon microfiltration membrane and preparation method thereof - Google Patents
High-pollutant-receiving high-strength nanofiber composite nylon microfiltration membrane and preparation method thereof Download PDFInfo
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Abstract
The invention provides a high dirt-receiving high-strength nanofiber composite nylon microfiltration membrane and a preparation method thereof, wherein the high dirt-receiving high-strength nanofiber composite nylon microfiltration membrane comprises a filtration membrane layer and a dirt-receiving layer, wherein the filtration membrane layer is a high-strength high-flux flat nylon microfiltration membrane; the pollutant carrying layer comprises an upper nylon nanofiber membrane and a lower flat nylon microfiltration membrane. The method comprises the steps of preparing a spinning solution, spinning the spinning solution on the surface of a flat nylon microfiltration membrane through a needleless electrostatic spinning machine, and sequentially forming a fine fiber layer and a coarse fiber layer to form a dirt containing layer. The method has the advantages that the nylon nanofiber membranes with different diameters are electrospun on the basis of the flat nylon microfiltration membrane with high strength and high flux, so that the pollutant carrying capacity of the filtration membrane is improved on the premise of ensuring the filtration precision of the filtration membrane; the nanofiber is prepared by utilizing the electrostatic spinning technology, the preparation method is simple, and the preparation process is controllable.
Description
Technical Field
The invention belongs to the technical field of filtration, and relates to a preparation method of a high-dirt-receiving high-strength nanofiber composite nylon microfiltration membrane.
Background
With the development of economy, the application field of microporous membranes is continuously expanded, and the microporous membranes are widely applied to various fields such as food, medical treatment, electronics, chemical industry and the like.
Polyamide (PA, commonly known as nylon) is a commonly used material for preparing microporous membranes, has good mechanical properties, heat resistance, abrasion resistance, chemical resistance and the like, and is widely used in filtration treatment of laboratory and industrial liquids.
The commonly used preparation method of microporous membranes is a phase inversion method, which is to perform mass transfer exchange between a solvent and a non-solvent on a polymer solution by a certain physical method, change the thermodynamic state of the solution, enable the solution to generate phase separation from a homogeneous polymer solution, convert the solution into a three-dimensional macromolecular network type gel structure, and finally solidify the gel structure to form a membrane. The flat membrane prepared by the method has small aperture, high filtration precision and excellent mechanical property, and the narrow aperture distribution and the small aperture easily cause the blockage of the filter membrane when filtering some larger particles, thereby influencing the service life of the filter membrane.
Nanofibers prepared by electrospinning is a porous material with small pore size and high porosity, and the electrospinning technique is considered to be the most versatile and efficient technique for producing continuous nanofibers with controlled morphology, structure and functional composition. The electrostatic spinning technology is that high-voltage static electricity is utilized to enable polymer solution or melt to carry thousands of volts of high-voltage static electricity, and charged polymer liquid drops overcome surface tension under the action of electric field force to form jet trickle. The thin stream evaporates or solidifies during the spraying process and eventually falls on the receiving device, forming a fiber film of tens of nanometers to several micrometers. The prepared nanofiber membrane has high porosity, small pore diameter and good interconnected pore structure. However, in the aspect of liquid filtration, due to the structural characteristics, the filtration precision is not enough, and the fiber membrane strength is low, so that the nanofiber membrane prepared by simply using electrostatic spinning at present cannot be well applied.
Therefore, the characteristics of the flat membrane and the nanofiber membrane are combined, and the nanofiber layer is electrospun on the flat membrane, so that the dirt containing performance of the filter membrane can be effectively improved, and the service life of the filter membrane is prolonged. Is applied to wider market fields.
Currently, there is less research related to the use of electrospinning technology in the filtration membrane industry.
Chinese patent CN112791596A discloses a preparation method of polyvinylidene fluoride hydrophilic membrane with acid, alkali and ethanol resistance, which comprises electrospinning PVDF and TBAC into nano-membrane, and performing hydrophilic treatment to prepare hydrophilic membrane for liquid filtration. Although the patent adopts the electrostatic spinning nanometer technology, the filtration precision is lower.
Chinese patent CN112978861A discloses a hydrophilic and hydrophobic nanofiltration membrane, which comprises a substrate nanofiltration membrane layer, a hydrophobic nanofiber membrane layer and a surface hydrophilic modification layer. The invention has complex process, firstly utilizes an electrostatic spinning method to spin the nano-fiber on the substrate nanofiltration membrane layer, then loads the carbon nano-tube on the surface of the nano-fiber, and finally carries out modification treatment.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of a high-dirt-receiving high-strength nanofiber composite nylon microfiltration membrane.
The technical scheme of the invention is as follows:
a high-dirt-receiving high-strength nanofiber composite nylon microfiltration membrane comprises a filtration membrane layer and a dirt receiving layer, wherein the filtration membrane layer is a high-strength high-flux flat nylon microfiltration membrane; the pollutant carrying layer comprises an upper nylon nanofiber membrane and a lower flat nylon microfiltration membrane.
Preferably, the nylon nanofiber membrane comprises fine fibers with the diameter of 10nm-500nm and coarse fibers with the diameter of 500nm-1000nm, the thickness of the fine fibers is set to be 10-100 mu m, and the thickness of the coarse fibers is set to be 10-100 mu m.
Preferably, the aperture of the lower-layer flat nylon microfiltration membrane is 0.22um or 0.45um, the flat nylon filtration membrane has high flux, the pure water flux of the filtration membrane meeting the aperture of 0.22um is not lower than 6ml/cm < 2 >/min under 0.07Mpa, or the flat nylon filtration membrane has high flux, the pure water flux of the filtration membrane meeting the aperture of 0.45um is not lower than 12ml/cm < 2 >/min under 0.07 Mpa.
Preferably, the flat nylon microfiltration membrane is a supported high-strength filtration membrane, and the tensile strength of the filtration membrane is 15-20MPa.
The invention discloses a preparation method of a high-nano-pollution high-strength nanofiber composite nylon microfiltration membrane, which comprises the following steps:
(1) Solution preparation: dissolving nylon slices in a solvent, and stirring to obtain a spinning solution;
(2) Preparing a stain containing layer: spinning the spinning solution on the surface of a flat nylon microfiltration membrane through a needleless electrostatic spinning machine to form a fine fiber layer and a coarse fiber layer in sequence.
Further, in the step (1), the spinning material comprises one or more of nylon 6 and nylon 66.
Further, in the step (1), the molecular weight of the nylon is 1.5-3 ten thousand.
Further, in the step (1), the solvent comprises one or more of formic acid and acetic acid;
further, in the step (1), the mass fraction of the fine fiber spinning solution is between 10 and 15 percent, and the mass fraction of the coarse fiber spinning solution is between 15 and 30 percent.
Further, in the step (1), the stirring time is 2-12h, and the stirring temperature is 25-65 ℃.
Further, in the step (2), the spinning voltage of electrostatic spinning is 50-70kV, and the receiving distance is 15-35cm.
Further, in the step (2), the ambient temperature of the electrostatic spinning is 25-30 ℃, and the humidity is 40-70%.
The invention has the beneficial effects that:
(1) The method has the advantages that the nylon nanofiber membranes with different diameters are electrospun on the basis of the flat nylon microfiltration membrane with high strength and high flux, so that the pollutant carrying capacity of the filtration membrane is improved on the premise of ensuring the filtration precision of the filtration membrane;
(2) The nanofiber is prepared by utilizing the electrostatic spinning technology, the preparation method is simple, and the preparation process is controllable.
Drawings
FIG. 1 is an electron microscope image of the nanofiber composite nylon microfiltration membrane of example 1.
FIG. 2 is an electron microscope image of the nanofiber composite nylon microfiltration membrane of example 2.
Detailed Description
The invention will be further illustrated with reference to specific embodiments without restricting the patent thereto.
Example 1
Step 1: 10g of nylon 66 chips having a molecular weight of 1.5 ten thousand were added to 90g of formic acid and stirred at 30 ℃ for 6 hours. Obtaining nylon 66 electrostatic spinning solution with the mass fraction of 10%;
step 2: spinning the electrostatic spinning solution on a flat nylon microfiltration membrane. The electrostatic spinning parameters are as follows: the ambient temperature is 26 ℃ and the humidity is 40%. Spinning voltage is 70kv, receiving distance is 20cm, and winding speed is 0.3m/min;
and step 3: 20g of nylon 66 chips having a molecular weight of 1.5 ten thousand were added to 80g of formic acid and stirred at 30 ℃ for 6 hours. Obtaining nylon 66 electrostatic spinning solution with the mass fraction of 20%;
and 4, step 4: and (3) spinning the electrostatic spinning solution in the step (3) on the nanofiber membrane prepared in the step (2) to obtain the nanofiber composite nylon microfiltration membrane. Wherein the electrostatic spinning parameters are the same as those in the step 2.
Example 2
Step 1: 15g of nylon 6 chips having a molecular weight of 1.5 ten thousand were added to 85g of formic acid and stirred at 30 ℃ for 4 hours. Obtaining nylon 6 electrostatic spinning solution with the mass fraction of 15%;
and 2, step: spinning the electrostatic spinning solution on a flat nylon microfiltration membrane. The electrostatic spinning parameters are as follows: the ambient temperature is 25 ℃ and the humidity is 40%. Spinning voltage is 70kv, receiving distance is 20cm, and winding speed is 0.1m/min;
and step 3: 25g of nylon 6 chips having a molecular weight of 1.5 ten thousand were added to 75g of formic acid and stirred at 30 ℃ for 4 hours. Obtaining 25% of nylon 6 electrostatic spinning solution by mass fraction;
and 4, step 4: and (3) spinning the electrostatic spinning solution in the step (3) on the nanofiber membrane prepared in the step (2) to obtain the nanofiber composite nylon microfiltration membrane. Wherein the electrostatic spinning parameters are the same as those in the step 2.
Example 3
Step 1: 8g of nylon 6 chips having a molecular weight of 1.5 ten thousand were added to 92g of formic acid and stirred at 30 ℃ for 4 hours. Obtaining 8% nylon 6 electrostatic spinning solution by mass fraction;
step 2: spinning the electrostatic spinning solution on a flat nylon microfiltration membrane. The electrostatic spinning parameters are as follows: the ambient temperature is 25 ℃ and the humidity is 40%. Spinning voltage is 70kv, receiving distance is 20cm, and winding speed is 0.1m/min;
and 3, step 3: 25g of nylon 6 chips having a molecular weight of 1.5 ten thousand were added to 75g of formic acid and stirred at 30 ℃ for 4 hours. Obtaining 25% of nylon 6 electrostatic spinning solution by mass fraction;
and 4, step 4: and (3) spinning the electrostatic spinning solution in the step (3) on the nanofiber membrane prepared in the step (2) to obtain the nanofiber composite nylon microfiltration membrane. Wherein the electrostatic spinning parameters are the same as those in the step 2.
Example 4
Step 1: 10g of nylon 6 chips having a molecular weight of 1.5 ten thousand were added to 90g of acetic acid, and stirred at 30 ℃ for 4 hours. Obtaining nylon 6 electrostatic spinning solution with the mass fraction of 90%;
and 2, step: spinning the electrostatic spinning solution on a flat nylon microfiltration membrane. The electrostatic spinning parameters are as follows: the ambient temperature is 25 ℃ and the humidity is 40%. Spinning voltage is 70kv, receiving distance is 15cm, and winding speed is 0.2m/min;
and step 3: 25g of nylon 6 chips with a molecular weight of 1.5 ten thousand are added to 75g of acetic acid and stirred for 4 hours at 30 ℃. Obtaining 25% of nylon 6 electrostatic spinning solution by mass fraction;
and 4, step 4: spinning the spinning solution in the step 3 on the nanofiber membrane prepared in the step 2 to obtain the nanofiber composite nylon microfiltration membrane. The electrostatic spinning parameters are as follows: the ambient temperature is 25 ℃ and the humidity is 40%. Spinning voltage is 70kv, receiving distance is 15cm, and winding speed is 0.1m/min.
The results of the dirt holding capacity and the percentage increase in dirt holding capacity (the improvement in dirt holding rate) of the example 1, example 2, example 3, example 4 and the original flat nylon microfiltration membrane are shown in the following table 1, and the test conditions are as follows: the amount of iced black tea was filtered after 2min under a pressure of 0.1 MPa.
TABLE 1
| Flat nylon microfiltration membrane | Example 1 | Example 2 | Example 3 | Example 4 | |
| Capacity of receiving dirt | 88g | 95g | 119g | 101g | 107g |
| Increase rate of pollutant collection | - | 8.0% | 35.2% | 14.8% | 21.6% |
From table 1, it can be seen that the fouling tolerance of the flat nylon microfiltration membrane can be effectively improved by electrospinning the nylon nanofiber membrane on the upper layer.
For example 1, exampleThe results of the water flux tests of example 2, example 3, example 4 and the raw flat nylon microfiltration membrane are as follows, and the test conditions are as follows: filter disc 47mm in diameter (membrane area 9.62 cm) 2 ) At a pressure of 0.07mpa, over a period of 100ml of water (25 ℃).
TABLE 2
| Flat nylon microfiltration membrane | Example 1 | Example 2 | Example 3 | Example 4 | |
| Water flux (time) | 29.54s | 30.92s | 33.01s | 35.20s | 30.35s |
It can be seen from the table that electrospinning the upper nylon nanofiber membrane on the flat nylon microfiltration membrane has little effect on the water flux of the original flat nylon microfiltration membrane. Therefore, the nylon nanofiber membrane electrospun on the flat nylon microfiltration membrane can effectively improve the dirt-holding capacity of the filtration membrane and does not influence the water flux of the filtration membrane.
A high-dirt-holding high-strength nanofiber composite nylon microfiltration membrane comprises a filtration membrane layer and a dirt holding layer, wherein the filtration membrane layer is a high-strength high-flux flat nylon microfiltration membrane; the pollutant carrying layer comprises an upper nylon nanofiber membrane and a lower flat nylon microfiltration membrane.
The nylon nanofiber membrane comprises fine fibers with the diameter of 10nm-500nm and coarse fibers with the diameter of 500nm-1000nm, the thickness of the fine fibers is set to be 10-100 mu m, and the thickness of the coarse fibers is set to be 10-100 mu m.
The dull and stereotyped nylon micro-filtration membrane aperture size of lower floor be 0.22um or 0.45 um's filter membrane, dull and stereotyped nylon filter membrane have high flux, satisfy the filter membrane in 0.22um aperture under 0.07Mpa, its pure water flux size is not less than 6ml/cm2/min, or dull and stereotyped nylon filter membrane have high flux, satisfy the filter membrane in 0.45um aperture under 0.07Mpa, its pure water flux size is not less than 12ml/cm2/min.
The flat nylon micro-filtration membrane is a high-strength filtration membrane with a support, and the tensile strength of the filtration membrane is 15-20Mpa.
Claims (10)
1. The utility model provides a dirty high strength nanofiber composite nylon microfiltration membrane is received to height, includes the rete and receives dirty layer, its characterized in that: the filter membrane layer is a flat nylon microfiltration membrane with high strength and high flux; the pollutant carrying layer comprises an upper nylon nanofiber membrane and a lower flat nylon microfiltration membrane.
2. The high-nano-stain high-strength nanofiber composite nylon microfiltration membrane according to claim 1 is characterized in that: the nylon nanofiber membrane comprises fine fibers with the diameter of 10nm-500nm and coarse fibers with the diameter of 500nm-1000nm, the thickness of the fine fibers is set to be 10-100 mu m, and the thickness of the coarse fibers is set to be 10-100 mu m.
3. The high-nano-stain high-strength nanofiber composite nylon microfiltration membrane according to claim 1 is characterized in that: the aperture size of the lower-layer flat nylon microfiltration membrane is 0.22um or 0.45um, the flat nylon filter membrane has high flux, the pure water flux of the filter membrane meeting the aperture of 0.22um is not less than 6ml/cm < 2 >/min under 0.07Mpa, or the flat nylon filter membrane has high flux, the pure water flux of the filter membrane meeting the aperture of 0.45um is not less than 12ml/cm < 2 >/min under 0.07 Mpa.
4. The high-nano-stain high-strength nanofiber composite nylon microfiltration membrane according to claim 1 is characterized in that: the flat nylon micro-filtration membrane is a high-strength filtration membrane with a support, and the tensile strength of the filtration membrane is 15-20Mpa.
5. The method for preparing the high-nano-contamination high-strength nanofiber composite nylon microfiltration membrane according to claim 1, 2, 3 or 4, wherein the method comprises the following steps: the preparation method comprises the following steps of (1) preparing a solution, namely dissolving nylon slices in a solvent, and stirring to obtain a spinning solution; (2) Preparing a dirt accommodating layer, namely spinning the spinning solution on the surface of the flat nylon microfiltration membrane by a needle-free electrostatic spinning machine to form a fine fiber layer and a coarse fiber layer in sequence.
6. The preparation method of the high-nano-pollution high-strength nanofiber composite nylon microfiltration membrane according to claim 5 is characterized in that: in the step (1), the spinning material comprises one or two of nylon 6 and nylon 66; in the step (2), the spinning voltage of electrostatic spinning is 50-70kV, and the receiving distance is 15-35cm.
7. The preparation method of the high-nano-pollution high-strength nanofiber composite nylon microfiltration membrane according to claim 5 is characterized in that: in the step (1), the molecular weight of the nylon is 1.5-3 ten thousand.
8. The preparation method of the nanofiber composite nylon microfiltration membrane with high nano-fouling and high strength according to claim 5 is characterized by comprising the following steps: in the step (1), the solvent comprises one or two of formic acid and acetic acid; in the step (2), the ambient temperature of electrostatic spinning is 25-30 ℃, and the humidity is 40-70%.
9. The preparation method of the nanofiber composite nylon microfiltration membrane with high nano-fouling and high strength according to claim 5 is characterized by comprising the following steps: in the step (1), the mass fraction of the fine fiber spinning solution is between 10 and 15 percent, and the mass fraction of the coarse fiber spinning solution is between 15 and 30 percent.
10. The preparation method of the nanofiber composite nylon microfiltration membrane with high nano-fouling and high strength according to claim 6 is characterized by comprising the following steps: in the step (1), the stirring time is 2-12h, and the stirring temperature is 25-65 ℃.
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