CN116212666B - Acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane and preparation method thereof - Google Patents
Acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane and a preparation method thereof, and relates to the technical field of membrane separation, and the method comprises the following steps: (1) Soaking a polytetrafluoroethylene hollow fiber microfiltration membrane in an organic solution of a nonionic surfactant for pre-modification to obtain a pre-modified membrane; (2) Soaking the pre-modified membrane in a polyphenol monomer solution, carrying out self-polymerization reaction under a closed condition after oxygenation, and constructing a mussel bionic coating on the surface of the membrane and in a membrane hole to prepare the acid-resistant high-water flux polytetrafluoroethylene hollow fiber microfiltration membrane; the polyphenol monomer contains catechol structure; the method has mild reaction conditions, simple process and low equipment requirements, and the modified acid-resistant high-water flux polytetrafluoroethylene hollow fiber microfiltration membrane not only improves the water permeation flux by 9-13 times, but also has excellent acid resistance, and has wide application prospects in the field of wastewater treatment.
Description
Technical Field
The invention relates to the technical field of membrane separation, in particular to an acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane and a preparation method thereof.
Background
The membrane technology is taken as a green and efficient water treatment technology, is one of technologies for innovatively driving green development and relieving water resource shortage, and the high-performance membrane material which is taken as a technical basis is an important guarantee for promoting the development and application of the membrane technology. The microfiltration membrane technology is based on the principle of pore size screening, and is used for intercepting bacteria, colloid, particulate matters and other substances in water under the drive of pressure, so that the purposes of purification, separation and concentration are achieved, and the microfiltration membrane technology is one of common wastewater treatment technologies. The polytetrafluoroethylene membrane has good thermal stability and chemical stability, has been widely applied to treatment of complex water quality, and can effectively separate suspended matters, bacteria, high molecular weight colloid and other substances. However, the polytetrafluoroethylene membrane has poor water permeability and is easy to cause organic pollution to reduce the service life, so that the polytetrafluoroethylene membrane is required to be modified to improve the filtering efficiency and prolong the service life.
The modification method of the polytetrafluoroethylene separation membrane at present mainly comprises a wet chemical method, a plasma treatment, a high-energy radiation treatment surface, a hydrophilic agent infiltration method, a mussel chemical method and the like, but the methods are still to be further improved, for example, the wet chemical method has the problem of serious damage to the membrane structure, and the plasma and high-energy radiation treatment can only modify the membrane surface and cannot realize the modification of the inside of a membrane hole (especially the modification of the inside of a hollow fiber membrane).
The Chinese patent document with publication number of CN108905649A discloses a preparation method of a hydrophilic polytetrafluoroethylene microfiltration membrane, which comprises the steps of self-polymerizing and introducing a polydopamine coating by using a surfactant to assist in the self-polymerization of the L-dopamine, and then crosslinking and curing in a curing agent aqueous solution to obtain the hydrophilic modified polytetrafluoroethylene separation membrane. However, in the method, the introduction process of the polydopamine coating is aqueous phase reaction, hydrophilic modification in holes is difficult to realize, and in addition, the curing process has more complicated steps, and the acid resistance of the hydrophilic modified film is not researched.
The chinese patent publication No. CN112473402a discloses a method for preparing a hydrophilic polytetrafluoroethylene micro-ultrafiltration membrane, which comprises treating polytetrafluoroethylene membrane with a thickener aqueous solution to improve the hydrophilicity of polytetrafluoroethylene membrane and reduce the pore diameter thereof, and immersing the membrane in polytetrafluoroethylene emulsion to obtain the hydrophilic polytetrafluoroethylene micro-ultrafiltration membrane, wherein the polytetrafluoroethylene emulsion contains fluorocarbon surfactant, which may have potential biosafety problem.
Disclosure of Invention
The invention provides a preparation method of an acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane, which has the advantages of mild reaction conditions, simple process and low equipment requirements, and the modified acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane not only has 9-13 times of water permeation flux, but also has excellent acid resistance, and has wide application prospects in the field of wastewater treatment.
The technical scheme adopted is as follows:
the preparation method of the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane comprises the following steps:
(1) Soaking a polytetrafluoroethylene hollow fiber microfiltration membrane in an organic solution of a nonionic surfactant for pre-modification to obtain a pre-modified membrane;
(2) Soaking the pre-modified membrane in a polyphenol monomer solution, carrying out self-polymerization reaction under a closed condition after oxygenation, and constructing a mussel bionic coating on the surface of the membrane and in a membrane hole to prepare the acid-resistant high-water flux polytetrafluoroethylene hollow fiber microfiltration membrane;
the polyphenol monomer contains catechol structure, and is at least one of dopa, dopamine, tannic acid, catechol or catechin compounds, wherein the catechin compounds comprise epicatechin, epigallocatechin, epicatechin gallate or epigallocatechin gallate.
In the prior art, the modification method of the polytetrafluoroethylene separation membrane is mostly based on an aqueous phase modification system, but the polytetrafluoroethylene separation membrane is hydrophobic, and the solute of the aqueous phase is difficult to modify in the membrane pores; according to the invention, the polytetrafluoroethylene hollow fiber microfiltration membrane is pre-modified by the organic solution of the nonionic surfactant, so that the membrane is endowed with excellent hydrophilicity and water permeability, then the membrane is coated by introducing the mussel bionic coating by utilizing the self-polymerization adhesion characteristic of the polyphenol substances, and the hydrophilic and acid-resistant modification of the polytetrafluoroethylene hollow fiber microfiltration membrane is completed, so that the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane is prepared.
Preferably, the polytetrafluoroethylene hollow fiber microfiltration membrane is cleaned, dried and subjected to a pre-modification step.
In the step (1), the nonionic surfactant comprises at least one of laurate polyoxyethylene ester, laureth, alkylphenol polyoxyethylene and fatty alcohol polyoxyethylene, and the organic solvent is at least one of ethanol, acetone and isopropanol.
The polytetrafluoroethylene hollow fiber microfiltration membrane is pre-modified by utilizing the organic solution of the nonionic surfactant, the organic solvent can wet the polytetrafluoroethylene separation membrane, the compatibility of the nonionic surfactant is good, and the nonionic surfactant can modify the polytetrafluoroethylene separation membrane surface and the inside of the pore canal.
Preferably, in the step (1), the mass concentration of the nonionic surfactant in the organic solution of the nonionic surfactant is 3-30wt% and the pre-modification time is 1-12h.
It is further preferred that in step (1), the mass concentration of the nonionic surfactant in the organic solution of the nonionic surfactant is 3 to 15wt%.
The organic solution pre-modification of the nonionic surfactant can obviously improve the hydrophilicity of the polytetrafluoroethylene hollow fiber microfiltration membrane, so that the water contact angle of the polytetrafluoroethylene hollow fiber microfiltration membrane is reduced from 121 degrees to 35-70 degrees, and the self-polymerization reaction of the subsequent monomer on the membrane surface and in the membrane pores is facilitated.
The pre-modified film is unstable and the surfactant is easily lost during operation. The polyphenol monomer containing catechol structure can realize self-polymerization under normal temperature condition, and the excellent adhesiveness of the polyphenol coating is utilized to relieve the loss of the surfactant coating and strengthen the stability of the surfactant coating on the film.
The polyphenol monomer solution is prepared by dissolving polyphenol monomers in Tris-HCl buffer solution or PBS buffer solution; the concentration of Tris-HCl buffer or PBS buffer is 5-20mmol/L, and the pH value is 8.0-9.0.
Preferably, the oxygenation time is 3-30min.
Preferably, in the polyphenol monomer solution, the mass concentration of the polyphenol monomer is 0.2-10g/L; in the self-polymerization reaction process, the higher the concentration of the monomer is, the faster the reaction rate is, the formed mussel bionic coating can be more stable, but the higher the concentration of the monomer is, the larger polyphenol particles can be generated, so that the problem of membrane pore channel blockage is caused.
Further preferably, the mass concentration of the polyphenol monomer in the polyphenol monomer solution is 0.2-5g/L.
Preferably, in the step (2), the self-polymerization time of the polyphenol monomer is 1-48 hours, the self-polymerization time of the monomer is too short, the polyphenol coating is difficult to introduce, the self-polymerization time is too long, and larger particles possibly generate to block the membrane holes.
Further preferably, the polyphenol monomer is self-polymerized for a period of time ranging from 1 to 24 hours.
The invention also provides the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane prepared by the preparation method of the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane.
The acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane is improved by 9-13 times compared with the original membrane by virtue of the further treatment of the mussel bionic coating on the pre-modified membrane, and the water flux can still be kept stable after being soaked in dilute hydrochloric acid with the pH value of 1 for 2 weeks.
The invention also provides application of the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane in the technical field of membrane separation, in particular application in the field of acid wastewater treatment.
Compared with the prior art, the invention has the beneficial effects that:
(1) The preparation method is simple, the reaction condition is mild, the raw material cost is low, and the acid-resistant high-water flux polytetrafluoroethylene hollow fiber microfiltration membrane can be prepared through two steps of pre-modification and self-polymerization deposition, so that the preparation method is convenient for large-scale production.
(2) The acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane prepared by the method disclosed by the invention is coated with the mussel bionic coating on the membrane surface and in the membrane pores, and the mussel bionic coating is not easy to run off in the running process due to the excellent adhesion property of the polyphenol coating, so that the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane has excellent hydrophilic performance, the water contact angle is as low as 36.1 degrees, the water permeation flux is 9-13 times higher than that of the original membrane, the water flux can still be kept above 90% after being soaked in dilute hydrochloric acid with the pH value of 1 for 2 weeks, and the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane has wide application prospect in the field of wastewater treatment and is especially suitable for treating general acidic or inorganic wastewater.
Drawings
FIG. 1 is a schematic representation of the reaction of dopamine autopolymerization process.
FIG. 2 is a graph showing the dynamic contact angle of the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane of example 1 over time.
FIG. 3 is a surface SEM image of various separation membranes, wherein (a) is the untreated polytetrafluoroethylene hollow-fiber microfiltration membrane of example 1, (b) is the composite membrane of comparative example 2, (c) is the pre-modified membrane of comparative example 3, and (d) is the acid-resistant high-water-flux polytetrafluoroethylene hollow-fiber microfiltration membrane of example 1.
FIG. 4 is a sectional SEM image of different separation membranes, wherein (a) is the untreated polytetrafluoroethylene hollow-fiber microfiltration membrane of example 1, (b) is the composite membrane of comparative example 2, (c) is the pre-modified membrane of comparative example 3, and (d) is the acid-resistant high-water-flux polytetrafluoroethylene hollow-fiber microfiltration membrane of example 1.
FIG. 5 is a graph showing XPS energy spectra of membrane surfaces of the polytetrafluoroethylene hollow fiber microfiltration membrane of example 1, the composite membrane of comparative example 2, the pre-modified membrane of comparative example 3, and the acid-resistant high water flux polytetrafluoroethylene hollow fiber microfiltration membrane of example 1.
Fig. 6 is an SEM image of the pre-modified membrane of comparative example 3 and the acid-resistant high water flux polytetrafluoroethylene hollow fiber microfiltration membrane of example 1 after continuous test for 6 hours of pure water, (a) the pre-modified membrane of comparative example 3, and (b) the acid-resistant high water flux polytetrafluoroethylene hollow fiber microfiltration membrane of example 1.
Detailed Description
The invention is further elucidated below in connection with the examples and the accompanying drawing. It is to be understood that these examples are for illustration of the invention only and are not intended to limit the scope of the invention. The methods of operation, under which specific conditions are not noted in the examples below, are generally in accordance with conventional conditions, or in accordance with the conditions recommended by the manufacturer.
Polytetrafluoroethylene hollow fiber microfiltration membranes are offered by the new materials technology company of li-de membrane (beijing).
Comparative example 1
Soaking the polytetrafluoroethylene hollow fiber microfiltration membrane in absolute ethyl alcohol for 1h, and drying in vacuum for later use.
Comparative example 2
Soaking a polytetrafluoroethylene hollow fiber microfiltration membrane in absolute ethyl alcohol for 1h, and drying in vacuum for later use; then placing the membrane in 2g/L dopamine Tris-HCl buffer solution, carrying out self-polymerization for 4h under a closed condition after oxygenation for 5min, wherein the concentration of the Tris-HCl buffer solution is 10mmol/L, the pH value is 8.5, and carrying out vacuum drying for later use after the reaction is finished, wherein the prepared composite membrane is named as PDA@PTFE; the reaction conditions are the optimal modification conditions which are explored through preliminary experiments, and under the reaction conditions, the water flux of the prepared composite membrane is maximum.
Comparative example 3
Soaking a polytetrafluoroethylene hollow fiber microfiltration membrane in absolute ethyl alcohol for 1h, and drying in vacuum for later use; then pre-modifying the membrane by soaking the membrane in ethanol solution of 12wt% polyoxyethylene laurate LAE-4 for 4 hours, and drying the membrane in vacuum for later use, wherein the prepared pre-modified membrane is named as PTFE-LAE; the reaction conditions are the optimal modification conditions which are explored through preliminary experiments, and the prepared pre-modified membrane has the maximum water flux under the reaction conditions.
Example 1
(1) Soaking a polytetrafluoroethylene hollow fiber microfiltration membrane in absolute ethyl alcohol for 1h, drying in vacuum to remove an ethanol solvent, and testing the water contact angle to be 121 degrees;
(2) Polyoxyethylene laurate LAE-4 was dissolved in absolute ethanol to prepare a 12wt% ethanol solution of LAE-4; soaking the polytetrafluoroethylene hollow fiber micro-filtration membrane cleaned in the step (1) in an ethanol solution of LAE-4 for 4 hours for pre-modification to prepare a pre-modified membrane, wherein the contact angle of test water is 56.3 degrees;
(3) Dissolving Dopamine (DA) in Tris-HCl buffer solution with pH value of 8.5 and 10mmol/L, wherein the DA concentration is 2g/L; immersing the pre-modified membrane in a DA-containing Tris-HCl buffer solution, carrying out self-polymerization reaction for 18h under a closed condition at normal temperature after oxygenating for 5min, and drying for 5h at a vacuum of 50 ℃ to obtain the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber micro-filtration membrane (the dopamine self-polymerization process is shown as a graph in figure 1), wherein the prepared acid-resistant high-water-flux polytetrafluoroethylene hollow fiber micro-filtration membrane is denoted as PDA@PTFE-LAE, the water contact angle of the test PDA@PTFE-LAE is 41.5 DEG, and the dynamic contact angle of the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber micro-filtration membrane can be reduced to 0 DEG at 1min as shown in figure 2.
The SEM pictures of the surfaces of the polytetrafluoroethylene hollow fiber microfiltration membranes without any treatment are shown in (a) of fig. 3, the SEM pictures of the surfaces of the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membranes are shown in (d) of fig. 3, and the surfaces of the membranes can be found to be successfully attached with hydrophilic coatings by comparing the SEM pictures before and after modification, and as can be seen from (b) and (c) of fig. 3, pda@ptfe and PTFE-LAE are also successfully modified; comparing the SEM of the sections (a) - (d) in fig. 4, it is known that the membrane pores modified by LAE pre-modification and the method of the present invention also achieve the adhesion of the hydrophilic coating, while the PDA modified membrane section has no obvious change compared with the original membrane, because the PDA modification process is aqueous phase, the monomer is hard to dip into the membrane to achieve the modification in the pores. The chemical environment changes of the film surface before and after modification are shown in fig. 5, and it can be found that the characteristic peaks of O1s and N1s appear in the PDA@PTFE-LAE compared with the original film, which shows that the LAE successfully realizes the construction of a hydrophilic coating, and the PDA coating is also successfully introduced into the film surface.
The stability was tested by continuous filtration for 6h using PDA@PTFE-LAE and the pre-modified membrane PTFE-LAE of comparative example 3, and after filtration, the morphology of the membrane was analyzed and the results are shown in FIG. 6, wherein (a) is PTFE-LAE and (b) is PDA@PTFE-LAE; compared with the pre-modified film, the PDA@PTFE-LAE hydrophilic coating has good stability, and the surface of the film cannot see the fiber of the body after pure water testing, which indicates that the introduction of the PDA layer can slow down the loss of the hydrophilic coating and can promote the hydrophilic timeliness of the film in the practical operation and use process.
Example 2
In this example, the preparation process of the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane is different from that of example 1 only in that the polytetrafluoroethylene hollow fiber microfiltration membrane is pre-modified by using an acetone solution of laureth-10 with a mass concentration of 9wt%, and the pre-modification time is 8 hours.
Example 3
In this example, the process for preparing the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane differs from example 1 only in that the polyphenol monomer is tannic acid and the monomer concentration is 1g/L.
Example 4
In this example, the preparation process of the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane is different from that of example 1 only in that the concentration of Tris-HCl buffer is 20mmol/L, the concentration of monomers in the Tris-HCl buffer is 1.5g/L, and the self-polymerization time is 24 hours.
Example 5
In this example, the preparation process of the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane is different from that of example 1 only in that the oxygenation time is 20min and the self-aggregation time is 10h.
Example 6
In this example, the preparation process of the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane is different from that of example 1 in that the buffer solution is PBS buffer solution, the polyphenol monomer is dopa, and the self-polymerization time is 24 hours.
Sample analysis
The separation membranes prepared in comparative examples 1 to 3 and examples 1 to 6 were subjected to a pure water flux test under a test pressure of 0.1MPa for 30 minutes before the test, and a pure water flux F in L m was calculated according to the following formula -2 h -1 。
Wherein: v represents the volume of water obtained by filtering for a certain time; s represents the effective area of the membrane and Δt represents the filtration time.
The acid resistance of the membrane was evaluated by the change in pure water flux of the membrane before and after the acid treatment; the acid treatment conditions are as follows: hydrochloric acid solution at ph=1, at 25 ℃, for 2 weeks.
The pure water fluxes before and after the acid treatment of the separation membranes prepared in comparative examples 1 to 3 and examples 1 to 6 are shown in Table 1. The results show that the flux of the unmodified polytetrafluoroethylene hollow fiber microfiltration membrane in comparative examples 2 and 3 is improved by 3-7 times compared with that of the unmodified polytetrafluoroethylene hollow fiber microfiltration membrane in comparative example 1, which shows that LAE infiltration and dopamine deposition can both obviously improve the water flux of the membrane, and the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane prepared by the method has better water permeability than that of the unmodified membrane by 9-13 times, and the water permeability of the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane obtained by modification in examples 1-6 after 2 weeks of acid soaking can still maintain a higher level.
TABLE 1 Water flux and acid resistance of separation membranes of examples 1 to 6 and comparative examples 1 to 3
While the foregoing embodiments have been described in detail in connection with the embodiments of the invention, it should be understood that the foregoing embodiments are merely illustrative of the invention and are not intended to limit the invention, and any modifications, additions, substitutions and the like made within the principles of the invention are intended to be included within the scope of the invention.
Claims (5)
1. The preparation method of the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane is characterized by comprising the following steps of:
(1) Soaking a polytetrafluoroethylene hollow fiber microfiltration membrane in an organic solution of a nonionic surfactant for pre-modification to obtain a pre-modified membrane;
(2) Soaking the pre-modified membrane in a polyphenol monomer solution, carrying out self-polymerization reaction under a closed condition after oxygenation, and constructing a mussel bionic coating on the surface of the membrane and in a membrane hole to prepare the acid-resistant high-water flux polytetrafluoroethylene hollow fiber microfiltration membrane;
the nonionic surfactant comprises at least one of polyoxyethylene laurate, laureth, alkylphenol ethoxylate and fatty alcohol ethoxylate;
in the step (1), the mass concentration of the nonionic surfactant in the organic solution of the nonionic surfactant is 3-30wt%, the pre-modification time is 1-12h, and the organic solvent is at least one of ethanol, acetone and isopropanol;
the polyphenol monomer contains catechol structure, which is at least one of dopa, dopamine, tannic acid, catechol or catechin compounds, wherein the catechin compounds comprise epicatechin, epigallocatechin, epicatechin gallate or epigallocatechin gallate; in the polyphenol monomer solution, the mass concentration of the polyphenol monomer is 0.2-10 g/L.
2. The method for preparing the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane according to claim 1, wherein the polyphenol monomer solution is prepared by dissolving polyphenol monomers in Tris-HCl buffer or PBS buffer; the oxygenation time is 3-30min.
3. The method for preparing an acid-resistant high-water-flux polytetrafluoroethylene hollow fiber micro-filtration membrane according to claim 1, wherein in the step (2), the self-polymerization time of the polyphenol monomer is 1-48 h.
4. The acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane prepared by the preparation method of the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane according to claim 1.
5. The use of the acid-resistant high-water-flux polytetrafluoroethylene hollow fiber microfiltration membrane as claimed in claim 4 in the technical field of membrane separation.
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