CN111701464A - Super-hydrophilic beta-FeOOH/PDAus/PVDF composite membrane and preparation and application thereof - Google Patents
Super-hydrophilic beta-FeOOH/PDAus/PVDF composite membrane and preparation and application thereof Download PDFInfo
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Abstract
The invention discloses a super-hydrophilic beta-FeOOH/PDAus/PVDF composite membrane as well as a preparation method and application thereof, belonging to the field of modification of a high polymer composite membrane. The invention firstly utilizes the Michael addition reaction between dopamine and PVDF to prepare the PDAus/PVDF composite membrane, and then prepares the composite membrane through the chelation between catechol hydroxyl on dopamine molecules and ferric ions, wherein dopamine microspheres and beta-FeOOH nanoparticles are fixed on the upper and lower surfaces of the PVDF membrane and in the membrane pore walls, so that the composite membrane reaches a super-hydrophilic state, and the defects of the PDAus/PVDF composite membrane such as hydrophilic instability and uncontrollable property are overcome. Meanwhile, due to the unique chemical characteristics of beta-FeOOH, the modified composite membrane has good dye removal performance, so that the composite membrane has good application value in the fields of water filtration and purification, industrial wastewater dye removal and the like.
Description
Technical Field
The invention belongs to the field of preparation, modification and application of a high-molecular composite membrane, and particularly relates to a beta-FeOOH/PDAus/PVDF composite membrane with excellent hydrophilic performance.
Background
Polyvinylidene fluoride (PVDF) is a crystalline polymer, is white granular or powdery, has good thermal stability and chemical stability, is not easily corroded by acid, alkali, oxidant and halogen at normal temperature, is stable to organic solvents such as aliphatic hydrocarbon, aromatic hydrocarbon, alcohol and aldehyde, and is only dissolved in a few polar solvents, fuming sulfuric acid, strong base and the like; the material has outstanding mechanical properties, and has the characteristics of good impact strength and toughness, high hardness and good wear resistance; and also has outstanding resistance to gamma rays, ultraviolet radiation, and the like. However, the hydrophobic nature of PVDF membranes makes it prone to adsorb organics, colloids, etc. during separation resulting in membrane fouling, and thus the effect of membrane fouling on membrane performance is one of the most serious challenges facing current polymer separation membranes.
According to the invention, the PVDF microfiltration membrane is modified by hydrophilic high molecular material dopamine microspheres, the catechol hydroxyl on dopamine molecules and beta-FeOOH nanoparticles with strong hydrophilicity are chelated, and the beta-FeOOH nanoparticles are subjected to low-temperature control and hydrolysis under an acidic condition, so that the chemical stability, mechanical strength, thermal stability and other aspects of the obtained composite membrane are obviously improved, the further functionalization of the material surface is realized, various performance defects of the membrane raw material are made up, and the obtained membrane has good hydrophilicity, anti-pollution performance and good dye removal capability, and has wide application value in the fields of water filtration and purification, biomedicine and the like.
Disclosure of Invention
The invention aims to provide a beta-FeOOH/PDAus/PVDF composite membrane with super-hydrophilic performance and a preparation method thereof. The preparation method has the advantages of simple preparation process, easy operation, obvious modification effect, low requirement on equipment and easy industrial implementation; the obtained composite membrane has good application value in the fields of water filtration and purification, industrial wastewater dye removal and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
an β -FeOOH/PDAus/PVDF composite membrane with super-hydrophilicity is prepared through the Michael addition reaction between dopamine and PVDF by using the unique biogel characteristics of dopamine, chelating with FeCl between catechol hydroxyl on dopamine molecule and ferric ion3And preparing a precursor solution, wherein the dopamine microspheres and β -FeOOH nanoparticles are fixed on the upper and lower surfaces of the PVDF membrane and in the pore wall of the membrane.
The specific preparation method of the super-hydrophilic beta-FeOOH/PDAus/PVDF composite membrane comprises the following steps:
(1) preparing a dopamine modified PVDF composite membrane: adding a Tris-phosphate neutral buffer solution into a mixed solution of water and absolute ethyl alcohol (the volume ratio of the water to the absolute ethyl alcohol is 1-5: 1) to prepare a solution with a Tris concentration of 10 mmol/L, adding dopamine powder into the solution, and stirring for 1 day to obtain a dopamine solution with a concentration of 0.5-2 mg/mL; adding the PVDF raw membrane into a dopamine solution, continuously stirring for 3 days, cleaning the membrane and airing the membrane for 2 days to obtain a modified PDAus/PVDF composite membrane;
(2) preparing β -FeOOH/PDAus/PVDF composite membrane with super-hydrophilicity by mixing FeCl3·6H2Dissolving O in water to prepare a solution of 5-50 mg/mL, adding 0.01mol/L of acid solution according to the volume ratio of 2: 1 to prepare a mineralized solution, placing the modified PDAus/PVDF composite membrane obtained in the step (1) into the mineralized solution, stirring and reacting for 6-24 h under the condition of a constant-temperature water bath at 60 ℃, cleaning the membrane after stirring is completed, and airing the membrane for 2 days to obtain the β -FeOOH/PDAus/PVDF composite membrane.
The acidic solution in the step (2) is HCl solution and H2SO4Solution or HNO3And (3) solution.
The obtained super-hydrophilic beta-FeOOH/PDAus/PVDF composite membrane can be used in the fields of water filtration and purification treatment or industrial wastewater dye removal and the like.
The invention has the following remarkable advantages:
(1) the dopamine micromolecule substance can synthesize functional molecule polydopamine microspheres according to the bionic principle. According to the invention, ferric ions are firmly anchored on the surface of the membrane material by utilizing the bionic structural unit of the polydopamine microsphere, so that the surface of the membrane material has better performance. The dopamine microspheres and the beta-FeOOH nanoparticles are not only fixed on the surface of the PVDF, but also a large amount of beta-FeOOH grows on the hole walls of the membrane, so that support is provided for the composite membrane, and the mechanical property of the composite membrane is enhanced.
(2) Compared with the original PVDF film, the prepared beta-FeOOH/PDAus/PVDF composite film has excellent hydrophilicity, pollution resistance and good dye removal capability, retains the good physical properties of the polyvinylidene fluoride film, and has wide application value in the fields of water filtration and purification, dye removal of industrial wastewater and the like.
(3) The beta-FeOOH/PDAus/PVDF composite membrane prepared by the invention has the following advantages: the hydrophilic nature is good; ② has good anti-pollution performance; the material has good stability and mechanical property; fourthly, the dye has good dye removing performance; the modification effect is obvious, the preparation process is simple, the operation is easy, the requirement on equipment is low, and the industrial implementation is easy.
Drawings
FIG. 1 is a scanning electron microscope image of PVDF raw film (M0) and PDAus/PVDF composite film (M1) and beta-FeOOH/PDAus/PVDF composite film (M2) prepared in example 3.
FIG. 2 is a graph showing the comparison of the contact angle between the PVDF raw film (M0) and the beta-FeOOH/PDAus/PVDF composite film (M2) prepared in example 3.
FIG. 3 is a graph showing the comparison of the removal ability of the beta-FeOOH/PDAus/PVDF composite film (M2) prepared in example 3 to methyl blue dye.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
Example 1
A preparation method of a beta-FeOOH/PDAus/PVDF composite membrane with super-hydrophilic performance comprises the following specific steps:
(1) preparing a dopamine modified PVDF composite membrane:
firstly, deionized water and absolute ethyl alcohol are mixed according to the volume ratio of 5: 1, adding a Tris-phosphate neutral buffer solution to prepare a solution with the Tris concentration of 10 mmol/L, then dissolving dopamine powder into the solution, stirring for 1 day to prepare a dopamine solution with the concentration of 0.5mg/ml, then adding a PVDF (polyvinylidene fluoride) raw membrane into the dopamine solution, continuously stirring for 3 days, and finally cleaning and airing the membrane for 2 days to obtain the modified PDAus/PVDF composite membrane.
(2) Preparing a beta-FeOOH/PDAus/PVDF composite membrane with super-hydrophilic performance:
FeCl is added3·6H2Dissolving O in 100ml of ultrapure water to prepare a solution with the concentration of 6mg/ml, adding 50ml of 0.01M HCl solution to prepare a mineralized solution, placing the PDAus/PVDF composite membrane prepared in the step (1) in the obtained mineralized solution, stirring for 6 hours in a constant-temperature water bath at 60 ℃, cleaning the membrane after stirring, and airing the membrane for 2 days to obtain the β -FeOOH/PDAus/PVDF composite membrane with the contact angle of about 60 degrees.
Example 2
A preparation method of a beta-FeOOH/PDAus/PVDF composite membrane with super-hydrophilic performance comprises the following specific steps:
(1) preparing a dopamine modified PVDF composite membrane:
firstly, deionized water and absolute ethyl alcohol are mixed according to the volume ratio of 5: 1, adding a Tris-phosphate neutral buffer solution to prepare a solution with the Tris concentration of 10 mmol/L, then dissolving dopamine powder into the solution, stirring for 1 day to prepare a dopamine solution with the concentration of 1 mg/ml, then adding a PVDF (polyvinylidene fluoride) raw membrane into the dopamine solution, continuing stirring for 3 days, finally cleaning and airing the membrane for 2 days to obtain the modified PDAus/PVDF composite membrane.
(2) Preparing a beta-FeOOH/PDAus/PVDF composite membrane with super-hydrophilic performance:
FeCl is added3·6H2Dissolving O in 100ml of ultrapure water to prepare a solution with the concentration of 12mg/ml, adding 50ml of 0.01M HCl solution to prepare a mineralized solution, placing the PDAus/PVDF composite membrane prepared in the step (1) in the obtained mineralized solution, stirring for 12 hours in a constant-temperature water bath at 60 ℃, cleaning the membrane after stirring, and airing the membrane for 2 days to obtain the β -FeOOH/PDAus/PVDF composite membrane with the contact angle of about 50 degrees.
Example 3
A preparation method of a beta-FeOOH/PDAus/PVDF composite membrane with super-hydrophilic performance comprises the following specific steps:
(1) preparing a dopamine modified PVDF composite membrane:
firstly, deionized water and absolute ethyl alcohol are mixed according to the volume ratio of 5: 2, adding a Tris-phosphate neutral buffer solution to prepare a solution with the Tris concentration of 10 mmol/L, then dissolving dopamine powder into the solution, stirring for 1 day to prepare a dopamine solution with the concentration of 1.5mg/ml, then adding a PVDF (polyvinylidene fluoride) raw membrane into the dopamine solution, continuously stirring for 3 days, and finally cleaning and airing the membrane for 2 days to obtain the modified PDAus/PVDF composite membrane.
(2) Preparing a beta-FeOOH/PDAus/PVDF composite membrane with super-hydrophilic performance:
FeCl is added3·6H2Dissolving O in 100ml of ultrapure water to prepare a solution with the concentration of 18mg/ml, adding 50ml of 0.01M HCl solution to prepare a mineralized solution, placing the PDAus/PVDF composite membrane prepared in the step (1) in the obtained mineralized solution, stirring for 24 hours in a constant-temperature water bath at 60 ℃, cleaning the membrane after stirring, and airing the membrane for 2 days to obtain the β -FeOOH/PDAus/PVDF composite membrane with the contact angle of about 40 degrees.
Example 4
A preparation method of a beta-FeOOH/PDAus/PVDF composite membrane with super-hydrophilic performance comprises the following specific steps:
(1) preparing a dopamine modified PVDF composite membrane:
firstly, deionized water and absolute ethyl alcohol are mixed according to the volume ratio of 5: 3, adding a Tris-phosphate neutral buffer solution to prepare a solution with the Tris concentration of 10 mmol/L, then dissolving dopamine powder into the solution, stirring for 1 day to prepare a dopamine solution with the concentration of 1.5mg/ml, then adding a PVDF (polyvinylidene fluoride) raw membrane into the dopamine solution, continuing stirring for 3 days, finally cleaning and airing the membrane for 2 days to obtain the modified PDAus/PVDF composite membrane.
(2) Preparing a beta-FeOOH/PDAus/PVDF composite membrane with super-hydrophilic performance:
FeCl is added3·6H2Dissolving O in 100ml of ultrapure water to obtain a solution with a concentration of 18mg/ml, adding 50ml of 0.01M H2SO4Placing the PDAus/PVDF composite membrane prepared in the step (1) in the obtained mineralized solution, stirring for 24 hours in a constant-temperature water bath at 60 ℃, cleaning the membrane after stirring is finished, and airing the membrane for 2 days to obtain the β -FeOOH/PDAus/PVDF composite membrane, wherein the contact angle of the composite membrane is about 30 degrees.
Example 5
A preparation method of a beta-FeOOH/PDAus/PVDF composite membrane with super-hydrophilic performance comprises the following specific steps:
(1) preparing a dopamine modified PVDF composite membrane:
firstly, deionized water and absolute ethyl alcohol are mixed according to the volume ratio of 5: 4, mixing, adding a Tris-phosphate neutral buffer solution to prepare a solution with the Tris concentration of 10 mmol/L, then dissolving dopamine powder into the solution, stirring for 1 day to prepare a dopamine solution with the concentration of 2mg/ml, then adding a PVDF (polyvinylidene fluoride) raw membrane into the dopamine solution, continuously stirring for 3 days, finally cleaning the membrane and airing the membrane for 2 days to obtain the modified PDAus/PVDF composite membrane.
(2) Preparing a beta-FeOOH/PDAus/PVDF composite membrane with super-hydrophilic performance:
FeCl is added3·6H2Dissolving O in 100ml of ultrapure water to prepare a solution with the concentration of 24mg/ml, and adding 50ml of 0.01M HNO3Preparing a mineralized solution from the solution; placing the PDAus/PVDF composite membrane prepared in the step (1) in the obtained mineralized solution, stirring for 24 hours in a constant-temperature water bath at 60 ℃, and finishing stirringAnd cleaning and airing the membrane for 2 days to obtain the β -FeOOH/PDAus/PVDF composite membrane with a contact angle of about 40 degrees.
FIG. 1 is a scanning electron microscope image of PVDF raw film (M0) and PDAus/PVDF composite film (M1) and beta-FeOOH/PDAus/PVDF composite film (M2) prepared in example 3. As can be seen, the PVDF raw membrane has a large amount of microfiltration membrane pores and an average pore diameter of 0.45 micron; dopamine microspheres with the average particle size of 300nm are immobilized on the surface of the PDAus/PVDF composite membrane; and the surface of the beta-FeOOH/PDAus/PVDF composite membrane is loaded with a large amount of needle-rod-shaped beta-FeOOH nano particles, so that the hydrophobic PVDF original membrane is completely covered.
FIG. 2 is a graph showing the comparison of the contact angle between the PVDF raw film (M0) and the beta-FeOOH/PDAus/PVDF composite film (M2) prepared in example 3. As can be seen from the figure, the contact angle of the PVDF film is 100 degrees, which belongs to the category of super-hydrophobicity, while the surface contact angle of the beta-FeOOH/PDAus/PVDF composite film is 0 degrees, which is completed within 0s, which indicates that the hydrophilicity of the modified composite film is greatly improved.
FIG. 3 is a graph comparing the removal of methyl blue dye by PVDF raw film (M0) and beta-FeOOH/PDAus/PVDF composite film (M2) prepared in example 3. As can be seen from the figure, the dye degradation rate of the beta-FeOOH/PDAus/PVDF composite membrane reaches 64.2 percent after 24 hours of treatment, and the specific unique dye degradation performance of the beta-FeOOH/PDAus/PVDF composite membrane is proved.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (7)
1. A process for preparing β -FeOOH/PDAus/PVDF composite membrane with super-hydrophilicity includes such steps as generating Michael addition reaction between dopamine and PVDF by the unique biologic glue characteristic of dopamine to obtain PDAus/PVDF composite membrane, chelating the hydroxyl group of catechol on dopamine molecule with ferric ion, and using FeCl3Preparing the β -FeOOH/PDAus/PVDF composite membrane with super-hydrophilicity from the precursor solution.
2. The method for preparing the super-hydrophilic beta-FeOOH/PDAus/PVDF composite membrane according to claim 1, which is characterized in that: the method specifically comprises the following steps:
(1) preparing a dopamine modified PVDF composite membrane: adding a Tris-phosphate neutral buffer solution into a mixed solution of water and absolute ethyl alcohol to prepare a solution with a Tris concentration of 10 mmol/L, and then adding dopamine powder into the solution and stirring for 1 day to obtain a dopamine solution; adding the PVDF raw membrane into a dopamine solution, continuously stirring for 3 days, cleaning the membrane and airing the membrane for 2 days to obtain a modified PDAus/PVDF composite membrane;
(2) preparing β -FeOOH/PDAus/PVDF composite membrane with super-hydrophilicity by mixing FeCl3·6H2Dissolving O in water to prepare a solution of 5-50 mg/mL, adding 0.01mol/L of acid solution according to the volume ratio of 2: 1 to prepare a mineralized solution, placing the modified PDAus/PVDF composite membrane obtained in the step (1) into the mineralized solution, stirring and reacting for 6-24 h under the condition of a constant-temperature water bath at 60 ℃, cleaning the membrane after stirring is completed, and airing the membrane for 2 days to obtain the β -FeOOH/PDAus/PVDF composite membrane.
3. The method for preparing the super-hydrophilic beta-FeOOH/PDAus/PVDF composite membrane according to claim 2, wherein: the volume ratio of water to absolute ethyl alcohol in the mixed solution in the step (1) is 1-5: 1.
4. the method for preparing the super-hydrophilic beta-FeOOH/PDAus/PVDF composite membrane according to claim 2, wherein: the concentration of the dopamine solution prepared in the step (1) is 0.5-2 mg/mL.
5. The method for preparing β -FeOOH/PDAus/PVDF composite membrane with super-hydrophilicity according to claim 2, wherein the acidic solution in step (2) is HCl solution, H2SO4Solution or HNO3And (3) solution.
6. A super-hydrophilic beta-FeOOH/PDAus/PVDF composite membrane prepared by the method of any one of claims 1-5.
7. Use of the super-hydrophilic beta-FeOOH/PDAus/PVDF composite membrane according to claim 6 in water filtration purification treatment or industrial wastewater dye removal.
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| CN117643806A (en) * | 2024-01-30 | 2024-03-05 | 中国科学院合肥物质科学研究院 | Double-channel composite membrane and preparation method and application thereof |
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Application publication date: 20200925 |