CN111203107A - Polyphenol-iron nano film and preparation method and application thereof - Google Patents
Polyphenol-iron nano film and preparation method and application thereof Download PDFInfo
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Abstract
本发明涉及一种多酚‑铁纳米薄膜及其制备方法和应用。该方法包括：将多孔支撑膜浸入到多酚水溶液中，浸泡，加入亚铁盐水溶液，震荡共沉积，然后继续反应，清洗。该方法所使用的原料安全绿色、容易获得且价格低廉，反应过程在水相溶液中进行，避免使用了有机试剂，符合绿色化学需求；制备得到的薄膜不仅能筛分水溶液中的一价和多价离子，还能实现有机溶剂中染料分子的高效截留。
The present invention relates to a polyphenol-iron nano film and a preparation method and application thereof. The method comprises: immersing the porous support film in the polyphenol aqueous solution, soaking, adding the ferrous salt aqueous solution, oscillating and co-depositing, then continuing the reaction and cleaning. The raw materials used in the method are safe, green, easy to obtain and inexpensive. The reaction process is carried out in an aqueous solution, avoiding the use of organic reagents and meeting the requirements of green chemistry; the prepared film can not only screen the monovalent and polyvalent in the aqueous solution Valence ions can also achieve efficient retention of dye molecules in organic solvents.
Description
Technical Field
The invention belongs to the field of nanofiltration membranes and preparation and application thereof, and particularly relates to a polyphenol-iron nano-film and a preparation method and application thereof.
Background
Polyphenols are an important class of natural molecules, widely found in various plants. The metal-polyphenol coating is a self-assembled supermolecular material, and a crosslinked network structure is formed by polyphenol units and metal ions through coordination bonds. Due to the wide selection range of polyphenol and metal ions and the universal adhesion of polyphenol, the coating can be adhered to the surface of almost any material, so that the metal-polyphenol coating is a research hotspot in the field of material science rapidly since the emergence of the metal-polyphenol coating.
At present, the membrane separation technology is widely applied and rapidly developed by virtue of the advantages of high efficiency, low energy consumption and no secondary pollution, and people successfully apply the membrane separation technology to a plurality of fields in production and life, such as water purification, seawater desalination, sewage treatment, material concentration and the like. The nanofiltration draws great attention and research interest of various research institutions and film material production enterprises by virtue of the separation performance of the nanofiltration membrane superior to that of an ultrafiltration membrane and the operation energy consumption far lower than that of a reverse osmosis membrane.
Interfacial polymerization is a method commonly used for preparing a thin-layer composite nanofiltration membrane at present, and the preparation of the thin-layer composite nanofiltration membrane is usually realized by quickly forming a selective separation skin layer which determines the separation performance through polycondensation reaction of polyamine and polybasic acyl chloride at the interface of a water phase and an organic phase. Although the method is the most mature and widely applied composite nanofiltration membrane preparation method at present, a plurality of problems which need to be solved exist, such as too fast monomer condensation reaction speed which is difficult to regulate and control, environmental pollution caused by using a large amount of organic reagents and toxic acyl chloride monomers, and the like.
Chinese patent CN104984666A discloses a metal polyphenol film and a preparation method and application thereof. The method prepares the metal-polyphenol film by mixing polyphenol and various metal salt solutions and depositing on a porous base film, and applies the metal-polyphenol film to dye retention. The metal-polyphenol film in the invention can play a role in separation, but can only intercept dye molecules to a certain degree, can not realize the separation of salt ions with different valence states, and has low permeation flux. In addition, the coordination speed of polyphenol and metal ions is very high, so that the precise regulation and control of the thickness and the separation performance of the film are difficult to realize.
Disclosure of Invention
The invention aims to solve the technical problem of providing a polyphenol-iron nano film, a preparation method and application thereof, so as to overcome the defect that the thickness and the separation performance of a nanofiltration film are difficult to control in the prior art.
The invention provides a polyphenol-iron nano film, which is prepared by immersing a porous support film into a polyphenol aqueous solution, soaking, adding a ferrous salt aqueous solution, oscillating for codeposition reaction, and then continuing the reaction.
The porous support membrane is a polymer ultrafiltration membrane, preferably one of a polysulfone ultrafiltration membrane, a polyether sulfone ultrafiltration membrane, a polyacrylonitrile ultrafiltration membrane, a hydrolyzed polyacrylonitrile ultrafiltration membrane and a cellulose acetate ultrafiltration membrane, and further preferably a polyacrylonitrile ultrafiltration membrane.
The polyphenol is one or more of tannic acid, dopamine, tea polyphenol, grape polyphenol and apple polyphenol, preferably tannic acid.
The ferrous salt is one or more of ferrous chloride, ferrous chloride tetrahydrate, ferrous sulfate, ferrous bromide, ferrous fluoride, ferrous sulfide and ferrous perchlorate, and preferably ferrous chloride tetrahydrate.
The invention also provides a preparation method of the polyphenol-iron nano film, which comprises the following steps:
and (2) immersing the porous support film into a polyphenol aqueous solution, soaking, adding a ferrous salt aqueous solution, oscillating for codeposition reaction, continuing to react, and cleaning to obtain the polyphenol-iron nano film, wherein the concentration of the polyphenol aqueous solution is 0.8-80 mg/mL, the concentration of the ferrous salt aqueous solution is 4.9-98 mg/mL, and the molar ratio of polyphenol to ferrous salt is 1: 1-1: 100.
The porous support membrane is cleaned by deionized water.
The aqueous solution of polyphenol is obtained by dissolving polyphenol in ultrapure water.
The ferrous salt water solution is obtained by dissolving ferrous salt in ultrapure water.
The concentration of the polyphenol water solution is 8 mg/mL.
The concentration of the ferrous salt water solution is 9.8 mg/mL.
The soaking time is 0-60 minutes, is not 0, and is preferably 5 minutes.
The oscillating codeposition reaction temperature is 10-50 ℃ (preferably 25 ℃), and the oscillating codeposition reaction time is 60-360 min (preferably 120 min).
The continuous reaction temperature is 60-80 ℃, and the continuous reaction time is 0-60 min.
The cleaning is carried out by adopting ultrapure water.
The invention also provides an application of the polyphenol-iron nano-film, such as nanofiltration separation.
The concentration of the polyphenol aqueous solution is 0.8-80 mg/mL, and a complete separation cortex cannot be formed when the concentration of the polyphenol aqueous solution is low, so that the separation performance of the nano film is influenced; when the concentration is too high, the separation efficiency of the nano-film is affected by the excessively thick separation skin layer.
According to the invention, the porous support membrane is soaked in the polyphenol water solution, the soaking time can influence the distribution of polyphenol on the surface of the porous support membrane, and the soaking time is too short, so that the polyphenol cannot be uniformly distributed on the surface of the porous support membrane; the soaking time is too long, and the polyphenol is oxidized by oxygen in the air, so that the separation performance of the nano film is influenced.
The codeposition involved in the invention is a reaction process of polyphenol aqueous solution and ferrous salt aqueous solution; the thickness of the separation skin layer can be influenced by the time of the codeposition process, and the complete separation skin layer cannot be formed due to too short reaction time, so that the separation performance of the nano film is reduced; too long a codeposition time can result in the formation of a too thick separation skin layer, thereby reducing the separation efficiency of the nanofilm.
The polyphenol-iron nano film separation skin layer contains polyphenol, and the polyphenol surface has a large number of hydroxyl groups, so that the hydrophilicity of the nano film can be improved, and the water flux of the nano film can be kept at a good level; meanwhile, polyphenol generally has universal adhesion, so that the coating is stably combined with various supporting base film interfaces.
The invention can effectively prolong the deposition time window of the metal-polyphenol film, improve the controllability of coating preparation and accurately control the thickness and compact structure of the separation film.
Compared with the Chinese patent CN104984666A, the invention has the advantages that the controllability of the coating preparation is improved, the thickness and the compact structure of the separation film can be accurately controlled, monovalent and multivalent ions in the aqueous solution can be screened, and the efficient interception of dye molecules in the organic solvent can be realized.
Advantageous effects
(1) The raw materials used in the invention are safe, green, easily available and low in price, the reaction process is carried out in aqueous phase solution, organic reagents are avoided, and the green chemical requirements are met.
(2) The invention controls the forming speed and the structure of the separation cortex by controlling the oxidation process of ferrous ions in the aqueous solution so as to obtain the compact and defect-free polyphenol-iron nano film. The thickness and the pore diameter of the polyphenol-iron nano film separation cortex can be effectively regulated and controlled by regulating reaction conditions such as deposition time, solution concentration and the like, so that the separation performance and the separation efficiency of the polyphenol-iron nano film are regulated and controlled.
(3) The polyphenol-iron nano film obtained by the invention not only can screen univalent and multivalent ions in an aqueous solution, but also can realize efficient interception of dye molecules in an organic solvent.
Drawings
FIG. 1 is a scanning electron micrograph of a polyphenol-iron nano-film prepared in example 1;
FIG. 2 is a scanning electron micrograph of a cross-section of the polyphenol-iron nano-film prepared in example 1.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The reagents used in the examples of the invention were as follows: tannic acid (Tannic acid), Sigma-Aldrich (USA); ferrous chloride tetrahydrate (Iron (ii) chloride tetrahydrate, national pharmaceutical group chemicals ltd; methyl blue (Methyl blue), AR, shanghai avadin reagent ltd; methanol (Methanol), analytically pure, chemical reagents of national drug group, ltd.
The porous support membrane used in each embodiment of the invention is an FE-MBR-1.0 polyacrylonitrile ultrafiltration membrane produced by Shanghai blue-scenery membrane technical engineering Co.
The polyphenol-iron nano film prepared by the invention is used for desalination, and the desalination rate and the water flux are two important parameters for evaluating the nano-filtration performance of the nano film.
The parameters are obtained by testing and calculating the nanofiltration performance by adopting a cross-flow filtration mode. The filtration performance test was carried out in a thermostatic water bath at 25 ℃ under a pressure of 0.4MPa using an inorganic salt solution having a concentration of 1000mg/L as a raw material solution. And respectively recording the time required by the nano-film to permeate 5mL, 7mL and 10mL of penetrating fluid, and calculating by a formula to obtain the salt rejection and the water flux.
Wherein the salt rejection is defined as:
wherein, CfRepresents the concentration of salt ions in the water before treatment; cpIndicates the concentration of salt ions in the solution after the treatment.
The water flux is defined as: volume of water per unit membrane area per unit time, unit of water per unit membrane area, at a given operating pressureIs L.m-2·h-1The formula is as follows:
wherein V represents the volume of the permeated solution and has a unit of L; a represents the effective membrane area in m2(ii) a t represents time in units of h.
The polyphenol-iron nano film prepared by the invention can also be used for dye separation in organic solvents.
The dye in the test example was methyl blue. The specific test method comprises the following steps: a methanol solution of methyl blue was prepared as a starting solution at a concentration of 100 ppm. Adding the raw material liquid into a rotary membrane pool, pressurizing the inside of the apparatus by nitrogen, controlling the pressure to be 1MPa, and collecting the filtrate. Respectively taking 3mL of raw material liquid and filtrate, detecting absorbance by using an ultraviolet-visible spectrophotometer, comparing with a standard curve to obtain the dye concentration in the raw material liquid and the filtrate, calculating the retention rate according to the formula (1), and calculating the solvent flux according to the formula (2).
Example 1
(1) Weighing a proper amount of tannic acid, and dissolving in 30ml of ultrapure water to obtain a polyphenol water solution with the polyphenol concentration of 8 mg/ml; an appropriate amount of ferrous chloride tetrahydrate is weighed and dissolved in 30ml of ultrapure water to obtain a ferrous salt solution with the ferrous chloride concentration of 9.8 mg/ml.
(2) And (2) immersing the polyacrylonitrile ultrafiltration membrane into the polyphenol water solution obtained in the step (1) for 5 minutes.
(3) And (3) transferring the ferrous salt aqueous solution obtained in the step (1) into the solution obtained in the step (2), quickly transferring a reaction vessel containing the two solutions into a water bath constant-temperature oscillator, and oscillating in a water bath at 25 ℃ for codeposition for 120 minutes.
(4) And (3) transferring the reaction vessel containing the solution from the water bath constant temperature oscillator into an oven, reacting for 10 minutes at 70 ℃, finally taking out the membrane, and washing with ultrapure water to obtain the polyphenol-iron nano film.
FIG. 1 shows that: successfully preparing the polyphenol-iron nano film.
Examples 2 to 6
The codeposition time was adjusted (as shown in table 1), and the polyphenol-iron nano-film was obtained under the same conditions as in example 1.
Test example 1
The polyphenol-iron nano-films prepared in examples 1 to 6 were tested. The results are shown in Table 1.
TABLE 1 Water flux and rejection rates for Polyphenol-iron nanofilms prepared in examples 1-6
As can be seen from the data in table 1, the water flux of the polyphenol-iron nano-film of the present invention decreases with the increase of deposition time, which is caused by the increase of the thickness of the separation skin layer; the deposition time is increased and the salt rejection rate is gradually increased, on one hand, due to the complete formation and densification of the separation skin layer, and on the other hand, due to the fact that the separation layer is not densified and the thickness is increased, the rejection rate is improved.
Examples 7 to 11
The concentration of tannic acid in the solution was adjusted (as shown in table 2), and the same conditions as in example 1 were applied to obtain a polyphenol-iron nano-film.
Test example 2
The polyphenol-iron nano-films prepared in examples 7 to 11 were tested. The results are shown in Table 2.
TABLE 2 Water flux and rejection rates for Polyphenol-iron nanofilms prepared in examples 7-11
As can be seen from the data in Table 2, as the concentration of tannic acid increases, the pH value of the reaction solution decreases due to the acidic substance of tannic acid, which is not favorable for the formation of polyphenol-iron nano-film, so the retention rate decreases and the water flux increases.
Examples 12 to 16
The concentration of ferrous chloride in the solution was adjusted (as shown in table 3), and the polyphenol-iron nano-film was obtained under the same conditions as in example 1.
Test example 3
The polyphenol-iron nano films prepared in examples 12 to 16 were tested. The results are shown in Table 3.
TABLE 3 Water flux and rejection rates for Polyphenol-iron nanofilms prepared in examples 12-16
As can be seen from the data in table 3, as the concentration of ferrous chloride increases, the formed polyphenol-iron nano-film becomes more compact, so that the water flux of the polyphenol-iron nano-film decreases, and the retention rate increases continuously until the film becomes stable.
Test example 4
The polyphenol-iron nano-film prepared in example 1 was tested. The results are shown in Table 4.
Table 4 rejection rates for different salts of polyphenol-iron nanofilms prepared in example 1
| Testing | Sodium sulfate rejection (%) | Magnesium sulfate rejection (%) | Magnesium chloride rejection (%) | Sodium chloride rejection (%) |
| Example 1 | 91.7 | 70.9 | 38.1 | 22.4 |
As can be seen from the data in table 4, the polyphenol-iron nano-film of the present invention can screen monovalent and multivalent ions in aqueous solution.
Test example 5
The polyphenol-iron nano-films prepared in examples 1 to 6 were tested. The results are shown in Table 5.
TABLE 5 solvent flux and dye retention of the polyphenol-iron nanofilms prepared in examples 1-6
As can be seen from the data in table 5, as the deposition time increases, the solvent flux of the polyphenol-iron nano-film decreases, the dye retention rate increases continuously until it stabilizes, and no dye adsorption occurs.
The above-mentioned embodiments are intended to illustrate the technical solutions and advantages of the present invention, and it should be understood that the above-mentioned embodiments are only specific embodiments of the present invention, and are not intended to limit the present invention, and any modifications, additions, equivalents, etc. made within the scope of the principles of the present invention should be included in the scope of the present invention.
Claims (9)
1. A polyphenol-iron nano film is characterized in that a porous support film is immersed into a polyphenol aqueous solution, soaked, added with a ferrous salt aqueous solution, vibrated for codeposition reaction, and then continuously reacted to obtain the polyphenol-iron nano film.
2. The membrane of claim 1, wherein the porous support membrane is one of a polysulfone ultrafiltration membrane, a polyethersulfone ultrafiltration membrane, a polyacrylonitrile ultrafiltration membrane, a hydrolyzed polyacrylonitrile ultrafiltration membrane, and a cellulose acetate ultrafiltration membrane.
3. The film of claim 1, wherein the polyphenol is one or more of tannic acid, dopamine, tea polyphenol, grape polyphenol and apple polyphenol.
4. The film according to claim 1, wherein the ferrous salt is one or more of ferrous chloride, ferrous chloride tetrahydrate, ferrous sulfate, ferrous bromide, ferrous fluoride, ferrous sulfide, and ferrous perchlorate.
5. A preparation method of a polyphenol-iron nano film comprises the following steps:
and (2) immersing the porous support film into a polyphenol aqueous solution, soaking, adding a ferrous salt aqueous solution, oscillating for codeposition reaction, continuing to react, and cleaning to obtain the polyphenol-iron nano film, wherein the concentration of the polyphenol aqueous solution is 0.8-80 mg/mL, the concentration of the ferrous salt aqueous solution is 4.9-98 mg/mL, and the molar ratio of polyphenol to ferrous salt is 1: 1-1: 100.
6. The method according to claim 5, wherein the soaking time is 0 to 60 minutes and is not 0.
7. The method according to claim 5, wherein the oscillating co-deposition reaction temperature is 10-50 ℃ and the oscillating co-deposition reaction time is 60-360 min.
8. The method according to claim 5, wherein the continuous reaction temperature is 60 to 80 ℃ and the continuous reaction time is 0 to 60 min.
9. Use of a film according to claim 1.
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| CN119656893A (en) * | 2024-12-23 | 2025-03-21 | 江南大学 | Composite nanofiltration membrane with surface enhanced Raman detection function and application thereof in drug separation detection |
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