CN114832640B - Method for relieving membrane protein pollution by FeOCl modified ceramic membrane in-situ coupling peroxyacetic acid catalytic filtration system - Google Patents
Method for relieving membrane protein pollution by FeOCl modified ceramic membrane in-situ coupling peroxyacetic acid catalytic filtration system Download PDFInfo
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Abstract
A method for relieving membrane protein pollution by a FeOCl modified ceramic membrane in-situ coupling peroxyacetic acid catalytic filtration system belongs to the technical field of membrane pollution treatment. According to the invention, feOCl loaded on a flat ceramic membrane is used as a catalyst, peroxyacetic acid is used as an oxidant, a FeOCl modified ceramic membrane in-situ coupling peroxyacetic acid catalytic filtration system is constructed, active oxygen substances are generated in situ in the membrane during filtration, bovine serum albumin is used as a protein model pollutant, and the effect of rapidly and efficiently relieving membrane protein pollution is realized. Compared with the traditional ceramic membrane filtration mode without oxidant, the FeOCl modified ceramic membrane activated peroxyacetic acid has the advantages that the membrane flux reduction degree is reduced by one time in the catalytic filtration mode, bovine serum albumin on the membrane surface and in the membrane hole is obviously degraded, and the application prospect of membrane pollution control is greatly shown.
Description
Technical Field
The invention belongs to the technical field of membrane pollution treatment. In particular to a method for relieving membrane protein pollution by a FeOCl modified ceramic membrane in-situ coupling peroxyacetic acid catalytic filtration system.
Background
The membrane separation water treatment technology has the advantages of no phase change, small occupied area, high treatment efficiency and the like, and is one of the leading technologies for water purification and recycling. Wherein, the inorganic ceramic membrane has the advantages of stable chemical and thermodynamic properties, high mechanical strength, corrosion resistance and the like, and is widely applied to the field of water treatment. However, ceramic membrane filtration suffers from serious problems of colloid and protein contamination, decreasing the ceramic membrane filtration efficiency and causing an increase in membrane filtration operation maintenance costs. Therefore, research on methods for effectively alleviating ceramic membrane pollution is important for further development of ceramic membrane water filtration treatment technology.
Aiming at the problem, the ceramic membrane is endowed with additional catalytic performance (such as modifying a carbon-based or metal-based high-activity catalyst in the ceramic membrane) by a chemical modification method, and the constructed catalytic ceramic membrane filtration system can be used for in-situ coupling catalytic oxidation reaction in the membrane, so that the dual effects of synchronously degrading pollutants and improving the pollution resistance of the membrane during filtration are realized. The catalytic ceramic membrane filtration systems reported so far mostly employ typical oxidants (e.g., hydrogen peroxide, chlorine, persulfates). It is worth noting that no ideal catalytic ceramic membrane filtration system is coupled with peroxyacetic acid oxidant at present, so that the ceramic membrane filtration efficiency is improved, and the ceramic membrane pollution is effectively relieved.
Disclosure of Invention
The invention aims to solve the problems that the existing ceramic membrane protein pollution cannot be effectively solved, the filtering efficiency is low and the operation and maintenance costs are high, and provides a method for relieving the membrane protein pollution by a FeOCl modified ceramic membrane in-situ coupling peroxyacetic acid catalytic filtering system.
The invention relates to a method for relieving membrane protein pollution by a FeOCl modified ceramic membrane in-situ coupling peroxyacetic acid catalytic filtration system, which comprises the following steps:
soaking a FeOCl modified ceramic membrane in deionized water for 6-12h, loading the soaked ceramic membrane into a membrane module, and then filtering for 15min by using the FeOCl modified ceramic membrane by taking Milli-Q water as a feed liquid to obtain initial pure water flux; then taking a protein solution added with an oxidant as a feed liquid, and filtering for 30-120min by utilizing a FeOCl modified ceramic membrane;
the preparation method of the FeOCl modified ceramic membrane comprises the following steps: dissolving ferric chloride hexahydrate solid in absolute ethyl alcohol, and uniformly stirring to obtain a mixed solution; placing the clean substrate ceramic membrane in a dry vessel, putting the substrate ceramic membrane into the mixed solution, performing ultrasonic treatment at 40kHz for 30-60min, and performing continuous shaking culture at 80rpm for 30-60min; subsequently, the ceramic membrane is calcined to 220 ℃ by programming the temperature, and the temperature rising rate is controlled to be 1-3 ℃ for min -1 The method comprises the steps of carrying out a first treatment on the surface of the And naturally cooling to room temperature, cleaning the membrane by deionized water, and then placing the membrane in a 50 ℃ drying box for 12-18h to obtain the FeOCl modified ceramic membrane.
Further, the filtration using FeOCl modified ceramic membranes is performed in a dead-end filtration mode.
Further, the oxidant is peracetic acid.
Further, the concentration of the peracetic acid is 1-5mmol L -1 。
Further, the protein solution is a bovine serum albumin solution.
Further, the protein solution is bovine serum albumin solution with the concentration of 20-200mg L -1 。
Further, the FeOCl modified ceramic membrane filtration is driven by constant pressure, the feed liquid enters the membrane assembly, the weight change of the filtrate after membrane filtration is measured in real time, and the flux is recorded every 5 seconds.
Further, the constant pressure is hydraulic driving pressure of 1bar provided by a nitrogen bottle, and the purity of the nitrogen is more than or equal to 99.999%.
Further, soaking the FeOCl modified ceramic membrane in deionized water for 8-12h, loading the soaked ceramic membrane into a membrane module, and then filtering for 15min by using the FeOCl modified ceramic membrane by taking Milli-Q water as a feed liquid to obtain initial pure water flux; and then taking the protein solution added with the oxidant as a feed liquid, and filtering for 60-100min by utilizing a FeOCl modified ceramic membrane.
Further, the ultrasonic treatment is carried out for 30-50min at 40kHz, and the continuous shaking culture is carried out for 30-50min at 80 rpm; subsequently, the ceramic membrane is calcined to 220 ℃ by programming the temperature, and the temperature rising rate is controlled to be 2-3 ℃ for min -1 Naturally cooling to room temperature, cleaning the membrane with deionized water, and then placing the membrane in a drying box at 50 ℃ for 12-14h to obtain the FeOCl modified ceramic membrane.
The invention has the following beneficial effects:
the FeOCl modified ceramic membrane in-situ coupling peroxyacetic acid catalytic filtration system provided by the invention can generate catalytic oxidation reaction inside the membrane pores during membrane filtration to generate active oxygen substances (hydroxyl free radicals and singlet oxygen) in situ, so that bovine serum albumin pollution on the membrane is efficiently degraded, and the anti-pollution performance of the membrane is improved. The system has great application potential in the process of alleviating membrane protein pollution.
Compared with the existing chemical oxidant catalytic membrane filtration technology, the peroxyacetic acid oxidant adopted by the invention has the characteristics of high oxidation efficiency, low tendency of forming disinfection byproducts and easier activation, and the peroxyacetic acid oxidation and the catalytic membrane filtration are coupled in situ to reduce membrane pollution, so that the peroxyacetic acid oxidant has wide application prospect. The in-situ catalytic oxidation filtration system fully utilizes the hydraulic condition of forced convection during membrane filtration and the micro-nano space limiting effect in the membrane pores, so that the oxidant fully contacts with the FeOCl nano-sheet catalyst in the membrane pores to generate active oxygen species with better oxidation capability, thereby obviously improving the anti-pollution efficiency of the membrane.
Drawings
FIG. 1 is a schematic illustration of the implementation flow in embodiment 1 of the present invention;
FIG. 2 is a physical image (FIG. a) of a FeOCl-modified ceramic film and a physical image (FIG. b) of a base ceramic film obtained in example 2 of the present invention;
FIG. 3 is a graph showing the variation of membrane normalized water flux in different filtration modes in example 3 of the present invention; wherein A is an operation mode I, namely a membrane filtration mode of adopting FeOCl modified ceramic membranes and adding peracetic acid oxidant during filtration; b is an operation mode II, namely a membrane filtration mode of adding a peroxyacetic acid oxidant during filtration by adopting a substrate ceramic membrane; c is an operation mode III, namely a membrane filtration mode in which FeOCl is adopted to modify a ceramic membrane and an oxidant is not added during filtration; d is an operation mode IV, namely a membrane filtration mode which adopts a substrate ceramic membrane and does not add an oxidant during filtration;
FIG. 4 is a scanning electron microscope photograph of the cross section and the surface of the FeOCl modified ceramic membrane contaminated in the operation mode I and the operation mode III (FIGS. 4a-4 b) and a scanning electron microscope photograph of the cross section and the surface of the FeOCl modified ceramic membrane cleaned before filtration (FIG. 4 c) in the embodiment 3 of the present invention;
FIG. 5 is a graph showing the degradation effect of bovine serum albumin in mode I and mode II of operation in example 3 of the present invention; wherein A is an operation mode II, and B is an operation mode II;
FIG. 6 is a graph showing pore size of FeOCl-modified ceramic membranes obtained in example 2 of the present invention; in the drawing the view of the figure,
is a commercial ceramic membrane (molecular weight cut-off 3 kDa),>
a FeOCl modified ceramic membrane; />
FIG. 7 is a graph showing the effect of different oxidizing agent coupling FeOCl ceramic membrane filter systems on the removal of bovine serum albumin; in the drawing the view of the figure,
is peroxyacetic acid, & lt- & gt>
Is peroxymonosulfate, & lt & gt>
Is hydrogen peroxide.
Detailed Description
For the purposes of clarity, technical solutions and advantages of embodiments of the present invention, the spirit of the present disclosure will be described in detail below, and any person skilled in the art, after having appreciated the embodiments of the present disclosure, may make changes and modifications to the techniques taught by the present disclosure without departing from the spirit and scope of the present disclosure.
The exemplary embodiments of the present invention and the descriptions thereof are intended to illustrate the present invention, but not to limit the present invention.
Example 1
The FeOCl modified ceramic membrane in-situ coupling peroxyacetic acid catalytic filtration system of the embodiment is constructed in the following manner:
membrane filtration was performed using FeOCl modified ceramic membranes as described in example 2. And soaking the prepared FeOCl modified ceramic membrane in deionized water for 12 hours, and filling the soaked ceramic membrane into a membrane assembly. First, milli-Q water was used as a feed liquid, and the initial pure water flux was obtained by filtration with FeOCl-modified ceramic membranes for 15 minutes. Secondly, taking a protein solution added with a peroxyacetic acid oxidant as a feed liquid, filtering for 30min by using a FeOCl modified ceramic membrane, and periodically measuring the water flux.
The specific filtering operation steps are as follows: the catalytic membrane filtration is carried out in a dead-end filtration mode, a nitrogen bottle is adopted to provide a transmembrane pressure difference of 1bar, a pressure is utilized to drive a feed liquid to enter a membrane assembly from an ultrafiltration cup through a hose, a filtrate after the membrane filtration is collected in a beaker on an electronic balance, the weight change of the filtrate is measured in real time, and a flux monitor is adopted to record flux every 5 seconds.
Example 2
The preparation method of the FeOCl modified ceramic membrane in-situ coupling peroxyacetic acid catalytic filtration system described in example 1 is as follows:
and preparing the FeOCl modified ceramic membrane by adopting a solution infiltration and heating roasting mode. Wherein, a flat circular ceramic membrane is used as a catalytic membrane substrate, the main components of the catalytic membrane substrate are titanium dioxide and zirconium dioxide, the molecular weight cut-off is 300kDa, the diameter is 47mm, and the thickness is 2.5mm. The purity of the ferric chloride hexahydrate needed by the preparation is more than or equal to 99 percent.
An amount of ferric chloride hexahydrate powder was weighed with an electronic balance and dissolved in absolute ethanol, and magnetically stirred at a rotation speed of 300rpm to obtain a uniform solution. The ceramic membrane substrate was placed in a dry glass petri dish and immersed in the above solution, followed by ultrasonic treatment at 40kHz for 30min and continuous shaking treatment at 80rpm for 30min, so that the ceramic membrane substrate was completely immersed in the solution. Subsequently, the ceramic film was calcined to 220℃with a muffle furnace temperature programming, the rate of heating being controlled at 3℃for min -1 Naturally cooling to room temperature. The membrane was rinsed with deionized water and then placed in a 50 ℃ oven for 12 hours.
Fig. 2 is a physical diagram of the FeOCl modified ceramic film (fig. a) and a physical diagram of the base ceramic film (fig. b) prepared. The FeOCl modified ceramic membrane has uniform reddish brown color.
Example 3
The FeOCl modified ceramic membrane in-situ coupled peroxyacetic acid catalytic filtration system described in example 1 has the following effect of alleviating membrane protein pollution:
the model pollutant adopted is bovine serum albumin, and the oxidant adopted is peracetic acid. Wherein, the operation mode I is a catalytic filtration mode of adopting FeOCl modified ceramic membrane and adding peracetic acid oxidant during filtration; the operation mode II is a membrane filtration mode which adopts a substrate ceramic membrane and is added with a peroxyacetic acid oxidant during filtration; the operation mode III is a membrane filtration mode in which FeOCl is adopted to modify a ceramic membrane and an oxidant is not added during filtration; the operation mode IV is a membrane filtration mode which adopts a substrate ceramic membrane and does not add an oxidant during filtration.
And (3) characterizing microscopic morphology of bovine serum albumin on the surface and the section of the ceramic membrane by utilizing a Scanning Electron Microscope (SEM), so as to analyze the pollution resistance of the FeOCl modified ceramic membrane.
And (3) characterizing degradation conditions of the bovine serum albumin by using a fluorescence spectrometer, and performing semi-quantitative detection on degradation effects of the bovine serum albumin by using fluorescence intensity. Measuring fluorescence intensity of bovine serum albumin solution under the conditions of excitation wavelength and emission wavelength of 280nm and 340nm respectively, to obtain fluorescence intensity A of bovine serum albumin before filtering 0 Calculating A/A under different filtering time 0 Thus reflecting the degradation of bovine serum albumin.
Figure 3 shows the normalized water flux change for the membranes of this example. After bovine serum albumin is filtered, the normalized water flux of the FeOCl modified ceramic membrane activated peroxyacetic acid filtration mode reaches 0.46 (operation mode I), which is nearly doubled compared with the normalized water flux of the single ceramic membrane filtration mode (operation modes III and IV) without adding an oxidant. In addition, in FeOCl modified ceramic membrane activated peroxyacetic acid catalytic filtration, membrane pollution in the initial stage of filtration is effectively relieved, namely membrane pore blocking is obviously relieved.
As can be seen from the SEM image of the ceramic membrane of this example of FIG. 4, when the FeOCl modified ceramic membrane was used, a clear fouling area was observed on the surface and cross section of the membrane after the filtration mode (operation mode III) in which peracetic acid was not added during filtration, and the fouling area was large and penetrated into the membrane pores. And after the FeOCl modified ceramic membrane is adopted to activate the peracetic acid filtration mode (operation mode I), bovine serum albumin particles deposited on the surface of the membrane or permeated into the membrane pores are obviously degraded. The dirt is mainly distributed near the upper surface of the membrane, and only dispersed bovine serum albumin particles are arranged on the surface of the membrane, which indicates that the FeOCl modified ceramic membrane activated peroxyacetic acid filtration mode has effective membrane pollution resistance.
FIG. 5 illustrates that the degradation rate of bovine serum albumin in the filtration mode (operation mode I) of the activated peroxyacetic acid by using the FeOCl modified ceramic membrane of this example is nearly doubled compared with the degradation rate of bovine serum albumin in the filtration mode (operation mode II) of the activated peroxyacetic acid by using the base ceramic membrane, which indicates that the FeOCl modified ceramic membrane in situ coupled peroxyacetic acid catalytic filtration system can effectively degrade protein contaminants on the membrane.
Through the pore size map of the membrane of this example, as shown in FIG. 6, the pore size range of the prepared FeOCl modified ceramic membrane was similar to that of a commercial fine ultrafiltration ceramic membrane having a molecular weight cut-off of 3 kDa. Therefore, the prepared FeOCl modified ceramic membrane is a fine ultrafiltration ceramic membrane.
The ratio of FeOCl/peracetic acid in the catalytic membrane filtration system of the embodiment is verified to examine the anti-pollution effect of the catalytic membrane filtration system under different ratios. For FeOCl modified ceramic membrane in-situ coupling peracetic acid catalytic filtration system, when the molar ratio of FeOCl/peracetic acid is 93-1860 (i.e. 0.1g mL) -1 FeOCl/10mM peracetic acid to 0.5g mL -1 When FeOCl/2.5mM peracetic acid, the catalytic membrane filtration system has good anti-protein pollution effect, and the anti-pollution effect of the catalytic membrane filtration system outside the interval is obviously reduced.
The peracetic acid coupled FeOCl ceramic membrane filtration system showed the best removal of bovine serum albumin compared to the two classes of typical oxidants, hydrogen peroxide and persulfate, which have similar structures to peracetic acid, as shown in fig. 7. FIG. 7 shows comparative data of removal of bovine serum albumin by FeOCl ceramic membrane in-situ coupled hydrogen peroxide system, feOCl ceramic membrane in-situ coupled peracetic acid system, feOCl ceramic membrane in-situ coupled persulfate system (equal concentrations of the three oxidants, all 2.5mM. BSA concentrations all 20 mg.L) -1 )。
The foregoing is a preferred embodiment of the present invention. However, the embodiments of the present invention are not limited to the above embodiments. Based on the description of the present invention, any modification, combination and simplification that do not deviate from the technical principle of the present invention should be equivalent substitution, and all modifications, combinations and simplifications are covered in the protection scope of the present invention.
Claims (9)
1. A method for relieving membrane protein pollution by a FeOCl modified ceramic membrane in-situ coupling peroxyacetic acid catalytic filtration system is characterized by comprising the following steps:
soaking a FeOCl modified ceramic membrane in deionized water for 6-12h, loading the soaked ceramic membrane into a membrane module, and then filtering the membrane module by using Milli-Q water as a feed liquid and using the FeOCl modified ceramic membrane for 15min to obtain initial pure water flux; then taking a protein solution added with an oxidant as a feed liquid, and filtering for 30-120min by utilizing a FeOCl modified ceramic membrane;
the preparation method of the FeOCl modified ceramic membrane comprises the following steps: dissolving ferric chloride hexahydrate solid in absolute ethyl alcohol, and uniformly stirring to obtain a mixed solution; placing the clean substrate ceramic membrane in a dry vessel, putting the substrate ceramic membrane into the mixed solution, performing ultrasonic treatment at 40kHz for 30-60min, and performing continuous shaking culture at 80rpm for 30-60min; subsequently, the ceramic membrane is calcined to 220 ℃ by programming the temperature, and the temperature rising rate is controlled to be 1-3 ℃ for min -1 The method comprises the steps of carrying out a first treatment on the surface of the Naturally cooling to room temperature, cleaning the membrane with deionized water, and placing the membrane in a 50 ℃ drying box to keep 12-18h, thus obtaining a FeOCl modified ceramic membrane; the protein solution is bovine serum albumin solution.
2. The method for alleviating membrane protein pollution by using a FeOCl modified ceramic membrane in-situ coupled peroxyacetic acid catalytic filtration system according to claim 1, wherein the filtration by using the FeOCl modified ceramic membrane is performed in a dead-end filtration mode.
3. The method for alleviating membrane protein pollution by a FeOCl modified ceramic membrane in-situ coupled peroxyacetic acid catalytic filtration system of claim 1, wherein the oxidant is peroxyacetic acid.
4. A method for alleviating membrane protein contamination by a FeOCl modified ceramic membrane in situ coupled peroxyacetic acid catalyzed filtration system according to claim 1 or 3, characterized in that said peroxyacetic acid catalyzed filtration system comprisesThe concentration of the oxyacetic acid is 1 to 5mmol L -1 。
5. The method for alleviating membrane protein pollution by using FeOCl modified ceramic membrane in-situ coupling peroxyacetic acid catalytic filtration system according to claim 1, wherein the protein solution is bovine serum albumin solution with the concentration of 20-200mg L -1 。
6. The method for alleviating membrane protein pollution by using the FeOCl modified ceramic membrane in-situ coupling peracetic acid catalytic filtration system of claim 1, wherein the FeOCl modified ceramic membrane filtration is driven by constant pressure, a feed liquid enters a membrane assembly, the weight change of a filtrate after membrane filtration is measured in real time, and the flux is recorded every 5s intervals.
7. The method for alleviating membrane protein pollution by using a FeOCl modified ceramic membrane in-situ coupling peroxyacetic acid catalytic filtration system according to claim 6, wherein the constant pressure is a hydraulic driving pressure of 1bar provided by a nitrogen cylinder, and the purity of nitrogen is more than or equal to 99.999%.
8. The method for alleviating membrane protein pollution by a FeOCl modified ceramic membrane in-situ coupling peracetic acid catalytic filtration system according to claim 1, wherein the method is characterized in that the FeOCl modified ceramic membrane is soaked in deionized water for 8-12-h, the soaked ceramic membrane is filled into a membrane module, milli-Q water is used as feed liquid, and the FeOCl modified ceramic membrane is used for filtration for 15min to obtain initial pure water flux; and then taking the protein solution added with the oxidant as a feed liquid, and filtering for 60-100min by utilizing a FeOCl modified ceramic membrane.
9. The method for alleviating membrane protein pollution by a FeOCl modified ceramic membrane in-situ coupled peroxyacetic acid catalytic filtration system according to claim 1, which is characterized in that the method comprises the steps of carrying out ultrasonic treatment at 40kHz for 30-50min and carrying out continuous shaking culture at 80rpm for 30-50min; subsequently, the ceramic membrane is calcined at a programmed temperatureControlling the temperature to 220 ℃ and the temperature rising rate to 2-3 ℃ min -1 Naturally cooling to room temperature, cleaning the membrane with deionized water, and placing in a 50 ℃ drying box to keep 12-14h, thus obtaining the FeOCl modified ceramic membrane.
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| US20160045874A1 (en) * | 2014-08-12 | 2016-02-18 | The Curators Of The University Of Missouri | Nanocomposite membranes with advanced antifouling properties under visible light irradiation |
| CN111760462A (en) * | 2020-07-17 | 2020-10-13 | 重庆理工大学 | Preparation method, device and use method of photo-Fenton ceramic membrane for water treatment |
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