CN112537823B - Method for controlling aging of ultrafiltration membrane by micro-nano bubble technology enhanced chemical cleaning - Google Patents
Method for controlling aging of ultrafiltration membrane by micro-nano bubble technology enhanced chemical cleaning Download PDFInfo
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Abstract
A method for strengthening chemical cleaning and controlling aging of an ultrafiltration membrane by utilizing a micro-nano bubble technology enhances the contact area of a chemical cleaning agent and membrane pollutants by utilizing the characteristics of stability, large specific surface area, high mass transfer and the like of a micro-nano bubble colloid, and promotes the analysis of organic pollutants by generating the action of active oxygen and pollutants due to high interface charge and cavitation. The invention mainly relates to three steps of pure water spray washing and back washing, micro-nano bubble technology strengthening a chemical cleaning agent with proper exposure dose to clean an ultrafiltration membrane, and pure water washing again, wherein the cleaning time of each step is within the range of 10-180 minutes. The invention not only achieves the required membrane cleaning effect and recovers the initial performance of the membrane, compared with the conventional chemical cleaning, the membrane flux recovery rate is improved by 0.5 to 2.6 times, and most importantly, the irreversible influence of chemical agents on the physical/chemical characteristics and the filtering performance of the membrane in the conventional chemical cleaning process of the ultrafiltration membrane at present is effectively relieved, so that the aging process of the membrane is controlled.
Description
Technical Field
The invention relates to the field of ultrafiltration membrane aging control, in particular to a method for controlling the aging of an ultrafiltration membrane by enhancing the chemical cleaning of the ultrafiltration membrane by a micro-nano bubble technology.
Background
Since 1990, the ultrafiltration process based on the principle of membrane pore screening is widely applied to the recycling of sewage and wastewater and the advanced treatment of drinking water by virtue of the advantages of strong adaptability, good effluent quality, low cost and the like, and can effectively remove bacteria, pathogens, colloids, macromolecular pollutants and even partial viruses in raw water. However, during operation, membrane fouling is severe and unavoidable, resulting in continuous attenuation of membrane flux and membrane performance, wherein organic polymers are the main ultrafiltration membrane contaminants and are widely distributed in various water bodies, such as water bodies containing algal organics, municipal and industrial wastewater containing intracellular and extracellular polymers, laundry wastewater containing cationic polymers, coagulation wastewater containing organic polymeric flocculants, and wastewater containing Anionic Polyacrylamide (APAM), resulting in frequent membrane cleaning and short cleaning cycle.
Membrane replacement typically accounts for 25-40% of the total cost of the membrane plant, and cleaning/disinfection procedures account for 15-20% of the operating costs. Conventional physical cleaning generally restores the membrane flux of the fouled membranes to a low level, almost impossible to remove for irreversible fouling, and therefore requires a combination of chemical cleaning. However, it has been found that organic membranes are sensitive to chemical exposure and mechanical stress, and although chemical cleaning is effective in controlling contamination, frequent cleaning affects the physical/chemical properties of the membrane, for example, hydrophilic additives in the membrane are lost, the membrane is modified, the mechanical strength of the membrane is damaged, and the like, thereby reducing the treatment performance and the service life of the ultrafiltration membrane, accelerating the aging process of the membrane, and shortening the service life of the membrane. Membrane fouling, cleaning and aging are central to the problems of industrial membrane applications. Based on this, the scholars propose the maximum life exposure dose of the chemical cleaning, which also indicates that the film aging is related to the factors such as the type, concentration and time of the chemical cleaning, and the film aging phenomenon is inevitably caused by the conventional chemical cleaning at present. How to correctly control the aging of the membrane and improve the service life of the membrane on the premise of achieving the cleanliness and recovering the initial performance of the membrane is an urgent problem to be solved.
In recent years, micro-nano bubbles are widely paid attention to as a novel cleaning mode by virtue of the advantages of high mass transfer efficiency, long hydraulic retention time, high interface potential and the like. Researches find that the method can effectively recover the membrane flux to be more than 90%, does not generate secondary pollution, provides a new idea for controlling the membrane aging, but has the defects of high cost and the like in single micro-nano bubble cleaning. Meanwhile, ions accumulated on the gas-liquid interface of the micro-nano bubbles can improve the reaction process, the contact area between a chemical agent and pollutants in the ultrafiltration membrane process is increased, the active oxygen and pollutants are generated due to high interface charges and cavitation, the organic pollutants are analyzed, the usage amount of the chemical agent is reduced due to synergistic use, the reaction time is shortened, and the theoretical basis is provided for the enhanced chemical cleaning of the micro-nano bubbles.
Disclosure of Invention
The invention aims to solve the key problems that chemical agents damage membrane materials and internal structures, affect membrane chemical stability, cause irreversible influence on membrane filtration performance, accelerate membrane aging process and the like during ultrafiltration membrane chemical cleaning, and provides a method for controlling ultrafiltration membrane aging by micro-nano bubble technology enhanced chemical cleaning.
The invention comprises the following steps: a method for controlling aging of an ultrafiltration membrane by strengthening chemical cleaning by a micro-nano bubble technology is implemented by the following steps:
(1) Carrying out pure water spray washing and back washing on the polluted membrane to remove reversible pollution on the surface of the membrane;
(2) Adding a specific chemical cleaning solution with a proper exposure dose, adjusting the pH, simultaneously starting a micro-nano bubble generator to introduce micro-nano bubbles into the solution, and after the whole process is stable in operation, cleaning the membrane until the membrane flux is recovered;
(3) And washing with purified water again to remove the chemical agent residue on the surface of the membrane.
The specific chemical cleaning agent is oxidation type cleaning agent such as sodium hypochlorite, hydrogen peroxide, etc., surfactant/chelating agent such as ethylene diamine tetraacetic acid salt, dodecyl trimethyl ammonium chloride, sodium dodecyl sulfonate, dioctadecyl dimethyl ammonium bromide, etc., one or more of the chemical cleaning agents.
When the chemical cleaning agent is an oxidation type cleaning agent, the mass concentration is controlled to be 0.001-0.2%, the pH =2-10, and the pH regulator is hydrochloric acid/sodium hydroxide.
The chemical cleaning agent has a concentration of 0.1-3.0CMC (critical micelle concentration) when surfactant is selected, and a molar concentration of 3.0-6.5mmol/L when sodium ethylenediaminetetraacetate is selected.
The micro-nano bubble generator is made of corrosion-resistant stainless steel such as 316L, the pressure and gas dissolving principle is adopted, the size range of micro-nano bubbles is 100nm-30 mu m, a specific micro-nano bubble generator is installed at the tail end of an outlet and is filled with solution, and the specific micro-nano bubble generator can be connected with a ceramic nanotube to obtain micro-nano bubbles with uniform and controllable sizes.
When the air source of the micro-nano bubble generator is air, the gas flow range is 200-400mL/min, and when other gases such as nitrogen, pure oxygen, hydrogen or combined gas are used as the air source, the gas flow is 400-500mL/min.
In the micro-nano bubble enhanced chemical cleaning process, the temperature of the solution is controlled within the range of 0-20 ℃ by adopting a cooling water circulator, and a chemical cleaning agent compounding or synergistic cleaning mode can be selected according to requirements when the chemical cleaning is selected and combined for cleaning.
The time of each cleaning step is in the range of 10-180 minutes.
The method can be used for cleaning ultrafiltration membranes polluted by treating polymer flooding oil extraction wastewater, municipal sewage containing intracellular and extracellular polymers, landfill leachate and other water bodies containing high-molecular organic polymeric pollutants, such as PVDF, PTFE, PES and other organic membranes, ceramic membranes and other inorganic membranes, and controlling the aging behavior of chemical cleaning on the membranes.
When above-mentioned micro-nano bubble reinforces chemical cleaning, can set up membrane reinforcing apparatus, put the membrane in the device fixed in order to prevent that the micro-nano bubble generator operation rivers impact force from causing the damage to the membrane, micro-nano bubble sees through reinforcing apparatus's the nanopore entering of evenly arranging simultaneously, makes micro-nano bubble wash more stable even.
The basic principle of the method for controlling the aging of the ultrafiltration membrane by enhancing chemical cleaning by the micro-nano bubble technology is as follows: micro-nano bubble can exist steadily and have micro-nano level size in aqueous, big specific surface area, and then showing and improving gas-liquid mass transfer efficiency, it is combined with the chemical cleaning medicament that suits to expose the dose, can improve the utilization ratio of chemical cleaning medicament, reduce the consumption of chemical medicament, micro-nano bubble self high interface Zeta electric potential simultaneously, and the shock wave that micro-nano bubble collapses the production can promote membrane adsorbed pollutant to compel to shift to the gas-liquid micro interface from solid-liquid interface, and then more do benefit to and react with the chemical medicament contact, and wash along with the water power and get rid of, both satisfied membrane cleaning demand and recovered membrane flux, and itself is very little to the damage of membrane material than conventional chemical cleaning, high-efficient control membrane is ageing, the life of milipore filter has been prolonged.
Compared with the prior art, the method for controlling the aging of the ultrafiltration membrane by strengthening chemical cleaning by the micro-nano bubble technology has the following advantages:
(1) On the premise of ensuring that the requirement of membrane cleaning is met, the method effectively avoids the problems that the chemical stability of the membrane is damaged and the filtering performance of the membrane is not reversible by the conventional membrane chemical cleaning, and the like, efficiently controls the aging process of the membrane and prolongs the service life of the membrane; (2) The method disclosed by the invention provides the appropriate exposure dose of the chemical cleaning agent under the action of the micro-nano bubbles, so that the membrane cleaning is more targeted, the chemical agent is ensured to play a role in the ultrafiltration membrane cleaning, and the aging effect of the chemical agent on the membrane is relieved;
(3) The method of the invention obviously shortens the membrane cleaning time, improves the reaction efficiency of the chemical agent and the pollutant, and simultaneously reduces the using amount of the chemical cleaning agent.
Drawings
The attached drawing is a diagram of the cleaning effect of the method for controlling the aging of the ultrafiltration membrane by enhancing chemical cleaning with the micro-nano bubble technology on the PVDF ultrafiltration membrane polluted by the anionic polyacrylamide in the specific embodiment 1. Wherein ^ represents the cleaning effect of sodium hypochlorite chemical cleaning with the mass concentration of 0.03% on the PVDF ultrafiltration membrane polluted by the anionic polyacrylamide, and is strengthened by a micro-nano bubble technology taking air as an air source; and a circle indicates the cleaning effect of the sodium hypochlorite chemical cleaning with the mass concentration of 0.03% on the PVDF ultrafiltration membrane polluted by the anionic polyacrylamide.
Detailed Description
The invention is further illustrated by the following specific embodiments.
Specific example 1:
the process conditions are as follows:
and (3) pollution film: an anionic polyacrylamide contaminated PVDF ultrafiltration membrane;
the cleaning mode is as follows: soaking the micro-nano bubbles and the liquid medicine;
cleaning temperature: 10 ℃;
cleaning time: all the steps are different;
preparing a cleaning solution: selecting purified water as a solvent;
sodium hypochlorite chemical cleaning solution suitable for exposure dose: the mass concentration of sodium hypochlorite is 0.03%, the pH value of the solution is adjusted to be =10 by hydrochloric acid, and the soaking time is 120min;
micro-nano bubble technology: air is used as an air source, the pressure is controlled to be 0.4-0.5MPa, the gas flow is 350-400mL/min, the liquid environment is 20 ℃, the size range of the micro-nano bubbles is 850nm-10 mu m, and the Zeta potential of the micro-nano bubble interface is-55 mV;
a cleaning step:
(1) Carrying out pure water spray washing and back washing on the polluted membrane to remove reversible pollution on the surface of the membrane, wherein the washing time is 15min;
(2) Adding sodium hypochlorite cleaning solution with the mass concentration of 0.03%, adjusting the pH value to be =10 by hydrochloric acid, starting a micro-nano bubble generator to introduce micro-nano bubbles into the solution, operating for 30min, stabilizing the process, cleaning the membrane, setting the flow to be 350-400mL/min, setting the cleaning time to be 120min, and setting the solution temperature to be 20 ℃;
(3) And washing with purified water again to remove chemical agent residue on the membrane surface for 10min.
The experimental results are as follows: the method for controlling the aging of the ultrafiltration membrane by strengthening chemical cleaning by the micro-nano bubble technology in the embodiment has the cleaning effect on the PVDF ultrafiltration membrane polluted by anion polyacrylamide as shown in the attached drawing, the micro-nano bubble technology taking air as an air source strengthens sodium hypochlorite chemical cleaning with the mass concentration of 0.03% so that the clear water flux of the membrane is recovered to 97.65% before the experiment is operated, the flux recovery rate of the sodium hypochlorite chemical agent statically soaking the ultrafiltration membrane under the same condition is 56.14%, the efficiency is improved by 74%, and no obvious hydrophilic membrane modification behavior is found through detection and analysis of mechanical strength, contact angle, fourier infrared spectrometer, scanning electron microscope and membrane aperture of the membrane, the chemical stability of the membrane is not damaged after cleaning, the membrane extensibility is good, the softening characteristic is not shown, and the aging process of the membrane is controlled.
Specific example 2:
the process conditions are as follows:
and (3) pollution film: treating a PVDF polluted membrane in the polymer flooding wastewater by an ultrafiltration process;
the cleaning mode is as follows: soaking the micro-nano bubbles and the liquid medicine;
cleaning temperature: 10 ℃;
cleaning time: all the steps are different;
preparing a cleaning solution: selecting purified water as a solvent;
sodium hypochlorite chemical cleaning solution suitable for exposure dose: the mass concentration of sodium hypochlorite is 0.01%, the pH of the solution is adjusted to be =10 by hydrochloric acid, and the soaking time is 30min;
dodecyl trimethyl ammonium chloride cleaning solution: the molar concentration is 2.0CMC (CMC is the critical micelle concentration of the surfactant), pH =7, and the soaking time is 40min;
micro-nano bubble technology: controlling the pressure to be 0.4-0.5MPa, the gas flow to be 450-500mL/min and the liquid environment to be 10 ℃ by taking nitrogen as a gas source;
a cleaning step:
(1) Carrying out pure water spray washing and back washing on the polluted membrane to remove reversible pollution on the surface of the membrane, wherein the washing time is 15min;
(2) Firstly, adding dodecyl trimethyl ammonium chloride with the molar concentration of 2.0CMC, adjusting the pH =7, starting a micro-nano bubble generator to introduce micro-nano bubbles into a solution, operating for 30min, stabilizing the process, cleaning a membrane, setting the flow to be 450-500mL/min, setting the cleaning time to be 40min, and setting the solution temperature to be 10 ℃;
then adding sodium hypochlorite cleaning solution with the mass concentration of 0.01%, adjusting the pH value to be =10 by hydrochloric acid, starting a micro-nano bubble generator to introduce micro-nano bubbles into the solution, operating for 30min, stabilizing the process, cleaning the membrane, setting the flow to be 450-500mL/min, setting the cleaning time to be 30min, and setting the solution temperature to be 10 ℃;
the process is circularly cleaned once;
(3) And washing with purified water for 10-20min to remove chemical agent residue on the surface of the membrane.
The experimental results are as follows: the high Zeta potential of the micro-nano bubble interface depends on the potential difference between electric double layers consisting of ion adsorption of the bubble interface and counter ions on the inner surface of the bubble, the micro-nano bubble is negatively charged, when the micro-nano bubble is combined with a cationic surfactant dodecyl trimethyl ammonium chloride cleaning solution, the charge is changed from negative to positive, the interface Zeta potential is 37 +/-2 mV under the conditions that the pH of a solution environment is =7 and the concentration is 2.0CMC, a positively charged dodecyl trimethyl ammonium chloride colloid is adsorbed on the surface of the micro-nano bubble, the micro-nano bubble has larger specific surface area, the hydraulic impact and bubble cavitation during operation promote pollutants on a medicament adsorption membrane, the gel layer is quickly deconstructed, the next optimal exposure dose of sodium hypochlorite chemical cleaning is promoted, the optimal exposure dose of sodium hypochlorite chemical cleaning is finally recovered to 101.72% before the experiment operation, the hydrophilic modification effect on the membrane is obviously lower than that of conventional cleaning, the overall extensibility of the membrane is stable after cleaning, the membrane structure is not damaged, and the oxidative type cleaning medicament under the optimal exposure dose does not cause the loss of the membrane hydrophilic modification, and the aging process of the membrane is controlled.
Specific example 3:
the process conditions are as follows:
and (3) pollution film: treating a polluted membrane in the polymer flooding oil extraction wastewater by an ultrafiltration process;
the cleaning mode comprises the following steps: soaking the micro-nano bubbles and the liquid medicine;
cleaning temperature: 10 ℃;
cleaning time: all the steps are different;
preparing a cleaning solution: selecting purified water as a solvent;
cleaning solution of disodium ethylene diamine tetraacetate: the concentration is 3.5mmol/L, the pH value is adjusted to be =7 by sodium bicarbonate, and the soaking time is 20min;
dodecyl trimethyl ammonium chloride cleaning solution: the molar concentration is 1.0CMC, the pH is not less than 7, and the soaking time is 30min;
micro-nano bubble technology: pure oxygen is taken as a gas source, the pressure is controlled to be 0.4-0.5MPa, the gas flow is 450-500mL/min, and the liquid environment is 10 ℃;
a cleaning step:
(1) Carrying out pure water spray washing and back washing on the polluted membrane to remove reversible pollution on the surface of the membrane, wherein the washing time is 15min;
(2) Adding disodium ethylene diamine tetraacetate cleaning solution with the concentration of 3.5mmol/L, adjusting the pH =7, starting a micro-nano bubble generator to introduce pure oxygen micro-nano bubbles into the solution, operating for 30min, stabilizing the process, cleaning the membrane, setting the flow at 450-500mL/min, setting the cleaning time at 20min, and setting the solution temperature at 10 ℃;
then adding dodecyl trimethyl ammonium chloride cleaning solution with the concentration of 1.0CMC, adjusting the pH to be =10 by hydrochloric acid, starting a micro-nano bubble generator to introduce micro-nano bubbles into the solution, operating for 30min, stabilizing the process, cleaning the membrane, setting the flow to be 450-500mL/min, setting the cleaning time to be 30min, and setting the solution temperature to be 10 ℃;
the process is circularly cleaned once;
(3) And washing with purified water again to remove chemical agent residue on the membrane surface for 15min.
The experimental results are as follows: the clear water flux is recovered to 106.5% before the experiment is run, compared with the conventional surfactant/chelating agent membrane cleaning agent, the hydrophilic modification effect on the membrane is obviously reduced, and meanwhile, the strong mass transfer efficiency of the micro-nano bubbles shortens the reaction time of the disodium ethylene diamine tetraacetate and the APAM-Ca-APAM complex by 47%, so that the cleaning time of a chemical agent is shortened on the basis of ensuring the cleaning efficiency, and the membrane aging behavior is not generated.
The above embodiments are merely preferred embodiments of the present invention, which should not be construed as limiting the scope of the present invention, but should be defined by the appended claims.
Claims (5)
1. A method for controlling aging of an ultrafiltration membrane by enhancing chemical cleaning by a micro-nano bubble technology is characterized by comprising the following steps: the method is implemented by the following steps:
(1) Carrying out pure water spray washing and back washing on the polluted membrane to remove reversible pollution on the surface of the membrane;
(2) Adding a specific chemical cleaning agent with proper exposure dose, adjusting the pH, simultaneously starting a micro-nano bubble generator to introduce micro-nano bubbles into the solution, and cleaning the membrane after the whole process is stable until the membrane flux is recovered;
(3) Washing with purified water again to remove chemical agent residues on the surface of the membrane;
the specific chemical cleaning agent is an oxidation type cleaning agent or a surfactant; the oxidation type cleaning agent is sodium hypochlorite or hydrogen peroxide, the surfactant is ethylene diamine tetraacetate, dodecyl trimethyl ammonium chloride, sodium dodecyl sulfonate or dioctadecyl dimethyl ammonium bromide, and the specific chemical cleaning agent is one or the combination of more of the components;
when the chemical cleaning agent is an oxidation type cleaning agent, the mass concentration of the chemical cleaning agent is controlled to be 0.001-0.2%, the pH =2-10, and the pH regulator is hydrochloric acid/sodium hydroxide;
when the chemical cleaning agent selects surfactant, the concentration is 0.1-3.0CMC (critical micelle concentration), and when the ethylene diamine tetraacetic acid sodium salt is selected, the molar concentration is 3.0-6.5mmol/L;
the material of the micro-nano bubble generator is corrosion-resistant 316L stainless steel, a pressurized gas dissolving principle is adopted, the size range of micro-nano bubbles is 100nm-30 mu m, a specific micro-nano bubble generator is installed at the tail end of an outlet and is filled with solution, and the specific micro-nano bubble generator can be connected with a ceramic nanotube to obtain micro-nano bubbles with uniform and controllable sizes;
when the air source of the micro-nano bubble generator is air, the gas flow range is 200-400mL/min, and when the air source is nitrogen, pure oxygen or hydrogen, the gas flow is 400-500mL/min.
2. The method for controlling aging of the ultrafiltration membrane by using micro-nano bubble technology to strengthen chemical cleaning according to claim 1, is characterized in that: in the micro-nano bubble strengthening chemical cleaning process in the step (2), a cooling water circulator is adopted to control the temperature of the solution within the range of 0-20 ℃, and chemical cleaning agents can be selected to be compounded or cooperatively cleaned according to requirements when the chemical cleaning is selected and combined for cleaning.
3. The method for controlling aging of the ultrafiltration membrane by using micro-nano bubble technology to strengthen chemical cleaning according to claim 1, is characterized in that: each washing step is in the range of 10-180 minutes.
4. The method for controlling aging of the ultrafiltration membrane by using micro-nano bubble technology to strengthen chemical cleaning according to claim 1, is characterized in that: the method can be used for cleaning an ultrafiltration membrane polluted by polymer flooding oil extraction wastewater, municipal sewage containing intracellular and extracellular polymers and landfill leachate; the ultrafiltration membrane is made of PVDF, PTFE, PES or ceramic membrane, and aging behavior of chemical cleaning on the type of membrane is controlled.
5. The method for controlling the aging of the ultrafiltration membrane by the micro-nano bubble technology reinforced chemical cleaning according to claim 1, which is characterized by comprising the following steps: when carrying out step (2) micro-nano bubble and strengthening chemical cleaning, can set up membrane reinforcing apparatus, put the membrane in the device fixed in order to prevent that micro-nano bubble generator from moving rivers impact force from causing the damage to the membrane, micro-nano bubble sees through reinforcing apparatus's the nanopore of evenly arranging and gets into simultaneously, makes micro-nano bubble wash more stable even.
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