CN111333067A - Preparation method of mesoporous activated carbon and application of mesoporous activated carbon in relieving filter membrane pollution caused by algae-containing water - Google Patents
Preparation method of mesoporous activated carbon and application of mesoporous activated carbon in relieving filter membrane pollution caused by algae-containing water Download PDFInfo
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28064—Surface area, e.g. B.E.T specific surface area being in the range 500-1000 m2/g
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- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
- B01J20/28076—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being more than 1.0 ml/g
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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Abstract
The invention relates to mesoporous activated carbon, which has the pore diameter of 2-4.5 nm and the specific surface area of 800-1000 m2(ii) a mesopore volume of 0.8 to 1.5cm3The preparation method comprises the following steps: adding a template agent into an aqueous solution containing sucrose and concentrated sulfuric acid, and uniformly stirring; heating at 100-120 deg.C and 160-180 deg.C for 5-10h to obtainGrinding the obtained solid into powder; uniformly dispersing the powder into an aqueous solution containing sucrose and concentrated sulfuric acid; then heating for 5-10h at the temperature of 100-120 ℃ and the temperature of 160-180 ℃ respectively; carbonizing at the temperature of 700-900 ℃ for 5-7h under the protection of nitrogen, and grinding the obtained solid into powder; and removing the template agent by adopting hydrofluoric acid solution, and washing by adopting ultrapure water to obtain the mesoporous activated carbon. The invention also relates to application of the mesoporous activated carbon in relieving filter membrane pollution caused by algae-containing water. The mesoporous activated carbon can remarkably relieve the pollution of the filter membrane caused by organic matters released by the water bloom algae after the algae-containing water is pretreated, can effectively improve the removal of the organic matters of the algae and the membrane flux of the filter membrane, and has very important practical significance for the water bloom algae in the membrane treatment application.
Description
Technical Field
The invention relates to the technical field of drinking water, in particular to mesoporous activated carbon and a preparation method and application thereof, and more particularly relates to a method for relieving pollution of algae-containing water to filter membranes (microfiltration membranes, ultrafiltration membranes and the like) by using hollow activated carbon.
Background
At present, lake and river water eutrophication and frequent outbreak of algae bloom seriously affect the quality of water supply and bring great harm to the health of people and the development of society. Meanwhile, algae and its produced metabolites pose serious challenges to drinking water treatment and water quality safety. The low-pressure membrane technology represented by microfiltration and ultrafiltration is considered to be a more effective removal method than the conventional process. However, fouling of membranes by algae and their metabolites is a problem that needs to be carefully treated. At present, researchers have proposed various technical measures for preventing membrane pollution, such as coagulation, activated carbon adsorption, ozone oxidation and the like, aiming at low-pressure membrane pollution. Through the pretreatment process, the accumulation of pollutants on the surface of the membrane can be reduced, and the interaction capacity of the membrane and pollutants is improved, so that the membrane pollution is reduced.
The pretreatment of the activated carbon is a common pretreatment mode in the low-pressure membrane treatment technology, but the currently adopted activated carbon has a non-ideal effect of removing organic matters and has very limited improvement on the membrane flux of the low-pressure membrane. Because the organic matters released by the algae in the growth process can cause the rapid reduction of the membrane flux, the development and popularization of the activated carbon suitable for relieving the membrane pollution and the water treatment technology become an urgent task for vast drinking water workers.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the mesoporous activated carbon and the preparation method thereof, and the mesoporous activated carbon is applied to relieving low-pressure membrane pollution caused by algae, so that the adding amount of a coagulant can be reduced, the organic matters of algae cells can be prevented from being crushed by a chemical reagent, and the mesoporous activated carbon has very important practical significance for the application of the algae in membrane treatment.
In order to achieve the purpose, the invention adopts the following technical scheme:
the first aspect of the invention provides mesoporous activated carbon, the aperture of which is 2-4.5 nm, and the specific surface area of which is 800-1000 m2(ii) a mesopore volume of 0.8 to 1.5cm3/g。
Further, the aperture of the mesoporous activated carbon is 3-4 nm, and the specific surface area is 850-950 m2(ii) a mesopore volume of 1.0 to 1.4cm3(ii)/g; further, the mesoporous activated carbon has a pore diameter of 3.5nm and a specific surface area of 884m2G, mesopore volume 1.2cm3/g。
Further, the algae-containing water treatment process is to remove algae by adopting a low-pressure membrane; further, the low-pressure membrane is a microfiltration membrane or an ultrafiltration membrane.
The second aspect of the present invention provides a method for preparing the mesoporous activated carbon, which comprises the following steps:
step a), adding a template agent with a preset dosage into a first aqueous solution containing cane sugar and concentrated sulfuric acid, and uniformly stirring;
step b) heating the uniformly mixed solution in the step a) to 100-;
step c) uniformly dispersing the first powder obtained in step b) into a second aqueous solution containing sucrose and concentrated sulfuric acid;
step d) heating the solution uniformly mixed in the step c) to 100-;
step e) carbonizing the solution after the heating treatment in the step d) at the temperature of 700-900 ℃ for 5-7h under the protection of nitrogen, and grinding the solid obtained after drying into second powder;
and f) removing the template agent from the second powder obtained in the step e) by adopting a hydrofluoric acid solution, washing by adopting ultrapure water, and drying to obtain the mesoporous activated carbon.
Further, in the above preparation method, the amount ratio of the templating agent to the first aqueous solution in step a) is 2 to 10 g: 20-100 ml.
Further, in the above production method, the ratio of the amount of the first aqueous solution in the step a) to the amount of the second aqueous solution in the step c) is 20 to 100 ml: 20-100ml, wherein in the first aqueous solution and the second aqueous solution, the content of sucrose is 2-10g/20-100ml, the content of concentrated sulfuric acid is 0.2-1.5ml/20-100ml, and the concentration is 70-98 wt%.
Further, in the above production method, the concentration of the hydrofluoric acid solution in the step f) is 5 to 20 wt%; the usage amount of the hydrofluoric acid solution and the ultrapure water is adaptively adjusted according to the usage amount of the template agent.
Further, in the above production method, the template is selected from one or more of non-silicon-based mesoporous materials; specifically, transition metal oxides, phosphates, sulfides, and the like may be included.
Further, in the above-mentioned production method, the equipment used in each operation step is any suitable equipment in the art, which can be adjusted adaptively according to the production scale of the activated carbon, for example, in a pilot test, magnetic stirring, heating with an oil bath, grinding with a mortar, drying with a drying oven, etc. can be used; in the pilot test, a conventional mixer can be used for stirring, a conventional heater is used for heating, a conventional grinder is used for grinding, and a high-temperature furnace is used for carbonization.
In a preferred embodiment, the preparation method specifically comprises the following operation steps:
(1) adding 2-10g of template agent into 20-100ml of aqueous solution containing 2-10g of cane sugar and 0.2-1.5ml of concentrated sulfuric acid, and uniformly stirring;
(2) respectively heating at 100-120 ℃ and 160-180 ℃ for 5-10h, and grinding the obtained dark brown solid into powder;
(3) then uniformly dispersing the powder into 20-30ml of aqueous solution containing 3-5g of cane sugar and 0.2-0.8ml of concentrated sulfuric acid;
(4) then heating at the temperature of 100-120 ℃ and the temperature of 160-180 ℃ for 5-10h respectively;
(5) carbonizing at 900 ℃ of 700-minus 4 ℃ for 5-7h under the protection of nitrogen, and grinding the obtained solid to powder;
(6) and washing the carbonized powder with hydrofluoric acid solution to remove the template agent, and washing with ultrapure water to obtain the mesoporous activated carbon.
The third aspect of the invention provides the application of the mesoporous activated carbon in an algae-containing water treatment process, wherein the algae-containing water treatment process is to remove algae by using low-pressure membranes.
Furthermore, the application is that the mesoporous activated carbon is adopted to relieve the pollution of the filter membrane caused by algae-containing water; wherein the mesoporous activated carbon removes organic matter and increases membrane flux.
In a fourth aspect of the invention, there is provided a method of mitigating filter membrane fouling by algae-containing water, comprising the steps of: adding mesoporous activated carbon with a preset dose into an aqueous solution containing an algae organic matter source; filtering the water solution treated by the mesoporous activated carbon by adopting a filter membrane; wherein the mesoporous activated carbon is any of the above mesoporous activated carbons or is produced by any of the above production methods.
Further, in the method, the dosage of the mesoporous activated carbon is 20mg/L-100 mg/L; more preferably 100 mg/L.
Further, in the above method, after filtration with a filter membrane, filtration may be carried out with a filtration apparatus. Further, the filtration apparatus is an ultrafiltration membrane, which is operated at a pressure of 0.1MPa, and the gas is high-purity nitrogen.
Further, measuring total organic carbon TOC, organic matter UV and membrane flux of a filter membrane in the effluent liquid before and after filtration; wherein, the removal rate of the total organic carbon TOC is 24-70%, the removal rate of the organic matter UV is 30-85% (more preferably 68-85%), and the membrane flux of the filter membrane is improved by 10-50%.
Further, in the above application or method, the filter membrane is an ultrafiltration membrane or a microfiltration membrane; still further, the filter membrane is a microfiltration membrane, specifically a cellulose filter membrane, such as a Millipore blend of cellulose esters, more specifically 80% to 100% nitrocellulose and 0% to 20% cellulose acetate.
Further, in the above application or method, the algae includes blue algae, diatom, green algae, cryptophyceae, euglena, chrysophyceae, dinoflagellate; the cyanobacteria forming the water bloom generally comprises microcystis, anabaena, synnema, cylindrocystis, nodocyclos, flounder and the like, and specifically comprises the following components: anabaena crispa, anabaena, Aphanizomenon flos-aquae, Microcystis aeruginosa, Microcystis viridis, Microcystis flos-aquae, Chlorella, Cyclotella, Scenedesmus, etc.
In one embodiment, the method for alleviating filter membrane fouling caused by algae-containing water comprises the following steps: and (3) pretreating the water containing the organic matters in the algae by using the prepared mesoporous activated carbon, filtering the pretreated water by using a microfiltration membrane experimental filtering device, collecting effluent to measure the total organic carbon TOC and UV of the effluent, and calculating the removal rate of the organic matters by using the mesoporous activated carbon and the improvement condition of the membrane flux after the mesoporous activated carbon is treated. The specific operation steps of the relevant verification experiment on the performance of the mesoporous activated carbon are as follows:
the first step is as follows: adding mesoporous activated carbon; adding mesoporous activated carbon (20-100 mg/L) with different doses into the raw water solution of algae organic matters with a certain concentration, quickly stirring for 30min, slowly stirring for 30min, and standing for half an hour;
the second step is that: filtering the supernatant with a small-scale filter device, wherein the membrane for experiment is a 0.1 μm mixed cellulose filter membrane;
the third step: measuring the removal rate of organic matters in the filtered water by adopting an ultraviolet spectrophotometer and a total organic carbon detector; and the membrane flux of the filter membrane was measured.
Compared with the prior art, the invention adopts the technical scheme, and has the following technical effects:
the invention synthesizes the mesoporous activated carbon, and applies the mesoporous activated carbon to the algae-containing water treatment process for the first time, the mesoporous activated carbon can obviously relieve the membrane pollution of the microfiltration membrane caused by organic matters released by the algal bloom algae after the algae-containing water is pretreated, and can be used as a treatment method for relieving the microfiltration membrane pollution in the algae-containing water treatment, the mesoporous activated carbon can reduce the machine throwing amount of a coagulant, can also avoid the breakage of chemical reagents to the organic matters of algal cells, and has very important practical significance for the algal bloom algae in the membrane treatment application;
the embodiment verifies that the removal rate of the mesoporous activated carbon to different algae organic matters UV can reach 68-85%, the removal rate of common commercial microporous activated carbon to different algae organic matters UV is only 35-62%, the removal rate of the mesoporous activated carbon synthesized by the method is about 27-50% higher than that of common commercial microporous activated carbon to UV, and the removal rate to TOC of microcystis Aeruginosa (AOM) is about 43% highest; the invention also researches the membrane flux after filtering different microcystis, and finds that the membrane flux can be improved by more than 45 percent after being pretreated by the mesoporous activated carbon of 100mg/L, particularly the membrane flux of a microfiltration membrane can be improved by 50 percent, thereby obviously relieving the pollution of organic matters released by the water bloom algae to the microfiltration membrane.
Detailed Description
The invention relates to mesoporous activated carbon, which has the pore diameter of 2-4.5 nm and the specific surface area of 800-1000 m2(ii) a mesopore volume of 0.8 to 1.5cm3The preparation method of the mesoporous activated carbon comprises the following steps: adding a template agent with a preset dosage into an aqueous solution containing sucrose and concentrated sulfuric acid, and uniformly stirring; heating at 100-120 deg.C and 160-180 deg.C for 5-10h respectively to obtain solid, and grinding into powder; uniformly dispersing the powder into an aqueous solution containing sucrose and concentrated sulfuric acid; then heating for 5-10h at the temperature of 100-120 ℃ and the temperature of 160-180 ℃ respectively; then carbonizing the mixture for 5 to 7 hours at the temperature of 700-900 ℃ under the protection of nitrogen, and grinding the obtained solid into powder; and removing the template agent from the powder by adopting a hydrofluoric acid solution, and washing by adopting ultrapure water to obtain the mesoporous activated carbon. The invention also relates to application of the mesoporous activated carbon in relieving filter membrane pollution caused by algae-containing water.
The following further describes embodiments of the present invention with reference to examples. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Experimental methods without specific conditions noted in the following examples, according to methods and conditions conventional in the art; the raw materials and reagents in the following examples are all commercially available products; the equipment used in the steps in the following examples is conventional.
EXAMPLE 1 preparation of mesoporous activated carbon
All reagents used in the present example are commercially available reagents, wherein the template agent is a titanium dioxide-based mesoporous material. This embodiment is a preferred method for preparing mesoporous activated carbon, which comprises the following steps:
(1) adding 3g of template agent into 50ml of aqueous solution containing 5g of cane sugar and 0.8ml of concentrated sulfuric acid (98 wt%), placing the solution into a flask, and stirring uniformly by adopting magnetic stirring for 20 min;
(2) heating the flask in oil bath at 110 deg.C and 170 deg.C for 7h, respectively, drying in oven to obtain dark brown solid, and grinding into powder with mortar;
(3) uniformly dispersing the powder into 50ml of aqueous solution containing 5g of cane sugar and 0.6ml of concentrated sulfuric acid (98 wt%) by magnetic stirring for 10min, and placing the solution into a flask;
(4) then heating the flask for 7 hours at 110 ℃ and 170 ℃ respectively by adopting oil bath;
(5) carbonizing at 800 ℃ for 6h in a high-temperature furnace under the protection of nitrogen, and grinding the obtained solid into powder by adopting a mortar after the temperature is restored to room temperature;
(6) and washing the powder obtained after carbonization by hydrofluoric acid solution (15 wt%) to remove the template agent, and washing the powder by ultrapure water to obtain the mesoporous activated carbon.
The relevant performance parameters of the neutral activated carbon obtained above are as follows: the mesoporous activated carbon has a pore diameter of 3.5nm and a specific surface area of 884m2G, mesopore volume 1.2cm3/g。
Example 2-use of mesoporous activated carbon to mitigate Membrane fouling (organic removal Rate)
This example is a preferred treatment method for mitigating microfiltration membrane fouling in algae-containing water treatment using mesoporous activated carbon prepared in example 1, comprising:
the first step is as follows: and (4) adding mesoporous activated carbon. Adding activated carbon with a certain dosage into the raw water solution of algae organic matters with a certain concentration, quickly stirring for 30min, slowly stirring for 30min, and standing for half an hour.
The second step is that: filtering the supernatant by using a 0.1um mixed cellulose filter membrane (80-100% of cellulose nitrate and 0-20% of cellulose acetate), wherein the filter device is a 400ml ultrafiltration membrane of millipore company, the operating pressure is 0.1MPa, the experimental gas is high-purity nitrogen, and the filtered water chain is balance and automatically records data by a computer);
the third step: and (3) measuring the removal rate of the organic matters in the filtered water by adopting an ultraviolet spectrophotometer and a total organic carbon detector.
In the steps, the content of total organic carbon in the algae water is 5mol/L, the adopted algae are microcystis aeruginosa, chlorella, synnema, anabaena, scenedesmus and cyclotella algae respectively, and the adding dosage of the active carbon is 20mg/L, 40mg/L and 100mg/L respectively.
According to experimental results, the best effect of adding 100mg/L of mesoporous activated carbon is known, and particularly, when the adding amount is 100mg/L, the TOC removal rates of the membrane to AOM (argon oxygen decarburization) of microcystis aeruginosa, chlorella, Aphanizomenon, anabaena, scenedesmus and Cyclotella microcystis are 65%, 52%, 48%, 46%, 45% and 28%, and the UV removal rates are 85%, 72%, 70%, 87%, 32% and 76%, respectively.
Example 3-use of mesoporous activated carbon to mitigate Membrane fouling (Membrane flux) from algae-containing Water
According to the experimental result of the embodiment 2, the water containing different microcystis is treated by adding 100mg/L of mesoporous activated carbon to measure the membrane flux, the steps are the same as the embodiment 2, the adopted microcystis are respectively microcystis aeruginosa, dactylium annulatum AOM, anabaena AOM, scenedesmus AOM and synnema AOM, and the experimental result shows that the membrane flux of the water containing algae is between 30 and 70 percent after the water containing algae is pretreated by adopting the newly synthesized mesoporous activated carbon, and the membrane flux of the microfiltration membrane is improved by about 10 to 50 percent compared with 15 to 20 percent of the water containing algae which is not treated by the activated carbon.
From the results, the pollution of organic matters released by different algae-containing waters to the microfiltration membrane can be remarkably relieved when the newly synthesized activated carbon is adopted for pretreatment.
Comparative example-use of common commercial microporous activated carbon to mitigate Membrane fouling from algae-containing Water
Membrane fouling by algae-containing water was mitigated by the procedure of example 2 using a common commercial microporous activated carbon having a specific surface area of 400 to 580.13m2The pore diameter is 1.5-1.86 nm. The measured organic removal rate and membrane flux were as follows: the membrane flux is about 20 percent, compared with the treatment without PAC, the membrane flux is not improved at all basically, the TOC removal rates of the microporous carbon pretreatment to microcystis aeruginosa, chlorella, Aphanizomenon, anabaena, scenedesmus and Cyclotella minutissima are 22 percent, 25 percent, 13 percent, 17 percent, 32 percent and 5 percent respectively, and the UV removal rates are 62 percent, 36 percent, 35 percent, 36 percent, 40 percent and 44 percent respectively.
Comparing the above results with examples 2 and 3, it can be seen that the removal rate of UV by the mesoporous activated carbon prepared in example 1 is improved by about 27% to 40% compared to the common commercial microporous activated carbon, and the removal rate of TOC of microcystis Aeruginosa (AOM) is improved by about 43% at the highest; after the pretreatment of the mesoporous activated carbon of 100mg/L, the membrane flux can be improved by more than 45 percent (the highest can be 50 percent), and the pollution of organic matters released by the water bloom algae to the microfiltration membrane is obviously relieved.
The embodiment and the comparative example show that the mesoporous activated carbon synthesized by the invention can obviously relieve the membrane pollution of the microfiltration membrane caused by organic matters released by the water bloom algae after the algae-containing water is pretreated, effectively improve the removal rate of different algae organic matters, and simultaneously effectively improve the membrane flux of the filtration membrane, and has very important practical significance for the water bloom algae in the application of membrane treatment.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.
Claims (10)
1. The mesoporous activated carbon for the algae-containing water treatment process is characterized by having a pore diameter of 2-4.5 nm and a specific surface area of 800-1000 m2(ii) a mesopore volume of 0.8 to 1.5cm3/g。
2. Mesoporous activated carbon according to claim 1, characterized in that said algae-containing water treatment process is the removal of algae with low pressure membranes.
3. A method of making mesoporous activated carbon as defined in claim 1, comprising the steps of:
step a), adding a template agent with a preset dosage into a first aqueous solution containing cane sugar and concentrated sulfuric acid, and uniformly stirring;
step b) heating the uniformly mixed solution in the step a) to 100-;
step c) uniformly dispersing the first powder obtained in step b) into a second aqueous solution containing sucrose and concentrated sulfuric acid;
step d) heating the solution uniformly mixed in the step c) to 100-;
step e) carbonizing the solution after the heating treatment in the step d) at the temperature of 700-900 ℃ for 5-7h under the protection of nitrogen, and grinding the solid obtained after drying into second powder;
and f) removing the template agent from the second powder obtained in the step e) by adopting a hydrofluoric acid solution, washing by adopting ultrapure water, and drying to obtain the mesoporous activated carbon.
4. A process for the production of mesoporous activated carbon as claimed in claim 3, wherein the amount ratio of template to first aqueous solution in step a) is 2-10 g: 20-100 ml.
5. A process for producing mesoporous activated carbon as claimed in claim 3, wherein the ratio of the amount of said first aqueous solution in step a) to the amount of said second aqueous solution in step c) is 20-100 ml: 20-100 ml; wherein, in the first aqueous solution and the second aqueous solution, the content of sucrose is 2-10g/20-100ml, the content of concentrated sulfuric acid is 0.2-1.5ml/20-100ml, and the concentration is 70-98 wt%.
6. A process for the production of mesoporous activated carbon as claimed in claim 3, wherein said templating agent is selected from one or more of non-silicon based mesoporous materials.
7. Use of a mesoporous activated carbon as defined in claim 1 in an algae-containing water treatment process to mitigate membrane fouling caused by algae-containing water; wherein the mesoporous activated carbon removes organic matter and increases membrane flux.
8. A method of mitigating filter membrane fouling caused by algae-containing water, comprising the steps of: adding mesoporous activated carbon with a preset dose into an aqueous solution containing an algae organic matter source; filtering the water solution treated by the mesoporous activated carbon by adopting a filter membrane;
wherein the mesoporous activated carbon is the mesoporous activated carbon according to claim 1 or produced by the production method according to any one of claims 3 to 6.
9. The method of claim 8, wherein the mesoporous activated carbon is used in an amount of 20mg/L to 100 mg/L.
10. The method of mitigating filter membrane fouling caused by algae-containing water according to claim 8, wherein the filtering is performed using a filter device.
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