CN218620540U - Internal circulating fluidized bed-photoproduction direct coupling reactor - Google Patents
Internal circulating fluidized bed-photoproduction direct coupling reactor Download PDFInfo
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Abstract
The utility model discloses an internal circulation fluidized bed-photoproduction direct coupling reactor, include: a photobioreactor and one or more magnetic rods disposed around the photobioreactor, the photobioreactor comprising: the aeration device comprises a first barrel, a second barrel and an aeration disc, wherein the first barrel is a cylindrical cavity with an open top surface, and the second barrel is a cylindrical cavity with an open top surface and an open bottom surface; the aeration disc is fixedly arranged on the inner wall of the bottom end of the first barrel, and the second barrel is positioned in the first barrel and is fixedly arranged on the aeration disc through a hollow bracket. The internal circulation fluidized bed-photoproduction direct coupling reactor avoids excessive photocatalytic oxidation and saves time and space required by reaction. Can affect the growth and metabolism of active groups and microorganisms in the photocatalyst, and play an auxiliary or synergistic promotion role in the photocatalytic process and the biodegradation process, thereby greatly improving the degradation rate and mineralization rate of the antibiotic and achieving the purpose of efficiently degrading the antibiotic.
Description
Technical Field
The utility model belongs to the technical field of sewage treatment, relate to an internal circulation fluidized bed-photoproduction direct coupling reactor particularly.
Background
The antibiotic as a medicament with wide application and difficult degradation organic pollutants exists in various aquatic environments, has persistence and is difficult to remove by the traditional water treatment process. The advanced oxidation method is an effective method for degrading macromolecular organic pollutants. However, complete mineralization of the advanced oxidation process is economically prohibitive and difficult to operate in practice, and any rapid chemical reaction in the advanced oxidation process often results in the accumulation of toxic by-products and excessive residual of oxidation products. In contrast, biodegradation methods have natural advantages in terms of mineralization of pollutants, and biological methods are low in operating cost and have mature experience for reference. Despite the promising biodegradation prospects of antibiotics, a serious bottleneck is the slow or no at all biodegradability of many antibiotics. At present, the indirect coupling of the advanced oxidation pretreatment process and the biodegradation process is widely used for treating antibiotic wastewater, but still has the problems of high energy consumption, difficult regulation, unsustainable detoxification and the like, and two reactors of advanced oxidation and biodegradation are needed, so that the occupied area is increased, and the reaction space is enlarged. The photocatalysis-biological direct coupling technology developed in recent years has great potential in improving the removal and mineralization of pollutants difficult to degrade, and can realize continuous detoxification of antibiotics. In a typical direct coupled system, the photocatalyst is coated on the outer surface of the macroporous support, while the biofilm is concentrated inside the macroporous support. Under uv or visible light irradiation, photocatalysis first attacks the recalcitrant contaminants, producing biodegradable intermediates, which are at the same time rapidly consumed and mineralized by the internal microorganisms. Because of the protection of the carrier, the biofilm is well protected from poisons and oxidants. With the repetition of the composite degradation process, the compound is effectively degraded. At present, the direct coupling technology is used for denitrification, dechlorination, degradation of dyes and antibiotics, and shows application potential in actual wastewater treatment. However, research shows that the photocatalytic-biological direct coupling technology is susceptible to environmental factors, so that the degradation of antibiotics is unstable, and the pollutant removal efficiency is reduced.
Disclosure of Invention
The utility model is not enough to prior art, an object of the utility model is to provide an interior circulating fluidized bed-photoproduction direct coupling reactor, after the catalyst that contains the microorganism was put into to interior circulating fluidized bed-photoproduction direct coupling reactor, this interior circulating fluidized bed-photoproduction direct coupling reactor can be through magnetic field, the antibiotic in visible light and the microorganism degradation waste water simultaneously, plus magnetic field not only produces the influence to active group in the catalyst, also take place the interact with the microorganism, realize microbial community evolution, improve the microbial degradation function, thereby realize the high-efficient degradation of system.
The purpose of the utility model is realized by the following technical proposal.
An internally circulating fluidized bed-photogeneration direct coupled reactor comprising: the device comprises a photobioreactor and one or more magnetic rods arranged around the photobioreactor, wherein the magnetic strength of the magnetic rods formed in the photobioreactor is 10-50 mT.
In the above technical solution, the photobioreactor comprises: the aeration device comprises a first barrel, a second barrel and an aeration disc, wherein the first barrel is a cylindrical cavity with an open top surface, and the second barrel is a cylindrical cavity with an open top surface and an open bottom surface; the aeration disc is fixedly arranged on the inner wall of the bottom end of the first barrel, and the second barrel is positioned in the first barrel and is fixedly arranged on the aeration disc through a hollow bracket.
In the technical scheme, the bottom end of the hollow support is provided with a truncated cone-shaped baffle, the baffle gradually shrinks from top to bottom, and the hollow support is located at the center of the baffle.
In the above technical solution, the method further comprises: and the pipeline between the aeration disc and the aeration pump is provided with a gas flowmeter.
In the technical scheme, the area ratio of the cross sections of the first barrel and the second barrel is (3-3.5): 1, and the ratio of the outer diameter to the height of the first barrel to the height of the second barrel is (3-5).
In the above technical solution, when the number of the magnetic rods is plural, the plural magnetic rods are arranged along the circumferential direction with the axis of the first barrel as the center of circle.
In the above technical scheme, the first barrel and the second barrel are both made of transparent materials, and a light source is arranged around the photobioreactor.
A method for degrading antibiotic wastewater by a magnetic field enhanced photocatalysis-biological direct coupling system comprises the following steps: putting a catalyst-biological coupling carrier and antibiotic wastewater into the internal circulating fluidized bed-photogenerated direct coupling reactor, starting an aeration disc, and degrading, wherein the method for preparing the catalyst-biological coupling carrier comprises the following steps:
1) Adding Bi (NO) 3 ) 3 ·5H 2 O、H 3 BO 3 Polyethylene glycolMixing the vinylpyrrolidone and the first mannitol aqueous solution to obtain a solution A, wherein the Bi (NO) is calculated according to the parts by mass 3 ) 3 ·5H 2 O、H 3 BO 3 And the ratio of the polyvinylpyrrolidone to the mannitol in the first aqueous mannitol solution is 26.2:1:21.6: (1-2);
and mixing NaCl and a second mannitol aqueous solution to obtain a solution B, wherein the ratio of the NaCl to the second mannitol in the second mannitol aqueous solution is 10: (1-2);
in the step 1), the concentration of mannitol in the first mannitol aqueous solution is 0.1-0.2 mol/L, and the concentration of mannitol in the second mannitol aqueous solution is 0.1-0.2 mol/L.
2) Under the condition of stirring, dropwise adding the solution B into the solution A, continuously stirring for at least 30min after dropwise adding is finished, adjusting the pH value to 11-12 by using a NaOH aqueous solution after stirring, carrying out hydrothermal treatment at 150-170 ℃ for 23-25 h, cooling to room temperature, centrifugally collecting solids, washing and drying to obtain B/Bi 3 O 4 A Cl catalyst, wherein the ratio of the solution A to the solution B is (4.5-5.5) in parts by volume: 1;
in the step 2), the concentration of NaOH in the NaOH aqueous solution is 1.5-2.5M.
In the step 2), deionized water and absolute ethyl alcohol are adopted for washing.
In the step 2), the temperature of the drying is 60 ℃.
3) B/Bi 3 O 4 Mixing a Cl catalyst, absolute ethyl alcohol and nitric acid, performing ultrasonic dispersion at 80 ℃ for at least 20min to obtain a suspension, adding a polyurethane sponge carrier into the suspension, performing ultrasonic dispersion at 80 ℃ for at least 20min, taking out, and drying to obtain B/Bi 3 O 4 A Cl sponge carrier, and B/Bi is added under the aeration condition 3 O 4 Immersing a Cl sponge carrier into the activated sludge for at least 24 hours to obtain a catalyst-biological coupling carrier, wherein the B/Bi is calculated according to the parts by weight 3 O 4 The ratio of the Cl catalyst to the absolute ethyl alcohol to the nitric acid is (900-1100): 10:1.
in the step 3), the ratio of the suspension to the polyurethane sponge carrier is 1 (0.8-1.2) by volume part, and the concentration of the nitric acid is 17-18M.
In the step 3), the aeration is air.
In the step 3), the B/Bi is calculated according to parts by mass 3 O 4 The ratio of the Cl sponge carrier to the activated sludge is (0.2-0.4): 1.
in the technical scheme, the B/Bi is calculated according to parts by weight 3 O 4 The ratio of the Cl catalyst to the polyurethane sponge carrier is (0.3-0.5): 1.
in the technical scheme, the light source applies visible light during degradation, and the illumination intensity of the visible light is more than or equal to 40mW/cm 2 。
In the technical scheme, the aeration quantity of the aeration disc is 2.5-3L/min.
The utility model discloses compare with traditional photocatalysis + biodegradable's technique (photocatalysis reaction degrades ciprofloxacin earlier and improves waste water biodegradability, goes out the further mineralization of water reentrant biological treatment technology), avoided excessive photocatalytic oxidation, practiced thrift required time and the space of reaction. Can affect the growth and metabolism of active groups and microorganisms in the photocatalyst, and play an auxiliary or synergistic promotion role in the photocatalytic process and the biodegradation process, thereby greatly improving the degradation rate and mineralization rate of the antibiotic and achieving the purpose of efficiently degrading the antibiotic.
Drawings
Fig. 1 is a schematic structural diagram of the internal circulating fluidized bed-photoproduction direct coupling reactor of the present invention, wherein, 1: magnetic bar, 2: first barrel, 3: second barrel, 4: light source, 5: aeration disc, 6: fretwork support, 7: baffle, 8: aeration pump, 9: a gas flow meter;
FIG. 2 is an SEM of a catalyst-bio-coupling carrier;
FIG. 3 is the total organic carbon removal for the processes of example 4 and comparative example 1;
FIG. 4 is a graph of ciprofloxacin removal rates for the methods of example 4 and comparative example 2;
FIG. 5 is the ciprofloxacin degradation pathway of the method in example 4;
FIG. 6 is the toxicity of the degradation products of ciprofloxacin obtained by the methods of example 4 and example 2.
Detailed Description
The technical solution of the present invention will be further described with reference to the following specific examples.
Aeration in the following examples is air.
The activated sludge is from a secondary sedimentation tank of a sewage treatment plant in a new coastal area in Tianjin.
Example 1
As shown in fig. 1, an internal circulating fluidized bed-photogeneration direct coupling reactor comprises: a photo bioreactor and two magnetic rods 1 arranged around the photo bioreactor.
Example 2
On the basis of example 1, the photobioreactor comprises: the device comprises a first barrel 2, a second barrel 3 and an aeration disc 5, wherein the first barrel 2 is a cylindrical cavity with an open top surface, and the second barrel 3 is a cylindrical cavity with an open top surface and an open bottom surface; the first round barrel 2 and the second round barrel 3 are made of transparent organic glass materials, the aeration disc 5 is fixedly arranged on the inner wall of the bottom end of the first round barrel 2, the second round barrel 3 is positioned in the first round barrel 2 and is fixedly arranged on the aeration disc 5 through a hollowed-out support 6, a truncated cone-shaped baffle 7 is arranged at the bottom end of the hollowed-out support 6, the baffle 7 is gradually reduced from top to bottom, and the hollowed-out support 6 is positioned at the center of the baffle 7. The top end edge of baffle 7 and the interior wall connection of first cask 2, the bottom edge of baffle 7 is connected with fretwork support 6 for in the water current guide entering fretwork support 6's the hollow out construction with flowing down between first cask 2 and the second cask 3, and then get into the inside of second cask 3, the water current that gets into the inside of second cask 3 is supreme flow from down in second cask 3 under the effect of aeration dish 5 aeration, and then gets into between first cask 2 and the second cask 3 from the top of second cask 3 again.
The first barrel 2 and the second barrel 3 are coaxially arranged, the area ratio of the cross sections of the first barrel 2 and the second barrel 3 is 3.44.
The two magnetic rods 1 are oppositely arranged and are arranged along the circumferential direction by taking the axis of the first round barrel 2 as the center of a circle.
The light source 4 is arranged around the photobioreactor, and visible light is applied by the light source 4.
Example 3
On the basis of embodiment 2, the method further comprises the following steps: an aeration pump 8 connected to the aeration disk 5, and a gas flow meter 9 is installed on a pipeline between the aeration disk 5 and the aeration pump 8.
Example 4
A method for degrading antibiotic wastewater by a magnetic field enhanced photocatalysis-biological direct coupling system comprises the following steps: putting a catalyst-biological coupling carrier (30 percent of the volume of the antibiotic wastewater) and the antibiotic wastewater (1L) into an internal circulating fluidized bed-photo-generated direct coupling reactor in example 3, enabling the liquid level in the internal circulating fluidized bed-photo-generated direct coupling reactor to be higher than the top edge of a second round barrel 3 (the volume of the second round barrel 3 is 320 mL), starting an aeration disc 5, starting a light source 4, applying a magnetic field by a magnetic rod 1, and degrading, wherein the antibiotic wastewater is a ciprofloxacin aqueous solution of 40mg/L, the aeration amount of the aeration disc 5 is 3L/min, and the illumination intensity of visible light is 42mW/cm 2 The magnetic bar 1 has a magnetic field strength of 40mT formed in the photobioreactor.
The method for preparing the catalyst-biological coupling carrier comprises the following steps:
1) Adding Bi (NO) 3 ) 3 ·5H 2 O、H 3 BO 3 Mixing polyvinylpyrrolidone and a first mannitol aqueous solution to obtain a solution A, wherein Bi (NO) is calculated according to the mass portion 3 ) 3 ·5H 2 O、H 3 BO 3 And the ratio of the polyvinylpyrrolidone to the mannitol in the first aqueous mannitol solution is 26.2:1:21.6:1.6, the concentration of mannitol in the first mannitol aqueous solution is 0.1mol/L;
and mixing NaCl and the second mannitol aqueous solution to obtain a solution B, wherein the mass portion ratio of the NaCl to the mannitol in the second mannitol aqueous solution is 10:1.1, the concentration of mannitol in the second mannitol aqueous solution is 0.1mol/L;
2) Under the condition of stirring, dropwise adding the solution B into the solution A,stirring for 30min after the dropwise addition is finished, adjusting the pH value to 11.5 by using a 2M NaOH aqueous solution after stirring, putting the mixture into a high-pressure reaction kettle, carrying out hydrothermal treatment for 24h at 160 ℃, cooling to room temperature of 20-25 ℃, centrifugally collecting solids, sequentially washing 3 times by respectively using deionized water and absolute ethyl alcohol, and drying for 12h under a vacuum condition at 60 ℃ to obtain B/Bi 3 O 4 A Cl catalyst, wherein the ratio of the solution A to the solution B is 5:1;
3) B/Bi 3 O 4 Mixing Cl catalyst, absolute ethyl alcohol and nitric acid, performing ultrasonic dispersion in an ultrasonic cleaner at 80 ℃ for 30min to obtain a suspension, adding a polyurethane sponge carrier (purchased from Jiangsu ai-Du environmental protection enterprise store) into the suspension, performing ultrasonic dispersion at 80 ℃ for 30min, taking out, and drying in a constant-temperature oven at 60 ℃ for 6h to obtain B/Bi 3 O 4 A Cl sponge carrier, under the aeration condition, adding B/Bi 3 O 4 And (2) immersing the Cl sponge carrier into the activated sludge for 24 hours to obtain a catalyst-biological coupling carrier, wherein the ratio of the suspension to the polyurethane sponge carrier is 1 3 O 4 The ratio of the Cl catalyst to the absolute ethyl alcohol to the nitric acid is 1000:10:1, the concentration of nitric acid is 18M, calculated by weight parts, B/Bi 3 O 4 The ratio of Cl sponge carrier to activated sludge is 0.3:1, based on parts by mass, B/Bi 3 O 4 The ratio of Cl catalyst to polyurethane sponge support was 0.4:1.
the SEM of the catalyst-bio-coupling carrier is shown in fig. 2, and it can be seen that the polyurethane sponge carrier inoculated with the activated sludge has a certain amount of biomass in the inner pore channels and the outer surface.
The proportion of the live bacteria in the embodiment 4 can reach 87 percent, the degradation efficiency of the ciprofloxacin is about 92 percent, the degradation rate constant is 0.17, the removal rate of Chemical Oxygen Demand (COD) of the effluent can reach about 95 percent, and the mineralization rate of the antibiotic wastewater is about 90 percent.
Comparative example 1
A method for degrading antibiotic wastewater by a photocatalysis-biological direct coupling system is basically the same as that in example 4, and the only difference is that two magnetic rods 1 around an internal circulating fluidized bed-photoproduction direct coupling reactor in example 4 are removed.
The total organic carbon removal rate with respect to the degradation time of example 4 and comparative example 1 is shown in fig. 3, and it can be seen from the graph that the mineralization rate was 90% when the antibiotic wastewater of example 4 was degraded for 12 hours, and the mineralization rate was 66% when the antibiotic wastewater of comparative example 1 was degraded for 12 hours.
The proportion of the live bacteria in the comparative example 1 can reach 65%, the degradation efficiency of the ciprofloxacin after the antibiotic wastewater is degraded for 12h is 74%, the degradation rate constant is 0.09, and the removal rate of Chemical Oxygen Demand (COD) of the effluent can reach 69%. It can be seen from comparative example 4 and comparative example 1 that the external magnetic field strategy can not only improve the biological activity but also enhance the photocatalytic oxidation.
Comparative example 2
A method for degrading antibiotic wastewater is substantially the same as that in example 4, except that "the catalyst-bio-coupling carrier (30% by volume of antibiotic wastewater) and the antibiotic wastewater (1L) in example 4 are placed in the internal circulating fluidized bed-photogenerated direct coupled reactor in example 3" instead of "B/Bi in example 4 3 O 4 The Cl sponge carrier (30% of the antibiotic wastewater volume) and the antibiotic wastewater (1L) were placed in the internal circulating fluidized bed-photogenerated direct coupled reactor of example 3 ".
The ciprofloxacin removal rates with degradation time of the antibiotic wastewater in the example 4 and the antibiotic wastewater in the comparative example 2 are shown in fig. 4, and it can be seen from the graph that the degradation efficiency of ciprofloxacin is 92% by testing after the antibiotic wastewater in the example 4 is degraded for 12 hours, and the degradation efficiency of ciprofloxacin is 76% by testing after the antibiotic wastewater in the comparative example 2 is degraded for 12 hours.
The degradation rate constant of ciprofloxacin in comparative example 2 is 0.09, which is 0.5 times that of example 4, the removal rate of Chemical Oxygen Demand (COD) of effluent is 49 percent, which is 0.5 times that of example 4, and the mineralization rate of antibiotic wastewater in comparative example 2 is 58 percent, which is 0.6 times that of example 4 after degradation for 12 hours.
In the degradation process of the methods of example 4 and comparative example 2, 2mL of liquid was taken every 2 hours, and then the liquid was passed through a 0.22um filter head to remove suspended matter, and the obtained filtrate was tested in a high performance liquid chromatography mass spectrometer to obtain the mass-to-charge ratio of the product in the filtrate, wherein in the test, mobile phase a was methanol, mobile phase B was water/formic acid (volume ratio was 9/1), mobile phase a: mobile phase B =80:20 (volume ratio), the column temperature is 40 ℃, the detection wavelength is 270nm, and the sample injection amount is 10uL.
Through tests, the ciprofloxacin degradation path of example 4 is shown in fig. 5, and as can be seen from the figure, the high performance liquid chromatography mass spectrometry test is performed on the liquid of the antibiotic wastewater of example 4 at different time points, so as to obtain 2 ciprofloxacin degradation paths, wherein the path 1 is that the quinolone ring of ciprofloxacin is attacked by oxygen-containing free radicals, the ethylenediamine and the alcohol group on the piperazine ring are gradually oxidized, and the defluorination is performed on G, so that main products of H, I, carbon dioxide and water are finally generated; the quinolone ring of pathway 2, ciprofloxacin, is attacked by oxygen-containing radicals, the piperazine ring is cleaved, and by decarbonylation of E, the major products are ultimately formed as F, carbon dioxide and water.
In addition, G and E were tested to be two of the major final degradation products produced in comparative example 2 (the remaining major final degradation products were carbon dioxide and water).
Example 4 and comparative example 2 toxicity comparison of products degrading antibiotic wastewater: the chemical formulas of the intermediate product and the final product for degrading the ciprofloxacin wastewater in the example 4 and the comparative example 2 are input into EPI software, and the acute toxicity and the chronic toxicity of the three nutrition levels of the fishes, the daphnia and the green algae are calculated and shown in figure 6, and the acute toxicity to the fishes and the daphnia is LC 50 Acute toxicity to green algae is EC 50 The acute toxicity of ciprofloxacin to fish, daphnia and green algae is 13131.42, 1240.43 and 1621.63mg/L respectively, and the chronic toxicity (ChVs) of ciprofloxacin to fish, daphnia and green algae is 1553.59, 81.27 and 455.22mg/L respectively, which indicates that ciprofloxacin is harmless to aquatic organisms.
For both the chronic and acute toxicity of the intermediates and final products, most chemical formulas, except G, are not harmful to 3 aquatic organisms. All products in the 2 degradation pathways had LC50 against fish and ChVs against daphnia greater than 100.0 and 10.0mg/L, respectively, indicating that these intermediates were not acutely toxic to fish and not chronically toxic to daphnia. The main final degradation product G of comparative example 2 is harmful to both fish and water fleas and has chronic toxicity to green algae. While example 4 degrades the final degradation products of ciprofloxacin, H, I and F, are not chronically and acutely toxic to fish, daphnia and green algae. After a sufficient reaction time, these intermediates can be decomposed into carbon dioxide and water by active species and microorganisms.
The above description of the invention is given by way of example only, and it is to be understood that any simple modifications, adaptations or equivalent replacements which can be carried out by a person skilled in the art without expending any inventive effort, fall within the scope of protection of the invention, without departing from the core of the invention.
Claims (10)
1. An internal circulating fluidized bed-photogeneration direct coupled reactor, comprising: a photobioreactor and one or more magnetic rods (1) arranged around the photobioreactor;
the photobioreactor includes: the device comprises a first barrel (2), a second barrel (3) and an aeration disc (5), wherein the first barrel (2) is a cylindrical cavity with an open top surface, and the second barrel (3) is a cylindrical cavity with an open top surface and an open bottom surface; the aeration disc (5) is fixedly arranged on the inner wall of the bottom end of the first barrel (2), and the second barrel (3) is positioned in the first barrel (2) and is fixedly arranged on the aeration disc (5) through a hollow bracket (6);
install baffle (7) of a round platform shape on the bottom of fretwork support (6), baffle (7) are from last convergent down, fretwork support (6) are located the center department of baffle (7), the top edge of baffle (7) and the inner wall connection of first cask (2), the bottom edge and the fretwork support (6) of baffle (7) are connected for in the hollow out construction that gets into fretwork support (6) with the rivers guide of downward flow between first cask (2) and second cask (3).
2. The internal circulating fluidized bed-photogeneration direct coupled reactor of claim 1, further comprising: and the aeration pump (8) is connected with the aeration disc (5).
3. The internally circulating fluidized bed-photogeneration direct coupled reactor of claim 2, characterized in that a gas flow meter (9) is installed on the piping between the aeration disc (5) and the aeration pump (8).
4. The internal circulating fluidized bed-photogeneration direct coupling reactor according to claim 1, wherein the area ratio of the cross sections of the first barrel (2) and the second barrel (3) is (3-3.5): 1.
5. The internal circulating fluidized bed-photogeneration direct coupling reactor as claimed in claim 1, wherein the ratio of the outer diameter to the height of the first barrel (2) is 1 (3-5).
6. The internal circulating fluidized bed-photogeneration direct coupling reactor as claimed in claim 1, wherein the ratio of the external diameter to the height of the second barrel (3) is 1 (3-5).
7. The internal circulating fluidized bed-photogeneration direct coupling reactor according to claim 1, wherein when the number of the magnetic rods (1) is multiple, the magnetic rods (1) are arranged along the circumferential direction with the axis of the first barrel (2) as the center.
8. The internal circulating fluidized bed-photogeneration direct coupling reactor according to claim 1, wherein the first barrel (2) and the second barrel (3) are both made of transparent materials, and a light source (4) is arranged around the photobioreactor.
9. The internal circulating fluidized bed-photogeneration direct coupling reactor according to claim 8, characterized in that the light source (4) applies visible light with the illumination intensity of 40mW/cm or more 2 。
10. The internal circulating fluidized bed-photogeneration direct coupling reactor according to claim 1, characterized in that the magnetic bar (1) has a magnetic field strength of 10-50 mT formed in the photobioreactor.
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