Method for water treatment with adsorbent renewal to target intermediate age

Abstract

The invention relates to a method for treating a fluid, in particular water, the method further comprising a renewal step (40) for restoring the adsorptive capacity of an adsorption bed (22), the step comprising: extracting (42) a sample of adsorbent from the adsorption bed (22); determining (44) a target average age of the extracted sample of adsorbent, in particular by regenerating at least a portion of the extracted sample of adsorbent, at which target average age the extracted adsorbent has a real abatement of pollutants corresponding to a predefined abatement target, regenerating (46) the adsorption bed (22) to the predefined target average age. The invention can improve the treatment of a fluid by adsorption, in particular taking into account new pollutants. The invention also relates to a device for treating according to the proposed method.

Description

[0001] Technical Field of the Invention

[0002] This invention relates to a method for treating fluids (particularly water, especially drinking water, and urban or industrial effluents), the method comprising an adsorption step. More specifically, the invention relates to an adsorbent renewal step, and the intermediate age of the mixed adsorbent is determined according to emission reduction targets. Background Technology

[0003] For fluid treatment, especially for drinking water production or effluent treatment, it can be recommended to reduce the amount of organic pollutants contained in the raw water or effluent through an adsorption step of the substance.

[0004] The increasing load of organic pollutants (natural organic matter and micropollutants of anthropogenic or natural origin) observed in resources has led manufacturers of drinking water and effluent purifiers to retrofit their treatment facilities that are no longer meeting quality targets. This increasing organic pollutant load also necessitates the design of new treatment units by drinking water producers. Finally, effluent purifiers (whether for industrial or tertiary sources before discharge into the natural environment, or for effluent intended for safe drinking (e.g., wastewater)) can also benefit from treatments that take into account higher organic pollutant levels. Consideration of this major pollution caused by organic pollutants can specifically include adding refining facilities during the design or retrofit phase, particularly using activated carbon, such as for filtration and / or adsorption, especially filtration and / or adsorption on granular activated carbon (GAC) beds.

[0005] For example, as known from document FR3003477, activated carbon filters or activated carbon reactors are used to retain organic matter or other natural or man-made pollutants. Document FR3003477 specifically proposes the use of upward flow of granular activated carbon beds without significant expansion, and a washing stage using filters formed from activated carbon beds. Washing is achieved through significant expansion of the bed. Document FR3003477 also proposes a periodic renewal stage for the activated carbon bed to update its adsorption capacity.

[0006] In this field of water treatment, consideration of the emergence of synthetically sourced organic micropollutants still needs improvement.

[0007] In particular, some of these emerging pollutants are almost non-adsorbable, regardless of whether they are in small molecule, polar, or hydrophilic form. They are primarily pesticide metabolites and can therefore be found downstream of adsorption steps (e.g., using granular activated carbon). If these pollutants are specifically regulated, or in any case represent a foreseeable risk associated with emerging pollutants that are not yet regulated, the levels of these emerging pollutants after treatment may exceed regulatory limits.

[0008] However, purification facilities that use activated carbon (even those that are regularly updated) are based on some traditional pollutants, rather than being designed to accommodate these emerging pollutants that are almost impossible to adsorb.

[0009] Therefore, there is a need to improve the treatment of fluids (such as water) through adsorption, especially to take into account these new, almost non-adsorbable pollutants. Summary of the Invention

[0010] More specifically, the present invention proposes a method for treating fluids (particularly water such as surface water or groundwater, and even effluents), the method comprising the step of adsorbing contaminants contained in the fluid to be treated through an adsorption bed, the method further comprising a renewal step of restoring the adsorption capacity of the adsorption bed, the renewal step comprising:

[0011] - Extract the adsorbent sample from the adsorption bed;

[0012] - Determine the target average age of the extracted adsorbent sample, in particular by regenerating at least a portion of the extracted adsorbent sample, at which the extracted adsorbent exhibits actual pollutant emission reductions corresponding to predetermined emission reduction targets.

[0013] - To regenerate the adsorption bed to the determined target average age.

[0014] According to a preferred embodiment, the present invention includes one or more of the following features:

[0015] - The update process can be triggered periodically at a predetermined update frequency;

[0016] - The update step can be triggered after the detection step of the quality defects of the fluid to be treated downstream of the adsorption step, preferably the detection step includes detecting quality defects by comparing the amount or level of contaminants between the upstream and downstream of the adsorption step.

[0017] - Detection of quality defects is performed during the treatment of the liquid to be treated. Preferably, the detection of quality defects is based on a measurement method selected from at least one of the following: chromatography, mass spectrometry, and fluorescence spectroscopy.

[0018] - The extraction of the adsorbent is carried out during the treatment stop phase of the fluid to be treated, preferably during the adsorbent washing phase, and more preferably during the adsorbent washing phase by injecting air.

[0019] - The extraction of the adsorbent is carried out by sampling at one or more points on the adsorption bed during the treatment of the fluid to be treated;

[0020] - When the target average age of the extracted adsorbent sample is determined, the actual emission reduction of pollutants is determined by sampling the fluid to be treated downstream of the adsorption step. Preferably, the fluid to be treated sampled downstream of the adsorption step is doped before the actual emission reduction of pollutants is determined.

[0021] - The target average age of the adsorbent sample is determined by measuring the actual emission reduction of pollutants in a mixture of young adsorbent and at least a portion of the adsorbent sample extracted from the adsorbent bed, and the adsorbent bed is regenerated to the determined average age by replacing the adsorbent bed with at least a portion of young adsorbent until the determined target average age of the adsorbent bed is obtained.

[0022] - The target average age of the adsorbent sample is determined by measuring the pollutant emission reduction in the adsorbent sub-samples obtained by mixing the extracted adsorbent with young adsorbent in different proportions. The combination of sub-samples has an intermediate average age range between the age of the extracted adsorbent and the age of the young adsorbent. The average age of the sub-samples shows the actual pollutant emission reduction that best corresponds to the predetermined emission reduction target of the target average age.

[0023] - The number of intermediate average ages of the adsorbent subsamples is 2 to 10, preferably 3 to 5, and the intermediate ages are preferably evenly distributed between the age of the extracted adsorbent and the age of the young adsorbent.

[0024] - The pollutant emission reduction of the adsorbent mixture is measured by short-bed adsorbent measurement, preferably on a bed with a volume of less than or equal to 100 mL, more preferably less than or equal to 50 mL, and even more preferably less than or equal to 20 mL.

[0025] - When determining the target average age of the extracted adsorbent sample, determine the actual emission reduction of at least one pollutant selected from the group consisting of: desethylhydroxyatrazine, metaldehyde, aminotriazole, metazachlorine, metazachlorine ESA, metalochlorine, metalochlorine ESA, desethylatrazine, chlortoluron, atrazine, terbuthylazine;

[0026] - The predetermined emission reduction target is defined as the minimum emission reduction value of each pollutant concentration in a group of pollutants to be tested. The minimum emission reduction value of each pollutant is preferably 50% to 90%, more preferably 60% to 80% or 70% to 80%. The minimum emission reduction value is optionally the same for each pollutant in the group of pollutants to be tested.

[0027] - The adsorption bed comprises granular activated carbon, and the adsorption step is carried out by passing the fluid to be treated, particularly water, in an upflow manner through the adsorption bed. The method preferably includes:

[0028] ○ At least one filtration / adsorption stage, in which the fluid velocity is low enough to prevent significant expansion of the activated carbon bed, ensuring filtration and adsorption of substances contained in the fluid;

[0029] ○ It also provides at least one expansion stage in which the fluid circulates at a sufficiently high rate to cause significant expansion of the activated carbon bed, after which the activated carbon bed is washed with the fluid.

[0030] A fluid processing apparatus according to the proposed processing method is also proposed, the apparatus comprising:

[0031] - A reactor for adsorbing contaminants contained in a fluid to be treated, wherein the adsorption bed is retained inside the reactor and the reactor is provided with orifices for removing at least a portion of the used adsorbent from the adsorption bed;

[0032] - A mixer that mixes the adsorbent sample extracted from the adsorption bed with young adsorbent;

[0033] - A measurement unit for the actual emission reduction of pollutants from a mixture of young adsorbent and adsorbent extracted from the adsorption bed, wherein the measurement unit is preferably a short-bed adsorbent measurement unit, and the test is preferably carried out on a bed with a volume of less than or equal to 100 mL, more preferably less than or equal to 50 mL, and even more preferably less than or equal to 20 mL.

[0034] Brief description of the attached figures

[0035] [ Figure 1 This image shows one embodiment of a water treatment facility that includes a pollutant adsorption step.

[0036] [ Figure 2 The proposed method is shown in the diagram.

[0037] [ Figure 3 The results are shown by HPLC-HR / MS measurements obtained from water leaving the adsorption step.

[0038] [ Figure 4 The results are shown by HPLC-HR&MS measurements obtained from the decanting water of the feed to the adsorption step.

[0039] [ Figure 5 The results are shown as measurements obtained from the raw water upstream of the decantation step by HPLC-HR&MS.

[0040] [ Figure 6 This shows the measured results of actual pollutant emission reductions for a mixture of subsamples with three intermediate average ages.

[0041] [ Figure 7 This shows the measured results of actual pollutant emission reductions for a mixture of subsamples with five intermediate average ages.

[0042] [ Figure 8 [Showing SBA test machine]

[0043] [ Figure 9 The image shows a bed of granular activated carbon flowing upwards, and illustrates the Carbazur UP method.

[0044] [ Figure 10 The image shows a comparative emission reduction test of 50,000 BVT activated carbon using SBA and Carbazur UP units on a pilot scale.

[0045] [ Figure 11 The image shows a comparative emission reduction test of 80,000 BVT activated carbon in SBA and Carbazur UP units on a pilot scale.

[0046] [ Figure 12 The diagram shows the proposed fluid processing device. Invention Details

[0048] The proposed treatment method aims to remove contaminants from the fluid to be treated. The fluid to be treated can be water, especially water intended for safe drinking, but it can also be urban or industrial effluents (especially lixiviates, which are liquid effluents from waste storage) before being discharged into the natural environment, or effluents intended for safe drinking, such as wastewater from urban effluents, either directly or indirectly.

[0049] In the remainder of this article, the term "contaminant" refers to both organic matter and microcontaminants. Microcontaminants can be defined as undesirable substances that can be detected in the environment at extremely low concentrations (micrograms per liter, or even nanograms per liter). The presence of microcontaminants in water is at least in part due to human activities (industrial methods, agricultural practices, or pharmaceutical or cosmetic residues). Microcontaminants are characterized by their ability to affect organisms at these extremely low concentrations due to their toxicity, persistence, and bioaccumulation, or due to sensory contamination (taste or odor, which is particularly important when treating water intended for safe drinking). The number of microcontaminants is vast (European regulations list over 110,000 molecules) and their variety is immense. This diversity allows for classification based on source, type, or highly differentiated chemical properties. For example, microcontaminants can be of natural origin (such as compounds derived from soil degradation, including geosmin, methylisoborneol-MIB, or bacterial residues), plant origin (such as algal metabolites, including microcystins), animal, or human origin. Micropollutants can be classified by type, such as polar organic compounds abbreviated as POC or organometallic compounds abbreviated as MOC. Micropollutants can have very different chemical properties, for example, detergents, metals, hydrocarbons, pesticides, cosmetics, or pharmaceutical products. Therefore, the proposed fluid treatment method is particularly suitable for pesticide compounds and related metabolites. The method is also particularly suitable for solvents. Furthermore, the method is particularly suitable for pharmaceutical residues or residues from industrial activities. Therefore, all these categories of pollutants or micropollutants receive special attention from the proposed method.

[0050] The proposed fluid treatment method includes an adsorption step for contaminants contained in the fluid to be treated.

[0051] This adsorption step is carried out using an adsorption bed. For example, the adsorbent (or adsorption medium) is activated carbon, particularly granular activated carbon (GAC). The particle size of the granular activated carbon used in the proposed method is, for example, 400 to 1700 μm for at least 85% to 90% of the particles, or preferably 800 to 1200 μm for at least the majority (50%) of the particles. The dimensions shown are the equivalent diameter dimensions of the particles for dry or wet sieving. Granular activated carbon can typically have an iodine value higher than 950 or 1000 mg / g when new. The iodine value refers to the number of milligrams of iodine adsorbed per gram of activated carbon. This value is used to quantify the adsorption capacity of a given adsorption medium. The iodine value can be specifically obtained according to the standard ASTM D4607–14.

[0052] Treatment methods with an adsorption step can correspond to [ Figure 1 The water treatment method shown in the figure. According to the method shown therein:

[0053] - The water 12 to be treated is first sampled at step 10. This water 12 is more broadly referred to as a resource or raw water, for example, taken from a waterway as shown in the figure. It is a typical example of surface water. The resource can also be sampled by drilling, in which case the water is referred to as groundwater. It can also be an effluent from urban sources (such as wastewater, also known as residual municipal wastewater) or an effluent from industrial sources.

[0054] The sampled water can then undergo a pretreatment step (clarification 14) including, for example, a settling tank or flotation unit to achieve separation, such as by coagulation to retain particulate or colloidal matter, optionally followed by filtration, particularly sand filtration as shown in the figure. The type of pretreatment can depend on the source of the fluid to be treated. If the resource to be treated is groundwater, this pretreatment step can be particularly avoided, as is the case with surface water. For the effluent, it is advantageous to provide pretreatment that also includes biodegradation (e.g., upstream of clarification).

[0055] - Subsequently, water undergoes adsorption step 18 through, for example, reactor 20.

[0056] - Following the adsorption step 18 and the optional filtration step (not shown), the treated water can be distributed in the distribution step 80.

[0057] The proposed method can be based on [ Figure 2 [Illustration]

[0058] The effectiveness of adsorption step 18 is improved by updating step 40. When an adsorbent (such as activated carbon) is used to adsorb pollutants, its adsorption capacity decreases. The media updating step allows the adsorption capacity of the adsorption bed to be restored.

[0059] In the proposed method, the updating step first involves extracting 42 adsorbent samples from the adsorption bed. Like the rest of the bed, this sample exhibits a decrease in adsorption capacity when further used as a pollutant adsorbent. This decrease in capacity is typically addressed using the concept of yield, which itself is often partially equivalent to the sample age. Therefore, the sample age equivalent to its yield can be quantified using the treated bed volume BVT or bed volume BV. The treated bed volume corresponds to the volume of fluid (particularly water) treated by the adsorbent relative to the adsorbent volume. Thus, the higher the adsorbent yield, the more fluid it treats, the more it is consumed or aged, and therefore its adsorption capacity can be considered reduced.

[0060] Based on the extracted and thus aged sample, the update in the proposed method includes determining a regeneration age of 44, at which the adsorbent sample can recover better pollutant reductions. This regeneration age is the target average age to be obtained, such that the adsorbent exhibits more satisfactory pollutant reductions at extraction than the adsorbent sample. The target average age is then defined as the age at which the extracted adsorbent demonstrates actual pollutant reductions corresponding to a pre-set reduction target.

[0061] To determine the average age of the target, at least a portion of the extracted adsorbent sample can be regenerated.

[0062] In a preferred embodiment, the regeneration is, for example, in the form of a mixture of at least a portion of the extracted adsorbent sample and a young adsorbent. "Young adsorbent" refers to an adsorbent younger than the extracted adsorbent sample (without it, simply mixing with the adsorbent will not result in regeneration). Specifically, the young adsorbent can be a fresh adsorbent, i.e., an adsorbent that has not yet been used as an adsorbent after production. The young adsorbent can also be a regenerated adsorbent, particularly activated carbon. A regenerated adsorbent corresponds to an adsorbent that, after being cycled as an adsorbent, has been treated, for example, thermally or chemically to restore its adsorption capacity to near that of a fresh adsorbent. When expressed in BVT, the age of either a fresh or regenerated adsorbent is considered zero. Therefore, regeneration results in a production reset to zero, equivalent to the age described above. Even if regeneration allows for the restoration of adsorption capacity, the regenerated adsorbent may exhibit a more limited adsorption capacity compared to the same adsorbent under new conditions. This more limited adsorption capacity after regeneration can be characterized, for example, by the iodine adsorption number or iodine value. The iodine value is the amount of iodine adsorbed in milligrams per gram of adsorbent and is used to quantify the adsorption capacity of the adsorption medium. For example, for fresh adsorbents, the iodine value can be higher than 950 or 1000 mg / g (for preferred activated carbon). Conversely, for used adsorbents, the iodine value can be lower than 400 mg / g. Regeneration of the adsorbent can result in a recovery of the iodine value, preferably higher than 600 mg / g or more preferably higher than 700 mg / g. Regeneration can be carried out off-site, particularly by the adsorbent supplier through reactivation, for example, heat treatment at above 800°C for adsorbents in the form of activated carbon. The iodine value obtained from such regeneration can be higher than 800 mg / g or even higher than 850 mg / g. Regeneration can also be carried out on-site at the treatment facility by chemical or thermal treatment, particularly at temperatures lower than those for reactivation at 800°C. This on-site regeneration advantageously allows for the recovery of partial adsorption capacity (iodine value of 600 to 800 mg / g) without necessarily requiring more stringent off-site reactivation.

[0063] After the extracted sample is regenerated and in order to determine the target mean age, the proposed method may include measuring pollutant reduction using the subsequently regenerated extracted adsorbent after mixing. This measurement of pollutant reduction can be performed directly by comparing pollutant concentrations upstream and downstream of the fluid treatment with the regenerated extracted adsorbent. Pollutant reduction can also be measured indirectly by measuring pollutant levels using methods such as iodine value measurement (e.g., discussed above) or by chromatography, mass spectrometry, or fluorescence spectroscopy (e.g., discussed below, and therefore particularly by HPLC, HPLC-HR, or HPLC-HR / MS). The pollutant levels thus determined can then be correlated with the actual concentrations of the pollutants, for example, using a predetermined scatter plot of the pollutants.

[0064] Pollutant emission reduction measurements were performed using samples from the regenerated adsorption bed and compared with pre-set emission reduction targets. When the target is achieved, the average age of the regenerated adsorption bed samples will form the target for regeneration of the entire adsorption bed.

[0065] The target average age has been determined, and the proposed method next involves regenerating the adsorption bed for 46 days to the determined target average age.

[0066] Regeneration of an adsorption bed can specifically include replacing at least partially the adsorption bed with younger adsorbent until a defined target average age of the adsorption bed is achieved. The amount of younger adsorbent to be added is calculated, for example, using the arithmetic mean of the amount of used adsorbent remaining in the bed and the amount of younger adsorbent added to the bed. Typically, to ensure that the adsorption bed has a near-constant volume, the amount of remaining used adsorbent should be reduced before adding younger adsorbent.

[0067] In a preferred embodiment, this regeneration, which involves at least partially replacing the adsorption bed with a younger adsorbent, can be carried out, in particular, by mixing the sample with the younger adsorbent to determine the target average age. In this case, the regeneration performed to determine the target average age is a replication of a smaller-scale regeneration of the entire adsorption bed. The advantage of this approach is the ability to have finer control over the adsorption capacity obtained by restoring the regenerated adsorption bed.

[0068] In the proposed method, the pollutant reduction of the regenerated extracted adsorbent is referred to as the "actual pollutant reduction" in order to determine the target average age of the carbon bed renewal. This reduction is called "real" because it is determined based on samples of adsorbent effectively used in the treatment method.

[0069] By determining this actual emission reduction, the proposed method is particularly different from, for example, existing methods that use adsorbents to theoretically assess pollutant emission reduction.

[0070] Some existing methods propose updating the adsorption bed by partially and periodically replacing it with fresh adsorbent, as described in references FR3003477 or FR2874913. In these methods, the theoretically limitable operational value of the treated bed volume, corresponding to a limitable mean age at or after which theoretical pollutant reductions are no longer considered satisfactory, is theoretically determined before industrial implementation. Programming the update cycle ensures theoretically satisfactory pollutant reductions while taking into account the limit determined before the industrial application of the method. For example, theoretical reductions can be determined using a homogeneous surface diffusion model (HSDM), particularly when the adsorbent is activated carbon.

[0071] However, for the same treatment bed volume, two adsorption beds can exhibit different pollutant reduction capacities, depending on the actual concentration variations and the type of pollutant actually treated in each of these adsorption beds. Furthermore, the theoretical adsorption capacity of a treatment bed volume is typically determined on a pollutant-by-pollutant basis, without considering competition between organic matter and micropollutants at adsorption sites or competition between micropollutants themselves (also known as the "cocktail effect"). For example, highly adsorbent micropollutants will tend to saturate adsorption sites before poorly adsorbed micropollutants are adsorbed. Therefore, competition for adsorption sites is particularly significant for compounds with low adsorption affinity (small polar molecules) such as pesticide metabolites. Thus, theoretical determinations of adsorption capacity based on treatment bed volume may overestimate the remaining adsorption capacity of actual adsorption beds.

[0072] Using the method proposed in this paper, a targeted age for emission reduction is obtained based on a sample extracted from an industrially operating adsorption bed. Therefore, this age target is not theoretically fixed by prior testing or modeling of equivalent adsorbent wear (e.g., by measuring the volume of bed treated). Instead, in the proposed method, the sample thus represents the true wear of the adsorption bed and specifically considers the competition between pollutants in the fluid at the adsorption sites actually treated by the adsorbent. Therefore, determining the target mean age from this sample, considering the true history of the adsorption bed, can optimize the regeneration of the adsorption bed.

[0073] Therefore, the proposed fluid treatment method addresses the new limitations posed by novel, difficult-to-adsorb pollutants by controlling the constant aging of the adsorbent to ensure the permanent and effective removal of both targeted and non-targeted pollutants. This can be achieved through continuous adsorbent renewal.

[0074] Adsorbent renewal (especially GAC renewal) can be achieved by extracting a portion of the adsorbent and replacing it with a younger adsorbent. Specifically for GAC, the younger adsorbent can be fresh GAC or regenerated GAC.

[0075] Continuous adsorbent renewal allows for variations in renewal volume and / or frequency, thus adapting to changes in raw water quality. In other words, the proposed method allows for pilot-scale treatment by adjusting the dosage of adsorbent to be renewed through adsorption, based on monitoring the actual saturation state of the adsorbent.

[0076] Therefore, the proposed method allows for better handling of fluids such as water, especially for novel adsorbents that are difficult to adsorb.

[0077] Furthermore, since the samples are extracted from the adsorption bed, the proposed method allows for the determination of the actual emission reductions of the samples, particularly in the fluids to be treated efficiently. Therefore, in a preferred embodiment, when determining the target average age of the extracted adsorbent sample, the actual pollutant emission reduction is determined by collecting samples of the fluid to be treated downstream of the adsorption step. The fluid to be treated is also referred to as the matrix, particularly in the field of wastewater treatment. The proposed method assesses the target average age at which the adsorption bed must regenerate and determines this target average age using samples of both the adsorbent and the fluid; thus, these samples correspond precisely to the future operating conditions of the adsorption bed with the determined target average age.

[0078] The target average age is determined by extracting adsorbent samples because it also takes into account actual matrix samples, allowing for further optimization of adsorbent regeneration.

[0079] This optimization is particularly advantageous compared to existing methods that determine remaining adsorption capacity based on pre-established models with a matrix that is individually sampled during model design and subsequently kept constant. Specifically, EP 3 153 475 proposes a treatment method using a reactor with an activated carbon bed, which controls bed renewal based on a model determined by sampling the matrix even before the reactor begins operation, according to the UV emission reduction yield associated with micropollutant reduction. Using the aforementioned methods, the regeneration rate of the adsorption bed is assessed based on a matrix that no longer corresponds to the matrix actually treated by the adsorbent. Therefore, such methods are no longer applicable to determining actual pollutant reductions in the case of newly emerging pollutants. This lack of adaptation to newly emerging pollutants (such as pesticide metabolites) becomes even more critical when they are almost unadsorbable. In contrast, the method proposed herein ensures that adsorption renewal is adapted to these pollutants that may be found in the matrix by allowing the target average age to be determined based on the current matrix.

[0080] Therefore, the proposed method, particularly by adjusting the adsorption bed renewal through the extraction of adsorbent samples, provides better treatment of fluids such as water, thus taking into account new contaminants, especially those that are almost impossible to adsorb.

[0081] In a preferred embodiment, the renewal step can be triggered when a quality defect is detected in the fluid to be treated. Therefore, the proposed method may include a step of detecting a quality defect in the fluid to be treated, subsequently triggering the renewal step. This step can be performed downstream of the adsorption step. This downstream detection localization allows determination of whether “breakthrough” has occurred in the adsorption bed. The terms bed breakthrough or filter breakthrough are used. Particularly in the water treatment field, filter breakthrough is said to occur when a filter allows contaminants or elements that the filter should retain to pass through. In other words, it is proposed to renew the adsorbent (e.g., granular activated carbon) by monitoring the quality parameters of the fluid to be treated (e.g., water) at the outlet of the adsorption filter. When a limiting value is reached, the renewal of the adsorption bed is triggered.

[0082] Regarding the detection of quality defects, this trigger allows for better consideration of novel contaminants that are virtually non-adsorbable. Quality defect detection of relatively targeted (or predetermined) contaminants can be achieved. In this case, the detection step is specifically aimed at some predetermined contaminants to be monitored. However, this detection step can also be implemented relative to non-targeted contaminants. The fluid to be treated (especially water) can be measured to allow the determination of the presence of impurities or contaminants without prior determination of the contaminant type.

[0083] The non-targeted detection of contaminants in water (or the fluid to be treated) can be specifically achieved by at least one of the measurement methods, including chromatography, mass spectrometry, and fluorescence spectroscopy (also known as 3D fluorescence). In a particularly preferred embodiment, the measurement method can be high-performance liquid chromatography (HPLC), especially high-resolution high-performance liquid chromatography (abbreviated as HPLC-HR), and particularly further combined with mass spectrometry (MS). [Figure 1] Figure 3 ]、[ Figure 4 ]、[ Figure 5 This corresponds to a graph of the measurement results obtained by the latter measurement method, HPLC-HR&MS. Each point in the graph corresponds to a molecule or molecule type that reacted in the chromatography. Therefore, each point corresponds to a mark of a contaminant or contaminant type. Metaphorically, the graph is also called a mark. For each point in the graph, these graphs represent the retention time of the molecule corresponding to that point along the X-axis, measured in minutes. Along the Y-axis, these graphs give the mass-to-charge ratio of the molecule corresponding to the point. This value is measured in m / z (i.e., mass per ion charge). Finally, for each point, these graphs represent the intensity of the chromatographic response, with black dots indicating high intensity, gray dots indicating medium intensity, and white dots surrounded by black circles indicating low intensity. The intensity of the chromatographic response is related to the concentration of the impurity or contaminant represented by that point.

[0084] Attached Figures Figure 3 The results of measurements of the fluid downstream of the treatment step via fluid adsorption are particularly shown, for example [ Figure 1Point 33 is shown in the figure. This graph can demonstrate the presence of impurities in the fluid being treated, particularly contaminants in water. This demonstration is not specific: when a point appears on the graph, it corresponds to the presence of an impurity or contaminant, without necessarily confirming the exact type of the contaminant or seeking specialized testing for it. Therefore, if [ Figure 3 If a point not present in previous measurements is observed at time t, the presence of a contaminant corresponding to that point might suggest penetration of the adsorption bed, suggesting that the contaminant is not specifically targeted. However, the non-targeted measurement method can specifically detect the penetration of newly emerging contaminants such as pesticide residues, whereas targeted measurement methods are typically used for more common contaminants.

[0085] Especially as shown in the attached image [ Figure 3 ]、[ Figure 4 ]、[ Figure 5 As shown in the attached figure, in a preferred embodiment, quality defects are detected by comparing the mass of the fluid to be treated between the upstream and downstream sections of the adsorption step. Figure 3 ]、[ Figure 4 ]and[ Figure 5 The measurements in [the image] were taken on the same treatment line from samples taken from the Seine River:

[0086] -[ Figure 4 The image shows the measurement results obtained after the first fluid treatment step, in this case, after the decantation step of the fluid to be treated, for example, in […]. Figure 1 Point 34 as shown in the image;

[0087] -[ Figure 5 The image shows the measurement results obtained at the sampling point of the fluid to be processed, for example, in […]. Figure 1 Point 35 as shown in the image;

[0088] In particular, based on the methods used to preserve these figures, the amount of contaminants upstream and downstream of the adsorption step can be compared. If a point appearing downstream of adsorption is unusually retained upstream, the adsorbent no longer retains that contaminant. Therefore, it may be advantageous to trigger the renewal of the adsorption bed. Similarly, if a point appears downstream of the adsorption step but is not present upstream, then the adsorption bed has released the contaminant it previously adsorbed. Again, here, it is advantageous to trigger the renewal of the adsorption bed. Alternatively or additionally, particularly by mass spectrometry or other measurement methods, it is also conceivable to compare the contaminant levels upstream and downstream of the adsorption step. [Figure 1] Figure 3 ]、[ Figure 4 ]、[ Figure 5This specifically demonstrates that the concentration of impurities is moderate or high based on the intensity of the displayed point. Based on this information about contaminant concentration or level, it may be advantageous to trigger bed renewal, particularly if the point intensity changes from low or moderate to high. In this preferred embodiment, where the mass of the fluid to be treated is compared between upstream and downstream of the adsorption step, the measurement method can be performed alternately upstream and downstream using a single analytical sensor shared by measurements at both points.

[0089] Preferably, the detection of quality defects in the fluid to be treated, whether upstream or downstream of adsorption, can be performed online during the treatment process. Monitoring can then be ensured by an online analyzer, particularly one based on fluorescence or chromatography, regardless of whether these methods are targeted or non-targeted (imprinting), as described above. This online monitoring allows for the detection of quality defects while the fluid is being treated, thereby optimizing the volume of the treated fluid. This online detection step can be performed continuously or nearly continuously, with the time between detections being shorter than, for example, the transit time of bed volume into the adsorbent bed. Furthermore, this detection step can also be performed upon operator request. In any case, it is not necessarily necessary to interrupt the production of the treated fluid in order to determine whether quality defects have become apparent and whether a bed renewal step must be triggered.

[0090] Alternatively or additionally, the renewal step can be triggered periodically at a predetermined renewal frequency. The renewal time can then be defined to limit the risk of adsorption bed breakthrough and to regenerate the adsorbent according to the proposed method. The nominal pollutant reduction can then be defined according to a pre-set emission reduction target based on the proposed method, for which it is determined that the remaining pollutant reduction after the renewal time is sufficient to meet the quality standards required by the operator.

[0091] Preferably, the pre-set emission reduction target is defined as the minimum emission reduction value for the concentration of each pollutant in a group of pollutants to be tested. This pollutant emission reduction is typically expressed as a percentage of the amount of pollutant retained relative to the amount of pollutant entering the group. Therefore, it is a relative value. Nevertheless, this relative value allows for reaching a threshold for adjusting the concentration of pollutants after treatment relative to a predictable concentration of entering pollutants. For each pollutant, the minimum emission reduction value can be 50% to 90%, preferably 60% to 80%, or even 70% to 80%. The minimum emission reduction value can be defined differently for different pollutants, or it can be defined the same for all pollutants to be tested. Specifically, in this embodiment, and more generally in the proposed method, the actual emission reduction of each pollutant in the group of pollutants to be tested can be determined individually.

[0092] The specific pollutants selected to determine actual emission reductions can be chosen from: desethylhydroxyatrazine, metaldehyde, aminotriazole, metazachlorine, metalochlorine, desethylatrazine, chlortoluron, atrazine, and terbuthylazine. If detection procedures for target pollutants are specified, particularly downstream of the adsorption bed, it is especially advantageous that pollutants identified as contributing to quality defects be integrated into the pollutant group used to determine actual emission reductions.

[0093] As mentioned above, in order to determine the actual emission reductions from the extracted regenerated adsorbent sample, it is preferable that the sample of the fluid to be treated should be obtained, particularly downstream of the adsorption step. More preferably, the fluid is doped with the pollutant as soon as it is sampled, before determining the actual emission reductions. This doping can shorten the time required to determine the actual emission reductions. For example, doping can be achieved by increasing the concentration of the pollutant under consideration in the sampled fluid. Typically, desethylhydroxyatrazine, metaldehyde, aminotriazole, metazachlorine, or metalochlorine can each be doped by increasing their concentration by 1 to 10 μg / L, preferably 1 to 2 μg / L, more preferably 1 to 2 μg / L. Similarly, desethylatrazine, chlortoluron, atrazine, and terbuthylazine can each be doped by increasing their concentration by 1 to 10 μg / L, preferably 9 to 10 μg / L.

[0094] As previously mentioned, the target average age of the adsorbent sample is preferably determined by measuring the actual emission reduction of pollutants in the adsorbent mixture, whether the sample uses a fluid to be treated or not, and whether the sampling fluid is doped or not. This adsorbent mixture corresponds to a mixture of young adsorbent (e.g., fresh adsorbent or particularly regenerated adsorbent) and at least a portion of the adsorbent sample extracted from the adsorption bed.

[0095] In a further preferred embodiment, actual emission reductions are measured on multiple subsamples obtained from the extracted adsorbent sample. These subsamples are obtained by mixing the extracted adsorbent with young adsorbent. Mixing is carried out in variable proportions to obtain subsamples, resulting in a combination of subsamples with a defined average age range. This average age range allows the intermediate age distribution to fall between the age of the extracted adsorbent and the age of the young adsorbent. This intermediate average age range allows for as many actual emission reduction measurements as possible, ensuring the closest possible age to the optimal age at which the extracted adsorbent should regenerate to exhibit actual emission reductions best corresponding to the predefined emission reduction target. Among these subsamples, one subsample with the most significant actual pollutant emission reductions that best meets the predefined emission reduction target is then used to determine the target average age of the proposed method. In particular, the target average age can be taken as the age of the mixture forming the subsample. Alternatively, the target average age can be taken as the average or extrapolated value of the age of the subsample mixture and the age of the immediately following subsample over an intermediate age range. For the determination of the target average age, the adsorption bed is regenerated until the target average age is obtained.

[0096] The number of intermediate ages in the subsample group can be 2 to 10, or preferably 3 to 5. A reasonable number of subsamples ensures an estimate of the target average age that is sufficiently close to the optimal age. Considering the number of subsamples, it is preferable that the intermediate ages be evenly distributed between the extracted adsorbent age and the age of younger adsorbents. This even distribution increases the likelihood of reaching the target average age, which is close to the optimal age for regeneration of the extracted adsorbent.

[0097] Attached Figures Figure 6 ]and[ Figure 7 The study provides measurements of actual pollutant emission reductions for mixed subsamples with 3 to 5 intermediate average ages. Figure 6 The results were obtained by measuring actual emission reductions based on adsorbent samples, in which the age of the granular activated carbon was 45,000 years, measured by bed volume treated, and the Seine water sampled near Mont Valérien was treated with 10 μg / l of pollutants. Figure 7The emissions reductions were obtained by measuring actual emissions reductions based on adsorbent samples, in which the age of the granular activated carbon was 140,000 years, based on the treated bed volume, and the Seine water sampled at Morsang sur Seine near the Seine was treated with 10 μg / L of co-pollutant. Emission reduction measurements were performed on water samples collected downstream of the adsorption step. These graphs show the reconstructed mean age of the subsamples, expressed in BVT, along the X-axis. Along the first Y-axis, these graphs show the fraction of adsorbent from the extracted samples and the fraction of fresh adsorbent, respectively. Along the second Y-axis, these graphs show the relationship between the actual emissions reductions measured for the subsamples and the pollutants tested.

[0098] In particular, the last column of these figures gives the actual emission reductions for each pollutant in the adsorption bed represented by the extracted sample before any regeneration. In this case, in [ Figure 6 In the [ ], for the sample extracted at 45000 BVT, the pollutant reduction from worst to best can be seen as follows: metaldehyde (dashed line), metazachlorine (mixed dashed line), metalochlorine (at the same point as desethylhydroxyatrazine) (both represented by thin solid lines), but before the common point, the reduction level of desethylhydroxyatrazine is higher than that of metalochlorine), and finally aminotriazole (thick solid line). Figure 7 In the figure, for the sample extracted at 140,000 BVT, the pollutant reduction from worst to best is as follows: metaldehyde (dashed line), aminotriazole (thin solid line), metazachlorine (mixed dashed line), and finally desethylhydroxyatrazine (thick solid line), which has the same curve as metalochlorine.

[0099] First, these two figures clearly demonstrate that, based on the actual history of the adsorption bed (in this case, granular activated carbon), for a given set of contaminants, breakthrough does not always occur at the same time and in the same order. In particular, in [ Figure 6 In [ ], aminotriazole did not cause bed penetration, while in [ Figure 7 In this study, the bed breakthrough of aminotriazole exceeded that of metazachlorine. This observation confirms the advantage of performing actual emission reduction measurements on the fluid sample obtained downstream of the adsorption step, as previously indicated.

[0100] These figures also demonstrate the advantage of the median regeneration age of the reconstructed (or simulated) adsorbent. In these figures, the adsorbent was regenerated using a mixture of young adsorbents with varying proportions. The reconstructed median age range optimally determines the reconstruction age at which emission reductions for all tested pollutants can be considered to meet pre-set emission reduction targets. In this case, if a 90% emission reduction for all these pollutants is sought, an adsorbent bed of 45,000 BVT can be regenerated to 15,000 BVT by replacing nearly 70% of the adsorbent bed with fresh adsorbent. Figure 6 For the same emission reduction target, by replacing nearly 30% of the adsorbent in the adsorption bed with fresh adsorbent, an adsorption bed with a capacity of 140,000 BVT can be regenerated to 100,000 BVT. Figure 7 ].

[0101] In a particularly advantageous embodiment, pollutant emission reduction of the adsorbent mixture is measured by a short-bed adsorbent test (SBA).

[0102] [ Figure 8 The image shows an SBA testing machine 60, which has eight filter cartridges 62, each filled with an adsorbent containing extracted samples and mixed with young adsorbent in different proportions.

[0103] The advantage of these SBA tests in the proposed methods is that they allow for testing with very little adsorbent to be extracted and provide results with relatively short contact times, such as approximately 6 minutes, corresponding to the contact time in the adsorbent bed from which the adsorbent sample is extracted. The contact time for the SBA test or the adsorbent bed from which the sample is extracted can range from 4 to 10 minutes, or from 5 to 20 minutes, with a maximum of 30 minutes, depending on operating conditions. These contact times are compatible with SBA beds with volumes less than or equal to 100 mL, 50 mL, or even 20 mL. With or without the SBA test, the adsorbent dose in the extracted sample can be less than 2 L, preferably less than 1 L, or even less than 200 mL or 100 mL.

[0104] In one embodiment of the proposed method, with or without the use of subsamples, particularly SBA subsamples, adsorbent extraction is performed during the treatment cessation phase of the fluid to be treated. Then, for this extraction to proceed, the cessation phase preferably corresponds to a cessation phase that serves a purpose other than the separate extraction of the adsorbent sample, such as an adsorbent washing phase, particularly an adsorbent washing phase by injecting air. Alternatively, adsorbent extraction is performed during the treatment of the fluid to be treated. Sampling is then performed at one or more points on the adsorbent bed to obtain adsorbent samples representative of the wear and tear of the entire adsorbent bed.

[0105] In a preferred embodiment, the proposed method is implemented as part of an upflow treatment method with activated carbon (hereinafter referred to as Carbazur UP), as disclosed in previously cited and referenced document FR 3003477. Specifically, the proposed treatment method can be a method of upward flow of fluid through a bed of granular activated carbon, the method comprising:

[0106] - At least one filtration / adsorption stage in which the fluid velocity is low enough to prevent significant expansion of the activated carbon bed, ensuring filtration and adsorption of substances contained in the fluid;

[0107] - and providing at least one expansion stage in which the fluid is circulated at a sufficiently high rate to cause significant expansion of the activated carbon bed, after which the activated carbon bed is washed with the fluid.

[0108] The specific implementation method is shown in [ Figure 9 ]middle,[ Figure 9 This shows a bed of granular activated carbon moving in an upward flow. Figure 9 A reactor 20 comprising a bed of granular activated carbon 22 is specifically shown. The bed 22 operates via an upflow of water 28 to be treated. The reactor 20 may include an inlet 24 and an outlet 26 for renewing the activated carbon bed. The reactor 20 may include an air inlet 34 to allow washing of the bed with air instead of just fluid. The reactor 20 may be adjacent to a filter 70. The filter 70 may include a downflow bed 72 of activated carbon, as shown. After filtration through the filter 70, the water is discharged through an outlet 33.

[0109] The representativeness of using the SBA test to determine actual pollutant emission reductions was evaluated by comparing it with the Carbazur UP method described above. Figures

[10] and [ Figure 11 The accompanying figure shows a pilot-scale comparative test between pollutant reduction measurements using SBA via adsorbents and pollutant reduction measurements using Carbazur UP units. These pilot-scale Carbazur UP units correspond to laboratory models designed to be representative of the same line of operation at industrial scale. [Figure 1] Figure 10 ]and[ Figure 11 The X-axis shows the different test pollutants, and the Y-axis shows the emission reduction rates of these pollutants. For each test pollutant, the left bar represents the emission reduction measured in pilot tests, and the right bar represents the emission reduction measured through SBA testing.

[0110] Attached Figures Figure 10The SBA and Carbazur UP tests were compared for granular activated carbon aged 50,000 BVT using Seine River water and a contact time of 6 minutes (contact time is empty bed contact time - EBCT). The contaminants tested, from left to right, were: desethylhydroxyatrazine, aminotriazole, metazachlorine, and metalochlorine.

[0111] Attached Figures Figure 11 The SBA and Carbazur UP tests were compared for granular activated carbon aged 80,000 BVT using Seine River water and an EBCT contact time of 10 minutes. The contaminants tested, from left to right, were: desethylhydroxyatrazine, aminotriazole, metazachlorine, metalochlorine, metazachlorine ESA, and metalochlorine ESA (ESA is an abbreviation for ethyl sulfonic acid).

[0112] like[ Figure 10 ]and[ Figure 11 As shown, the emission reduction levels measured by these two methods are largely comparable. The SBA test, implemented innovatively, is a method for characterizing the saturation level of a specific compound and represents a pilot. The design and scale of the pilot take into account relevant factors of the industrial unit (bed height, contact time, etc.). Therefore, the SBA test represents a pilot and thus also represents the industrial unit.

[0113] A fluid treatment apparatus for implementing the above method on all variants is also proposed, the apparatus comprising measuring the actual emission reduction of pollutants in a mixture of young adsorbent and adsorbent extracted from the adsorption bed. Therefore, the proposed apparatus includes a measurement unit. The proposed apparatus also includes an adsorption reactor. The reactor contains an adsorption bed in which the adsorption bed is held. The reactor allows for the adsorption of pollutants contained in the fluid to be treated.

[0114] The reactor was seen previously [ Figure 9 [or as detailed below] Figure 12 ] will be explained in detail.

[0115] like[ Figure 12As shown, the proposed apparatus 90 includes a reactor 20 with orifices 26 for at least partial discharge of used adsorbent from an adsorption bed 22. As shown, the adsorption bed 22 is capable of operating with an upflow of the fluid to be treated 28. In the proposed apparatus, a sample of adsorbent is directed to a mixer 92. Therefore, the proposed apparatus may include the mixer 92. This mixer ensures that the used adsorbent sample is mixed with young adsorbent (e.g., a reservoir 94 derived from young adsorbent). The proposed apparatus may include the reservoir 94. The mixer 92 may allow obtaining the intermediate age of a single sample, or a subsample combination with an intermediate average age ranging between the extracted adsorbent age and the young adsorbent age. In the proposed apparatus, whether forming a single sample or a subsample combination, the resulting mixture is directed to a measurement unit 96. This measurement unit 96 measures the actual pollutant reduction in the mixture of young adsorbent and adsorbent extracted from the adsorption bed.

[0116] As described above, the measuring unit 96 is preferably a short bed adsorber (SBA), and the test is preferably performed with a bed with a volume of less than or equal to 100 mL, more preferably less than or equal to 50 mL, and even more preferably less than or equal to 20 mL.

[0117] As previously described, the measuring unit 96 preferably allows determination of the target average age of the extracted adsorbent sample relative to a group of contaminants selected from the following: desethylhydroxyatrazine, metaldehyde, aminotriazole, metazachlorine, metazachlorine ESA, metalochlorine, metalochlorine ESA, desethylatrazine, chlortoluron, atrazine, and terbuthylazine. Optionally, the contaminant group also includes contaminants identified as contributing to quality defects in the fluid to be treated that trigger the renewal step.

[0118] Finally, in a particularly preferred embodiment, the measuring unit 96 also receives the fluid processed by the reactor 20, thereby obtaining the measurement values ​​as close as possible to the future conditions of the adsorption bed.

[0119] Obviously, the present invention is not limited to the examples and embodiments described and illustrated, but can be modified in many ways.

[0120] Specifically, in one variant, the method for detecting water quality defects is through fluorescence 3D analysis, allowing for online monitoring of water quality between entry and exit from the adsorbent. This method is particularly suitable for effluents loaded with contaminants or resources representing algal blooms. Therefore, this method is advantageous for industrial effluents or leachates formed from liquid effluents from waste storage.

[0121] In another variation, the adsorbent is not limited to granular activated carbon; it can also be resin, clay, zeolite for capturing metals, or other specific micro-pollutants. These other adsorbents preferably have a millimeter size.

[0122] The adsorbent can also be micro-particulate activated carbon, i.e., having a finer particle size than granular carbon. For example, the adsorbent can be micro-particulate activated carbon with a particle size of 300 μm to 800 μm for at least 85% to 90% of the particles, or preferably 400 to 600 μm for at least the majority (50%) of the particles. The dimensions shown are the equivalent diameter dimensions of the particles for dry or wet sieving.

[0123] In other variations, the proposed method is achieved by employing an adsorption step directly on the raw water, thus being particularly effective in the absence of pre-decantation or flotation.

[0124] Furthermore, the proposed method is applicable to a wide range of fluid velocities. Fluid velocities are selected from, for example, 2 m / h to 20 m / h, preferably 5 m / h to 20 m / h, more preferably 10 m / h to 20 m / h, or 5 m / h to 15 m / h. The fluid velocity can be selected, in particular, based on the water temperature.

Claims

1. A method for treating fluids, characterized in that, The method includes an adsorption step (18) in which contaminants contained in the fluid to be treated are adsorbed through an adsorption bed (22), and the method further includes a renewal step (40) in which the adsorption capacity of the adsorption bed (22) is restored, the renewal step including: - Extract (42) adsorbent sample from the adsorption bed (22); - The target average age of the extracted adsorbent sample is determined by regenerating at least a portion of the extracted adsorbent sample, at which the extracted adsorbent exhibits actual pollutant emission reductions corresponding to a predetermined emission reduction target, wherein, when determining the target average age of the extracted adsorbent sample, the actual pollutant emission reductions are determined by sampling the fluid to be treated downstream of the adsorption step, and the regeneration is in the form of a mixture of at least a portion of the extracted adsorbent sample and a young adsorbent. - Regenerate the adsorption bed (22) (46) to the determined target average age.

2. The method for treating fluids as described in claim 1, wherein, The update step (40) is triggered periodically at a predetermined update frequency.

3. A method for treating a fluid as described in claim 1 or 2, wherein, The update step (40) is triggered after the detection step of quality defects of the fluid to be treated downstream of the adsorption step (18), the detection step including detecting quality defects by comparing the amount or level of contaminants between the upstream and downstream of the adsorption step.

4. A method for treating fluids as described in claim 3, wherein, The detection of quality defects is performed during the treatment of the liquid to be treated, and the detection of quality defects is based on a measurement method selected from at least one of the following measurement methods: chromatography, mass spectrometry, and fluorescence spectroscopy.

5. A method for treating fluids as described in claim 1, wherein, The adsorbent is extracted during the treatment stop phase of the fluid to be treated.

6. A method for treating a fluid as described in claim 1, wherein, The adsorbent is extracted during the adsorbent washing stage.

7. A method for treating fluids as described in claim 1, wherein, The adsorbent is extracted during the adsorbent washing stage by injecting air.

8. A method for treating fluids as claimed in claim 1, wherein, The adsorbent is extracted by sampling at one or more points on the adsorption bed during the treatment of the fluid to be treated.

9. A method for treating a fluid as claimed in claim 1, wherein, The fluid sampled downstream of the adsorption step is doped before the actual emission reduction of pollutants is determined.

10. A method for treating a fluid as claimed in claim 1, wherein: - Determining the target average age of the adsorbent sample (44) is achieved by measuring the actual emission reduction of pollutants in a mixture of young adsorbent and at least a portion of the adsorbent sample extracted from the adsorption bed, and wherein - The adsorption bed (22) is regenerated (46) to the determined target average age by replacing the adsorption bed at least partially with a young adsorbent until the determined target average age of the adsorption bed (22) is obtained.

11. A method for treating a fluid as described in claim 10, wherein, The target average age of the adsorbent sample (44) is determined by measuring the emission reduction of pollutants in the adsorbent sub-samples obtained by mixing the extracted adsorbent with young adsorbents in different proportions. The combination of sub-samples has an intermediate average age range between the age of the extracted adsorbent and the age of the young adsorbents. The average age of the sub-samples corresponds best to the actual emission reduction of pollutants that best corresponds to the pre-set emission reduction target of the determined target average age.

12. A method for treating a fluid as claimed in claim 11, wherein, The number of intermediate average ages of the adsorbent subsamples ranged from 2 to 10.

13. A method for treating a fluid as claimed in claim 11, wherein, The average age of the adsorbent subsamples ranged from 3 to 5.

14. A method for treating a fluid as described in claim 11, wherein, The intermediate age is evenly distributed between the age of the extracted adsorbent and the age of the young adsorbent.

15. A method for treating a fluid as claimed in any one of claims 10 to 14, wherein, Pollutant emission reduction measurements of adsorbent mixtures are performed using short-bed adsorbents.

16. A method for treating a fluid as described in claim 15, wherein, The test was conducted on a bed with a volume of 100 mL or less.

17. A method for treating a fluid as described in claim 15, wherein, The test was conducted on a bed with a volume of 50 mL or less.

18. A method for treating a fluid as described in claim 15, wherein, The test was conducted on a bed with a volume of 20 mL or less.

19. A method for treating a fluid as claimed in claim 1, wherein, When determining the target average age of the extracted adsorbent sample, determine the actual emission reduction of at least one pollutant selected from the group consisting of: deethylated hydroxyatrazine, polyacetaldehyde, aminotriazole, pyrazole, pyrazole ESA, metal thiocyanate, metal thiocyanate ESA, deethylated atrazine, green meron, atrazine, terbutaline.

20. A method for treating a fluid as described in claim 3, wherein, When determining the target average age of the extracted adsorbent sample, determine the actual emission reduction of at least one pollutant selected from the group consisting of: deethylated hydroxyatrazine, polyacetaldehyde, aminotriazole, pyrazole, pyrazole ESA, metal thiocyanate, metal thiocyanate ESA, deethylated atrazine, green meron, atrazine, terbutaline.

21. A method for treating a fluid as claimed in claim 1, wherein, The predetermined emission reduction target is defined as the minimum emission reduction value of each pollutant concentration in a set of pollutants to be tested. The minimum emission reduction value of each pollutant is 50% to 90%, and the minimum emission reduction value is optionally the same for each pollutant in the set of pollutants to be tested.

22. A method for treating a fluid as described in claim 21, wherein, The minimum emission reduction for each pollutant is 60% to 80%.

23. A method for treating a fluid as described in claim 21, wherein, The minimum emission reduction for each pollutant is 70% to 80%.

24. A method for treating a fluid as claimed in claim 1, wherein, The adsorption bed (22) comprises granular activated carbon, and the adsorption step (18) is carried out by passing the fluid to be treated through the adsorption bed in an upflow manner, the method comprising: - At least one filtration / adsorption stage in which the fluid velocity is low enough to prevent significant expansion of the activated carbon bed, ensuring filtration and adsorption of substances contained in the fluid; - and providing at least one expansion stage in which the fluid is circulated at a sufficiently high rate to cause significant expansion of the activated carbon bed, after which the activated carbon bed is washed with the fluid.

25. An apparatus for treating a fluid according to any one of claims 1-24, characterized in that, The device (90) includes: - A reactor (20) for adsorbing contaminants contained in a fluid to be treated, wherein an adsorption bed (22) is retained in the reactor (20), and the reactor (20) is provided with orifices (26) for removing at least a portion of the used adsorbent from the adsorption bed (22); - A mixer (92) for mixing adsorbent samples extracted from the adsorption bed with young adsorbents. - Measurement unit for actual emission reduction of pollutants from a mixture of young adsorbents and adsorbents extracted from the adsorption bed (96).

26. The apparatus for processing fluids as claimed in claim 25, wherein, The measuring unit (96) is a short-bed adsorbent measuring unit.

27. The apparatus for processing fluids as claimed in claim 26, wherein, The test was conducted on a bed with a volume of 100 mL or less.

28. The apparatus for processing fluids as claimed in claim 26, wherein, The test was conducted on a bed with a volume of 50 mL or less.

29. The apparatus for processing fluids as claimed in claim 26, wherein, The test was conducted on a bed with a volume of 20 mL or less.

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