EP3359492A1 - Verfahren zur entfernung von verunreinigungen aus wasser durch adsorption an aktivkohle - Google Patents
Verfahren zur entfernung von verunreinigungen aus wasser durch adsorption an aktivkohleInfo
- Publication number
- EP3359492A1 EP3359492A1 EP16782030.7A EP16782030A EP3359492A1 EP 3359492 A1 EP3359492 A1 EP 3359492A1 EP 16782030 A EP16782030 A EP 16782030A EP 3359492 A1 EP3359492 A1 EP 3359492A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- activated carbon
- reactor
- treatment
- grain
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 387
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 238000000034 method Methods 0.000 title claims abstract description 46
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 38
- 238000011282 treatment Methods 0.000 claims abstract description 112
- 230000009467 reduction Effects 0.000 claims abstract description 37
- 238000000605 extraction Methods 0.000 claims description 34
- 238000002347 injection Methods 0.000 claims description 32
- 239000007924 injection Substances 0.000 claims description 32
- 239000003245 coal Substances 0.000 claims description 28
- 239000002351 wastewater Substances 0.000 claims description 25
- 238000005406 washing Methods 0.000 claims description 22
- 230000008569 process Effects 0.000 claims description 21
- 229910052799 carbon Inorganic materials 0.000 claims description 17
- 238000002835 absorbance Methods 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 15
- 238000000926 separation method Methods 0.000 claims description 13
- 239000003643 water by type Substances 0.000 claims description 13
- 239000003610 charcoal Substances 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 7
- 238000001033 granulometry Methods 0.000 claims description 5
- 238000011084 recovery Methods 0.000 claims description 4
- 238000011481 absorbance measurement Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000011954 pollution control method Methods 0.000 claims 2
- 230000009194 climbing Effects 0.000 claims 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims 1
- 230000000630 rising effect Effects 0.000 abstract 1
- 238000009826 distribution Methods 0.000 description 13
- 239000010842 industrial wastewater Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 4
- -1 organostanneux Chemical class 0.000 description 4
- 239000000575 pesticide Substances 0.000 description 4
- HEFNNWSXXWATRW-UHFFFAOYSA-N Ibuprofen Chemical compound CC(C)CC1=CC=C(C(C)C(O)=O)C=C1 HEFNNWSXXWATRW-UHFFFAOYSA-N 0.000 description 3
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 3
- 239000012964 benzotriazole Substances 0.000 description 3
- 230000000903 blocking effect Effects 0.000 description 3
- FFGPTBGBLSHEPO-UHFFFAOYSA-N carbamazepine Chemical compound C1=CC2=CC=CC=C2N(C(=O)N)C2=CC=CC=C21 FFGPTBGBLSHEPO-UHFFFAOYSA-N 0.000 description 3
- 229960000623 carbamazepine Drugs 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- DCOPUUMXTXDBNB-UHFFFAOYSA-N diclofenac Chemical compound OC(=O)CC1=CC=CC=C1NC1=C(Cl)C=CC=C1Cl DCOPUUMXTXDBNB-UHFFFAOYSA-N 0.000 description 3
- 229960001259 diclofenac Drugs 0.000 description 3
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 description 3
- 229960003883 furosemide Drugs 0.000 description 3
- 239000004009 herbicide Substances 0.000 description 3
- 229960001680 ibuprofen Drugs 0.000 description 3
- DKYWVDODHFEZIM-UHFFFAOYSA-N ketoprofen Chemical compound OC(=O)C(C)C1=CC=CC(C(=O)C=2C=CC=CC=2)=C1 DKYWVDODHFEZIM-UHFFFAOYSA-N 0.000 description 3
- 229960000991 ketoprofen Drugs 0.000 description 3
- ADIMAYPTOBDMTL-UHFFFAOYSA-N oxazepam Chemical compound C12=CC(Cl)=CC=C2NC(=O)C(O)N=C1C1=CC=CC=C1 ADIMAYPTOBDMTL-UHFFFAOYSA-N 0.000 description 3
- 229960004535 oxazepam Drugs 0.000 description 3
- AQHHHDLHHXJYJD-UHFFFAOYSA-N propranolol Chemical compound C1=CC=C2C(OCC(O)CNC(C)C)=CC=CC2=C1 AQHHHDLHHXJYJD-UHFFFAOYSA-N 0.000 description 3
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- 229960005404 sulfamethoxazole Drugs 0.000 description 3
- JLKIGFTWXXRPMT-UHFFFAOYSA-N sulphamethoxazole Chemical compound O1C(C)=CC(NS(=O)(=O)C=2C=CC(N)=CC=2)=N1 JLKIGFTWXXRPMT-UHFFFAOYSA-N 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 2
- 230000001174 ascending effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000010908 decantation Methods 0.000 description 2
- 239000003651 drinking water Substances 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 125000005498 phthalate group Chemical class 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 238000011144 upstream manufacturing Methods 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 235000012206 bottled water Nutrition 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229940126601 medicinal product Drugs 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 239000004476 plant protection product Substances 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000007420 reactivation Effects 0.000 description 1
- 230000003134 recirculating effect Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/008—Control or steering systems not provided for elsewhere in subclass C02F
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/305—Endocrine disruptive agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/306—Pesticides
Definitions
- the present invention relates to the field of water treatment, particularly wastewater, such as urban and industrial wastewater. More particularly, the present invention relates to a method of water purification by adsorption on activated carbon grain in an upflow treatment reactor and expanded bed.
- the removal of micropollutants by adsorption on activated charcoal grain can be carried out in treatment reactor as described in the patent FR2874913, preferably for the treatment of groundwater and surface low organic pollution.
- treated water discharged into the natural environment must meet increasingly stringent regulatory requirements, in particular it must be controlled that micropollutants are not present beyond certain thresholds.
- Discharges from wastewater treatment plants also impact the quality of the resource for the production of drinking water. It is therefore important to control the quality of the water to drink.
- wastewater is classified into two categories: urban water and industrial water from, for example, the chemical and pharmaceutical industries.
- activated carbon adsorption processes especially granular activated carbon, as described in patent FR2874913.
- Potable water is a third category of water where activated carbon adsorption treatments are also very suitable.
- the amount of activated carbon to be injected into the reactors depends on the concentration of micropollutants to be treated.
- the volume or mass of granular activated carbon employed in the treatment reactor is optimal to obtain effective percentage of abatement of organic micropollutants from water.
- a method for controlling and / or monitoring the reduction of micropollutants in water in order to regulate the concentrations of activated carbon necessary for the removal of micropollutants in wastewater is described in particular in the patent application FR3009789. Nevertheless, this method does not make it possible to determine the optimum volume or mass (e), i.e. necessary and sufficient in AGC, to obtain a percentage of abatement of the micropollutants previously fixed.
- the present invention relates to a process for the depollution of water, typically wastewater, containing organic micropollutants by adsorption on activated charcoal grain in an upflow treatment reactor and expanded bed, so as to reduce a percentage of micropollutants previously fixed, said method comprising at least the following steps:
- FIG. 1 represents a particular embodiment of the treatment reactor used in the depollution process according to the present invention.
- Figure 2 is a graph depicting the percent reduction of micropollutants in water based on UV decay performance by activated carbon adsorption grain treatment.
- Figure 3 is a graph depicting the percent abatement of micropollutants as a function of the applied coal treatment rate.
- Figure 4 is a graph depicting the percentage of UV abatement as a function of the applied coal treatment rate.
- FIG. 5 is a graph representing the percentage of UV reduction as a function of time according to a first particular embodiment (initially empty reactor).
- FIG. 6 is a graph representing the percentage of UV reduction as a function of time according to a second particular embodiment (reactor with an initial charge).
- FIG. 7 is a graph representing the upward velocity, the evolution of the bed height of activated carbon and the MES at the outlet of the treatment reactor during washing.
- Fig. 8 is a diagram showing the particle size distribution of grain activated carbon according to a particular embodiment.
- FIG. 9 represents the effective size of the activated carbon in grain according to the height of the coal bed.
- micropollutant (s) refers to micropollutants which may be selected from alkylphenols, pharmaceuticals for human or animal use, polycyclic aromatic hydrocarbons, pesticides, herbicides, insecticides, phthalates, adsorbable organic halogens, organostanneux, phenols and their combinations.
- the micropollutants are selected from pesticides, herbicides, phthalates, pharmaceutical substances and combinations thereof.
- micropollutant (s) can specifically refer to pharmaceutical substances, especially pharmaceutical substances selected from carbamazepine, oxazepam, diclofenac, ibuprofen, ketoprofen, furosemide, atanolol, propanolol, sulfamethoxazole and benzotriazole.
- clean water refers to the condition of the water after coming into contact with a bed of granular activated carbon.
- cleaned and decanted water refers to the condition of the water after treatment according to the present invention.
- waters refers to wastewater or water to be treated.
- treatment rate refers to the mass of activated carbon (in grams) based on the volume of water to be treated (in m 3 ).
- the Applicant has developed a process for the depollution of water, typically wastewater, containing organic micropollutants by adsorption on activated charcoal grain in an upflow treatment reactor, which makes it possible to optimize the mass or the volume of activated carbon by grain in the reactor, for a given treatment rate, and thus size the reactor.
- the method makes it possible to determine the optimum mass or volume of granular activated carbon in the required reactor and sufficient to obtain a percentage of reduction of the previously fixed organic micropollutants (% Mw).
- the present invention relates to a process for the depollution of water, typically wastewater, containing organic micropollutants by adsorption on charcoal granular active agent in an upflow treatment reactor, so as to reduce a pre-fixed percentage of micropollutants, comprising injecting water into the lower part of the reactor containing a bed of activated carbon so as to create an expansion of said activated carbon in in parallel ensuring the gravitational separation between the cleaned water and the activated carbon particles and the overflow recovery of the cleaned and decanted water in the upper part of the reactor, said process comprising at least the following steps:
- the performance control of the activated carbon adsorption grain treatment advantageously comprises the following steps;
- Steps (1), (2), and (3) for controlling the UV reduction efficiency are advantageously repeated over time.
- the control of the UV C reduction efficiency is carried out continuously or regularly. When the control is carried out regularly, it is advantageously carried out at least once a day.
- the present invention relates to a process for the depollution of water, typically wastewater, containing organic micropollutants by adsorption on activated charcoal grain in an upflow treatment reactor, in order to remove a percentage of micropollutants previously fixed, comprising the injection of water in the lower part of the reactor containing a bed of activated carbon so as to create an expansion of said activated carbon while ensuring the gravitational separation between the cleaned water and the particles of activated carbon and overflow recovery of the decontaminated and decontaminated water at the top of the reactor, said process comprising at least the following steps:
- steps 1 ') and 3') are carried out as stated above.
- steps 1 ') and 3') are carried out as stated above.
- the percentage of abatement of micropollutants (% Mp) fixed is between 50 and 100% for urban water.
- step (iii) measuring the effective concentration of the organic micropollutant (s) selected in step (ii) in said samples and measuring the absorbance of said samples at a given wavelength ⁇ ;
- step (v) measuring, for each dose of activated carbon tested, the effective concentration of the organic micropollutants selected in step (ii) in said samples after treatment according to step (iv);
- the performance control of the activated carbon adsorption grain treatment corresponds to the control of the UV reduction efficiency.
- the treatment of the samples according to step (iv) is carried out by contacting the samples with increasing doses of activated carbon.
- activated carbon In general, at least four doses of activated charcoal are tested.
- the contact time can vary from 15 to 120 minutes, preferably it is 60 minutes. During the contact time, the samples are advantageously stirred.
- the measurement of the effective concentrations of the micropollutants according to steps (iii) and (v) is carried out according to methods that are well known to those skilled in the art.
- the effective concentrations of the micropollutants selected can be determined by liquid chromatography or gas phase.
- the abatement percentages of micropollutants (% Mp d0S ei , % Mp d0S e2,% Mp d0S e3) and the UV reduction yields (% UV d0S ei,% UV dose 2,% UV dose 3) as a function of doses granular activated carbon (dose 1, dose 2, dose 3) are determined by simple calculation.
- the values obtained can be represented on a graph with the abscissa yield UV and on the ordinate the percentages of abatement of micropollutants ((% UV dose i;% Mp dose i), (% UV dose2 ;% Mp d0S e 2 ), ((% UV dose3 ,% Mp dose3 ), etc.)
- the graph eventually allows us to determine the equation of the relationship expressing the percent reduction of micropollutants (% Mp) as a function of the abatement yield ( % UV) ( Figure 2). Performance check
- step (ii) described above typically comprises the selection of the micropollutant or organic micropollutants that the activated carbon adsorption treatment is specifically designed to eliminate .
- the nature of the micropollutant (s) likely to be contained in industrial wastewater is often known, thus making easy the control and / or monitoring of this or these micropollutant (s).
- the activated carbon adsorption depollution referred to in steps 1) and 2) or 2 ') and 3') can be carried out upstream or downstream of a reactor.
- biological wastewater treatment plant the wastewater may be industrial wastewater previously cleaned or not, by biological treatment.
- step (ii) described above includes the selection of these micropollutants and steps (iii) and (v) comprise the measurement of the total effective concentration of these micropollutants. Micropollutants other than those previously listed may be further quantified.
- the process according to the invention is particularly suitable for the depollution of water containing organic micropollutants such as carbamazepine, oxazepam, diclofenac, ibuprofen, ketoprofen, furosemide, atanolol, propanolol, sulfamethoxazole and benzotriazole.
- organic micropollutants such as carbamazepine, oxazepam, diclofenac, ibuprofen, ketoprofen, furosemide, atanolol, propanolol, sulfamethoxazole and benzotriazole.
- the absorbance measurements before treatment ( ⁇ ⁇ ⁇ ) and after treatment ( ⁇ ⁇ ⁇ ⁇ ) of the water in the treatment reactor (steps (1) and (2) or 2 ') and 3')) can be measured by means of UV or photometer probes as described in the patent application FR3009789.
- the wavelength ⁇ is preferably chosen in the ultraviolet range (200-380 nm), preferably from 200 to 300 nm.
- the absorbance can be measured at 254 nm.
- the rate of treatment of activated carbon grain is a standard rate set for urban wastewater, the rate being between 5 and 30g / m 3 , preferably between 10 and 25g / m 3 .
- the reactor is operated by injection of water at a rate of rise of between 7 and 20 m 3 / m 2 .h, advantageously between 12 and 15 m 3 / m 2 .h , so as to obtain a dense suspension of activated carbon in an upflow treatment reactor and expanded bed surmounted by a decanted clear water height.
- the treatment reactor is initially empty.
- the determination of said mass or volume of granular activated carbon necessary and sufficient in the reactor to obtain said previously fixed% MP f comprises at least the following steps:
- the The treatment reactor is considered to be stabilized and the mass or volume of granular activated carbon present in the reactor is necessary and sufficient (optimal) to obtain said% MP f ( Figure 5) .
- an extraction of activated charcoal in grain corresponding to the quantity of granular activated charcoal injected daily is carried out. The injection and the extraction thus ensure the renewal of the active carbon grain.
- the daily injection of granular activated carbon into the treatment reactor is carried out once or several times a day.
- the extraction makes it possible to extract the granular activated carbon from the moment when the mass or volume of granular activated charcoal necessary and sufficient to obtain said% MP f has been obtained.
- the extraction is carried out 1 to 7 times a week.
- the reactor contains an initial charge of granular activated carbon so as to obtain at least the percentage of abatement of the micropollutants previously fixed (% MP f ) as soon as the reactor is put into service.
- the determination of said mass or volume of granular activated carbon necessary and sufficient in the reactor to obtain said previously fixed% MP f comprises at least the following steps:
- the beginning of the daily injection of activated carbon into the reactor is determined by UV control and starts when the% UV C is such that:% UV f ⁇ % UV C ⁇ % UV f + 15%.
- the UV control determines when the mass or volume of granular activated carbon present in the reactor is considered optimal (necessary and sufficient) to obtain said% MP f.
- an extraction of activated charcoal in grain corresponding to the quantity of granular activated charcoal injected daily is carried out.
- the injection and the extraction thus ensure the renewal of the active carbon grain.
- the rate of treatment of activated carbon injected in step c ') can be increased in order to speed up the commissioning.
- the daily injection of granular activated carbon into the treatment reactor is carried out once or several times a day.
- the extraction makes it possible to extract the granular activated carbon from the moment when the mass or volume of granular activated charcoal necessary and sufficient to obtain said% MP f has been obtained.
- the extraction is carried out 1 to 7 times a week.
- the UV control makes it possible to monitor the maintenance of the performances of the process according to the invention.
- the extraction of activated carbon in expanded grain is carried out from at least two extraction levels (4 and 4 ') (FIG. 1) of the activated carbon bed.
- a decreasing concentration gradient from the bottom of the reactor upwards is generally created within the activated carbon bed.
- the concentration gradient varies according to the particle size distribution of the activated carbon used. Since the settling speed of the grains is proportional to the granulometry of the grains (between 0.3 and 1 mm) (FIG. 8), the distribution of these particles in the bed is therefore made from the largest down to the smallest upwards. ( Figure 9).
- the time of exhaustion or saturation of the active carbon being proportional to the particle diameter of the grains, it is important during the extraction to keep the larger grains longer than the small ones.
- an extraction is carried out from at least two levels of extraction of the activated carbon bed, one level being located in the upper part of the coal bed to extract the finest grains and another level in the lower part. to extract the larger grains.
- the extraction heights are between 1, 5 and 2 m, even more advantageously at 2 m for the extraction level in the upper part of the coal bed and between 0.1 and 1 m, still more advantageously at 0.5 m for the extraction level located in the lower part of the coal bed.
- the frequency of the extractions for the same volume or mass of coal is proportionally determined as a function of the effective grain sizes, ie typically an extraction for the lower level and two for the higher level.
- the depollution process according to the invention comprises at least one step of washing the activated carbon grain used.
- the washing of the activated carbon can be carried out inside the treatment reactor, in particular by blowing air and washing water at the base of the reactor.
- the water supply circuit to be treated is advantageously used for the introduction of washing water at the base of the reactor or a recirculation pump in addition to the feed rate.
- the washing air is injected by the same water supply circuit or with its own ramp and branching device.
- the step of washing the activated carbon bed is carried out when the measured height of the activated carbon bed is 20% higher than the theoretical height under steady state conditions.
- a theoretical height is determined for a given speed in steady state, the height of expansion of the bed depending on the rate of climb.
- the measurement of the height of the activated carbon bed is carried out daily or continuously.
- the washing is carried out when h e ⁇ h p + 10 to 50% (h p ), advantageously h e ⁇ h p + 10 to 20% (h p ), h e representing the height of the dirty expanded bed and h p the height of the washed bed.
- the dirty expanded bed corresponding to the bed containing the MES and the washed bed corresponding to the bed without the MES.
- the washing step comprises an expansion phase and a settling phase.
- the activated carbon bed formed by the accumulation of injected doses has the ability to retain a large part of the suspended matter (MES) entering the treatment reactor.
- MES suspended matter
- the age of this active carbon remaining in the reactor promotes the development of a biofilm. It is necessary to evacuate these MES and biofilm because without extraction of these, an increase in the volume of the bed can cause a leak of MES and / or activated carbon. The purpose of this washing is to separate these MES coal without damaging it.
- the expansion phase consists in applying to the active charcoal bed an ascending velocity advantageously of between 20 and 50 m 3 / m 2 .h and more advantageously 30 m 3 / m 2 .h, allowing the separation of activated carbon from the suspended solids present in the water and thus a sufficient expansion of the coal so that the MES migrate above the bed.
- the duration of the expansion is between 5 and 15 minutes, advantageously between 7 and 11 minutes, and advantageously said washing is carried out 1 to 7 times a week, even more advantageously 1 to 3 times a week.
- the settling phase makes it possible to decant the MES and the activated carbon in expanded grain during the expansion phase.
- the settling phase of the washing step can be carried out with the reactor operating at a minimum rate of rise enabling efficient decantation, said speed advantageously being less than or equal to 15 m 3 / m 2 .h or with the reactor shut down. When the reactor is stopped, said shutdown has a duration of between 3 and 10 min, advantageously 5 min.
- a draining phase allowing evacuation of the water slice comprising the MESs is typically carried out to an all-water station and / or a coal drip hopper from an evacuation valve. located at a emptying height (h v ) ( Figure 1).
- the emptying phase has a duration of between 5 and 30 minutes, advantageously between 5 and 10 minutes.
- a rinsing phase is typically carried out by resuming the feed at the flow rate preceding the water injection washing step in the lower portion of the treatment reactor.
- the drain valve is open to allow the evacuation of all the water injected into the lower part of the reactor, so the water does not under any circumstances overflow through the chutes.
- the rinsing phase advantageously has a duration of between 5 and 20 minutes, advantageously between 5 and 10 minutes.
- the reactor further comprises injection means (3) of new activated carbon, extraction means (4 and 4 ') of used activated carbon.
- the means for extracting spent active carbon are generally included in the reaction zone (A) comprising the expanded coal bed (FIG. 1).
- the treatment reactor :
- the treatment can be carried out in a treatment reactor as described in the patent FR2874913.
- the contacting of the water with granular activated charcoal allows the elimination of organic micropollutants of natural or synthetic origin, such as the residues of plant protection products, pesticides, pharmaceutical molecules, by adsorption of micropollutants on the particles of activated carbon. grain.
- the treatment is carried out in a treatment reactor (1) with an expanded bed of activated carbon grain operating in ascending flow and comprising two distinct zones of operation:
- reaction zone (A) in the lower part of the reactor consisting of an expanded bed of activated carbon ensuring the removal of organic micropollutants by adsorption thereof on the particles of activated carbon grain;
- the reactor also comprises a developed zone (C) located under the reaction zone ensuring the admission and the homogeneous distribution of the water to be treated.
- a water distribution ramp (2) is present in the developed area.
- the developed area contains a blocking bed, such as a bed of gravel surmounted by a bed of sand.
- the blocking bed prevents granular activated carbon from entering the distribution ramp.
- the blocking bed ensures a homogeneous distribution of water at the bottom of the reactor and ensures a homogeneous suspension of the activated carbon bed within the reaction zone, thus avoiding any dead water zone at near the base of the coal bed.
- the height of the developed zone is established according to the height of the distribution ramp and its positioning in the bottom of the structure. In particular, its height can be between 25 and 30 cm above the intake of water.
- the distribution manifold is chosen and arranged to distribute the water homogeneously to the base of the reactor.
- a good distribution of water can particularly be obtained when the distribution manifold is a distributor on which are arranged equidistant sets of branches and pierced with orifices at identical intervals, preferably directed towards the alternating staggered bottom.
- the distribution ramp is usually embedded in a bed of gravel.
- the flow of water injected into the lower part of the reactor through the distribution manifold allows the suspension (or expansion) and the suspension suspension of the activated carbon grain.
- the concentration of activated carbon can reach several hundred grams per liter and effectively exert a depolluting action, without generating clogging or loss of load, as can be the case with the use of fixed bed activated carbon systems.
- the average active carbon concentration in the expanded bed is 100 to 450 g / l. It is generally less than or equal to 2 mg / l in the upper part of the separation zone.
- the height of the separation zone (B) typically varies from 0.5 m to 2.0 m. It is usually close to 1, 5 m.
- coagulation or flocculation agents may be added upstream of the reactor in the wastewater to improve the efficiency of the reduction in organic matter and organic micropollutants.
- the height of the expanded bed of granular activated carbon in the reaction zone is between 1 and 2 m, advantageously 1.5 m.
- the granulometry of the granular activated carbon and the upward velocity of the water are chosen so as to obtain a suspension of activated carbon in the form of an expanded bed, surmounted by a height of cleared water corresponding to the zone of separation.
- the term "rate of climb” refers to the ratio of the hydraulic flow rate of water injected into the reactor on the ground surface of the treatment reactor.
- the granulometry of the granular activated carbon is between 100 and 1000 ⁇ , more advantageously between 300 and 800 ⁇ , more advantageously between 600 and 800 ⁇ .
- several types of activated carbons of different particle sizes or densities can be used in the same reactor (FIG. 8). The present invention thus makes it possible to treat a wide variety of micropollutants present in waters with varying degrees of adsorbability depending on the coals used.
- the granulometry of the granular activated carbon is between 300 and 1000 ⁇ , more advantageously between 600 and 800 ⁇ , and / or the upward velocity of the water varies between 7 and 20 m 3 / m 2. .h, more preferably 12 to 15 m 3 / m 2 .h
- the contact time of the water with activated carbon is defined according to the rate of rise of the water and the height of the expanded coal bed.
- the contact time generally varies from 5 to 60 min, advantageously from 5 to 30 min, even more advantageously from 8 to 15 min.
- the choice of a particular particle size of coal associated with the choice of a particular rate of rise of the waters allows a gravitational separation of the coal particles from the cleaned water with the obtaining of the cleaned and decanted water in the upper part of the reactor, with very low residual active carbon content.
- the injection of new granular activated carbon into the reactor is typically carried out above the (expanding) coal bed, preferably by one or more injection systems (3) typically composed of 'a pipe of section between 100 and 200 mm depending on the amount of granular activated carbon to be introduced.
- the injection of activated carbon in new grain is carried out using a hydroéjecteur which allows to bring the active carbon in the upper part of the reactor (separation zone (B)).
- the injection system (s) (3) in particular one or more injection rods, are placed parallel to the walls of the reactor and are terminated by a 45 ° elbow which is always at above the growing activated carbon bed.
- the elbow is between 1, 5 and 2 m below the level of discharge of process water (return chutes (5)).
- the end of this or these injection pipe (s) is (are) so as to form a bevel which will facilitate the flow of activated carbon to the surface of the bed of this active carbon.
- the advantage of this system lies in the fact that a clogging of this equipment is difficult or impossible.
- new active charcoal as opposed to the term “spent or expanded active charcoal”, refers to activated charcoal that has not been in contact with organic micropollutants.
- the cleaned and decanted water can be collected by overflow in the upper part of the reactor.
- the recovery chutes (5) are arranged in the upper part of the reactor.
- the upflow and expanded bed treatment reactor may further comprise means for recirculating water that has been depolluted inside the reactor, so as to maintain a sufficient rate of expansion or fluidization allowing a minimum expansion of the coal bed for prevent the reactor from being degraded during the shutdown phases.
- the granular activated carbon may be regenerable or reactivatable coal.
- the used grain activated carbon is then extracted and stored before being sent to essentially reactivation or regeneration centers by thermal means.
- the depollution process according to the invention is suitable for wastewater and water to be treated, even more advantageously wastewater.
- Example 1 Reactor initially empty 1) Percentage of reduction of fixed micropollutants contained in the wastewater: 70-80%;
- the micropollutant abatement percentage of 70-80% corresponds to a percentage of UV abatement of approximately 30% and is obtained with a treatment rate of 20 g / m 3 of activated carbon grain;
- the mass or volume of granular activated carbon in the reactor is then considered as optimal, an extraction of activated carbon is then carried out once a week from two levels of extraction of the activated carbon bed (a first level is located in the upper part of the coal bed, the second level is in turn located in the lower part), the mass or volume of extracted coal corresponding to the mass or volume of activated carbon introduced between two extractions.
- the treatment reactor according to the present invention is an upflow treatment reactor, thus the water to be treated containing MES, as in most cases an accumulation of these MES occurs.
- a washing comprising the following phases is then carried out:
- Expansion phase increase of the rate of expansion of the granular activated carbon by the commissioning of the recirculation pump in addition to the feed rate. During washing, the expansion rate goes from 15 m 2 / m 3 .h to 30 m 2 / m 3 .h. This desired speed allows expansion necessary and sufficient to extract the MES from the activated carbon bed.
- Decantation phase the end of the expansion phase of the granular activated carbon corresponding to the beginning of the settling phase is determined when the MES concentration at the chutes increases by a few mg / l (the concentration in MES from 1 to 2.5 g / L in 7 minutes (FIG. 7)), the concentration of MES being measured by a MES probe (Solitax from LANGE).
- Rinsing phase resumption of the feed by injection of water in the lower part of the treatment reactor at a rate of rise of 15 m 2 / m 3 .h for a period of 10 minutes, the drain valve being open.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Engineering & Computer Science (AREA)
- Hydrology & Water Resources (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Carbon And Carbon Compounds (AREA)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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EP15306586.7A EP3153475B8 (de) | 2015-10-08 | 2015-10-08 | Verfahren zur reinigung von wasser durch adsorption von aktivkohle |
PCT/EP2016/074247 WO2017060536A1 (fr) | 2015-10-08 | 2016-10-10 | Procédé de dépollution des eaux par adsorption sur charbon actif |
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EP3359492A1 true EP3359492A1 (de) | 2018-08-15 |
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EP15306586.7A Active EP3153475B8 (de) | 2015-10-08 | 2015-10-08 | Verfahren zur reinigung von wasser durch adsorption von aktivkohle |
EP16782030.7A Withdrawn EP3359492A1 (de) | 2015-10-08 | 2016-10-10 | Verfahren zur entfernung von verunreinigungen aus wasser durch adsorption an aktivkohle |
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EP15306586.7A Active EP3153475B8 (de) | 2015-10-08 | 2015-10-08 | Verfahren zur reinigung von wasser durch adsorption von aktivkohle |
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US (1) | US11040893B2 (de) |
EP (2) | EP3153475B8 (de) |
BR (1) | BR112018007009B1 (de) |
CA (1) | CA3001113C (de) |
CL (1) | CL2018000904A1 (de) |
CO (1) | CO2018004095A2 (de) |
ES (1) | ES2933706T3 (de) |
MX (1) | MX2018004294A (de) |
PE (1) | PE20181106A1 (de) |
PL (1) | PL3153475T3 (de) |
PT (1) | PT3153475T (de) |
SA (1) | SA518391293B1 (de) |
WO (1) | WO2017060536A1 (de) |
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US20210269889A1 (en) * | 2020-03-02 | 2021-09-02 | Exxonmobil Research And Engineering Company | Lignocellulosic biomass treatment methods and systems for production of biofuels and biochemicals |
FR3114093B1 (fr) | 2020-09-17 | 2024-08-23 | Suez Groupe | Procédé de traitement d’une eau avec renouvellement de l’adsorbant à un âge intermédiaire ciblé |
FR3122104A1 (fr) | 2021-04-22 | 2022-10-28 | Suez Groupe | Methode de determination de la capacite restante d’un adsorbant et procede de traitement d’un fluide utilisant ladite methode |
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US5997812A (en) * | 1996-06-20 | 1999-12-07 | Coolant Treatment Systems, L.L.C. | Methods and apparatus for the application of combined fields to disinfect fluids |
US6568900B2 (en) * | 1999-02-01 | 2003-05-27 | Fantom Technologies Inc. | Pressure swing contactor for the treatment of a liquid with a gas |
JP2002166265A (ja) * | 2000-11-30 | 2002-06-11 | Toshiba Corp | 蛍光分析計を用いた水処理制御システム |
WO2006013235A1 (fr) | 2004-07-05 | 2006-02-09 | Societe D'amenagement Urbain Et Rural | Procede de depollution de fluide contenant des micropolluants organiques par adsorption sur charbon actif dans un reacteur de traitement |
FR2946333B1 (fr) * | 2009-06-09 | 2012-08-03 | Saur | Installation de traitement de fluide aqueux par contact avec un lit fluidise de charbon actif coagule |
US10040699B2 (en) * | 2013-07-08 | 2018-08-07 | Sensor Electronics Technology, Inc. | Ultraviolet water disinfection system |
FR3009789B1 (fr) | 2013-08-23 | 2017-07-28 | Saur | Methode de controle et de suivi de l'abattement des micropolluants organiques dans les eaux usees |
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2015
- 2015-10-08 PT PT153065867T patent/PT3153475T/pt unknown
- 2015-10-08 PL PL15306586.7T patent/PL3153475T3/pl unknown
- 2015-10-08 ES ES15306586T patent/ES2933706T3/es active Active
- 2015-10-08 EP EP15306586.7A patent/EP3153475B8/de active Active
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2016
- 2016-10-10 CA CA3001113A patent/CA3001113C/fr active Active
- 2016-10-10 US US15/766,446 patent/US11040893B2/en active Active
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- 2016-10-10 BR BR112018007009-2A patent/BR112018007009B1/pt active IP Right Grant
- 2016-10-10 WO PCT/EP2016/074247 patent/WO2017060536A1/fr active Application Filing
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- 2016-10-10 EP EP16782030.7A patent/EP3359492A1/de not_active Withdrawn
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MX2018004294A (es) | 2018-08-09 |
PL3153475T3 (pl) | 2023-01-09 |
US20180312411A1 (en) | 2018-11-01 |
CL2018000904A1 (es) | 2018-08-31 |
BR112018007009A2 (pt) | 2018-10-16 |
CO2018004095A2 (es) | 2018-07-10 |
WO2017060536A1 (fr) | 2017-04-13 |
EP3153475A1 (de) | 2017-04-12 |
ES2933706T3 (es) | 2023-02-13 |
BR112018007009B1 (pt) | 2023-02-07 |
CA3001113A1 (fr) | 2017-04-13 |
EP3153475B1 (de) | 2022-10-19 |
US11040893B2 (en) | 2021-06-22 |
EP3153475B8 (de) | 2022-12-07 |
PE20181106A1 (es) | 2018-07-12 |
SA518391293B1 (ar) | 2022-04-25 |
CA3001113C (fr) | 2023-09-05 |
PT3153475T (pt) | 2022-12-13 |
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