US005364534A United States Patent 19 11 Patent Number: 5,364,534 Anselme et al. 45 Date of Patent: Nov. 15, 1994

54 PROCESS AND APPARATUS FOR 4,872,991 10/1989 Kartels et al...... 210/651 TREATING WASTE LIQUIDS 5,093,072 8/1991 Hitotsuyanagi et al...... 210/650 5,154,830 10/1992 Paul et al...... 210/639 75 Inventors: Christophe Anselme, Le Vesinet; Isabelle Baudin, Nanterre, both of FOREIGN PATENT DOCUMENTS France 2628337 9/1989 France . 73 Assignee: Lyonnaise Des Eaux - Dumez, 4018994 1/1992 Japan ...... 210/195.2 Nanterre, France Primary Examiner-Frank Spear (21) Appl. No.: 129,387 Assistant Examiner-Ana Fortuna Attorney, Agent, or Firm-Pollock, Vande Sande & 22 Filed: Sep. 30, 1993 Priddy (30) Foreign Application Priority Data 57 ABSTRACT Oct. 2, 1992 FR France ...... 92 1699 Process for purifying and filtering fluids, especially 51l Int. Cl...... BOD 61/00 water, containing suspended contaminants and using 52 U.S. Cl...... 210/650; 210/660; gravity separation means as well as membrane separa 210/800; 210/805; 210/195.1; 210/195.2; tion means, in a finishing stage, comprising the step of 210/257.2 introducing a pulverulent reagent into the fluid stream 58) Field of Search ...... 210/650, 639, 800, 790, to be treated downstream of the gravity separation and 210/195.1, 195.2, 295, 805, 900, 257.2, 660 upstream of the membrane separation, wherein said 56) References Cited pulverulent reagent is recycled from the purge of the U.S. PATENT DOCUMENTS membrane separation means to the upstream of the gravity separation means. 4,525,278 6/1985 Frost, III ...... 210/650 4,610,792 9/1986 Van Gils et al. . ... 20/639 4,732,859 3/1988 Sugimoto et al...... 210/805 7 Claims, 1 Drawing Sheet

RECYCLING OF THE PULVERULENT REAGENT

PULVERULENT REAGENT

UNTREATED TREATED WATER WATER

GRAVITY SEPARATOR

U.S. Patent Nov. 15, 1994 5,364,534

7(9/-/

5,364,534 1 2 untreated water, containing suspended contaminants PROCESS AND APPARATUS FOR TREATING and using gravity separation means as well as membrane WASTE LIQUIDS separation means, in a finishing stage, according to which a pulverulent reagent is introduced into the fluid FIELD OF THE INVENTION stream to be treated downstream of the gravity separa The present invention relates to a process and to a tion and upstream of the membrane separation, this device intended for providing for the treatment of a process being characterized in that: liquid effluent containing especially dissolved contami the said pulverulent reagent is recycled from the nants. purge of the membrane separation means to the up 10 stream of the gravity separation means. BACKGROUND OF THE INVENTION According to the present invention, the pulverulent Such processes and devices use gravity separation reagent can consist of adsorbing agents, especially ac means, for example known systems of the clarifier type. tive charcoal, ion exchangers or complexing agents. It is known that, during treatment of a liquid effluent Another subject of the invention is a device for treat containing, inter alia, dissolved contaminants, it may be 15 ment of a liquid effluent, especially of an untreated necessary to use additions of pulverulent reactive agents such as especially adsorbing agents (for example active water, containing dissolved contaminants, constituting charcoal), ion exchangers and complexing agents. The a treatment line containing, in particular, gravity sepa addition of these reagents to the line for the treatment of ration means and membrane separation means, in a fin the liquid effluent is most often carried out at the same 20 ishing stage, as well as means which make it possible to time as another reagent which promotes coagulation, introduce a pulverulent reagent into the treatment line, flocculation and gravity separation of the particulate before the membrane separation and downstream of the impurities contained in the dissolved contaminants. gravity separation, this device being characterized in Such a use thus makes it possible, in a single treatment that it comprises a loop for recycling the pulverulent works, to remove the particulate, colloidal and dis 25 reagent, from the purge of the membrane separation solved impurities from the liquid effluent stream to be means as far as the pipe in which the liquid effluent to be treated. However, it is recognized that this type of treated moves, upstream of the gravity separation process is not entirely efficient, the yields of the various caS. processes used not being equal to 100%. Other characteristics and advantages of the present The advent of membrane separation techniques and 30 invention will emerge from the description given here especially the applications of microfiltration and ultra inbelow with reference to the appended drawings filtration to the treatment of liquid effluents containing which illustrate an implementational example thereof dissolved contaminants, for example of untreated water, free of any limiting nature. In the drawings: made it possible to improve the overall yield of the clarification operations, the membranes having a sepa 35 BRIEF DESCRIPTION OF THE FIGURE ration yield equal to 100% for the particles which are FIG. 1 is a schematic representation of a treatment larger than the separating power of the membranes device using the process which is the subject of the used. This has therefore led to the installation of treat invention, and, ment lines containing gravity separation means and membrane separation means in a finishing stage. The DETAILED DESCRIPTION OF THE present invention refers to this type of plant. INVENTION Plants are already known (FR-A-2,628,337) for puri It is seen, by referring to FIG. 1, that the device fying fluids by means of membranes in which an adsorb according to the present invention comprises, as ing agent, for example pulverulent active charcoal, is known, a gravity separation means, denoted by Refer introduced, this adsorbing agent being introduced into 45 ence 1, which can consist of a clarifier, and a membrane the fluid stream to be purified before the filtration mem separation means 2 produced, for example, in the form branes. of micro- or ultrafiltration devices. Plants for the treatment of contaminated water are According to the invention, this device allows for the also known (U.S. Pat. No. 4,610,792) which contain introduction of a pulverulent reagent downstream of clarification means and membrane separation means, in 50 a finishing treatment. In this known plant, a pulverulent the gravity separator I and upstream of the membrane reagent, for example active charcoal, is introduced into separator 2, it being possible for this introduction to be the line for treatment of untreated water between the carried out via a recirculation chamber 3. The invention clarification means and the membrane separation also provides for recycling of the pulverulent reagent means. In this known plant, the pulverulent reagent is 55 arising from the purge 4 of the membrane separator, recirculated in the filtration loop between the clarifica using a loop 5 which supplies the pulverulent reagent, tion means and the membrane separation means. thus recycled, to a point 6, situated on the pipe for Simpler systems for addition of pulverulent reagents supplying the untreated water, upstream of the gravity are also known according to which the reagent is in separator 1. jected into the treatment line directly upstream of the Thus, with respect to the known art, as defined espe gravity separation. cially in U.S. Pat. No. 4,610,792, the invention differs in In starting from this state of the art, the present inven that the pulverulent reagent is recycled from the purge tion introduces an improved process and device which 4 of the membrane separation 2 to a point situated up in particular makes it possible, as will be seen hereinbe stream of the gravity separation means 1, By virtue of low, to simplify the treatment plants and to improve the 65 this device, the gravity separation/membrane separa yields thereof. tion system contains only a single outlet for the sus Consequently, the first subject of this invention is a pended particles, this outlet consisting of the purge 7 of process for purifying and filtering fluids, especially the gravity separator. 5,364,534 3 4. With respect to the other known technique explained that of Configuration 1 is obtained but with 10 ppm of hereinabove (FR-A-2,638,337), the invention differs in PAC in place of 30 ppm and that, at equivalent doses of that, while circulating the pulverulent reagent counter PAC, Configuration 3 makes it possible to obtain larger currentwise with respect to the liquid effluent flow, the flows, reduced water losses and a better quality of water upstream operation is a conventional gravity separation 5 than Configuration 2 (Total Organic Carbon, TOC, operation (for example a clarification) in which the much lower). partially exhausted pulverulent reagent is in contact Of course, it remains that the present invention is not with an untreated fluid (for example untreated water) in the least limited to the implementational example and which thus makes it possible, on the one hand, to ex to the embodiment described and mentioned above but haust it completely and, on the other hand, to weigh 10 that it encompasses all the variants thereof. down the flakes. We claim: With respect to the other known processes using the 1. A system for purifying water comprising: combination: gravity separation means/membrane sepa gravity separation means having an inlet for receiving ration means, the invention introduces in particular the untreated water having suspended contaminants; following advantages: 15 an outlet of the gravity separation means providing the addition of pulverulent reagents to a clarified clarified untreated water to a container; effluent (for example a clarified water having a low means for introducing a pulverulent reagent into the Total Organic Carbon, TOC) promotes the adsorption container for mixing with the clarified water; of compounds having rapid adsorption kinetics (pesti membrane separation means connected at an inlet cides), thereof to an outlet of the container for separating the recycling of the pulverulent reagent, saturated to particles from water; 50%, from the membrane separation means to the up a first outlet of the membrane separation means pro stream of the gravity separation means (with a long viding treated water flow; residence time) makes it possible to saturate this pulver a second outlet of the membrane separation means ulent reagent and to promote the adsorption of the 25 connected to the inlet of the gravity separation organic compounds having slower kinetics present in means for recycling the pulverulent reagent, intro the untreated water, duced into the container, thus increasing contact the discarded material from the membranes of the time between the pulverulent reagent and the membrane separation means, containing the pulverulent water being treated; reagent, is conveyed to the sludges arising from the 30 the recycled pulverulent reagent being completely gravity separator, which simplifies the problem of the extracted from a purge in the gravity separation treatment of the sludges from the treatment line. e2S. In order for the advantages introduced by the present 2. The system set forth in claim 1 wherein the gravity invention to emerge better, results are given hereinbe separation means is a clarifier. low of comparative tests between, on the one hand, a 35 3. The system set forth in claim 1 wherein the mem plant using the process of the invention (in accordance brane separation means is either ultrafiltration or mi with FIG. 1) and, on the other hand, plants using pro crofiltration. cesses according to the prior state of the art. 4. A process for purifying water comprising the steps: In these known plants, the pulverulent reagent is performing gravity separation for initially untreated respectively introduced into the treatment line between water, having suspended contaminants, thereby the gravity separator 1 and the membrane separator 2 clarifying the untreated water; and upstream of the gravity separator 1. temporarily containing the clarified water; The comparative tests, the results of which are given introducing a pulverulent reagent into the contained in the table hereinbelow, were carried out on Seine clarified water and mixing with the clarified water; water and the pulverulent reagent used was fresh active 45 allowing reagent mixed water to flow along a treat charcoal (PAC). ment path; TABLE filtering the flowing reagent mixed water for separat Config. 1 Config. 2 Config. 3 (invention) ing particles therefrom; FIG.2 FIG. 3 FIG. 50 tapping a first portion of the filtered water to provide PAC Dose 30 30 10 25 treated water flow; mg/1 recycling the remaining treated water, containing Flow (1 h-lm-2) 200 110 195 200 partially spent pulverulent reagent, to mix with at 20 C. initially untreated water thereby increasing contact Backwashing A180 1/30 1A30 1/180 duration/frequency 55 time between the pulverulent reagent and the minute/minute water being treated; and Water loss % <3 25 15 <3 completely purging recycled pulverulent reagent TOC, untreated 3 3 2.9 3 from the clarified water. water mg/1 TOC, clarified 2 1.4 1.2 5. The process set forth in claim 4 wherein the pulver water mg/1 ulent reagent is selected from the group consisting of: TOC, filtered 0. 1.1 0.5 60 adsorbing agents, ion exchangers, and complexing water (UF or MF) agents. mg/l 6. The process set forth in claim 5 wherein the ad sorbing agent is active charcoal. The advantages introduced by the process which is 7. The process set forth in claim 4 wherein the filter the subject of the invention (Configuration 3, FIG. 1) 65 ing step is accomplished by ultrafiltration or microfiltra emerge clearly from the examination of the above table. tion. In particular, it is noticed that behaviour equivalent to