WO2000004969A1 - Procede et dispositif pour la separation d'emulsions contenues dans des eaux de processus et/ou usees - Google Patents

Procede et dispositif pour la separation d'emulsions contenues dans des eaux de processus et/ou usees Download PDF

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Publication number
WO2000004969A1
WO2000004969A1 PCT/EP1999/005012 EP9905012W WO0004969A1 WO 2000004969 A1 WO2000004969 A1 WO 2000004969A1 EP 9905012 W EP9905012 W EP 9905012W WO 0004969 A1 WO0004969 A1 WO 0004969A1
Authority
WO
WIPO (PCT)
Prior art keywords
container
wastewater
hydrophobic
temperature stratification
water
Prior art date
Application number
PCT/EP1999/005012
Other languages
German (de)
English (en)
Inventor
Michael Betz
Matthias Nomayo
Original Assignee
Michael Betz
Matthias Nomayo
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Michael Betz, Matthias Nomayo filed Critical Michael Betz
Priority to DE19981352T priority Critical patent/DE19981352D2/de
Priority to AU51598/99A priority patent/AU5159899A/en
Publication of WO2000004969A1 publication Critical patent/WO2000004969A1/fr

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D21/00Separation of suspended solid particles from liquids by sedimentation
    • B01D21/009Heating or cooling mechanisms specially adapted for settling tanks
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D21/00Separation of suspended solid particles from liquids by sedimentation
    • B01D21/01Separation of suspended solid particles from liquids by sedimentation using flocculating agents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D21/00Separation of suspended solid particles from liquids by sedimentation
    • B01D21/24Feed or discharge mechanisms for settling tanks
    • B01D21/2433Discharge mechanisms for floating particles
    • B01D21/2438Discharge mechanisms for floating particles provided with scrapers on the liquid surface for removing floating particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D21/00Separation of suspended solid particles from liquids by sedimentation
    • B01D21/30Control equipment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D3/00Differential sedimentation
    • B03D3/02Coagulation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/22Nature of the water, waste water, sewage or sludge to be treated from the processing of animals, e.g. poultry, fish, or parts thereof
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/02Temperature

Definitions

  • the invention relates to a method for separating process and / or waste water with a predetermined concentration of coagulable, hydrophobic constituents into a hydrophobic phase and a clear phase.
  • DE-C 30 11 025 has disclosed a process for separating, if appropriate with degreasing, solids, in particular organic substances, from liquids, the liquids containing solid substances which can be aggregated and / or dewatered by the action of heat.
  • the known method by aggregating particles in the liquid and / or reducing the water content thereof by the action of heat and then separating
  • REPLACEMENT SHEET (RULE 23) the particles worked out of the liquid and drying.
  • a corresponding system is equipped with a collection container, a quick heater and a heat treatment unit.
  • the invention is based on the technical problem of specifying a process for the separation of process water and / or waste water with a predetermined concentration of coagulable, hydrophobic constituents of the type described at the outset, which provides a perfect separation of the hydrophobic phase and clear phase - even at a high concentration of coagulable, hydrophobic components organic components - enables.
  • a particularly suitable system should be specified.
  • the invention relates to a process for separating process and / or waste water with a predetermined concentration of coagulable, hydrophobic constituents into a hydrophobic phase and a clear phase with the following process steps:
  • the wastewater to be separated is poured into a container, especially a concentration tank, at the top and drawn off as clear water in the bottom area;
  • the filled wastewater is heated on the foot side of the container by setting an inverse temperature stratification with at least two layers of different temperature in the container;
  • the hydrophobic components coagulate when sinking in a predetermined coagulation layer height and rise from there due to the inverse temperature gradient to the near-surface hydrophobic phase, where they are skimmed off;
  • a heater adapted to the cross section of the container is provided, which, for. B. is heated by means of steam or electrical energy.
  • the inverse temperature stratification is generally set so that temperatures between 80 ° C. to 95 ° C. are established in the layer immediately above the heating device, temperatures between 55 ° C. and 75 ° C. are present in the area of the layer with the coagulation layer height and Finally, temperatures of approx. 30 ° C to 50 ° C can be reached in the near-surface layer, the temperature stratification being set as a function of the nature and quantity of the waste water introduced and the coagulation temperature of the hydrophobic constituents.
  • the temperature stratification is largely set in a controlled manner, at least the temperature of a layer and the amount of incoming wastewater being used as control input variables and the heating energy required for heating the heating device being used as a control variable.
  • a convection counteracting the temperature stratification is preferably prevented by baffles arranged in the direction of the temperature gradient of the layers.
  • the invention recommends introducing fresh water into the container near the surface in order to reduce the salt content of the hydrophobic phase.
  • the invention is based first of all on the knowledge that waste water contaminated with coagulable, hydrophobic, organic constituents not only damage the environment, but that the abovementioned organic constituents can be advantageously recovered.
  • These organic components can be proteins that are produced in fish meal production.
  • these proteins are discharged into the sea with virtually no clarification and contribute to a not inconsiderable level of pollution. They are also irretrievably lost for further processing and accordingly represent an economic loss in fish meal processing.
  • the invention has now recognized that these hydrophobic organic constituents, ie insoluble sediments, usually coagulate within a certain temperature range, in other words can be converted into sedimentable precipitates by physicochemical processes.
  • the coagulation temperature ie the temperature at which the aforementioned coagulation process begins, is approximately 60 ° C to 70 ° C.
  • the filled waste water is generally heated on the foot side of the container by means of steam bubbles which emerge from the heating device, rise in the container and give off energy while heating.
  • the height of the container is dimensioned such that the vapor bubbles have disappeared or been resorbed or converted at the top of the container.
  • the desired inverse temperature stratification is achieved by the (cold or colder) waste water filled in at the head, the heating on the foot side and the constant removal of the waste water from the floor area, as will be explained in more detail with reference to the figure description.
  • a relatively cold wastewater layer forms in the upper region of the tank (on the head side), which is constantly supplied with fresh water. The warmer water layers underneath tend to rise within the tank through convection.
  • protein molecules consist of hundreds to thousands of amino acid residues which are linked to one another by peptide bonds. This means that, like cellulose and starch, proteins are macromolecular natural substances with molecular weights between 10,000 and several million. Proteins that are absorbed by water form colloidal solutions because the diameter of their molecules is 10 to 10 cm; accordingly, they do not diffuse through a membrane and can therefore be separated out (up to a certain concentration in water) using membrane filters.
  • the invention now enables a perfect separation into the hydrophobic phase and the clear phase.
  • the proteins change their coagulation layer height when they clot or coagulate, their structure and their chemical and physical properties
  • skimmed off hydrophobic phase can be processed further to a dry substance which has a high organic content and is therefore particularly suitable for (fish meal) processing.
  • the invention also relates to a device which is particularly suitable for carrying out the method described and is described in claims 10 to 17.
  • Fig. 1 shows the device according to the invention and Fig. 2 shows a plant for wastewater treatment, which has the device of FIG. 1.
  • the figures show a device for separating process and / or waste water with a predetermined concentration of coagulable, hydrophobic constituents into a hydrophobic phase and a clear phase.
  • this device has a (rotationally symmetrical) cylindrical container 1, in particular a concentration tank 1, with a (waste) water inlet 2 at the head.
  • the container 1 or concentration tank 1 has a conical base 3 with a sediment discharge 4.
  • This heating device 5 has (not shown) internal (flow) holes for (water) steam and is supplied with the required heating energy via a control device 6.
  • an electrical or other type of heating of the heating device 5 is also possible.
  • the aforementioned heating device 5 serves to set the previously described inverse temperature stratification in the container 1 with layers A, B and C of different temperatures in the container 1.
  • the (throughflow) bores in the heating device 5 are made in a sintered plate and are dimensioned such that this sintered plate or the heating device 5 leave vapor bubbles with a diameter of approximately 2 mm and below and rise in the container 1.
  • this sintered plate or the heating device 5 leave vapor bubbles with a diameter of approximately 2 mm and below and rise in the container 1.
  • the use of an end plate drilled by means of laser beams is also conceivable at this point, as long as appropriately small steam bubbles be generated.
  • These ensure the necessary energy transfer to the filled wastewater, which is heated by means of steam at a temperature of approx. 100 ° C (pressure: 1.1 bar) in the manner described below. It has been found that a height of approximately 2.50 m is sufficient for the container 1 to be able to represent the desired heat transfer from the steam to the waste water with the help of the steam bubbles.
  • each layer A, B and C is assigned its own temperature sensor 7.
  • Layer B which forms above layer A, has temperatures between 55 ° C. and 75 ° C.
  • the coagulation of the hydrophobic constituents of the waste water takes place in this second layer B, specifically at a certain coagulation layer height, which ultimately depends on the low temperature of the components.
  • the inverse temperature stratification in the container 1 is set so that the coagulation layer height is arranged approximately in the middle of the rotationally symmetrical cylinder container or concentration tank 1.
  • layer C with temperatures of approx. 30 ° C to 50 ° C, in which the hydrophobic phase forms on the surface.
  • a skimmer 8 near the surface according to the exemplary embodiment a rotating paddle 8 with an overflow 9, is realized for the flotate.
  • the hydrophobic phase consequently forms in layer C
  • the clear phase or clear water phase is arranged in layer A, so that a sharp separation of the two phases is achieved.
  • a clear water drain 10 is provided in the area of the clear phase.
  • the heating device 5 is designed as a circular disk adapted to the cylinder cross section of the container or concentration tank 1.
  • the aforementioned devices 7, 13 provide control input variables for the control device 6, which controls the heating energy supplied to the heating device 5 on the output side as a function thereof.
  • the heating energy supplied is the manipulated variable of the control device 6.
  • the further possibility of controlling the water outflow via the clear water drain 10 in terms of quantity and / or temperature which can also be done via the control device 6.
  • These additional options are represented by dashed connecting lines to the control device 6 in FIG. 1. It is always ensured that the temperature and amount of the waste water supplied via the water inlet 2 as well as the temperature and amount of the clear water discharged by means of the clear water drain 10 are set such that the temperature profile described is obtained.
  • the water drawn off by means of the skimming device 8 is also taken into account, although its effect is marginal due to the small amount.
  • containers 1 whose volume is below 1 m 3 , preferably below 0.6 m 3 .
  • the base area is approximately 0.1 m 2 , so that a volume content of approximately 0.3 m 3 is established.
  • a container 1 in the form of a round concentration tank 1 with approximately 1 m can also be used
  • Diameter can be used, which is evenly in four 90 ° circle segment sections with approximately 0.5 m edge width is divided.
  • the floor space realized in this way is approx. 0.2 m 2 , so that there is a volume of approximately 0.5 m 3 .
  • a suction pump with a possibly connected suction nozzle can also be provided in order to be able to remove the flakes which form or the hydrophobic phase.
  • the amount of wastewater drawn off in relation to the amount of water in the concentration tank 1 is adjusted so that a larger amount is drawn off on the foot side via the clear water drain 10 than with the aid of the pump device described above. This is necessary in order to maintain the inverse temperature stratification described unchanged.
  • an inert gas is supplied via the heating device 5 in addition to the (hot) water vapor.
  • This inert gas can be air, which is added to the water vapor in small quantities.
  • Hydrogen is even more suitable here, because of its special adsorption capacity and the achievable rate of buoyancy due to the low Weight.
  • CO 2 or nitrogen can also be used in the present case.
  • FIG. 2 shows a flow diagram of a wastewater treatment in connection with the previously described device with inverse temperature stratification.
  • An input buffer 14 with sludge discharge (dashed line) is provided on the input side.
  • the wastewater drawn off from this has a temperature of approximately 20 ° C. and a protein content of approximately 4% by weight. It also contains about 3% by weight fish oil.
  • This (waste) water is heated via two heat exchangers 15, 16 to temperatures of approximately 30 ° C. after the first heat exchanger 15 and approximately 50 ° C. after the second heat exchanger 16.
  • the (waste) water then passes through the (waste) water inlet 2 into the container or concentration tank 1.
  • the inverse temperature stratification already described and the associated metastable equilibrium are established.
  • the average temperature of the (waste) water in concentration tank 1 is approx. 70 ° C.
  • the heating device 5 is heated with steam.
  • a flotate is drawn off via the overflow 9, which has about 8% by weight of protein and about 7% by weight of fish oil.
  • This flotate has a temperature of approx. 40 ° C to 50 ° C.
  • the flotate is heated to approximately 70 ° C. by means of a third heat exchanger 17 and fed to a coagulator 18 and a tricanter 19.
  • the tricanter 19 is used to concentrate the protein and to separate (fish) oil and water. Some of the proteins not coagulated in the water are removed from the tricanter 19 and, if necessary, returned to the concentration tank 1.
  • the concentrate from the tricanter 19 is fed to further processing and has more than 20% by weight of protein in the dry substance.
  • the branch leaving Tricanter 19 also represents the separated (fish) oil.
  • the clear water obtained from the concentration tank 1 is drawn off via the clear water drain 10 and the heat exchanger 16 and only has about 1% by weight of organic constituents.
  • the (waste) water is saline
  • fresh water can be introduced into the concentration tank 1 near the surface in order to achieve a reduction in the salt content of the hydrophobic phase, which would be disadvantageous in the subsequent treatment to the end product.

Abstract

L'invention concerne un procédé et un dispositif pour la séparation d'eaux de processus et/ou usées, avec une concentration prédéterminée en composants coagulables hydrophobes, en une phase hydrophobe et une phase claire. Les eaux usées à séparer sont introduites côté tête, dans un contenant (1), et retirées dans la zone du fond. Les eaux usées introduites sont, du côté de la base du contenant (1), réchauffées, ce qui entraîne, dans le contenant (1), la formation de couches dont la température varie de façon inversée. Les composants hydrophobes se coagulent en descendant jusqu'à une profondeur prédéterminée correspondant à la couche de coagulation et montent, à partir de cette couche, en raison de la chute de température inverse, en direction de la phase hydrophobe proche de la surface, phase dans laquelle ils sont prélevés. En-dessous de la hauteur correspondant à la couche de coagulation se forme la phase claire proche du fond, laquelle est retirée.
PCT/EP1999/005012 1998-07-22 1999-07-15 Procede et dispositif pour la separation d'emulsions contenues dans des eaux de processus et/ou usees WO2000004969A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
DE19981352T DE19981352D2 (de) 1998-07-22 1999-07-15 Verfahren und Vorrichtung zur Trennung von Prozess-und/oder Abwässern mit vorgegebener Konzentration an koagulierbaren, hydrophoben Bestandteilen in eine Hydrophobphase und eine Klarphase
AU51598/99A AU5159899A (en) 1998-07-22 1999-07-15 Method and device for separating emulsions from process and/or waste water

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19832916A DE19832916A1 (de) 1998-07-22 1998-07-22 Verfahren und Vorrichtung zur Trennung von Prozeß- und/oder Abwässer mit vorgegebener Konzentration an koagulierbaren, hydrophoben Bestandteilen in eine Hydrophobphase und eine Klarphase
DE19832916.4 1998-07-22

Publications (1)

Publication Number Publication Date
WO2000004969A1 true WO2000004969A1 (fr) 2000-02-03

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ID=7874887

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP1999/005012 WO2000004969A1 (fr) 1998-07-22 1999-07-15 Procede et dispositif pour la separation d'emulsions contenues dans des eaux de processus et/ou usees

Country Status (4)

Country Link
AU (1) AU5159899A (fr)
DE (2) DE19832916A1 (fr)
PE (1) PE20001163A1 (fr)
WO (1) WO2000004969A1 (fr)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3950891A (en) * 1975-01-03 1976-04-20 Florida Celery Exchange Seed coating composition and coated seed
US4174751A (en) * 1978-01-23 1979-11-20 Occidental Oil Shale, Inc. Method of breaking shale oil-water emulsion
GB1569269A (en) * 1977-01-13 1980-06-11 Iws Nominee Co Ltd Treatment of emulsions
US5240617A (en) * 1989-12-07 1993-08-31 Hopf Karl Heinz Phase-separation equipment and method for thermally separating an emulsion, in particular a water-oil emulsion

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
HU184673B (en) * 1979-03-21 1984-09-28 Richter Gedeon Vegyeszet Method and apparatus for yielding the solid material from fluids e.g. colloidlike solutions, sludges and suspensions containing protein and grease the solid content of which may be granulated by heat effect and/or the moisture content of solid content of which may be decreased by heat effect

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3950891A (en) * 1975-01-03 1976-04-20 Florida Celery Exchange Seed coating composition and coated seed
GB1569269A (en) * 1977-01-13 1980-06-11 Iws Nominee Co Ltd Treatment of emulsions
US4174751A (en) * 1978-01-23 1979-11-20 Occidental Oil Shale, Inc. Method of breaking shale oil-water emulsion
US5240617A (en) * 1989-12-07 1993-08-31 Hopf Karl Heinz Phase-separation equipment and method for thermally separating an emulsion, in particular a water-oil emulsion

Also Published As

Publication number Publication date
DE19981352D2 (de) 2001-07-26
DE19832916A1 (de) 2000-02-03
AU5159899A (en) 2000-02-14
PE20001163A1 (es) 2000-11-18

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