EP1347840B1 - Verfahreen, vorrichtung und anlage zum reinigen von verunreinigten teilen mit einer unter druck stehenden flüssigkeit - Google Patents

Verfahreen, vorrichtung und anlage zum reinigen von verunreinigten teilen mit einer unter druck stehenden flüssigkeit Download PDF

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Publication number
EP1347840B1
EP1347840B1 EP01980606A EP01980606A EP1347840B1 EP 1347840 B1 EP1347840 B1 EP 1347840B1 EP 01980606 A EP01980606 A EP 01980606A EP 01980606 A EP01980606 A EP 01980606A EP 1347840 B1 EP1347840 B1 EP 1347840B1
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EP
European Patent Office
Prior art keywords
fluid
cleaning
parts
pressurised
basket
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.)
Expired - Lifetime
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EP01980606A
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English (en)
French (fr)
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EP1347840A1 (de
Inventor
Frédéric Barth
Serge Bassan
Guy Lumia
Guy Perre
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Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
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Commissariat a lEnergie Atomique CEA
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Publication of EP1347840A1 publication Critical patent/EP1347840A1/de
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
    • B08B7/0021—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by liquid gases or supercritical fluids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/02—Cleaning by the force of jets or sprays
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/045—Cleaning involving contact with liquid using perforated containers, e.g. baskets, or racks immersed and agitated in a liquid bath
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations

Definitions

  • the present invention relates to a method for cleaning polluted contaminated parts, contaminated with a dense fluid under pressure, in particular by a supercritical fluid, such as supercritical carbon dioxide CO 2 .
  • the invention also relates to a device and an installation for cleaning contaminated parts, by a dense fluid under pressure, in particular by a supercritical fluid.
  • the technical field of the invention may, in general, be defined as that of cleaning dirty, contaminated, polluted parts.
  • the cleaning of materials and parts is a fundamental step in the manufacture and development of intermediate or final products in a very large number of diverse and diverse industries encompassing sectors, such as the automotive industry, fine mechanics, electronics, watchmaking, connectors, computing, the aerospace industry, medical equipment, packaging, which use multiple alloys, such as steels, stainless steels, aluminum and copper, and sectors, such as optics and armament, which can use, besides these alloys, composite materials, such as polycarbonates and borosilicate-based glasses, etc.
  • the cleaning of parts and materials is particularly necessary before or during machining operations, manufacturing, assembly, assembly, gluing, application of paint, varnish, coating; surface treatment, chromating, physical vapor deposition.
  • Cleaning techniques consist in using organic solvents, or detergents or surfactants in aqueous solutions by soaking, spraying or wiping.
  • the solvents used differ in particular, depending on the nature of the pollutant, contaminating, dispersing.
  • organic solvents are: hydrocarbons; halogenated alkanes, alkenes and alkynes (chlorinated and / or fluorinated), such as trichlorethylene, dichloromethane and other CFCs and HCFCs; alcohols and ethylene glycol.
  • the Montreal Protocol put in place by most industrial countries, aims to limit the release of VOCs or Volatile Organic Compounds, which are responsible for the destruction of the ozone layer.
  • the aim is to achieve a zero discharge of these VOCs in 2015, whether for old installations in service or for new installations under construction.
  • CO 2 cleaning processes have been developed for a variety of components ranging from simple automotive and aerospace parts to complex circuits such as electronic components, optical systems or missile gyroscopes.
  • the cleaning by the supercritical fluid can be achieved by simple soaking, immersion in the supercritical fluid, possibly stirred by blades, or the parts to be cleaned can be subjected to the action of supercritical fluid jets .
  • the documents US-A-5,267,455 and US-A-5,412,958 relate to a dry cleaning installation, using a supercritical fluid, such as CO 2 , in which the parts to be cleaned are placed in a drum or basket rotating inside an autoclave.
  • a supercritical fluid such as CO 2
  • the rotating drum or basket is supported by two sets of rollers and is magnetically coupled to a motor, preferably electric.
  • a motor preferably electric.
  • other drive means are possible, but they are not described.
  • the autoclave has no filter or spray device.
  • a method and a device for cleaning parts by the action of a jet of a supercritical fluid (CO 2 ) are known from the document EP-A-0 893 166 .
  • the object of the present invention is to provide a method and a device for cleaning with a dense fluid under pressure, which meets, inter alia, the needs mentioned above.
  • the object of the present invention is further to provide a method and a device for cleaning with a fluid under pressure, which does not have the disadvantages, limitations, defects and disadvantages of the methods and devices of the prior art and which solves the problems of the prior art.
  • the process associates several mechanical effects with the simple contacting, or simple soaking, of polluted, contaminated parts with the dense fluid under pressure, these mechanical effects are, respectively, the stirring effect, stirring due to the movement of the basket or the drum in which the parts are located and, on the other hand, the stripping effect due to the impact of the jets of dense fluid at high speed on the parts.
  • This high-speed jet makes it possible to perfect the cleaning and to eliminate any residual contamination of the parts.
  • the basket or drum set in motion by a shaft in direct contact with drive means there is no limitation to the amount and weight of the parts that can be cleaned, as is the case. case when the basket, generally rotating, is actuated by a magnetic system, for example.
  • the fact that the shaft is in direct contact with the drive means ensures a quasi torque unlimited, which depends only on the power of the drive means, such as an electric motor, ensuring generally rotational movements.
  • the method according to the invention eliminates all the torque limitations that are encountered in the processes where the agitation is provided by blades, by magnetic drive or by a system based on reaction forces due to jets. fluid.
  • the simultaneous continuous separation, during the cleaning, of the solid and / or liquid particles insoluble in the dense fluid by separation means provided inside the pressure vessel itself makes it possible to trap the contaminants and / or extracted pollutants, generated by cleaning, agitation action, and the effect of jets at high speed and to avoid the redeposition of contaminants and / or pollutants on the parts being cleaned and already clean.
  • the drum or basket may be rotated; the direction of rotation possibly being periodically reversed.
  • the drum or rotating basket can also be animated by a pendulum movement.
  • high-speed jet generally means a fluid velocity of 1 to 500 m / sec, which makes it possible to ensure optimum stripping of the part subjected to the action of this jet. that is to say, struck by this jet.
  • the rotational speed is generally 5 to 500 revolutions per minute.
  • the continuous separation of the solid and / or insoluble liquid particles generated is generally carried out by a filtration operation, possibly preceded, followed or associated with an absorption operation, which ensures extremely efficient separation and trapping of said solid particles and or insoluble liquids.
  • the fluid in the dense state under pressure is preferably brought into contact with the parts to be cleaned at a pressure of 100 to 300 bars and at a temperature of 15 to 80.degree. at 60 ° C.
  • the treatment conditions are much less severe than those of the processes of the prior art using dense fluids under pressure, which results in considerable energy savings for the process of the invention.
  • the milder conditions namely low temperatures, low pressures and low treatment time of the process of the invention, are precisely due to the combination, according to the invention, of the agitation caused by the drum or basket in motion, of the action of the high-speed jet of dense fluid, and the continuous separation of solid and / or fluid-insoluble liquid particles, from the dense fluid under pressure.
  • the process according to the invention has, of course, all the inherent advantages associated with the use for cleaning a dense fluid under pressure, instead of a conventional solvent, in particular of the halogenated hydrocarbon type.
  • said dense fluid under pressure is a fluid in the liquid state and / or supercritical, that is to say that the dense fluid is under a pressure and at a temperature, such that the fluid is in the state liquid and / or supercritical, more preferably the fluid is in the supercritical state.
  • a gaseous compound is used, for example, under normal conditions of temperature and pressure, and its density is increased by increasing its pressure.
  • the temperature By also changing the temperature, one will thus be placed in the field where the fluid is in the dense state and under pressure, preferably in its liquid and / or supercritical state. This field can be easily determined by the skilled person in this field of the art.
  • the extractive properties of the fluid can be varied in a controlled manner by acting on the two parameters of temperature and pressure, while remaining in the dense and under pressure range, preferably the liquid and / or supercritical of the fluid in question: thus, the increase in pressure and temperature increase the solubilization capacity, while the Decreasing the pressure decreases the viscosity and increases the diffusivity.
  • compression / decompression cycles preferably very fast with, for example, an amplitude of the pressure variation of 10 to 100 bars, and time intervals. from 10 seconds to a few minutes, for example, 10 minutes, all, for example, for one to a few hours, for example, 10 hours.
  • the fluid used may be chosen, for example, from carbon dioxide, sulfur hexafluoride, nitrous oxide, nitrous oxide, light alkanes having, for example, from 1 to 5 carbon atoms, such as methane, ethane, propane, butane, isobutane, pentane, alkenes, such as ethylene and propylene, as well as certain organic liquids, such as methanol and ethanol, etc.
  • Carbon dioxide is preferred because it has the advantage of being relatively easy to implement: it is cheap, non-toxic, non-flammable and has easily accessible critical conditions (critical pressure: Pc of 7.3 MPa and critical temperature). Tc 31.1 ° C).
  • the CO 2 in the dense state under pressure, liquid or supercritical, solubilizes most organic compounds with molar masses less than or equal to 2000 g / mol. It is therefore an excellent solvent, particularly vis-à-vis organic compounds, called “undesirable", forming the bulk of contaminants, and pollutants.
  • the low viscosity of CO 2 in the dense state makes it possible to clean complex parts by their shapes and their physical characteristics, in particular when in the presence of adsorption phenomena, whether on the surface or in the heart of the room.
  • the two characteristics of pressure and temperature make it possible to control a fluid whose solubility is variable in terms of solubilization, in particular of contaminants, pollutants, undesirable compounds, parts and extraction kinetics.
  • Treatment in CO 2 atmosphere can avoid the risk of oxidation and improve the final surface state of the room.
  • a compound called "cosolvent”
  • cosolvent is added to the dense fluid, under pressure.
  • cosolvent ensures extraction, elimination, selective unwanted organic compounds, while sparing the constituent compounds of the parts.
  • said cosolvent is chosen, for example, from water, aqueous solutions, alcohols, for example aliphatic alcohols of 1 to 5 C, such as ethanol, methanol, butanol, ketones, such as acetone, and mixtures thereof.
  • alcohols for example aliphatic alcohols of 1 to 5 C, such as ethanol, methanol, butanol, ketones, such as acetone, and mixtures thereof.
  • aqueous solutions mention may be made of detergent solutions such as anionic and / or cationic surfactants, solutions of complexing agents, chelating agents, buffer solutions, for example of phosphate and / or hydrogen phosphosphate, etc. ; solutions of antioxidants, such as ascorbic acid, to stabilize the material.
  • detergent solutions such as anionic and / or cationic surfactants, solutions of complexing agents, chelating agents, buffer solutions, for example of phosphate and / or hydrogen phosphosphate, etc.
  • solutions of antioxidants such as ascorbic acid
  • said cosolvent is added to the dense fluid, under pressure, in a proportion of from 0.01 to 10% by weight, preferably from 0.02 to 1% by weight, more preferably from 0.02 to 0, 1% by weight.
  • Cosolvent if it is water, may be partly present in the parts to be cleaned, and we will not add to the fluid supercritical than the amount needed to give the concentrations mentioned above.
  • the dense fluid, under pressure, located in the pressure vessel, and added with a cosolvent, preferably in the proportions mentioned above, is also subject to to the action of ultrasonic waves.
  • the dense fluid under pressure is CO 2 and the cosolvent is water or an aqueous solution.
  • the frequency of said ultrasonic waves preferably varies from 20 kHz to 100 MHz, more preferably from 20 to 1000 kHz or from 1 to 100 MHz, such ultrasonic waves are also qualified, respectively, of ultrasound or megasons .
  • the duration during which the fluid is subjected to the action of ultrasonic waves is generally from 1 to 60 minutes.
  • the ultrasounds are multifrequency ultrasounds of 20 to 1000 kHz or multifrequency megasons of 1 to 100 MHz, such ultrasounds or megasons are produced either by probes whose emission covers several frequencies, or by the association of single-frequency probes whose resulting emission covers several frequencies.
  • sonotrode models there are several sonotrode models, some not specific allow the emission of a "bouquet" of frequencies from 20 to 100 kHz, as we used for the tests described in Example 8 below.
  • sonotrodes whose spectrum is narrower, for example from 20 to 25 kHz. It is then possible to envisage a device comprising two or three or more sonotrodes, which makes it possible to cover a very wide area, thanks to their couplings, for example: it will be possible to associate a sonotrode of 20 kHz and one of 200 kHz, etc.
  • any type of room can be treated by the method of the invention.
  • the material (s) of these pieces can (wind) be organic (s), mineral or other.
  • Parts can be parts composites comprising the combination of several materials.
  • the method of the invention knows no limitation as to the size and / or the weight of the parts to be treated, in particular, thanks to the specific drive mode chosen.
  • the materials, which can be cleaned by the process of the invention are generally solid materials, such as metals, metal alloys, possibly plated, such as aluminum, titanium, steel, stainless steel, copper, brass, and any other alloy, or metal plated.
  • the parts made of these materials will therefore be, for example, aeronautical, automobile, timepiece and micromechanical parts, electrical and electronic connectors, microelectronic silicon components, such as wafer plates, medical tools. , etc.
  • cleaning is meant, in general, the elimination, extraction of pollutant compounds, undesirable contaminants, which are not normally part of the constituent material parts.
  • pollutant and contaminant compounds to be extracted can be found both on the surface of the room, but they can also be inside the material of the room, within, for example, its porosity.
  • the method according to the invention makes it possible to clean the parts of any contaminating contaminating inorganic and organic compound found in or on the part.
  • the inorganic and / or organic compounds may be products present accidentally or naturally on the parts, but they may also be, in particular, products introduced into and / or applied to the parts, during previous operations, entering their process. manufacturing and / or assembly.
  • oils used in metalworking such as cutting, machining, quenching and dyeing oils.
  • the extracted inorganic compounds removed by the cleaning method according to the invention are, for example, free metals or metalloids or compounds of metals or metalloids.
  • compounds of metals or metalloids are meant all compounds derived from these metals or metalloids, in particular their oxides or salts, organometallic derivatives, etc.
  • the salts mention may be made of nitrates, sulphates and chlorides. , etc., hydrated or not.
  • the process according to the invention is therefore particularly advantageous in the context of the decontamination of materials contaminated with radioactive products, for example organic compounds, contaminated with radioelements such as strontium, cesium, iodine, americium, plutonium, uranium, thorium. , tritiated organic compounds, etc.
  • radioactive products for example organic compounds, contaminated with radioelements such as strontium, cesium, iodine, americium, plutonium, uranium, thorium. , tritiated organic compounds, etc.
  • the organic compounds which can also be removed by the process according to the invention, are all the organic compounds likely to be found in or on the material of the parts accidentally, naturally or for purposes, other, for example, during treatments entering in their manufacturing process and / or assembly.
  • low-viscosity lubricants of the type of cutting oils such as Mobil Mobilube ® , Mobil DTE 24 ® , Castrol Variocut B27 + ® , paraffin oils such as Shell Neatcut XF15 ® , machining oils.
  • fatty acids from, for example, fingerprints on optical materials can also be cited.
  • the ranges of temperature and pressure used during the cleaning operation may vary, provided that the fluid always remains a dense fluid under pressure, preferably in a liquid and / or supercritical state, likewise as mentioned above, compression / decompression cycles can be performed.
  • the ranges of temperature and pressure are a function, in particular, of the nature of the fluid used.
  • Such conditions can be maintained for the duration of the process, or only at the beginning of the cleaning or treatment process, where such conditions corresponding to a high density and a high temperature - the predominant phenomenon being solubilization - allow to extract, to eliminate, very quickly the compounds outside the matrix forming the part.
  • the duration of the cleaning treatment is 1 or a few minutes, for example.
  • 10 minutes at one or a few hours, for example, 5 hours, depending on the flow rate of the fluid and the amount of material to be treated.
  • this time is low compared to the duration of the processes involving neither stirring in the drum or rotating basket, nor action of a jet of fluid at high speed, nor continuous separation.
  • the level of solvent used that is to say the weight of dense fluid - solvent, preferably liquid and / or supercritical, implemented relative to the surface of the room (s) to clean, can vary from 0 to 100 kg of fluid / cm 2 of room (s). According to a further advantage of the invention, the level of solvent used is significantly lower, thanks to the effects of agitation and fluid jets, to that of the prior art.
  • the method according to the invention comprises, after cleaning, a recycling of the fluid, after one or more physico-chemical separation steps to separate the fluid extracts, and the gaseous fluid is recycled, reconditioned to the cleaning step, to the pressure vessel.
  • the first separation steps consist of a decrease in the density of the fluid by a series of successive detents and reheating, in order to approach the gaseous state.
  • the solvent power of the fluid decreases and thus part of the previously solubilized extracts are recovered during the cleaning or extraction step.
  • the method, according to the invention of cleaning parts makes it possible to recover physically at the end of treatment, on the one hand, the cleaned parts, on the other hand, undesirable products, including the handling, the treatment or the elimination can be done specifically and therefore easily controlled, while the gas or fluid can advantageously be recycled, to achieve a new extraction or cleaning.
  • the process may comprise, inter alia, a step of distillation of the dense fluid allowing almost complete purification, in accordance with the document FR 85 13246 of 06/03/1985 which describes a method and a device for the extraction of constituents by a supercritical fluid.
  • the cleaning or extraction process can be carried out in a closed circuit or in a loop, which advantageously means that, thanks to an initial and constant fluid load, such as CO 2 , it is possible to progressively eliminate parts, contaminating compounds, unwanted pollutants.
  • the process according to the invention advantageously comprises one or more steps, for example up to 3 physicochemical separation steps, in which the density of the fluid is reduced by example by a series of detents and reheating successively to the number, preferably from 1 to 3, to approach the gaseous state.
  • the conditions prevailing in these successive stages will be, for example, the following: 90 bars and 50 ° C., 70 bars and 40 ° C. and 50 bars and 40 ° C.
  • These extracts are in the form of more or less fluid concentrated liquids, and can be specifically treated and usually they are destroyed.
  • the gas obtained at the end of the separation is preferably recycled to the cleaning and extraction stage, where it is reconditioned, in order to put it back under conditions of temperature and pressure so that it is in a supercritical state, the gas can thus be first cooled to atmospheric pressure, stored in liquid form, then heated and compressed before being sent to the cleaning or extraction process itself.
  • the fluid Prior to recycling, the fluid is preferably purified by one or more adsorption and / or liquefaction and / or distillation steps.
  • the adsorption can be carried out, for example, with activated charcoal or other adsorbent, such as zeolite ® and the (re) distillation is preferably carried out using the specific device disclosed in FR 85 131246 .
  • This purification carried out by adsorption for example, by passage through activated carbon and / or by distillation and / or by liquefaction makes it possible to eliminate traces of organic products. volatile and / or insoluble in CO 2 and mechanically driven by it during the previous steps of separation.
  • a final step is taken to relax, depressurize or decompress the pressure vessel with the cleaned parts that are there.
  • the dense fluid under pressure (initial fluid) is replaced by another lower enthalpy fluid which is chemically inert.
  • this other fluid, chemically inert may be selected from nitrogen, helium, neon and dry air, etc.
  • a regulation can take place between the temperature of the wall (using a probe) and the opening percentage of the expansion valve.
  • the expansion is then continued to atmospheric pressure and a temperature of 50 to 10 ° C.
  • the invention further relates to a cleaning installation comprising the device.
  • FIG. 1 An example of a device according to the invention is described on the figure 1 .
  • the device comprises, firstly, a closed sealed chamber (1), more commonly known autoclave, may be pressurized and can withstand the working pressures, implemented according to the invention.
  • the enclosure or autoclave (1) will therefore be designed to withstand pressures generally equal to or greater than 120 bar.
  • the material used to make the autoclave is preferably a material compatible with contact with a dense fluid under pressure, thus, the enclosure will usually be stainless steel.
  • the enclosure or autoclave usually has, as shown on the figure 1 a straight cylinder shape, of a diameter, preferably from 1 to a few tens of centimeters, for example 10 cm to 1 to several meters, for example 20 m; and a length of a few tens of cm, for example 20 cm to several m, for example, 20 m.
  • the volume of the autoclave is variable depending on the parts to be cleaned and will be, for example, 1 1 to 10 m 3 , but does not, in principle, limited in accordance with the invention.
  • the autoclave or cylindrical chamber is preferably placed so that its main axis and its generatrices are horizontal. This arrangement allows easy loading of the parts to be cleaned.
  • one of the circular bases of the cylinder Preferably, opposed to the drive means, form a door (2) loading-unloading, preferably with a quick opening-closing system, allowing a fast loading and unloading and front parts.
  • the autoclave can be positioned vertically, while retaining all the quick-closing devices.
  • the autoclave or enclosure is generally provided with a jacket (not shown) supplied with heat transfer fluid to adjust the temperature inside the enclosure in the required temperature ranges, including supercritical.
  • a basket or drum in motion (3) in which are placed the parts to be treated.
  • this drum or basket (3) is a rotating drum or basket, that is to say it is driven by a rotational movement.
  • the rotational speed can range, for example, from 5 to 500 rpm, the rotational movement can be periodically reversed.
  • the movement can also be pendulum.
  • This revolving drum or basket is, like the autoclave, generally in the form of a straight, horizontal cylinder whose main axis (of rotation) merges, preferably, with the main axis of the autoclave .
  • the autoclave and the basket are therefore like two horizontal straight cylinders of common horizontal main axis, the cylinder forming the autoclave containing the smaller cylinder forming the basket or drum.
  • the drum or rotating basket has a diameter of 1 to a few tens of cm, for example 10 cm to several meters, for example, 5 m; and a length of a few tens of cm, for example 20 cm to several meters, for example, 20 m.
  • the mass of the loaded parts can thus go, for example, from 1 kg to 10 tons.
  • This drum or basket is openwork, with openings of varying shapes, it may be, for example, consisting of a lattice or a grid and thus defined a "squirrel cage" with more or less loose mesh.
  • This drum or basket is made of a material supporting the conditions in the chamber and the contact with a dense fluid, under pressure, this material is generally similar to the material constituting the autoclave.
  • the piece or parts are arranged inside the drum or basket rotating on or in supports, such as clamps, claws, "racks" or lockers, fixed or mobile, for example animated by a translation, rotation or other motion.
  • supports such as clamps, claws, "racks” or lockers, fixed or mobile, for example animated by a translation, rotation or other motion.
  • the movement of the support (s) can be printed by a tree in direct or indirect contact with the driving means, for example, with the rotor of the electric motor, preferably this shaft is also the drive shaft of the drum.
  • the basket or drum is generally rotated about its horizontal axis, via a horizontal shaft (4) located in the extension of the horizontal axis of the cylindrical basket or drum, and fixed to the circular base (5). ) of the drum, on the opposite side to the loading-unloading door (2) of the autoclave (1).
  • This shaft passes through the wall or walls of the autoclave, namely the circular base of the cylinder (6) opposite to the base forming the door (2) or loading opening, in the center of the latter.
  • the tightness through the wall of the enclosure or autoclave is provided by a rotating seal (7) pressure-tight, up to a pressure that can go, for example up to 350 bar.
  • This shaft or shaft (7) which can be defined as an axis or transmission shaft is preferably a shaft or hollow shaft, which thus conveniently provides the supply (8) of the enclosure and the drum in dense fluid under pressure, such as CO 2 , and its evacuation (9).
  • the shaft is in direct engagement via a coupling block (10) with drive means, such as an electric motor (11) of adequate power, located outside the enclosure.
  • drive means such as an electric motor (11) of adequate power
  • the loading / unloading door of the autoclave can itself be provided with an orifice connected by a flexible cord, resistant to pressure and not impeding its movement, which allows the evacuation and / or feeding of the autoclave.
  • the autoclave in dense fluid under pressure.
  • the device according to the invention further comprises means for subjecting the parts, simultaneously with their contact with the fluid or to their immersion in the dense fluid under pressure, to the action of a jet at high speed. dense fluid under pressure.
  • These means consist of one or more nozzle (s) or nozzle (s) for spraying fluid at a very high speed, which allow mechanical etching surfaces.
  • This second mechanical effect is added to the first mechanical effect due to the rotating basket and the solvent effect due to the dense fluid under pressure in contact with the parts. It has indeed been shown that during the expansion of the fluid through a restrictor, the fluid, such as CO 2 , does not instantly lose its density. It decreases rapidly, but gradually in the jet at the restrictor outlet. The speed and residual kinetic energy are sufficient to create a significant mechanical effect to extract and strip contaminants on the surface of parts to be cleaned.
  • the supply pressure of the dense fluid under pressure arriving at the nozzle (s) is generally 10 to 500 bar.
  • a pressure differential generally 500 to 10 bar, can be reached between the upstream portion and the downstream portion of the restrictor device (s) or nozzles.
  • the nozzle (s) can (wind) be fixed (s) or mobile (s) and this or these nozzle (s) can (wind), likewise be placed (s) on one or more support (s) fixed (s) and / or mobile (s).
  • This or these support (s) can (wind) occur, for example, in the form of arms, ramps, crowns or others, fixed or animated with a rotational movement, translation, for example, type back and forth , or others.
  • the nozzles may be attached to an arm or rotating crown.
  • Each support can carry from 1 to 100 nozzles, depending on the size of the autoclave and depending on the geometry of the parts to be cleaned.
  • Each nozzle (13) may generate one or more jets (14) of conical or flat shape, thus scanning the entire basket and the parts to be cleaned.
  • the nozzle or nozzles and / or their support is (are) in motion, the latter is printed by a shaft in direct or indirect engagement with the drive means, for example, with the rotor of the electric motor.
  • the movement of the nozzle (s) and / or their support (s) can be associated, in addition to the movement of the basket or drum, the movement of the support of the parts, which allows to expose the whole different faces to clean, the effect of the jet or jets under one or more angles: this is particularly interesting in the case of cleaning complex parts.
  • the nozzle or nozzles can be fed with dense fluid under pressure, such as CO 2 , or by the main circuit, that is to say by the same circuit that allows the filling of the autoclave by the shaft.
  • dense fluid under pressure such as CO 2
  • the main circuit that is to say by the same circuit that allows the filling of the autoclave by the shaft.
  • hollow see description of the installation, below
  • its compression pump or by a secondary circuit, wherein all or part of the fluid, such as CO 2 , is recycled by a recirculating auxiliary pump.
  • the device according to the invention also comprises means for continuously separating, within the closed enclosure, the solid and / or liquid particles of the dense fluid under pressure. These separation means are intended to trap solid and / or insoluble liquid particles of contaminants or other, extracted, entrained, so as to avoid the recontamination of clean cleaned parts, by redeposition of these particles.
  • the filtration means are generally constituted by filtration means, possibly combined with absorption means.
  • the filtration means will take the form of a filter, called “anti-redeposition filter” (15) or “pollution trap”. It is generally a filter of specific shape, preferably removable, and metallic. This filter can thus have a semi-cylindrical shape (see figure 1 ) and be provided with windows or slots judiciously oriented relative to the direction of rotation of the basket, which makes it possible to trap in particular the solid particles, such as the metal particles and the non-soluble fraction of the eliminated contaminants, and to avoid that these These are redeposited on the clean rooms.
  • the windows or slots must be oriented in the direction of rotation.
  • the solid particles or “chips” are removed in part by the centrifugal force due to the basket rotation, as it rotates clockwise or vice versa, and these slots will have to be rotated to capture the particles that escape the basket and cleaning parts to the filter without allowing them to escape and return to the basket to recontaminate the parts.
  • the filter may, in other words, be in the form of a filter, for example, a metal in the form of a semicircle perforated by windows of particular shapes, which take into account the direction of rotation, in which an absorbent material, such as paper or absorbent fabric, may be placed and which collects and traps liquid particles from the non-soluble fraction in the fluid, such as CO 2 , set in motion by circular agitation and / or mechanical effects induced by the ramp (s) nozzle (s), as well as solid particles, chipes "and” microchips "of metal and other, completely random forms, produced during the machining of parts, in particular metal, being the subject of an operation of cleaning.
  • a filter for example, a metal in the form of a semicircle perforated by windows of particular shapes, which take into account the direction of rotation, in which an absorbent material, such as paper or absorbent fabric, may be placed and which collects and traps liquid particles from the non-soluble fraction in the fluid, such as CO 2 , set in motion by circular agit
  • the device according to the invention may comprise means (not shown) for subjecting the dense fluid under pressure located inside the chamber to the action of ultrasonic waves.
  • These means generally comprise one or more devices, more sonotrode frequency generators, for generating sound waves, ultrasound and / or megasons, for example a mono or multifrequency frequency generator and from one to ten sonotrodes.
  • sonotrodes are generally placed at regularly spaced points inside the enclosure, for example in the longitudinal axis of the autoclave (a sonotrode) or in the radial axis of the autoclave (from one to ten sonotrodes). spaced a few centimeters (5 cm) to a few tens of centimeters (20 cm) depending on the size of the enclosure.
  • the sonotrode Only the sonotrode can be placed in the enclosure, thanks to a pressure-tight passage that nevertheless allows its vibration. Or, the sonotrode plus the transducer can be placed in the enclosure, which then requires only a sealed passage for the power supply cable of the sonotrode to the frequency generator.
  • the sonotrode (s) is only a block with the transducer part and is (are) connected to the frequency generator by a coaxial cable for the generation of sound waves of adequate frequency (s) (s), etc.
  • the figure 2 represents, schematically, a sectional side view of the installation according to the invention.
  • the installation according to the invention is substantially analogous to a conventional installation for the treatment or cleaning of parts by a dense fluid under pressure, for example supercritical, except that it implements instead of autoclaves conventional, a specific autoclave or extractor, as described in figure 1 .
  • the autoclave can also be driven by a movement, for example, rotation, preferably, being driven by the same shaft or axis as the basket or rotating drum.
  • the autoclave is capable of withstanding the pressure used in the process of the invention and is also provided with heating and temperature control means in the form of, for example, a thermostatically controlled double jacket (not shown ), in which circulates a suitable heat transfer fluid.
  • the volume of the autoclave is variable, it depends in particular on the volume of the parts to be treated, it can be easily determined by the skilled person.
  • the extractor or autoclave receives the parts to be cleaned (25), which are preferably placed on one or more support (s) or grid (s), inside the basket or rotating drum (22).
  • the installation shown has only one extractor or autoclave (21), it is obvious that the installation can include several extractors, for example, from 2 to 10, arranged, for example, in series.
  • the installation also comprises means for bringing a fluid, such as CO 2 in the dense state and under pressure, for example in the supercritical state.
  • a fluid such as CO 2 in the dense state and under pressure, for example in the supercritical state.
  • the fluid for example, CO 2
  • a recycling pipe (26) and / or optionally a storage tank and, for example, of CO 2 (27) penetrates t it, via a valve (28) in a liquefaction tank (29) provided with temperature regulation means in the form of a thermostatically controlled double jacket (210), in which circulates a suitable heat transfer fluid ( 211, 212).
  • Said fluid such as CO 2
  • a flowmeter (213) for example, a compression pump type membrane or piston or, for example, a compressor to the autoclave (21).
  • the fluid for example, the CO 2 pumped
  • a heat exchanger 216
  • said exchanger "supercritical" in which it is reheated to be in conditions where it is in the form of a dense fluid under pressure, in particular a supercritical dense fluid.
  • the fluid is, in this exchanger warmed beyond its critical temperature which is, for example, 31.1 ° C, in the case of CO 2 .
  • the fluid is (see figure 1 ) preferably introduced into the autoclave, via the drive shaft of the basket or rotating drum, which is hollow.
  • the same circuit also feeds the nozzles or spray nozzles provided in the autoclave.
  • cosolvent injection means are also shown in the form of a high-pressure pump (217) fed by a cosolvent tank (218), which allows the gradual addition of a known amount of cosolvent into the compressed fluid, via a pipe (219) connected to the fluid supply pipe of the extractor (21), upstream of the exchanger (216) and downstream of the compression pump ( 214).
  • the fluid or, optionally, the fluid and cosolvent mixture comes into contact with the parts and cleans them in the enclosure of the extractor (21), while the same fluid is sprayed at high speed over the parts .
  • the pollutant pollutant compounds are thus extracted.
  • one or more pieces will be processed simultaneously.
  • the supercritical fluid will be, for example, a homogeneous solution of fluid, such as CO 2 alone or CO 2 with cosolvent.
  • the stream of fluid such as CO 2 in which the polluting compounds, contaminants, and extracts removed from the parts are solubilized, is then preferably sent via the same hollow shaft used for feeding, or through an orifice located at side on the same side or placed on the opposite side on the door allowing the opening of the autoclave for loading - unloading parts, to separation means connected to the extractor or autoclave (21) and comprising, for example , three cyclone separators (220, 221, 222) connected in series, each of which is preceded by an automatic expansion valve (23, 24, 25).
  • separation means connected to the extractor or autoclave (21) and comprising, for example , three cyclone separators (220, 221, 222) connected in series, each of which is preceded by an automatic expansion valve (23, 24, 25).
  • the expansion to which the fluid is subjected operates at a constant temperature.
  • each separator a separation or demixing takes place, on the one hand, extracted organic compounds which are in liquid form and, on the other hand, a gas, for example, CO 2 .
  • the compounds extracted from the parts are withdrawn (226, 227, 228), for example, at the base of the separators, and recovered, then possibly subjected to new operations of separation, extraction or purification, for example, centrifugation, decantation or liquid / liquid extraction, or destroyed.
  • the gas resulting from the separation, such as CO 2 is purified and then sent into the fluid recycling means, which essentially comprise a pipe (26) and a "cold" exchanger (229) or liquefier, for example, in the form of a thermostatically controlled enclosure, to be directed to the liquid reservoir (29) at low temperature, maintained by means of a cooling bath which cools and liquefies the fluid (211, 212), such as CO 2 .
  • the fluid recycling means which essentially comprise a pipe (26) and a "cold" exchanger (229) or liquefier, for example, in the form of a thermostatically controlled enclosure, to be directed to the liquid reservoir (29) at low temperature, maintained by means of a cooling bath which cools and liquefies the fluid (211, 212), such as CO 2 .
  • the purification means (230) have been represented on the figure 2 by a reflux column or an activated carbon column (230) placed on the fluid recycling means.
  • the dense fluid under pressure can be recirculated continuously during cleaning by means of a recirculation pump (231).
  • the insoluble particles are trapped on the filter inside the autoclave (not shown).
  • the particles trapped on the filter are generally recovered at the end of the cleaning operation, when opening the autoclave and removed as solid waste or recovered for the purpose of recycling.
  • the device may furthermore comprise means for introducing another lower enthalpy fluid than the dense fluid under pressure, inside. pressure chamber, and replace all or part of it during a final step of relaxation.
  • the introduction of the lower and chemically inert enthalpy fluid is through the top or bottom of the autoclave according to the respective densities of the lower enthalpy fluid and chemically inert and the dense fluid under pressure to be removed.
  • control means (not shown), in particular the pressure, in the various parts of the process, which comprise a control chain composed of pressure sensors, regulators and pneumatically controlled needle valves.
  • regulation can take place between the wall temperature (using a probe) and the opening percentage of the expansion valve.
  • the samples to be cleaned are specimens and / or pieces of complex shapes of aluminum, previously contaminated with various oils used in metalworking, such as a water-soluble machining oil, a cutting oil, a dye oil as respectively oils available commercially as Cimstar 560 ® , Mobil Mobilube ® , Drawsol 2345 N ® .
  • the specimen is placed more than 5 cm from the outlet of the nozzle.
  • the contaminant mass is determined by weighing before and after cleaning with CO 2 .
  • Table 1 presents this comparison, with the nature of the contaminant, the surface contamination and the operating conditions.
  • Table 1 ⁇ / u> Comparison of supercritical CO 2 cleaning efficiencies by dipping and spraying through a nozzle, on a 20% machining oil Cleaning Supercritical CO 2 by soaking CO 2 supercritical by jet Contaminant 20% machining oil 20% machining oil Surface contamination before cleaning in ⁇ g / cm 2 121 70 Operating conditions 300 bar, 44 ° C, 2 h 100 bar, 40 ° C, 1 h Surface contamination after cleaning in ⁇ g / cm 2 17 ⁇ 1 Cleaning efficiency 86% 100%
  • This example shows an improvement of the cleaning efficiency induced by the mechanical effects brought about by the use of CO 2 sprayed at high speed.
  • the nature of the contaminant which is in this case a relatively viscous mineral oil, is modified.
  • the supply of mechanical energy through jets shows that it is possible to maintain very good cleaning performance, while decreasing by a factor of 2, the treatment time.
  • the gain induced by the invention will be on the amount of solvent and is therefore energy.
  • Examples 4 and 5 below relate to the cleaning of real parts.
  • This example involves coating contaminants with real aluminum parts and complex shapes comprising several faces, as well as one or more holes for drilling.
  • the overall size of these pieces does not exceed 10 cm in length and 6 cm in height.
  • the evaluation of the efficiency is carried out by weighing the tare and the contaminant before and after cleaning and the efficiency is determined by the formula given above. In this case, it is used in this formula, the overall mass of contaminant and not the basis weight, as in the previous examples, the surface of a real part being difficult to obtain accurately.
  • the selected contaminants are those of the preceding examples: the water-soluble 20% water-based machining oil (of Example 1), the cutting oil (of Example 2) and the dyeing / inking oil (from Example 3).
  • This example 4 is the reference for a supercritical CO 2 cleaning operation, without any mechanical effect and based on the unique power of dissolution, vis-à-vis the contaminants studied and shown in the following Table 4.
  • This example consists of treating pieces of complex shapes contaminated with different oils identical to Example 4.
  • the parts, 15 in number per test are treated in the rotating autoclave, but not equipped with the jet device. and anti-redeposition filter, that is to say that the parts are subjected to agitation due to the single rotary movement of the basket or drum.
  • Table 5 shows the contaminants, their masses, the treatment conditions and the efficiencies obtained.
  • the efficiency remains optimal at 100%, with a net gain over time of treatment, which goes from 1 hour, for example 4, to 1 ⁇ 2 hour, for example 5.
  • the gain is essentially energetic, thanks to a reduction of treatment time, and therefore of the CO 2 solvent level.
  • the efficiency reaches 94%, with stirring, in about 1 hour, against 90% efficiency in 2 hours of treatment (for example 4 reference). In this case, the efficiency is improved while reducing the treatment time.
  • a nozzle manifold for projecting CO 2 , at very high speed, was implemented, as well as a perforated metal filter and absorbent paper, all to allow trapping the insoluble particles of the contaminant detached from the surface of the parts by the jet of CO 2 and the rotary movement of the basket.
  • This example shows that for the water-soluble machining oil, the use of nozzles and a filter retaining the fraction insoluble in CO 2 makes it possible to obtain an efficiency very close to 100%. for a treatment time not exceeding 1 ⁇ 2 h. In this case, a gain is obtained jointly on the efficiency and the time of treatment, but also on the working pressure where one goes from 300 bars (example 5) to 100 bars.
  • the cleaning efficiency is maintained at 94%, with an equivalent treatment time of about 70/75 minutes.
  • the CO 2 treatment conditions are significantly different. Indeed, these conditions evolve from 300 bar, 80 ° C, for example 5, 100 bar, 40 ° C, in this example, with nozzles and filter, which is a considerable energy gain.
  • the temperature is monitored using a thermocouple placed inside the enclosure.
  • Test n ° 1 shows that during a relaxation considered fast of 8'15 '', the final decompression temperature reaches -50 ° C, with formation of dry ice for a pressurized fluid at 240 bar and 43 ° C.
  • test No. 2 shows that a final temperature of the fluid in the autoclave of 17 ° C is obtained for a total depressurization time of 11'. 30.
  • the difference obtained between the two tests is + 67 ° C for only 4'15 '' more relaxation time.
  • Test n ° 3 comparable to tests n ° 1 and n ° 2, shows that by decreasing the relaxation time from 11'30 to 10 ', the final temperature of the chamber remains positive, at 2 ° C.
  • Table 8 which follows, gives the operating conditions of the various tests carried out. ⁇ u> Table 8 ⁇ / u> testing Operating conditions: dense CO 2 under pressure State of the fluid Adding a cosolvent Time Remarks 8 - 1 20 ° C; 100 bars liquid no 15 min. audible sound waves 8 - 2 20 ° C; 100 bars liquid Yes Same Highly audible sound waves 8 - 3 40 ° C; 100 bars supercritical no Same low audible sound waves 8 - 4 20 ° C; 100 bars supercritical Yes Same Highly audible sound waves 8 - 5 40 ° C; 300 bars supercritical no Same low audible sound waves 8 - 6 40 ° C; 300 bars supercritical Yes Same Highly audible sound waves
  • This test commonly used by experimentalists in the field of ultrasound, reflects, on the one hand, the existence of a wave propagation of the sonotrode to the sample and, on the other hand, the creation of cavitation by the creation of bubbles that implode in the vicinity of the sample, thus creating an alteration of the surface, visualized by the photos.
  • test 8-2 carried out under the same conditions as test 8-1, but in the presence of cosolvent, it is found that the screening of the sample is greater and results in the appearance of a hole in aluminum foil several centimeters in diameter (4 cm). In this case, the phenomenon is confirmed by a very significant increase in the audible level during the test. This proves that the presence of cosolvent in the dense CO 2 under pressure reveals the ultrasound phenomenon by amplifying it.
  • Tests 8 - 4 and 8 - 6, respectively identical to tests 8 - 3 and 8 - 5, but carried out in the presence of a cosolvent shows that the leaves of aluminum are more heavily screened with the appearance of holes of a few centimeters in diameter (from 1 to 1.5 cm), as well as a very important noise level outside the pressure vessel, tangible testimony of a phenomenon of propagation and / or increased cavitation. This demonstrates that it is the presence of cosolvent that acts as a developer and amplifier of ultrasonic phenomena in supercritical CO 2 .

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Claims (43)

  1. Verfahren zur Reinigung von kontaminierten Teilen durch In-Kontakt-Bringen mit einem dichten Druckfluid, in welchem:
    - die zu reinigenden Teile in einer Trommel oder einem Korb platziert werden, die/der sich in einem Druckbehälter befindet, der das dichte Druckfluid enthält, wobei diese Trommel oder dieser Korb durch eine direkt an außerhalb des Behälters befindliche Antriebseinrichtungen angeschlossene Welle in Bewegung versetzt wird,
    wobei dieses Verfahren dadurch gekennzeichnet ist:
    - dass die Teile außerdem simultan der Wirkung eines Hochgeschwindigkeitsstrahls des dichten Fluids ausgesetzt werden; und
    - dass simultan die im Wesentlichen durch die Reinigung erzeugten in dem dichten Fluid unlöslichen festen und/oder flüssigen Partikel durch im Innern des Behälters vorgesehene Trenneinrichtungen kontinuierlich von dem dichten Fluid getrennt werden.
  2. Verfahren nach Anspruch 1, in dem die Trommel oder der Korb in eine Rotationsbewegung versetzt wird.
  3. Verfahren nach Anspruch 2, in dem die Rotationsrichtung periodisch umgekehrt wird.
  4. Verfahren nach Anspruch 1, in dem die Trommel oder der Korb in eine Pendelbewegung versetzt wird.
  5. Verfahren nach Anspruch 1, in dem die Geschwindigkeit des Fluidstrahls 1 bis 500 m/s beträgt.
  6. Verfahren nach Anspruch 1, in dem das dichte Druckfluid eine Temperatur von 15 bis 80 °C und einen Druck von 100 bis 300 bar aufweist.
  7. Verfahren nach Anspruch 1, in dem das genannte dichte Druckfluid sich im flüssigen und/oder überkritischen Zustand befindet.
  8. Verfahren nach Anspruch 1, in dem das genannte dichte Druckfluid sich im überkritischen Zustand befindet.
  9. Verfahren nach einem der Ansprüche 1 bis 8, in dem man Kompressions/Dekompressionszyklen durchführt.
  10. Verfahren nach Anspruch 9, in dem die genannten Kompressions/Dekompressionszyklen mit einer Druckvariationsamplitude von 10 bis 100 bar und Zeitintervallen von 10 Sekunden bis 10 Minuten realisiert werden.
  11. Verfahren nach Anspruch 1, in dem das genannte Fluid ausgewählt wird unter Kohlendioxid; Schwefelhexafluorid; Stickoxid; Distickstoffmonoxid; leichten Alkanen mit zum Beispiel 1 bis 5 Kohlenstoffatomen wie Methan, Propan, Butan, Isobutan und Pentan; Alkenen wie Ethylen und Propylen; und bestimmten organischen Flüssigkeiten wie Methanol und Ethanol.
  12. Verfahren nach einem der Ansprüche 1 bis 11, in dem dem dichten Druckfluid ein Co-Solvent oder Hilfslösemittel beigemischt wird.
  13. Verfahren nach Anspruch 12, in dem das genannte Hilfslösemittel ausgewählt wird unter Wasser; wässrigen Lösungen; Alkoholen, zum Beispiel den aliphatischen Alkoholen mit 1 bis 5 Kohlenstoffatomen wie Ethanol, Methanol, Butanol; Ketonen; Hydrofluorethern; Terpenen; Cyclohexanen und ihren Mischungen.
  14. Verfahren nach Anspruch 13, in dem die genannten wässrigen Lösungen Lösungen von Detergenzien wie anionische und/oder kationische Oberflächenaktivstoffe; Lösungen von Komplexierungsmitteln, Chelatbildnern; Pufferlösungen, z.B. von Phosphat und/oder Hydrogenphosphat usw.; Lösungen von Antioxidationsmitteln, wie Ascorbinsäure, sind.
  15. Verfahren nach einem der Ansprüche 12 bis 14, in dem das Hilfslösemittel dem dichten Fluid unter Druck mit einem Anteil von 0,01 bis 10 Gew.-% beigemengt wird.
  16. Verfahren nach einem der Ansprüche 12 bis 15, in dem das sich in dem Druckbehälter befindliche dichte Druckfluid außerdem der Wirkung von Ultraschallwellen ausgesetzt wird.
  17. Verfahren nach Anspruch 16, in dem die Frequenz der genannten Ultraschallwellen von 20 kHz bis 100 MHz variiert.
  18. Verfahren nach Anspruch 17, in dem die genannten Ultraschallwellen Ultraschall mit einer Frequenz von 20 bis 1 000 kHz oder Megaschall mit einer Frequenz von 1 bis 100 MHz entsprechen.
  19. Verfahren nach einem der Ansprüche 16 bis 18, in dem das Fluid während einer Dauer von 1 bis 60 Minuten der Wirkung von Ultraschallwellen ausgesetzt wird.
  20. Verfahren nach einem der Ansprüche 13 bis 19, in dem das dichte Druckfluid CO2 ist und das Hilfslösemittel Wasser oder eine wässrige Lösung ist.
  21. Verfahren nach einem der Ansprüche 1 bis 20, in dem im Anschluß an die Reinigung durch das dichte Druckfluid das Fluid und die Extrakte durch einen oder mehrere physikalisch-chemische Trennschritte getrennt werden und das Fluid in Gasform recycelt wird.
  22. Verfahren nach Anspruch 21, in dem das gasförmige Fluid vor seinem Recycling durch einen (oder mehrere) Schritt(e) der Adsorption und/oder Verflüssigung und/oder Destillation (Redestillation) gereinigt wird.
  23. Verfahren nach einem der Ansprüche 1 bis 22, in dem man am Ende der Reinigung einen Endschritt zur Entspannung des Druckbehälters, in dem sich die gereinigten Teile befinden, durchführt, wobei man im Laufe dieser Entspannung die Gesamtheit oder einen Teil dieses dichten Druckfluids durch ein anderes und chemisch inertes Fluid mit niedrigerer Enthalpie ersetzt.
  24. Verfahren nach Anspruch 23, in dem das dichte Druckfluid CO2 ist, und das andere Fluid mit niedrigerer Enthalpie ausgewählt wird unter Stickstoff, Helium, Neon und Trockenluft.
  25. Vorrichtung zur Reinigung von kontaminierten Teilen mit einem dichten Druckfluid, umfassend:
    - einen geschlossenen Druckbehälter (1);
    - eine Trommel oder einen Korb (3), welche(r) sich im Innern des genannten Behälters befindet und die zu reinigenden Teile aufnimmt, wobei diese Trommel oder dieser Korb durch eine direkt an außerhalb des Behälters (1) befindliche Antriebseinrichtungen (11) angeschlossene Welle (4) in Bewegung versetzt wird;
    wobei diese Vorrichtung gekennzeichnet ist durch:
    - Einrichtungen (12, 13), um die Teile der Wirkung eines Hochgeschwindigkeitsstrahls (14) des dichten Fluids auszusetzen; und
    - Einrichtungen (15), um in dem geschlossenen Behälter kontinuierlich die in dem Fluid unlöslichen festen und/oder flüssigen Partikel von dem dichten Druckfluid zu trennen.
  26. Vorrichtung nach Anspruch 25, bei der der geschlossene Behälter (1) die Form eines geraden Zylinders hat, dessen Hauptachse und Mantellinien horizontal verlaufen.
  27. Vorrichtung nach Anspruch 26, bei der eine - den Antriebseinrichtungen (11) vorzugsweise entgegengesetzte - kreisförmige Basis des Zylinders eine Beladungs/Entladungstür (2) bildet.
  28. Vorrichtung nach Anspruch 25, bei der die Trommel oder der Korb (3) in eine Rotationsbewegung versetzt wird.
  29. Vorrichtung nach Anspruch 28, bei der die Trommel oder der Korb (3) die Form eines geraden horizontalen Zylinders hat, dessen Rotationshauptachse mit der Hauptachse des geschlossenen Behälters zusammenfällt.
  30. Vorrichtung nach Anspruch 29, bei der die Welle (4), die den Korb oder die Trommel in eine Bewegung bzw. Drehung um seine/ihre horizontale Achse versetzt, sich in der Verlängerung der horizontalen Achse des Korbs oder der Trommel befindet und an der zur Beladungs-/Entladungstür des Behälters entgegengesetzten kreisförmigen Basis (5) des Korbs oder der Trommel befestigt ist.
  31. Vorrichtung nach Anspruch 30, bei der die Welle die zur Beladungs/Entladungstür (2) des Behälters entgegengesetzte kreisförmige Basis (6) des geschlossenen Behälters durchquert, wobei die Dichtheit der Durchquerung der Wand des Behälters durch eine druckdichte Wellendichtung (7) gewährleistet ist.
  32. Vorrichtung nach einem der Ansprüche 25 bis 31, bei der die den Korb oder die Trommel in Bewegung bzw. Drehung versetzende Welle (4) eine Hohlwelle ist, welche die Speisung (8) des Behälters mit dichtem Druckfluid sowie seine Entleerung (9) gewährleistet.
  33. Vorrichtung nach einem der Ansprüche 25 bis 32, bei der die Einrichtungen, die ermöglichen, die zu reinigenden Teile einem Hochgeschwindigkeitsstrahl des dichten Fluids auszusetzen, durch eine (oder mehrere) ortsfeste oder bewegliche Düse(n) (13) oder Stutzen zum Spritzen des Fluids mit hoher Geschwindigkeit gebildet wird (werden), die sich eventuell auf einem (oder mehreren) festen und/oder beweglichen Träger(n) (12) befindet (befinden).
  34. Vorrichtung nach Anspruch 33, bei der jede Düse einen (oder mehrere) Strahl(en) (14) von konischer oder flacher Form erzeugt.
  35. Vorrichtung nach einem der Ansprüche 25 bis 34, bei der die Trenneinrichtungen (15) durch Filtereinrichtungen gebildet werden, eventuell kombiniert mit Absorptionseinrichtungen.
  36. Vorrichtung nach Anspruch 35, bei der die Filtereinrichtungen (15) durch einen durchbrochenen bzw. gelochten halbzylindrischen Filter gebildet werden.
  37. Vorrichtung nach einem der Ansprüche 25 bis 36, bei der der geschlossene Behälter (1) ebenfalls in eine Bewegung versetzt wird, zum Beispiel eine Rotation, vorzugsweise indem er durch dieselbe Welle oder Achse angetrieben wird wie der Korb oder die Trommel (3).
  38. Vorrichtung nach einem der Ansprüche 25 bis 37, außerdem Einrichtungen umfassend, um ein anderes und chemisch inertes Fluid mit einer niedrigeren Enthalpie als das dichte Druckfluid ins Innere des Behälters unter Druck einzuspeisen und dort während eines Entspannungs-Endschritts die Gesamtheit oder einen Teil des dichten Druckfluids auszutauschen.
  39. Vorrichtung nach Anspruch 38, bei der die Einspeisung des chemisch inerten Fluids mit einer niedrigeren Enthalpie durch die Oberseite oder die Unterseite des Autoklaven (1) erfolgt, in Abhängigkeit von der jeweiligen Dichte des chemisch inerten Austauschfluids mit niedrigerer Enthalpie und des zu eliminierenden dichten Druckfluids.
  40. Vorrichtung nach einem der Ansprüche 25 bis 39, Einrichtungen umfassend, um das im Innern des Behälters befindliche dichte Druckfluid der Wirkung von Ultraschallwellen des Typs Mega- oder Ultraschall auszusetzen.
  41. Vorrichtung nach Anspruch 40, bei der die genannten Einrichtungen, um das Fluid der Wirkung von Ultraschallwellen des Typs Mega- oder Ultraschall auszusetzen, sich in Form einer (oder mehrerer) Sonotrode(n) präsentieren.
  42. Reinigungsanlage, die Vorrichtung nach einem der Ansprüche 25 bis 41 umfassend.
  43. Anlage nach Anspruch 42 umfassend Einrichtungen zum Einspritzen eines Co-Solvents oder Hilfslösemittels in das komprimierte Fluid.
EP01980606A 2000-10-20 2001-10-19 Verfahreen, vorrichtung und anlage zum reinigen von verunreinigten teilen mit einer unter druck stehenden flüssigkeit Expired - Lifetime EP1347840B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR0013453A FR2815559B1 (fr) 2000-10-20 2000-10-20 Procede, dispositif et installation de nettoyage de pieces contaminees, par un fluide dense sous presssion
FR0013453 2000-10-20
PCT/FR2001/003249 WO2002032593A1 (fr) 2000-10-20 2001-10-19 Procede, dispositif et installation de nettoyage de pieces contaminees, par un fluide dense sous pression

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EP1347840A1 EP1347840A1 (de) 2003-10-01
EP1347840B1 true EP1347840B1 (de) 2008-09-24

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JP5626513B2 (ja) * 2010-06-16 2014-11-19 東洋製罐株式会社 容器の殺菌、洗浄方法
CN103017506A (zh) * 2012-12-05 2013-04-03 东台市食品机械厂有限公司 一种转鼓干燥器密闭罩的不拆机清洗装置
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CN109778483B (zh) * 2018-12-18 2020-05-29 珠海格力电器股份有限公司 一种摆钟式洗衣机
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DE60135929D1 (de) 2008-11-06
FR2815559A1 (fr) 2002-04-26
EP1347840A1 (de) 2003-10-01
FR2815559B1 (fr) 2002-11-29
DK1347840T3 (da) 2009-02-09
WO2002032593A1 (fr) 2002-04-25

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