EP2547452B1 - Procédé de fragmentation de déchets électroniques et de verre technique à des fins de recyclage - Google Patents

Procédé de fragmentation de déchets électroniques et de verre technique à des fins de recyclage Download PDF

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Publication number
EP2547452B1
EP2547452B1 EP11765105.9A EP11765105A EP2547452B1 EP 2547452 B1 EP2547452 B1 EP 2547452B1 EP 11765105 A EP11765105 A EP 11765105A EP 2547452 B1 EP2547452 B1 EP 2547452B1
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EP
European Patent Office
Prior art keywords
extraction
process according
shock wave
treatment
individual pieces
Prior art date
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Not-in-force
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EP11765105.9A
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German (de)
English (en)
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EP2547452A2 (fr
Inventor
Jörg BECKMANN
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00—Other disintegrating devices or methods
    • B02C19/18—Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00—Other disintegrating devices or methods
    • B02C19/0056—Other disintegrating devices or methods specially adapted for specific materials not otherwise provided for
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00—Other disintegrating devices or methods
    • B02C19/18—Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
    • B02C19/186—Use of cold or heat for disintegrating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00—Other disintegrating devices or methods
    • B02C19/18—Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
    • B02C2019/183—Crushing by discharge of high electrical energy

Definitions

  • the invention relates to a method of shredding electronic waste, i. generally electronic components, such as e.g. Circuit boards, chips and parts containing electronic components, as well as technical glass, such as picture tubes, fluorescent tubes and the like.
  • electronic components i. generally electronic components, such as e.g. Circuit boards, chips and parts containing electronic components, as well as technical glass, such as picture tubes, fluorescent tubes and the like.
  • the processing of these materials is very difficult, since different substances are present in the composite and the content of the individual materials can be very different.
  • metals various polymers, glass, semimetals and semiconductors (especially silicon), adhesives, inorganic fillers, organic chemical auxiliaries, such as. containing often bromides, oils, waxes, greases and many other possible substances.
  • the metals mainly include copper, iron, lead, zinc, tin, gold, silver, palladium and platinum.
  • the brominated flame retardants eg tetrabromobisphenol A - mass fraction up to 30%
  • these flame retardants form other brominated hydrocarbons, some of which have an even higher risk potential.
  • Such degradation products can be stored and accumulated by organisms in adipose tissue and show partial carcinogenic effects. Since since 2006 the use of bromine-containing materials in the Federal Republic of Germany is only permitted to a limited extent, old equipment is subject to a special burden.
  • a first treatment step is generally mechanical pre-shredding, for example shredding. From the shredder fraction or generally mechanically pretreated good magnetic metals can be separated with Magnettrennem, but separated depending on the degree of division not clean without additives. Organic components are often decomposed by thermal pyrolysis or wet chemical oxidative Furthermore, the electronic waste is also used as a supplement in the metal extraction in metallurgy, which corresponds to a substantial recovery of the metals in pyrolytic removal of organic components In alternative treatment methods, the leaching of the metals is operated.
  • shock wave crushing One method of obtaining relatively fine debris is shock wave crushing. From the DE 195 34 232 C2 is a basic apparatus for a concept developed by the Düsseldorf Research Center for the destruction of essentially non-metallic solids, such as mineral solids. The shock waves are triggered by rapid discharge of an electrical energy store. The material to be comminuted is located in a non-conductive or only slightly conductive process liquid.
  • the DE 100 61 386 is therefore concerned with the provision of a special four-pass reactor and reactor to handle wet oxidation in supercritical water.
  • the process developed therein does not yet solve the problem of being able to separate the other different materials within the electronic scrap, such as glass, ceramics, metals and inorganic residues, eg mixed oxides of previous treatment stages.
  • the object of the invention is to be able to process environmentally harmful scrap from complex composite multistage systems, in this case electronic waste and used technical glass, economically and ecologically efficient. Contained hazardous substances should be isolated and destroyed or returned. Base materials, such as metals and glass, are to be made available for recycling.
  • the invention is based on the idea to use a separation of substances by fine division on the one hand and targeted physical-chemical extractive treatment of the starting materials and / or the particles on the other hand in combination.
  • the method does not include the treatment of elastomeric, especially rubber-elastic and purely thermoplastic materials, which has been previously described. Rather, the method is directed to the treatment of composites of metals, polymers such as in particular polycarbonates, phenolic resins, phenol-formaldehyde resins, polyesters, polyvinyl chloride and polyolefins, optionally glass, ceramics and other reinforcements, and organic chemical auxiliaries.
  • piece goods any lumpy starting material. This may be a shredder fraction of electronic waste, which however may contain small components as such. Small components can represent general cargo per se and may not need to be mechanically pre-shredded. Frequently, mechanical pre-shredding will serve to homogenize the material to obtain a piece with particles of reasonably uniform size as the starting material.
  • the process can be carried out batchwise, ie in batch mode, continuously or semicontinuously.
  • starting material is continuously fed to an extractor designed for this purpose, for example a countercurrent extractor, taken off continuously and passed through the reaction space of a shockwave system, such as in the US 5,758,831 already shown.
  • an extractor designed for this purpose, for example a countercurrent extractor, taken off continuously and passed through the reaction space of a shockwave system, such as in the US 5,758,831 already shown. Both procedures can be combined, for example, by sequentially and separately treating larger batches of unitary starting materials in a plant designed for continuous operation.
  • devices for the treatment of materials with electrically ignited shock waves or, in other words, methods for electrohydraulic fragmentation are not only among the cited documents DE 195 34 232 C2 and US 5,758,831 known. Such devices can be used for the method according to the invention.
  • the extractant gaseous at relaxation, so that the organic residues remain behind and in part - depending on the resulting mixture - can be recovered. If the extractant is supercritical CO 2 , it is particularly preferred that supercritical CO 2 is used as the shock wave medium.
  • the organic fraction When using supercritical water as the extraction agent, the organic fraction will also separate after relaxation of the water phase and can be further treated accordingly. It is particularly preferred to use the extractant supercritical water in combination with the shockwave medium water.
  • the subsequent work-up will comprise, for example, a rectification or adsorptive separation.
  • the shock wave treatment is then carried out preferably also in an organic solvent and more preferably with the solvent selected as the extraction agent.
  • the addition of a mild oxidizing agent is preferred.
  • the solvent used is acetylacetone in a solution containing hydrochloric acid, nitric acid or halo-nitric acid and N-thiobenzoyl-N-phenylhydroxylamine is added thereto.
  • the single particle will be either metal, ceramic, glass, another inorganic base, or a high solution resistant polymer.
  • Other polymers and low molecular weight organic substances were already separated by the extraction before the shock wave treatment and disturb the separation here no longer.
  • the temperature to be selected during the shock wave treatment depends on the treatment task and the fluid medium used (the dielectric and shock wave transmission medium or the process fluid).
  • the fluid dielectric medium water, an organic liquid or supercritical carbon dioxide is used.
  • the organic liquid may preferably be a hydrocarbon, a ketone such as acetone or an alcohol, preferably methanol, ethanol, propanol, isopropanol or higher alcohols.
  • the alcohol may also be a polyol, in particular a glycol such as ethylene glycol or propylene glycol, generally a diol or a triol, in the latter preferably glycerol.
  • hydrocarbons for example hexane, heptane, cyclohexane, xylene, benzene, toluene, ethereal solvents, for example dioxane, diisopropyl ether, tetrahydrofuran or chlorinated hydrocarbons, in particular chloroform, dichloromethane, tetrachlorohydrocarbon or dichloroethylene.
  • the dielectric medium may be a liquid mixture.
  • the shock wave treatment is carried out within the inventive method at a temperature between - 80 ° C and + 50 ° C.
  • both the extraction and the shock wave treatment are carried out with supercritical carbon dioxide. This makes it possible to connect the streams of extractant and fluid shockwave medium. The use (and partial disposal) of organic liquids is avoided.
  • the piece goods are treated with acid or suspended in aqueous acid before or during the extraction.
  • the process can be carried out so that an oxidizing agent is allowed to act on the piece goods at the same time as the extraction medium.
  • Suitable are mild oxidants such as atmospheric oxygen or oxidants with a similar or lower oxidation potential than oxygen.
  • Strong oxidizing agents, eg peroxides, are not uncritical in handling and have a strong corrosive effect on the process apparatus. They should therefore be avoided.
  • the extraction medium and / or the dielectric medium are cleaned and recycled.
  • the cleaning processes can be connected in terms of process technology.
  • the extraction and the shockwave treatment follow one another directly. Intermediate steps are not required.
  • the process parameters (pressure, temperature) for the extractant and the shock wave medium can be set identical, so that the transfer of the substances to be treated and the connection of the process cycles between extraction and shock wave treatment is simplified.
  • a reduction in pressure takes place between extraction and shock wave treatment, for example by spontaneous relaxation after extraction.
  • the piece goods should be mechanically crushed before extraction as far as necessary. Already fine-particle cargo does not need to be further pretreated. However, pretreatment steps, such as pre-cleaning or dedusting of the material, are generally not excluded.
  • the product of the shock wave treatment is subjected to a post-treatment.
  • the aftertreatment may include, for example, surface conditioning, e.g. a plasma treatment.
  • the aftertreatment may also consist in a screening or classification of the particles. It may be a physical or chemical aftertreatment. The aftertreatment depends on the planned reuse of the solid meal.
  • a post-treatment with a chemical functionalization of the solid-flour polymers is particularly preferred.
  • a surface functionalization of the particles is provided, as is known in the art in principle.
  • the functionalization is carried out with OH groups (hydroxyl groups), amine groups, amide groups, halogen groups, oxygen groups, in particular -COOH or acid halide groups.
  • Mixed functionalizations with chemically different groups can also be performed.
  • the inventive method provides products in particulate form with a relatively uniform size distribution.
  • the energy supplied to the parameter, the duration of treatment, the degree of pre-grinding, the particle sizes obtained and the degrees of distribution can be influenced.
  • particle sizes below 30 microns are well reproducible, preferably for certain applications, particle sizes are set and obtained to only 100 nm.
  • the method starts in this example with a mechanical pre-shredding 1 of the piece goods, for example of used boards, for example in the form of printed circuit boards.
  • a mechanical pre-shredding 1 of the piece goods for example of used boards, for example in the form of printed circuit boards.
  • In the pre-crushing is generally desired to bring the particle size under a maximum of 5 cm in diameter, preferably less than 1 cm in diameter (or longest particle size). Even more preferred is a maximum particle size of 10 mm, more preferably 1 mm.
  • This can be a shredding or cutting, breaking or grinding in a mill.
  • the shredded or ground material is then transferred to an extraction stage 2 .
  • the extraction is carried out according to the invention with supercritical carbon dioxide, supercritical water or an organic solvent in a suitable extractor.
  • Preferred examples here are the extraction by means of acetylacetone from halogenated and / or nitric acid solutions and N-thiobenzoyl-N-phenylhydroxylamine.
  • the temperature can be adjusted.
  • a relaxation at position 3 takes place in this example.
  • the pressure reduction step is omitted at this point.
  • the excess pressure from the extraction stage is reduced here or reduced to atmospheric pressure.
  • the starting material still has its initial particle size in this stage of the process, but is already freed from low molecular weight substances and soluble polymers by the extraction step. Additives such as flame retardants (bromides), oils, silicones and the like are removed. Subsequently, the material thus treated is subjected to the shock wave crushing 4.
  • the shock wave treatment takes place in a fluid medium, for example, in an alcohol.
  • the fluid is recirculated here and purified again before returning to the shock wave stage.
  • the treatment with shock waves creates a fine particulate flour from the treated material.
  • the grain size depends on several parameters, including the type of scrap used, the degree of pre-shredding, the energy used and the duration of the treatment, but can be well adjusted to the desired range.
  • particulate products A solid particles
  • a treatment 5 is carried out, which may for example consist of additional separation operations or in which the particles are surface-functionalized. Suitable processes for surface functionalization of the particles obtained are known to the person skilled in the art and need not be described here. Refined and / or fractionated products A are obtained by way of the treatment 5 .
  • the extracting agent (extraction medium) leaving the extraction stage 2 carries the substances extracted from the starting material. These are unloaded in process stage 6 in a container or reactor.
  • the CO 2 extract is residue-free with respect to the extractant and can be recycled directly or further separated. Other extractants must be separated here. By further purification, various products B can be obtained.

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  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Processing Of Solid Wastes (AREA)
  • Extraction Or Liquid Replacement (AREA)

Claims (11)

  1. Procédé de traitement de marchandise en morceaux sous la forme de déchets électroniques et de verre technique, caractérisé en ce que la marchandise est soumise à une extraction avec du dioxyde de carbone surcritique, avec de l'eau surcritique ou avec un solvant organique, et en ce que la marchandise ainsi traitée est ensuite soumise à un traitement aux ondes de choc avec des ondes choc déclenchées au moyen d'une haute tension, dans un milieu fluide diélectrique, le milieu à ondes de choc étant de l'eau, un liquide organique ou du dioxyde de carbone surcritique.
  2. Procédé selon la revendication 1, caractérisé en ce que la procédure aux ondes de choc est effectuée à une température entre -80°C et +50°C.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que, avant ou pendant l'extraction, la marchandise est traitée à l'acide ou se présente en suspension dans un acide aqueux.
  4. Procédé selon l'une des revendications 1 à 3, caractérisé en ce que simultanément avec le milieu d'extraction, on laisse agir un agent oxydant sur la marchandise.
  5. Procédé selon l'une des revendications 1 à 4, caractérisé en ce que les substances extraites hors du milieu d'extraction sont récupérées et en ce que l'extrait dans son ensemble, au moins une fraction de l'extrait ou au moins une matière pure obtenue depuis l'extrait forme un produit du procédé.
  6. Procédé selon l'une des revendications 1 à 5, caractérisé en ce que le milieu d'extraction et/ou le milieu diélectrique sont purifiés et recyclés.
  7. Procédé selon l'une des revendications 1 à 6, caractérisé en ce que l'extraction et le traitement aux ondes de choc sont directement consécutifs.
  8. Procédé selon l'une des revendications 1 à 7, caractérisé en ce qu'une réduction de pression est effectuée entre l'extraction et le traitement aux ondes de choc.
  9. Procédé selon l'une des revendications 1 à 8, caractérisé en ce que la marchandise est grossièrement broyée de façon mécanique avant l'extraction.
  10. Procédé selon l'une des revendications 1 à 9, caractérisé en ce que le produit du traitement aux ondes de choc est soumis à un traitement ultérieur.
  11. Procédé selon la revendication 10, caractérisé en ce que le traitement ultérieur comprend une fonctionnalisation chimique des polymères solides à partir du matériau initial.
EP11765105.9A 2010-03-18 2011-03-18 Procédé de fragmentation de déchets électroniques et de verre technique à des fins de recyclage Not-in-force EP2547452B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE201010011937 DE102010011937B4 (de) 2010-03-18 2010-03-18 Verfahren zum Zerkleinern von Elektronikschrott und technischem Glas für die Wiederverwertung
PCT/DE2011/000285 WO2011124195A2 (fr) 2010-03-18 2011-03-18 Procédé de fragmentation de déchets électroniques et de verre technique à des fins de recyclage

Publications (2)

Publication Number Publication Date
EP2547452A2 EP2547452A2 (fr) 2013-01-23
EP2547452B1 true EP2547452B1 (fr) 2016-09-14

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EP (1) EP2547452B1 (fr)
DE (1) DE102010011937B4 (fr)
WO (1) WO2011124195A2 (fr)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014070193A1 (fr) * 2012-11-02 2014-05-08 Empire Technology Development Llc Traitement de déchets électroniques par des gaz rares supercritiques
DE102014013857B4 (de) * 2014-09-24 2016-09-22 Jörg Beckmann Verwendung eines Schockwellenverfahrens
AT516381B1 (de) * 2014-12-04 2016-05-15 Andritz Ag Maschf Verfahren zur Aufbereitung elektrischer und elektronischer Bauteile zur Rückgewinnung von Wertstoffen
FR3030317B1 (fr) * 2014-12-23 2017-02-10 Brgm Procede de recyclage de dechets d'equipements electriques et electroniques
DE102015216932A1 (de) * 2015-09-03 2017-03-09 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Verfahren zum Recycling von Kompositwerkstoffen sowie recycelte Kompositwerkstoffe

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19534232C2 (de) * 1995-09-15 1998-01-29 Karlsruhe Forschzent Verfahren zur Zerkleinerung und Zertrümmerung von aus nichtmetallischen oder teilweise metallischen Bestandteilen konglomerierten Festkörpern und zur Zerkleinerung homogener nichtmetallischer Festkörper
US5758831A (en) 1996-10-31 1998-06-02 Aerie Partners, Inc. Comminution by cryogenic electrohydraulics
JP2000246132A (ja) * 1999-02-26 2000-09-12 Kobe Steel Ltd 放電処理装置
DE10061386A1 (de) * 2000-12-09 2002-09-05 Daimler Chrysler Ag Verfahren und Vorrichtung zur überkritischen Nassoxidation

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Publication number Publication date
WO2011124195A2 (fr) 2011-10-13
WO2011124195A3 (fr) 2012-06-07
EP2547452A2 (fr) 2013-01-23
DE102010011937A1 (de) 2011-09-22
DE102010011937B4 (de) 2012-02-02

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