EP1687317A1 - Method for agglomerating and passivating a used mass or organohalosilane production fines - Google Patents

Method for agglomerating and passivating a used mass or organohalosilane production fines

Info

Publication number
EP1687317A1
EP1687317A1 EP04805476A EP04805476A EP1687317A1 EP 1687317 A1 EP1687317 A1 EP 1687317A1 EP 04805476 A EP04805476 A EP 04805476A EP 04805476 A EP04805476 A EP 04805476A EP 1687317 A1 EP1687317 A1 EP 1687317A1
Authority
EP
European Patent Office
Prior art keywords
fines
mass
agglomerates
spent
binder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP04805476A
Other languages
German (de)
French (fr)
Inventor
Gérard Simon
Daniel Bajolet
André Acloque
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Elkem Silicones France SAS
Original Assignee
Rhodia Chimie SAS
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 Rhodia Chimie SAS filed Critical Rhodia Chimie SAS
Publication of EP1687317A1 publication Critical patent/EP1687317A1/en
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00—Obtaining copper
    • C22B15/0026—Pyrometallurgy
    • C22B15/0056—Scrap treating
    • C22B15/0058—Spent catalysts
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
    • C07F7/02—Silicon compounds
    • C07F7/08—Compounds having one or more C—Si linkages
    • C07F7/20—Purification, separation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/14—Agglomerating; Briquetting; Binding; Granulating
    • C22B1/24—Binding; Briquetting ; Granulating
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/14—Agglomerating; Briquetting; Binding; Granulating
    • C22B1/24—Binding; Briquetting ; Granulating
    • C22B1/242—Binding; Briquetting ; Granulating with binders
    • C22B1/243—Binding; Briquetting ; Granulating with binders inorganic
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the present invention relates to an agglomeration process allowing the deactivation or passivation, the transport and the valorization of pulverulent spent masses and / or pulverulent residual fines resulting from the production of organohalosilanes, and more particularly from the production of methyl chlorosilanes, by direct synthesis.
  • the invention also relates to the products resulting from this agglomeration process as well as to the use of these products for the recovery in particular of residual silicon metal and of metals such as copper.
  • the industrial implementation of the direct methylchlorosilane synthesis process following the Rochow reaction reaction of silicon metal with gaseous methyl chloride in the presence of copper-based catalyst
  • reaction of silicon metal with gaseous methyl chloride in the presence of copper-based catalyst is generally carried out in a fluidized bed.
  • spent masses and synthetic residual fines are powdery and contain, alongside the metal silicon, optionally silicon oxides and elements such as chlorine, hydrogen, oxygen as well as elements such as copper, carbon, iron, aluminum, zinc, calcium, tin, manganese, etc.
  • silicon oxides and elements such as chlorine, hydrogen, oxygen as well as elements such as copper, carbon, iron, aluminum, zinc, calcium, tin, manganese, etc.
  • These spent masses and these powdery fines have a very reactive nature which makes their handling and transport in the state very difficult, if not impossible. In particular, they react with water in liquid or vapor form, with evolution of hydrogen and have a self-heating character in contact with air. Used materials must therefore be subjected to deactivation treatment.
  • US-A-5 342 430 describes a passivation process in which the spent mass is reacted with an aqueous medium comprising water and a surfactant, optionally at elevated temperature, then a binder such as a lignosulfonate, montmorillonite or bentonite, this treatment can be followed by elimination of water.
  • a binder such as a lignosulfonate, montmorillonite or bentonite
  • EP-A-0 287 934 describes a passivation process by agglomeration of the spent mass (formation of pellets) and the impregnation of the agglomerates with an organic binder to increase the cohesion of the agglomerates and isolate them from ambient humidity.
  • the binder can be a liquid organic binder having a sufficiently low viscosity to ensure its penetration into the agglomerate, or it can be applied in solution or in emulsion with an organic solvent or water. If water is the preferred means, both have disadvantages according to the terms of this document.
  • Organic solvents pose the usual emission problems. Water reacts with silicon, induces heating and the operating conditions must therefore be vigorously controlled.
  • Organic binders include glucose, gums, glues, bitumens, waxes, starch and preferably lignin, in a liquid form and in particular in dilute aqueous solution.
  • EP-A-201 199 recommends combining the pulverulent spent mass with water, carrying out a granulation, and covering the aggregates with an inert inorganic powder. From 5 to 50% of water by weight (relative to the mixture of spent mass + water) are used to convert the silicon into silicon dioxide (which makes it possible to deactivate the silicon).
  • WO-A-02 46119 describes that aluminum silicates make it possible to deactivate spent masses.
  • the mixing is carried out in conventional mixers. The process preferably provides for the presence of an amount of water which can range from 10 to 40% by adding water to the mixture of spent mass + aluminum silicate or by the use of an aluminum silicate mud.
  • the present invention therefore aims to propose a new process for treating used masses and / or fines from direct synthesis, allowing efficient deactivation or passivation of these used masses and / or these fines, and obtaining '' a stable solid product, not reactive with air or air humidity and not self-heating, transportable, manipulable, and which can in particular be directly subjected to recovery operations, in particular recovery of metals such as silicon and copper by the metallurgical industry.
  • Another objective of the invention is to provide such a process which can be carried out at the lowest cost and in particular with a minimum number of steps.
  • the subject of the present invention is therefore a process for agglomerating the pulverulent spent mass and / or pulverulent fines obtained from the production of organohalosilanes, comprising: (i) mixing this spent mass and / or the fines with a binder chosen from aluminum silicates; (ii) the production of a solid agglomerated product by compression, in an appropriate press.
  • This process allows the production of a non-pulverulent product, in the form of solid, hard, rigid agglomerates, of defined shape.
  • the agglomerated product is pacified or inert, that is to say that it does not react on contact with air and air humidity and that it is not self-heating; the agglomerates have a cohesion allowing their handling and their transport; and the absence of free water allows them to be easily treated in recovery operations, for example in metallurgy.
  • the expressions used mass and residual fines have the usual meanings. It can be specified that these are used materials and fines resulting from direct synthesis, therefore essentially comprising silicon metal and possibly silicon oxides and small quantities of other materials such as chlorine, hydrogen, oxygen, copper. , carbon, iron, aluminum, zinc, calcium, tin, titanium, manganese, etc.
  • the binder used is in a solid, dry form, but can nevertheless be hydrated to varying degrees.
  • the method according to the invention does not provide for the addition of water. However, the provision of a limited amount of water leading in particular to the hydration of the binder is not excluded from the invention. Likewise, if this is not sought, the presence or the addition of a residual or reduced quantity of free water in the binder is nevertheless not excluded, provided that the generally dry and solid character of the binder and the subsequent agglomeration operation will not be called into question. Most preferably, the binder does not contain free water.
  • aluminum silicates or aluminosilicates mention may be made of bentonite, kaolin, diatonite, Fuller's earth and more generally any hydrated form of aluminum silicate. Bentonite is a preferred embodiment. For economic reasons, natural aluminosilicates are preferably used. The particle size is not a critical parameter and in any case, the skilled person can very easily conduct routine tests to select the appropriate aluminosilicates. As an indication, it can be specified that the bentonite used in the examples had an average particle diameter of approximately 35 ⁇ m (50% by number of particles ⁇ 35 ⁇ m, 90% by number of particles ⁇ 1 1 1 ⁇ m).
  • the binder / used mass ratio can range in particular from 0.1 / 1 to 1.5 / 1, and is preferably between 0.3 / 1 and 1/1, by weight. It should be noted that throughout the description and claims and unless otherwise stated, when it comes to ranges of values, the bounds are included.
  • the press advantageously has means intended to give a defined shape to the agglomerated product, by compression molding. Any type of compression press can be used (of the type used for compression molding or agglomeration in a shape, cavity or mold), such as a piston press and a tangent wheel press.
  • the presses used therefore include cavities, shapes or molds in which the product is agglomerated by compression and which give the agglomerated product its final shape, its cohesion and its mechanical stability.
  • presses with tangent wheels constitute a preferred mode of implementation. They include two rollers placed facing each other (parallel axes), at least one of which is arranged so that it can be driven in rotation and at least one of which has cavities of defined shape. Most often, the two rollers can be rotated and in particular in opposite directions. Pressure can be exerted between the two rollers and this is adjustable. One of the rollers can be fixed in position on its axis, and the other roller can be brought into pressure against the previous one using appropriate means, in particular by hydraulic means such as pistons or jacks.
  • the two rollers can be moved towards one another to ensure the desired pressure, by the use for example of hydraulic means as already mentioned.
  • the tangent wheel press therefore applies a pressure, preferably adjustable, on the material which passes between the rollers, which material is molded in the cavities of defined shape which are provided on the surface of at least one of these rollers.
  • the two rollers Preferably, the two rollers have cavities of complementary shapes.
  • the final molded-pressed material can be given any desired shape by choosing the shape of the cavities presented by the roller (s).
  • the pressure can be adjusted between 10 and 80 kN / cm wheel width (roller).
  • agglomerates having a unit volume which can vary between 0.5 and 20 cm 3 it goes without saying that these values are given only for illustrative purposes.
  • the present invention makes it possible to produce inert agglomerates having good cohesion, which can be handled and transported without requiring any special precautions; in particular, they are easily pourable, which facilitates loading and unloading into or from a grab, silo or the like.
  • Tangents wheel presses are designed and manufactured by companies such as his. hut-Conreur in Raismes, France and KR Komarek Inc. in Elk Grave Village, Illinois, USA.
  • the initial mixing is carried out in a suitable mixer or homogenizer. It can be any type of solid mixer.
  • the mixing time can be of the order of a few minutes.
  • Presses with tangential wheels are generally fed by a feeding device intended to push the material between the rollers. It may especially be a screw device or the like, eg placed vertically above the facing surfaces of the two rollers. According to an optional feature, the mixture from the mixer passes through this feed device, then into the press.
  • the agglomerates obtained according to the process of the invention are not self-heating, nor reactive with water. They can therefore be handled and transported without special measures dictated by official regulations being required.
  • agglomerates free of free water can also be used as a raw material for the recovery of silicon metal and other metals such as copper. They can in particular be used in activities such as silicon metallurgy, copper metallurgy, iron metallurgy and foundry. Agglomerates can also be used in the manufacture of ceramics, refractory compounds, etc.
  • the solid agglomerated products obtained or capable of being obtained by implementing the method according to the invention are also objects of the present invention.
  • the present invention also relates to an agglomerated product comprising spent mass and / or fines resulting from direct synthesis, a binder chosen from aluminum silicates, according to a binder / used mass ratio of between 0, 1/1 and 1, 5/1, preferably between 0.3 / 1 and 1/1, by weight, not containing free water.
  • This agglomerate is in the form of a solid and rigid product, for example molded, for example in the form of rollers, briquettes or pellets, of simple circular or semi-circular geometric shapes, cylindrical or semi-cylindrical or the like, eg of unit volume between 0.5 and 20 cm 3 . It is in particular an agglomerated product as obtained by implementing the method according to the invention.
  • the binder is preferably bentonite.
  • the present invention also relates to the use of agglomerates in accordance with the invention, as a raw material for the recovery of a metal or more of the metals present in the spent or residual fine masses. These metals have been mentioned above; this use is more particularly aimed at the recovery of silicon metal and / or copper and / or iron.
  • the invention therefore particularly relates to the use of these agglomerates in silicon metallurgy, copper metallurgy or iron metallurgy.
  • the invention also relates to the use of agglomerates in accordance with the invention as a raw material in the manufacture of ceramics, refractory compounds, etc.
  • Example 1 In a solid mixer-homogenizer (mixer type device
  • EXAMPLE 2 Under the same operating conditions as for Example 1, for 3000 grams of used mass, 1285 grams of powdered bentonite are charged, ie 43% of the weight of used mass. The agglomerates obtained are measured not self-heating in the BOWES CAMERON test (sample subjected to an enclosure temperature equal to 140 ° C. for 24 hours) and do not react on contact with water.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Glanulating (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Processing Of Solid Wastes (AREA)
  • Silicon Compounds (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

The inventive method for agglomerating and passivating a used powdery mass and/or powdery organohalosilane production fines consists in mixing said used mass and/or fines with a binder selected from aluminium silicates and in producing a solid agglomerated product by compressing in a press such as a screw press. The thus obtained agglomerated product and the use thereof for upgrading certain metals such as silicon or copper are also disclosed.

Description

Procédé d'agglomération et de passivation de la masse usée ou des fines issues de la production d'organohalosilanes Process for agglomeration and passivation of the spent mass or of the fines resulting from the production of organohalosilanes
La présente invention est relative à un procédé d'agglomération permettant la désactivation ou passivation, le transport et la valorisation des masses usées pulvérulentes et/ou des fines résiduelles pulvérulentes issues de la production d'organohalosilanes, et plus particulièrement de la production des méthylchlorosilanes, par synthèse directe. L'invention est également relative aux produits issus de ce procédé d'agglomération ainsi qu'à l'utilisation de ces produits pour la valorisation notamment du silicium métal résiduel et de métaux tels que le cuivre. La mise en œuvre industrielle du procédé de synthèse directe des méthylchlorosilanes suivant la réaction de Rochow (réaction du silicium métal avec le chlorure de méthyle gazeux en présence de catalyseur à base de cuivre) est généralement réalisée en lit fluidisé. Le procédé nécessite une vidange régulière ou une purge du lit fluidisé, conduisant à ce- qu'il est convenu d'appeler les masses usées et les fines résiduelles de synthèse. Ces masses usées et/ou fines résiduelles sont pulvérulentes et contiennent au côté du silicium métal, éventuellement des oxydes de silicium et des éléments tels que du chlore, de l'hydrogène, de l'oxygène ainsi que des éléments tels que cuivre, carbone, fer, aluminium, zinc, calcium, étain, manganèse, etc. Ces masses usées et ces fines pulvérulentes présentent un caractère très réactif qui rend leur manipulation et leur transport en l'état très difficile, voire impossible. En particulier, elles réagissent avec l'eau sous forme liquide ou vapeur, avec dégagement d'hydrogène et présentent un caractère auto-échauffant au contact de l'air. Les masses usées doivent pour cette raison être soumises à un traitement de désactivation. Par ailleurs, les masses usées et les fines contiennent des proportions importantes de constituants tels que le silicium et le cuivre qu'il serait intéressant de pouvoir récupérer. Le brevet US-A-5 342 430 décrit un procédé de passivation dans lequel on fait réagir la masse usée avec un milieu aqueux comprenant de l'eau et un tensioactif, éventuellement à température élevée, puis l'on introduit un liant tel qu'un lignosulfonate, de la montmorillonite ou de la bentonite, ce traitement pouvant être suivi d'une élimination d'eau. EP-A-0 287 934 décrit un procédé de passivation par agglomération de la masse usée (formation de pellets) et l'imprégnation des agglomérats avec un liant organique pour augmenter la cohésion des agglomérats et les isoler de l'humidité ambiante. Le liant peut être un liant organique liquide ayant une viscosité suffisamment basse pour assurer sa pénétration dans l'agglomérat, ou bien il peut être appliqué en solution ou en émulsion avec un solvant organique ou de l'eau. Si l'eau est le moyen préféré, les deux présentent des inconvénients selon les propres termes de ce document. Les solvants organiques posent les problèmes d'émission habituels. L'eau réagit avec le silicium, induit un échauffement et les conditions opératoires doivent donc être vigoureusement contrôlées. Les liants organiques incluent le glucose, des gommes, colles, bitumes, cires, de l'amidon et de préférence de la lignine, sous une forme liquide et notamment en solution aqueuse diluée. EP-A-201 199 préconise de combiner la masse usée pulvérulente à de l'eau, d'effectuer une granulation, et de recouvrir les granulats avec une poudre inerte inorganique. De 5 à 50 % d'eau en poids (par rapport au mélange masse usée + eau) sont employés, pour convertir le silicium en dioxyde de silicium (ce qui permet de désactiver le silicium). WO-A-02 46119 décrit que les silicates d'aluminium permettent de désactiver les masses usées. Le mélange est réalisé dans des mélangeurs classiques. Le procédé prévoit de préférence la présence d'une quantité d'eau pouvant aller de 10 à 40 % par ajout d'eau au mélange masse usée + silicate d'aluminium ou par l'emploi d'une boue de silicate d'aluminium. La présence d'eau permet de faire passer le mélange dans une extrudeuse, avant de procéder au recyclage de la composition dans la fabrication de produits céramiques. Les procédés de l'art antérieur posent des problèmes sur le plan des conditions de mise en œuvre en raison de l'emploi de solvants volatiles ou d'eau et/ou conduisent à des produits comportant des teneurs en eau peu compatibles avec leur transport, leur manipulation et leur valorisation, par exemple dans les industries métallurgiques. La présente invention a donc pour objectif de proposer un nouveau procédé de traitement des masses usées et/ou des fines issues de la synthèse directe, permettant une désactivation ou passivation performante de ces masses usées et/ou de ces fines, et l'obtention d'un produit solide stable, non réactif avec l'air ou l'humidité de l'air et non auto-échauffant, transportable, manipulable, et pouvant être notamment directement soumis à des opérations de valorisation, en particulier valorisation de métaux tels que silicium et cuivre par l'industrie métallurgique. Un autre objectif de l'invention est de fournir un tel procédé qui puisse être réalisé au moindre coût et notamment avec un nombre minimum d'étapes. II a été trouvé de manière inattendue que des objectifs, ainsi que d'autres, peuvent être atteints par un procédé d'agglomération spécifique en l'absence d'eau libre, de solvant ou de liant liquide, en solution, dispersion, etc. La présente invention a ainsi pour objet un procédé d'agglomération de la masse usée pulvérulente et/ou des fines pulvérulentes issues de la production d'organohalosilanes, comprenant : (i) le mélange de cette masse usée et/ou des fines avec un liant choisi parmi les silicates d'aluminium ; (ii) la production d'un produit aggloméré solide par compression, dans une presse appropriée. Ce procédé permet, la production d'un produit non pulvérulent, se présentant sous forme d'agglomérats solides, durs, rigides, de forme définie. Le produit aggloméré est pacifié ou inerte, c'est-à-dire qu'il ne réagit pas au contact de l'air et de l'humidité de l'air et qu'il n'est pas auto-échauffant ; les agglomérats présentent une cohésion permettant leur manipulation et leur transport ; et l'absence d'eau libre leur permet d'être facilement traités dans des opérations de valorisation, par exemple en métallurgie. Les expressions masse usée et fines résiduelles ont les significations usuelles. On peut préciser qu'il s'agit des matières usées et des fines issues de la synthèse directe, comprenant donc essentiellement du silicium métal et éventuellement des oxydes de silicium et de faibles quantités d'autres matériaux tels que chlore, hydrogène, oxygène, cuivre, carbone, fer, aluminium, zinc, calcium, étain, titane, manganèse, etc. Le liant utilisé se présente sous une forme solide, sèche, mais peut néanmoins être hydraté à des degrés divers. Le procédé selon l'invention ne prévoit pas d'ajout d'eau. Cependant, l'apport d'une quantité d'eau limitée conduisant notamment à l'hydratation du liant n'est pas exclu de l'invention. De même, si ceci n'est pas recherché, la présence ou l'apport d'une quantité résiduelle ou réduite d'eau libre dans le liant n'est néanmoins pas exclu, pour autant que le caractère globalement sec et solide du liant et l'opération d'agglomération subséquente ne soient pas remis en cause. De manière tout à fait préférée, le liant ne comporte pas d'eau libre. Parmi les silicates d'aluminium ou aluminosilicates préférés, on peut citer la bentonite, le kaolin, la diatonite, la terre de Fuller et plus généralement toute forme hydratée de silicate d'aluminium. La bentonite constitue un mode de réalisation préféré. Pour des raisons économiques, on utilisera de préférence des aluminosilicates naturels. La granulométrie n'est pas un paramètre critique et de toute manière, l'homme du métier peut très aisément conduire des essais de routine pour sélectionner les aluminosilicates appropriés. A titre indicatif, on peut préciser que la bentonite utilisée dans les exemples présentait un diamètre moyen de particules de 35 μm environ (50 % en nombre de particules < 35 μm, 90 % en nombre de particules < 1 1 1 μm). Le rapport liant/masse usée peut aller notamment de 0,1/1 à 1 ,5/1 , et se situe de préférence entre 0,3/1 et 1/1 , en poids. Il convient de noter que dans ensemble de la description et des revendications et sauf mention contraire, lorsqu'il est question d'intervalles de valeurs, les bornes sont incluses. La presse présente avantageusement des moyens destinés à conférer une forme définie au produit aggloméré, par moulage par compression. On peut utiliser tout type de presse de compression (du type utilisé pour le moulage ou l'agglomération par compression dans une forme, cavité ou moule), tel que presse à piston et presse à roues tangentes. Les presses utilisées comportent donc des cavités, formes ou moules dans lesquels le produit est aggloméré par compression et qui confèrent au produit aggloméré sa forme finale, sa cohésion et sa stabilité mécanique. Dans la présente invention, on préférera des formes de galet, briquette ou pastille, des formes géométriques simples circulaires ou semi-circulaires, cylindriques ou semi-cylindriques ou similaires. Les presses à roues tangentes («rail type briquet machine ») constituent un mode de mise en œuvre préféré. Elles comprennent deux rouleaux placés au regard l'un de l'autre (axes parallèles) dont l'un au moins est agencé de manière à pouvoir être entraîné en rotation et l'un au moins comporte des cavités de forme définie. Le plus souvent, les deux rouleaux peuvent être entraînés en rotation et en particulier dans des directions opposées. Une pression peut être exercée entre les deux rouleaux et ce de façon réglable. L'un des rouleaux peut être fixe en position sur son axe, et l'autre rouleau peut être amené en pression contre le précédent à l'aide de moyens appropriés, en particulier par des moyens hydrauliques tels que des pistons ou vérins. Il est également possible que les deux rouleaux soient déplaçables l'un vers l'autre pour assurer la pression souhaitée, par l'utilisation par exemple de moyens hydrauliques comme déjà mentionnés. La presse à roues tangentes applique donc une pression, de préférence réglable, sur le matériau qui passe entre les rouleaux, lequel matériau se trouve moulé dans les cavités de forme définies qui sont prévues à la surface de l'un au moins de ces rouleaux. De préférence, les deux rouleaux présentent des cavités de formes complémentaires. On peut donner au matériau moulé-pressé final toute forme voulue en choisissant la forme des cavités présentées par le ou les rouleaux. Afin d'obtenir une bonne agglomération, il est possible d'ajuster la pression appliquée dans la presse. Typiquement pour une presse à roues tangentes, la pression peut être réglée entre 10 et 80 kN/cm de largeur de roue (rouleau). A titre illustratif, on pourra produire des agglomérats ayant un volume unitaire pouvant varier entre 0,5 et 20 cm3, il va de soi que ces valeurs sont données uniquement à titre illustratif. La présente invention permet de produire des agglomérats inertes et ayant une bonne cohésion, qui peuvent être manipulés et transportés sans nécessiter de précautions particulières ; ils sont notamment facilement deversables ce qui facilite le chargement et le déchargement dans ou à partir d'une benne, silo ou analogue. Des presses à roues tangentes sont conçues et fabriquées par des sociétés telles que Sa.hut-Conreur à Raismes, France et K.R. Komarek Inc. à Elk Grave Village, Illinois, USA. Le mélange initial est réalisé dans un mélangeur ou homogénéiseur approprié. II peut s'agir de tout type de mélangeur à solides. La durée de mélange peut être de l'ordre de quelques minutes. L'homme du métier est parfaitement en mesure de déterrminer les conditions de mélange pour réaliser un mélange aussi homogène que possible. Les presses à roues tangentes sont généralement alimentées par un dispositif d'alimentation destiné à pousser le matériau entre les rouleaux. Il peut s'agir notamment d'un dispositif à vis ou analogue, e.g. placé verticalement au-dessus des surfaces en regard des deux rouleaux. Suivant une caractéristique optionnelle, le mélange issu du mélangeur passe dans ce dispositif d'alimentation, puis dans la presse. Les agglomérats obtenus selon le procédé de l'invention ne sont pas auto- échauffants, ni réactifs à l'eau. Ils peuvent donc être manipulés et transportés sans que des mesures particulières dictées par une réglementation officielle ne soient requises. Ces agglomérats exempts d'eau libre peuvent également être utilisés comme matière première en vue de la valorisation du silicium métal et d'autres métaux tels que le cuivre. Ils peuvent notamment être utilisés dans des activités telles que la métallurgie du silicium, la métallurgie du cuivre, la métallurgie du fer et la fonderie. Les agglomérats peuvent être également utilisés dans la fabrication de céramiques, de composés réfractaires, etc. Les produits agglomérés solides obtenus ou susceptibles d'être obtenus par la mise en œuvre du procédé selon l'invention sont aussi des objets de la présente invention. La présente invention a également pour objet un produit aggloméré comprenant de la masse usée et/ou des fines issue(s) de la synthèse directe, un liant choisi parmi les silicates d'aluminium, selon un rapport liant/masse usée compris entre 0,1/1 et 1 ,5/1 , de préférence entre 0,3/1 et 1/1 , en poids, ne comportant pas d'eau libre. Cet agglomérat se présente sous la forme d'un produit solide et rigide, par exemple moulé, par exemple sous forme de galets, briquettes ou pastilles, de formes géométriques simples circulaires ou semi-circulaires, cylindriques ou semi- cylindriques ou similaires, e.g. de volume unitaire entre 0,5 et 20 cm3. Il s'agit en particulier d'un produit aggloméré tel qu'obtenu par la mise en œuvre du procédé selon l'invention. Dans cet agglomérat, le liant est de préférence de la bentonite. La présente invention a encore pour objet l'utilisation des agglomérats conformes à l'invention, comme matière première en vue de la valorisation d'un métal ou de plusieurs des métaux présents dans les masses usées ou fines résiduelles. Ces métaux ont été mentionnés supra ; cette utilisation vise plus particulièrement la valorisation du silicium métal et/ou du cuivre et/ou du fer. L'invention a donc particulièrement pour objet l'utilisation de ces agglomérats en métallurgie du silicium, en métallurgie du cuivre ou en métallurgie du fer. L'invention a également pour objet l'utilisation des agglomérats conformes à l'invention comme matière première dans la fabrication de céramiques, de composés réfractaires, etc. La présente invention va être maintenant décrite à l'aide d'exemples décrivant des modes de réalisation de l'invention pris à titre d'exemples non limitatifs. Exemple 1 Dans un mélangeur-homogénéiseur à solide (appareil type mélangeurThe present invention relates to an agglomeration process allowing the deactivation or passivation, the transport and the valorization of pulverulent spent masses and / or pulverulent residual fines resulting from the production of organohalosilanes, and more particularly from the production of methyl chlorosilanes, by direct synthesis. The invention also relates to the products resulting from this agglomeration process as well as to the use of these products for the recovery in particular of residual silicon metal and of metals such as copper. The industrial implementation of the direct methylchlorosilane synthesis process following the Rochow reaction (reaction of silicon metal with gaseous methyl chloride in the presence of copper-based catalyst) is generally carried out in a fluidized bed. The process requires regular emptying or purging of the fluidized bed, leading to what is commonly known as spent masses and synthetic residual fines. These spent and / or fine residual masses are powdery and contain, alongside the metal silicon, optionally silicon oxides and elements such as chlorine, hydrogen, oxygen as well as elements such as copper, carbon, iron, aluminum, zinc, calcium, tin, manganese, etc. These spent masses and these powdery fines have a very reactive nature which makes their handling and transport in the state very difficult, if not impossible. In particular, they react with water in liquid or vapor form, with evolution of hydrogen and have a self-heating character in contact with air. Used materials must therefore be subjected to deactivation treatment. Furthermore, the spent masses and the fines contain significant proportions of constituents such as silicon and copper which it would be advantageous to be able to recover. US-A-5 342 430 describes a passivation process in which the spent mass is reacted with an aqueous medium comprising water and a surfactant, optionally at elevated temperature, then a binder such as a lignosulfonate, montmorillonite or bentonite, this treatment can be followed by elimination of water. EP-A-0 287 934 describes a passivation process by agglomeration of the spent mass (formation of pellets) and the impregnation of the agglomerates with an organic binder to increase the cohesion of the agglomerates and isolate them from ambient humidity. The binder can be a liquid organic binder having a sufficiently low viscosity to ensure its penetration into the agglomerate, or it can be applied in solution or in emulsion with an organic solvent or water. If water is the preferred means, both have disadvantages according to the terms of this document. Organic solvents pose the usual emission problems. Water reacts with silicon, induces heating and the operating conditions must therefore be vigorously controlled. Organic binders include glucose, gums, glues, bitumens, waxes, starch and preferably lignin, in a liquid form and in particular in dilute aqueous solution. EP-A-201 199 recommends combining the pulverulent spent mass with water, carrying out a granulation, and covering the aggregates with an inert inorganic powder. From 5 to 50% of water by weight (relative to the mixture of spent mass + water) are used to convert the silicon into silicon dioxide (which makes it possible to deactivate the silicon). WO-A-02 46119 describes that aluminum silicates make it possible to deactivate spent masses. The mixing is carried out in conventional mixers. The process preferably provides for the presence of an amount of water which can range from 10 to 40% by adding water to the mixture of spent mass + aluminum silicate or by the use of an aluminum silicate mud. The presence of water makes it possible to pass the mixture through an extruder, before recycling the composition in the manufacture of ceramic products. The processes of the prior art pose problems in terms of the conditions of implementation due to the use of volatile solvents or water and / or lead to products having water contents which are hardly compatible with their transport, their handling and recovery, for example in the metallurgical industries. The present invention therefore aims to propose a new process for treating used masses and / or fines from direct synthesis, allowing efficient deactivation or passivation of these used masses and / or these fines, and obtaining '' a stable solid product, not reactive with air or air humidity and not self-heating, transportable, manipulable, and which can in particular be directly subjected to recovery operations, in particular recovery of metals such as silicon and copper by the metallurgical industry. Another objective of the invention is to provide such a process which can be carried out at the lowest cost and in particular with a minimum number of steps. It has been unexpectedly found that objectives, as well as others, can be achieved by a specific agglomeration process in the absence of free water, solvent or liquid binder, in solution, dispersion, etc. The subject of the present invention is therefore a process for agglomerating the pulverulent spent mass and / or pulverulent fines obtained from the production of organohalosilanes, comprising: (i) mixing this spent mass and / or the fines with a binder chosen from aluminum silicates; (ii) the production of a solid agglomerated product by compression, in an appropriate press. This process allows the production of a non-pulverulent product, in the form of solid, hard, rigid agglomerates, of defined shape. The agglomerated product is pacified or inert, that is to say that it does not react on contact with air and air humidity and that it is not self-heating; the agglomerates have a cohesion allowing their handling and their transport; and the absence of free water allows them to be easily treated in recovery operations, for example in metallurgy. The expressions used mass and residual fines have the usual meanings. It can be specified that these are used materials and fines resulting from direct synthesis, therefore essentially comprising silicon metal and possibly silicon oxides and small quantities of other materials such as chlorine, hydrogen, oxygen, copper. , carbon, iron, aluminum, zinc, calcium, tin, titanium, manganese, etc. The binder used is in a solid, dry form, but can nevertheless be hydrated to varying degrees. The method according to the invention does not provide for the addition of water. However, the provision of a limited amount of water leading in particular to the hydration of the binder is not excluded from the invention. Likewise, if this is not sought, the presence or the addition of a residual or reduced quantity of free water in the binder is nevertheless not excluded, provided that the generally dry and solid character of the binder and the subsequent agglomeration operation will not be called into question. Most preferably, the binder does not contain free water. Among the preferred aluminum silicates or aluminosilicates, mention may be made of bentonite, kaolin, diatonite, Fuller's earth and more generally any hydrated form of aluminum silicate. Bentonite is a preferred embodiment. For economic reasons, natural aluminosilicates are preferably used. The particle size is not a critical parameter and in any case, the skilled person can very easily conduct routine tests to select the appropriate aluminosilicates. As an indication, it can be specified that the bentonite used in the examples had an average particle diameter of approximately 35 μm (50% by number of particles <35 μm, 90% by number of particles <1 1 1 μm). The binder / used mass ratio can range in particular from 0.1 / 1 to 1.5 / 1, and is preferably between 0.3 / 1 and 1/1, by weight. It should be noted that throughout the description and claims and unless otherwise stated, when it comes to ranges of values, the bounds are included. The press advantageously has means intended to give a defined shape to the agglomerated product, by compression molding. Any type of compression press can be used (of the type used for compression molding or agglomeration in a shape, cavity or mold), such as a piston press and a tangent wheel press. The presses used therefore include cavities, shapes or molds in which the product is agglomerated by compression and which give the agglomerated product its final shape, its cohesion and its mechanical stability. In the present invention, forms of pebble, briquette or pellet, simple circular or semi-circular geometric shapes, cylindrical or semi-cylindrical shapes or the like will be preferred. Presses with tangent wheels ("rail type lighter machine") constitute a preferred mode of implementation. They include two rollers placed facing each other (parallel axes), at least one of which is arranged so that it can be driven in rotation and at least one of which has cavities of defined shape. Most often, the two rollers can be rotated and in particular in opposite directions. Pressure can be exerted between the two rollers and this is adjustable. One of the rollers can be fixed in position on its axis, and the other roller can be brought into pressure against the previous one using appropriate means, in particular by hydraulic means such as pistons or jacks. It is also possible that the two rollers can be moved towards one another to ensure the desired pressure, by the use for example of hydraulic means as already mentioned. The tangent wheel press therefore applies a pressure, preferably adjustable, on the material which passes between the rollers, which material is molded in the cavities of defined shape which are provided on the surface of at least one of these rollers. Preferably, the two rollers have cavities of complementary shapes. The final molded-pressed material can be given any desired shape by choosing the shape of the cavities presented by the roller (s). In order to obtain good agglomeration, it is possible to adjust the pressure applied in the press. Typically for a tangent wheel press, the pressure can be adjusted between 10 and 80 kN / cm wheel width (roller). By way of illustration, it is possible to produce agglomerates having a unit volume which can vary between 0.5 and 20 cm 3 , it goes without saying that these values are given only for illustrative purposes. The present invention makes it possible to produce inert agglomerates having good cohesion, which can be handled and transported without requiring any special precautions; in particular, they are easily pourable, which facilitates loading and unloading into or from a grab, silo or the like. Tangents wheel presses are designed and manufactured by companies such as his. hut-Conreur in Raismes, France and KR Komarek Inc. in Elk Grave Village, Illinois, USA. The initial mixing is carried out in a suitable mixer or homogenizer. It can be any type of solid mixer. The mixing time can be of the order of a few minutes. A person skilled in the art is perfectly capable of determining the mixing conditions in order to produce a mixture as homogeneous as possible. Presses with tangential wheels are generally fed by a feeding device intended to push the material between the rollers. It may especially be a screw device or the like, eg placed vertically above the facing surfaces of the two rollers. According to an optional feature, the mixture from the mixer passes through this feed device, then into the press. The agglomerates obtained according to the process of the invention are not self-heating, nor reactive with water. They can therefore be handled and transported without special measures dictated by official regulations being required. These agglomerates free of free water can also be used as a raw material for the recovery of silicon metal and other metals such as copper. They can in particular be used in activities such as silicon metallurgy, copper metallurgy, iron metallurgy and foundry. Agglomerates can also be used in the manufacture of ceramics, refractory compounds, etc. The solid agglomerated products obtained or capable of being obtained by implementing the method according to the invention are also objects of the present invention. The present invention also relates to an agglomerated product comprising spent mass and / or fines resulting from direct synthesis, a binder chosen from aluminum silicates, according to a binder / used mass ratio of between 0, 1/1 and 1, 5/1, preferably between 0.3 / 1 and 1/1, by weight, not containing free water. This agglomerate is in the form of a solid and rigid product, for example molded, for example in the form of rollers, briquettes or pellets, of simple circular or semi-circular geometric shapes, cylindrical or semi-cylindrical or the like, eg of unit volume between 0.5 and 20 cm 3 . It is in particular an agglomerated product as obtained by implementing the method according to the invention. In this agglomerate, the binder is preferably bentonite. The present invention also relates to the use of agglomerates in accordance with the invention, as a raw material for the recovery of a metal or more of the metals present in the spent or residual fine masses. These metals have been mentioned above; this use is more particularly aimed at the recovery of silicon metal and / or copper and / or iron. The invention therefore particularly relates to the use of these agglomerates in silicon metallurgy, copper metallurgy or iron metallurgy. The invention also relates to the use of agglomerates in accordance with the invention as a raw material in the manufacture of ceramics, refractory compounds, etc. The present invention will now be described with the aid of examples describing embodiments of the invention taken by way of nonlimiting examples. Example 1 In a solid mixer-homogenizer (mixer type device
LODIGUE horizontal ou mélangeur à train valseur), on charge et mélange pendant quelques minutesLODIGUE horizontal or mixer with waltz train), load and mix for a few minutes
3000 grammes de masses usées en poudre et 3000 grammes de bentonite en poudre soit 100 % du poids de masse usée. On introduit le mélange dans une presse à roues tangentes, alimentée par l'intermédiaire d'un dispositif d'alimentation à vis.3000 grams of used powdered mass and 3000 grams of bentonite powder, ie 100% of the weight of used mass. The mixture is introduced into a tangent wheel press, fed by means of a screw feeder.
Vitesse de rotation du dispositif d'alimentation à vis: 18 tours/minuteRotation speed of the screw feeder: 18 rpm
Caractéristiques de la presse à roues tangentes (Sahut Conreur type D150) :Characteristics of the tangent wheel press (Sahut Conreur type D150):
Entrefer : 7/10 mm Volume des alvéoles : 0,7 cm3 Air gap: 7/10 mm Cell volume: 0.7 cm 3
Vitesse de rotation des roues : 5 tours/minuteWheel rotation speed: 5 rpm
Pression : 50 kNewton/cm linéaire de largeur de roue. Les agglomérats obtenus sont mesurés non auto-échauffants au test de BOWES CAMERON (échantillon soumis à une température d'enceinte égale à 140°C pendant 24 heures, selon les Recommandations relatives au Transport des Marchandises Dangereuses, Manuel d'épreuves et de critères, Troisième édition révisée, Nations Unies, New York et Genève, 1999) et ne réagissent pas au contact de l'eau.Pressure: 50 kNewton / linear cm of wheel width. The agglomerates obtained are measured not self-heating in the BOWES CAMERON test (sample subjected to an enclosure temperature equal to 140 ° C for 24 hours, according to the Recommendations on the Transport of Dangerous Goods, Manual of tests and criteria, Third revised edition, United Nations, New York and Geneva, 1999) and do not react on contact with water.
Exemple 2 Dans les mêmes conditions opératoires que pour l'exemple 1 , pour 3000 grammes de masses usées, on charge 1285 grammes de bentonite en poudre soit 43 % du poids de masse usée. Les agglomérats obtenus sont mesurés non auto-échauffants au test de BOWES CAMERON (échantillon soumis à une température d'enceinte égale à 140°C pendant 24 heures) et ne réagissent pas au contact de l'eau.EXAMPLE 2 Under the same operating conditions as for Example 1, for 3000 grams of used mass, 1285 grams of powdered bentonite are charged, ie 43% of the weight of used mass. The agglomerates obtained are measured not self-heating in the BOWES CAMERON test (sample subjected to an enclosure temperature equal to 140 ° C. for 24 hours) and do not react on contact with water.
Exemple 3Example 3
Dans les mêmes conditions opératoires que pour l'exemple 1 , pour 3000 grammes de masses usées, on charge 900 grammes de bentonite en poudre soit 30 % du poids de masse usée.Under the same operating conditions as for Example 1, for 3000 grams of spent mass, 900 grams of powdered bentonite is charged, ie 30% of the weight of spent mass.
Les agglomérats obtenus sont mesurés non auto-échauffants au test de BOWES CAMERON (échantillon soumis à une température d'enceinte égale à 140°C pendant 24 heures) et ne réagissent pas au contact de l'eau. II doit être bien compris que l'invention définie par les revendications annexées n'est pas limitée aux modes de réalisation particuliers indiqués dans la description ci-dessus, mais en englobe les variantes qui ne sortent ni du cadre ni de l'esprit de la présente invention. The agglomerates obtained are measured not self-heating in the BOWES CAMERON test (sample subjected to an enclosure temperature equal to 140 ° C. for 24 hours) and do not react on contact with water. It should be understood that the invention defined by the appended claims is not limited to the particular embodiments indicated in the description above, but encompasses variants thereof which do not depart from the scope or the spirit of the present invention.

Claims

REVENDICATIONS
1. Procédé d'agglomération et de passivation de la masse usée pulvérulente et/ou des fines pulvérulentes issues de la production d'organohalosilanes, comprenant :1. Process for agglomeration and passivation of the pulverulent spent mass and / or of the pulverulent fines resulting from the production of organohalosilanes, comprising:
(i) le mélange de cette masse usée et/ou des fines avec un liant choisi parmi les silicates d'aluminium ; (ii) la production d'un produit aggloméré solide par compression dans une presse. (i) mixing this spent mass and / or the fines with a binder chosen from aluminum silicates; (ii) the production of a solid agglomerated product by compression in a press.
2. Procédé selon la revendication 1 , caractérisé en ce que le silicate d'aluminium est de la bentonite.2. Method according to claim 1, characterized in that the aluminum silicate is bentonite.
3. Procédé selon la revendication 1 ou 2, caractérisé en ce que le rapport liant/masse usée et/ou fines va de 0,1/1 à 1 ,5/1 en poids.3. Method according to claim 1 or 2, characterized in that the binder / used and / or fine mass ratio ranges from 0.1 / 1 to 1.5 / 1 by weight.
4. Procédé selon la revendication 3, caractérisé en ce que le rapport liant/masse usée et/ou fines va de 0,3/1 à 1/1 en poids.4. Method according to claim 3, characterized in that the binder / used and / or fine mass ratio ranges from 0.3 / 1 to 1/1 by weight.
5. Procédé selon l'une quelconque des revendications 1 à 4, caractérisé en ce que l'étape (ii) est conduite à l'aide d'une presse munie de moyens de moulage par compression.5. Method according to any one of claims 1 to 4, characterized in that step (ii) is carried out using a press provided with compression molding means.
6. Procédé selon la revendication 5, caractérisé en ce que l'on emploie une presse à roues tangentes.6. Method according to claim 5, characterized in that a tangent wheel press is used.
7. Procédé selon l'une quelconque des revendications 1 à 6, caractérisé en ce que l'on produit des agglomérats ayant un volume unitaire compris entre 0,5 et 20 cm3.7. Method according to any one of claims 1 to 6, characterized in that agglomerates having a unit volume of between 0.5 and 20 cm 3 are produced .
8. Procédé selon l'une quelconque des revendications 1 à 7, caractérisé en ce que l'on produit des agglomérats non auto-échauffants.8. Method according to any one of claims 1 to 7, characterized in that non-self-heating agglomerates are produced.
9. Produit aggloméré solide et inerte, non auto-échauffant, susceptible d'être obtenu par la mise en œuvre du procédé selon l'une quelconque des revendications 1 à 8.9. A solid and inert agglomerated product, not self-heating, capable of being obtained by implementing the method according to any one of claims 1 to 8.
10. Produit aggloméré solide, inerte et non auto-échauffant, comprenant de la masse usée et/ou des fines résiduelles issues de la production d'organohalosilane, et un silicate d'aluminium, et ne comportant pas d'eau libre. 10. Solid agglomerated product, inert and not self-heating, comprising spent mass and / or residual fines from the production of organohalosilane, and an aluminum silicate, and containing no free water.
11. Produit selon la revendication 10, caractérisé en ce que le rapport silicate d'aluminium/masse usé et/ou fines va de 0,1/1 à 1 ,5/1 en poids.11. Product according to claim 10, characterized in that the aluminum silicate / used and / or fine mass ratio ranges from 0.1 / 1 to 1.5 / 1 by weight.
12.*Produit selon la revendication 11 , caractérisé en ce que ce rapport va de 0,3/1 à 1/1 en poids. 12. * Product according to claim 11, characterized in that this ratio ranges from 0.3 / 1 to 1/1 by weight.
13. Produit selon l'une quelconque des revendications 10 à 12, caractérisé en ce que les agglomérats ont un volume unitaire compris entre 0,5 et 20 cm3.13. Product according to any one of claims 10 to 12, characterized in that the agglomerates have a unit volume of between 0.5 and 20 cm 3 .
14. Utilisation d'un produit aggloméré selon l'une quelconque des revendications 9 à 13, pour la valorisation d'un ou plusieurs des métaux présents dans la masse usée et/ou les fines issues de la production d'organohalosilane. 14. Use of an agglomerated product according to any one of claims 9 to 13, for the recovery of one or more of the metals present in the spent mass and / or the fines resulting from the production of organohalosilane.
15. Utilisation selon la revendication 14, pour la valorisation du silicium métal.15. Use according to claim 14, for the recovery of silicon metal.
16. Utilisation selon la revendication 14, pour la valorisation du cuivre. 16. Use according to claim 14, for the recovery of copper.
EP04805476A 2003-11-27 2004-11-18 Method for agglomerating and passivating a used mass or organohalosilane production fines Withdrawn EP1687317A1 (en)

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FR0313927A FR2862956B1 (en) 2003-11-27 2003-11-27 METHOD FOR AGGLOMERATION AND PASSIVATION OF WEEE MASS OR FINES FROM THE PRODUCTION OF ORGANOHALOSILANES
PCT/FR2004/002939 WO2005063775A1 (en) 2003-11-27 2004-11-18 Method for agglomerating and passivating a used mass or organohalosilane production fines

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FR2855176B1 (en) * 2003-05-21 2005-07-08 Rhodia Chimie Sa METHOD OF AGGLOMERATING THE WEEE MASS OR FINE FROM THE PRODUCTION OF ORGANOHALOSILANES
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EP0201199B1 (en) 1985-04-09 1989-07-19 Toray Silicone Company Limited Method for treating activated silicon powder
EP0287934A3 (en) 1987-04-22 1989-03-22 General Electric Company Deactivation of spent silicon powder
AT399887B (en) * 1993-06-21 1995-08-25 Voest Alpine Ind Anlagen METHOD FOR PRODUCING COLD-PRESSED IRON-CONTAINED BRIQUETTES
US5342430A (en) * 1993-07-28 1994-08-30 Grocela Kathe Teresa A Passivation of methylchlorosilane fines
GB0029774D0 (en) 2000-12-07 2001-01-17 Dow Corning Clay composition
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