EP2935100A1 - Procédé permettant de traiter des matières solides sous forme de fines particules lors de la production de chlorosilanes - Google Patents

Procédé permettant de traiter des matières solides sous forme de fines particules lors de la production de chlorosilanes

Info

Publication number
EP2935100A1
EP2935100A1 EP13795225.5A EP13795225A EP2935100A1 EP 2935100 A1 EP2935100 A1 EP 2935100A1 EP 13795225 A EP13795225 A EP 13795225A EP 2935100 A1 EP2935100 A1 EP 2935100A1
Authority
EP
European Patent Office
Prior art keywords
pressure
finely divided
divided solids
pressing
different
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Withdrawn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
EP13795225.5A
Other languages
German (de)
English (en)
Inventor
Janaina MARINAS PÉREZ
Ekkehard MÜH
Hartwig Rauleder
Frank Kropfgans
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.)
Evonik Operations GmbH
Original Assignee
Evonik Degussa GmbH
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 Evonik Degussa GmbH filed Critical Evonik Degussa GmbH
Publication of EP2935100A1 publication Critical patent/EP2935100A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
    • C01B33/10742—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K11/00—Use of ingredients of unknown constitution, e.g. undefined reaction products
    • C08K11/005—Waste materials, e.g. treated or untreated sewage sludge

Definitions

  • the invention relates to a process for the preparation of finely divided solids, which in the
  • Chlorosilanes such as silicon tetrachloride (SiC, abbreviated STC), trichlorosilane (HS1CI3, abbreviated to TCS) and dichlorosilane (H 2 SiCl 2 ) represent an important class of substances with a broad class
  • Silicon (Si) and hydrogen chloride (HCl) and / or chlorine (Cl) are dissolved in a reactor, e.g. As fluidized bed reactor or fixed bed reactor or stirred bed reactor, which forms inorganic chlorosilanes such as S1CI 4 and / or HS1CI3 and / or H 2 SiCl 2 or mixtures thereof and leave as product gases the reactor and then treated further.
  • a reactor e.g. As fluidized bed reactor or fixed bed reactor or stirred bed reactor, which forms inorganic chlorosilanes such as S1CI 4 and / or HS1CI3 and / or H 2 SiCl 2 or mixtures thereof and leave as product gases the reactor and then treated further.
  • the product gases contain production-related solids such as powder and / or dust containing silicon, iron, iron chloride and / or aluminum chloride.
  • production-related solids such as powder and / or dust containing silicon, iron, iron chloride and / or aluminum chloride.
  • ferric chloride and aluminum chloride are reaction by-products resulting from the fact that the raw silicon used contains these metals in small amounts as contaminants, which remain in the liquid phase after liquefaction of the product gases, the so-called vapors and settle in the container for the liquid phase. As a result, they can be separated from the chlorosilane mixture formed.
  • Silicon tetrachloride these solids in the form of powder, dust, for example, filter dust, and / or ash, for example hot gas filter ash on.
  • Such solids are summarized in the context of the invention by the term "/ one-part solids".
  • the particulate solids are mainly silicon and iron, and may also contain chlorine compounds. Together with the chlorine compounds which are gaseous reaction products under the reaction conditions, for example TCS and STC, the finely divided solids are carried out of the reactor.
  • ground metallurgical silicon having a diameter of about 500 ⁇ m is reacted with hydrogen chloride. During the course of the reaction, the silicon particles become smaller and smaller and can finally exit the reactor as dusts. These dusts are usually separated by means of filters or cyclones before the
  • TCS and STC are condensed. Because they are very fine and besides iron still contain a large amount of silicon, they are a valuable raw material.
  • silicon-containing solids accumulate in the production of silicon from monosilane by deposition processes. Such solids are often mixtures of product coarse fractions which are separated from the process via sieves, are also analytical residues and goods which do not conform to specifications. The silicon content is often more than 99%.
  • the patent DE 10 2009 037 155 B3 provides for the dust discharged from the fluidized bed to be converted into a second connected fluidized bed reactor. This method has the disadvantage that the bulk of the solid is discharged due to its extreme fineness also from the second reactor without being materially reacted.
  • the object is achieved by a process for the preparation of finely divided solids and by the compacts obtained according to this method.
  • the invention relates to a process for the preparation of finely divided solids in the production of chlorosilanes, which is characterized in that the finely divided
  • Solids are pressed hydraulically to bodies of increased density.
  • the procedure of hydraulically pressing the finely divided solids is in the context of the invention synonymous with the fact that the finely divided solids are pressed in a hydraulic press.
  • a cylindrical sleeve of ceramic preferably of high-strength silicon nitride ceramic, as press-vacuum.
  • the upper and lower punches of the hydraulic press can be selected from hardened steel be.
  • stamps can be used in cylindrical form, but also any other shape is possible, for example, edged stamp, which give cube or cuboid compacts, or hemispherical shapes. Since the finely divided solids contain chlorine compounds, the pellets on contact with water or moisture on their surface hydrochloric acid, which decomposes both insufficiently alloyed steel and unpainted components of the hydraulic press. Therefore, the use of a ceramic sleeve is made
  • Silicon nitride, S1 3 N 4 as a press vacuum advantageous.
  • Hydrogen chloride also attacks the mucous membranes, skin and eyes of humans. It is therefore important to ensure that in the case of a manual implementation of the method personal protective equipment is worn, which prevents the direct contact of the finely divided solids used and the compacts obtained according to the invention with skin, eyes and mucous membranes.
  • inorganic binders preferably silicas, aluminates,
  • binders containing organic compounds for example silicic acid esters, or a mixture of these binders. If organic binders are used, the organic portion must be removed in a calcination step prior to use in chlorosilane production.
  • hydrolyzable silicon-halogen bonds which adhere to the solids, which thus have an acidic pH. This is neutralized by the binder (s). The unpleasant property of the compacts to release hydrogen chloride can thus be at least partially lifted.
  • a pressing pressure in the process according to the invention which is at most 14 kN / cm 2 , preferably from 10 kN / cm 2 to 12 kN / cm 2 .
  • Ambient pressure of 1013 hPa at 20 ° C which is applied to the finely divided solids in the hydraulic press. At a pressing pressure of zero so just the ambient pressure is exerted and thus achieved no compression. At a pressing pressure of at most 14 kN / cm 2 surprisingly stable pellets are obtained, because they can be handled, for example, conveyed via a conveyor belt in a reactor for the production of chlorosilanes without breaking or breaking into chunks.
  • Density gradients so-called layers have.
  • the layers can be extended transversely, longitudinally or in any other direction within the volume of the compact and with respect to the direction of action of the pressing pressure and have a non-woven or lens-like shape.
  • the formation of such layers, the so-called layer formation occurs particularly increased above a
  • the pressing pressure can be expended by the pressure beginning at zero with a selected one
  • Press speed is approached.
  • the pressing speed is within the scope of the invention, the quotient of pressing pressure and the time during which the pressure is increased monotonically increasing up to the pressing pressure, synonymous with the fact that the pressing pressure is started during this period.
  • Pressing speed of 0.1 to 1 kN / cm 2 s, preferably from 0.5 kN / cm 2 s are approached until the pressing pressure is reached, and then for a period of 0.5 to 1.5 s, preferably from 1 s, and then degraded to zero over a period of 0.5 to 1.5 seconds, preferably 1 second.
  • the initial pressure is selected smaller than the pressing pressure. It has been found that when filling a press vacuum with the finely divided solids before starting the pressure, the press vacuum up to 77 vol .-% air or gas. As the pressure starts to rise, the finely divided solids are gradually compressed and the air or trapped gas must escape. However, the smaller the sizes of the particles of finely divided solids are, the longer it takes for trapped air or gas to escape. If at least one venting stroke is carried out in the process according to the invention, compacts having greater strength are obtained than without at least one venting stroke.
  • a at an initial pressure pi a with the durations Ai a and 5i a , b at an initial pressure pi b , with the periods Ai b and 5i b , and pi a and pi b are the same or different , are preferably different, and the durations Ai a and ⁇ ⁇ are the same or different, preferably different, and the periods 5i a and 5i b are the same or different, preferably different.
  • Each venting stroke can be carried out with or without vacuum, preferably without vacuum, and with 0.2 to 1 kN / cm 2 , preferably 0.5 kN / cm 2 pressing pressure, and for 2 to 10 s, preferably 5 s duration.
  • a fill factor is understood to mean the ratio of the height at which the press vacuum is filled with the finely divided solids to the height of the compact produced according to the invention. If, for example, the vacancy has been filled up to a height of 96 mm and, after carrying out the method according to the invention, a compact having a height of about 22 mm is obtained, this compact lies with a filling factor of
  • This filling factor is unexpectedly high compared to filling factors of ordinary molding compounds, for example commercial sands, ceramic granules for the sintering for the production of tiles. For example, it is about 2 times lower for pure sand and the same pressure.
  • the subject of the invention is also a compact obtained according to the claimed process and characterized by a filling factor of the finely divided solids to be hydraulically pressed from 3.9 to 4.5.
  • the finely divided solids were filter dust from the hot filter of a fluidized-bed reactor for the production of chlorosilanes, so-called hot gas filter ash, in the examples described below.
  • Each press vacuum was filled up to a height of 96 mm with the hot gas filter ash.
  • the tests differed by the pressing pressure, which was 6, 8, 10, 12 or 14 kN / cm 2 and each had been started at a pressing speed of 0.5 kN / cm 2 s.
  • the ejection force was 7.5 kN / cm 2 in each case.
  • Table 1 Overview of the determined sizes of the compacts as a function of the pressing pressure.
  • the second venting stroke was started at 4 kN / cm 2 pressure at 0.5 kN / cm 2 s for 8 s, held for 1 s and degraded within 1 s.
  • the pellets obtained according to the invention Withstood a drop from about 2 m in height without shattering. Thus, they had a sufficiently good stability to be able to return them to the reactor.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Press-Shaping Or Shaping Using Conveyers (AREA)

Abstract

L'invention concerne un procédé permettant de traiter des matières solides sous forme de fines particules lors de la production de chlorosilanes, caractérisé en ce que les matières solides sous forme de fines particules sont compactées hydrauliquement pour former des corps de densité élevée. L'invention concerne également une pièce compactée obtenue selon le procédé de l'invention, caractérisée par un facteur de compression des matières solides sous forme de fines particules à compacter hydrauliquement compris entre 3,9 et 4,5.
EP13795225.5A 2012-12-21 2013-11-21 Procédé permettant de traiter des matières solides sous forme de fines particules lors de la production de chlorosilanes Withdrawn EP2935100A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102012224182.5A DE102012224182A1 (de) 2012-12-21 2012-12-21 Verfahren zur Aufbereitung feinteiliger Feststoffe bei der Herstellung von Chlorsilanen
PCT/EP2013/074376 WO2014095220A1 (fr) 2012-12-21 2013-11-21 Procédé permettant de traiter des matières solides sous forme de fines particules lors de la production de chlorosilanes

Publications (1)

Publication Number Publication Date
EP2935100A1 true EP2935100A1 (fr) 2015-10-28

Family

ID=49639873

Family Applications (1)

Application Number Title Priority Date Filing Date
EP13795225.5A Withdrawn EP2935100A1 (fr) 2012-12-21 2013-11-21 Procédé permettant de traiter des matières solides sous forme de fines particules lors de la production de chlorosilanes

Country Status (8)

Country Link
US (1) US9593021B2 (fr)
EP (1) EP2935100A1 (fr)
JP (1) JP6049905B2 (fr)
KR (1) KR101760584B1 (fr)
CN (1) CN104854025B (fr)
CA (1) CA2895836C (fr)
DE (1) DE102012224182A1 (fr)
WO (1) WO2014095220A1 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3088358A1 (fr) * 2015-04-28 2016-11-02 Evonik Degussa GmbH Procédé de préparation d'une matière solide en fines particules lors de la production de chlorosilanes
EP3100978A1 (fr) * 2015-06-02 2016-12-07 Evonik Degussa GmbH Traitement d'une matière solide en fines particules lors de la production de chlorosilanes par agglomération et compactage
EP3100979A1 (fr) * 2015-06-02 2016-12-07 Evonik Degussa GmbH Préparation d'une matière solide en fines particules lors de la production de chlorosilanes par frittage à basses températures

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5126203A (en) 1987-04-22 1992-06-30 General Electric Company Deactivation of spent silicon powder
US4892694A (en) * 1987-04-22 1990-01-09 General Electric Company Deactivation of spent silicon powder
EP0287934A3 (fr) 1987-04-22 1989-03-22 General Electric Company Désactivation de poudre de silicium usé
JPH0214882A (ja) * 1988-06-30 1990-01-18 Hitachi Metals Ltd 乾電池の電解質剤成形用ダイス
CN1205266A (zh) * 1997-07-16 1999-01-20 卢文开 热固性荧光或夜光塑料制品的制造方法及其制品
JP4630993B2 (ja) * 2008-08-31 2011-02-09 北京中晶華業科技有限公司 高純度シリコンの製造方法
DE102009020143A1 (de) 2009-05-04 2010-11-11 Pv Silicon Forschungs- Und Produktionsgesellschaft Mbh Verfahren zur Aufbereitung von Sägeabfällen zur Rückgewinnung von Silizium für die Herstellung von Solarsilizium
DE102009037155B3 (de) 2009-08-04 2010-11-04 Schmid Silicon Technology Gmbh Verfahren und Anlage zur Herstellung von Trichlorsilan
US20120261269A1 (en) 2009-12-22 2012-10-18 Wataru Kagohashi Process for production of polysilicon and silicon tetrachloride
JP2012017247A (ja) * 2010-06-08 2012-01-26 Osaka Titanium Technologies Co Ltd シリコン含有ペレットの製造方法
WO2012109459A1 (fr) * 2011-02-09 2012-08-16 Hariharan Alleppey V Récupération de valeur de silicium dans des rebuts de coupe de silicium
DE102013201742A1 (de) 2012-12-21 2014-06-26 Evonik Industries Ag Verfahren zur Aufbereitung von Silizium-haltigem feinkörnigen Material bei der Herstellung von Chlorsilanen

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
None *
See also references of WO2014095220A1 *

Also Published As

Publication number Publication date
CA2895836A1 (fr) 2014-06-26
KR20150097518A (ko) 2015-08-26
KR101760584B1 (ko) 2017-07-21
JP6049905B2 (ja) 2016-12-21
CN104854025B (zh) 2017-03-22
JP2016506319A (ja) 2016-03-03
DE102012224182A1 (de) 2014-07-10
CN104854025A (zh) 2015-08-19
US20150315030A1 (en) 2015-11-05
CA2895836C (fr) 2017-05-16
WO2014095220A1 (fr) 2014-06-26
US9593021B2 (en) 2017-03-14

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