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EP3962861A1 - Procédé pour la production de trichlorosilane comprenant des particules de silicium à structure optimisée - Google Patents

Procédé pour la production de trichlorosilane comprenant des particules de silicium à structure optimisée

Info

Publication number
EP3962861A1
EP3962861A1 EP19721256.6A EP19721256A EP3962861A1 EP 3962861 A1 EP3962861 A1 EP 3962861A1 EP 19721256 A EP19721256 A EP 19721256A EP 3962861 A1 EP3962861 A1 EP 3962861A1
Authority
EP
European Patent Office
Prior art keywords
silicon
grain
particles
mass
fluidized bed
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.)
Pending
Application number
EP19721256.6A
Other languages
German (de)
English (en)
Inventor
Karl-Heinz RIMBÖCK
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.)
Wacker Chemie AG
Original Assignee
Wacker Chemie AG
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 Wacker Chemie AG filed Critical Wacker Chemie AG
Publication of EP3962861A1 publication Critical patent/EP3962861A1/fr
Pending 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
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00584—Controlling the density
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00654—Controlling the process by measures relating to the particulate material
    • B01J2208/00672—Particle size selection
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1809—Controlling processes

Definitions

  • the invention relates to a method for producing
  • Silicon contact mass containing structurally optimized silicon particles in a fluidized bed reactor Silicon contact mass containing structurally optimized silicon particles in a fluidized bed reactor.
  • the starting material for the production of chips or solar cells is usually made by decomposing its volatile
  • Halogen compounds especially trichlorosilane (TCS, HSXCI3).
  • Polycrystalline silicon can be produced in the form of rods using the Siemens process, with polysilicon being deposited on heated filament rods in a reactor.
  • the process gas is usually a
  • polysilicon granules can be produced in a fluidized bed reactor. Silicon particles are thereby produced using a
  • WO2016 / 198264A1 is based on the following reactions:
  • chlorosilanes can be made from silicon (usually metallurgical silicon Si mg ) with the addition of hydrogen chloride (HCl) in one
  • Fluidized bed reactor are produced, the reaction being exothermic.
  • TCS and STC are usually obtained as the main products.
  • chlorosilanes in particular TCS, is the thermal conversion of STC and hydrogen in the gas phase in the presence or absence of a catalyst.
  • the low temperature conversion (LTC) according to reaction (2) is a weakly endothermic process and is usually carried out in the presence of a catalyst (for example copper-containing catalysts or catalyst mixtures).
  • the NTK can take place in a fluidized bed reactor in the presence of Si mg under high pressure (0.5 to 5 MPa) at temperatures between 400 and 700 ° C. An uncatalyzed reaction procedure is under
  • the high temperature conversion according to reaction (3) is an endothermic process. This process usually takes place in a reactor under high pressure at temperatures between 600 and 1200 ° C. In principle, the known methods are complex and energy-intensive. The necessary energy supply, which is usually electrical, represents a considerable cost factor.
  • the operational performance of the NTK in the fluidized bed reactor depends, in addition to adjustable reaction parameters, primarily on the raw materials used. Furthermore, it is necessary for a continuous process management, the educt components silicon, hydrogen and STC as well
  • Chlorosilanes per time unit and reaction volume Chlorosilanes per time unit and reaction volume
  • the most important parameters that influence the performance of the NTK are basically the TCS selectivity, the silicon use and the formation of by-products.
  • the present invention was based on the object of providing a particularly economical process for producing chlorosilane via NTK.
  • the invention relates to a process for the preparation of chlorosilanes of the general formula 1
  • n means values from 1 to 3
  • Means grain mixture which is introduced into the fluidized bed reactor, contains at least 1% by mass of silicon-containing particles S, which are described by a structural parameter S, where S has a value of at least 0 and is calculated as follows: Equation (1),
  • r F is mean particle solids density [g / cm 3 ].
  • the particles S with a structural parameter S of> 0 preferably have lower mean particle sizes than those particles with a structural parameter S of ⁇ 0, whereby the mean
  • the method according to the invention has a
  • “Granulation” is understood to mean a mixture of silicon-containing particles which can be produced, for example, by atomizing or granulating silicon-containing melts and / or by comminuting lumpy silicon by means of crushing and grinding systems Particle size of> 10 mm, particularly preferably> 20 mm, in particular> 50 mm
  • Grain sizes can essentially be classified into fractions by sieving and / or sifting.
  • a mixture of different grain sizes can be referred to as a grain mixture and the grains of which the grain mixture is made up as grain fractions.
  • Grain fractions can be divided relative to one another according to one or more properties of the fractions, such as, for example, into coarse grain fractions and fine grain fractions. Basically with a
  • Grain mixing possible to divide more than one grain fraction into fixed relative fractions.
  • the working grain denotes that grain or
  • Granular mixture that is introduced into the fluidized bed reactor.
  • the symmetry-weighted sphericity factor f s results from the product of the symmetry factor and sphericity.
  • Both Shape parameters can be determined by means of dynamic image analysis in accordance with ISO 13322, the values obtained representing the volume-weighted mean over the respective sample of the corresponding particle mixture of the working grain.
  • the symmetry-weighted sphericity factor of the particles S is preferably at least 0.70, particularly preferably at least 0.72, very particularly preferably at least 0.75, in particular at least 0.77 and at most 1.
  • the sphericity of a particle describes the relationship between the surface area of a particle image and the circumference. Accordingly, a spherical particle would have a sphericity close to 1, while a jagged, irregular particle image would have a roundness close to zero.
  • the center of gravity of a particle image is first determined. Then, in each measurement direction, distances from edge to edge are laid through the specific center of gravity and the ratio of the two resulting route sections is measured. The value of the symmetry factor is calculated from the smallest ratio of these radii. For highly symmetrical figures such as circles or squares, the value of the respective symmetry factor is 1.
  • the bulk density is defined as the density of a mixture of a particulate solid (so-called bulk material) and a continuous fluid (e.g. air) which fills the spaces between the particles.
  • the bulk density of the grain fraction of the working grain with structure parameter S 3 0 is
  • the bulk density can be determined by the
  • the mean, mass-weighted particle solids density of the particles of the grain fraction with structure parameters S> 0 is preferably 2.20 to 2.70 g / cm 3 , particularly preferably 2.25 to 2.60 g / cm 3 , very particularly preferably 2.30 to 2.40 g / cm 3 , in particular 2.31 to 2.38 g / cm 3 .
  • the determination of the density of solid substances is described in DIN 66137-2: 2019-03.
  • the grain fraction with structural parameter S 3 0 is preferably present in the working grain in a mass fraction of at least 1 mass%, particularly preferably at least 5 mass%, very particularly preferably at least 10 mass%, in particular at least 20 mass%.
  • particles with S 3 0 have one
  • Particle size parameter d 50 which is 0.5 to 0.9 times the particle size parameter d 50 of the particles with S ⁇ 0.
  • the working grain preferably has a
  • Particle size parameters d 50 from 70 to 1500 ⁇ m, particularly preferably from 80 to 1000 ⁇ m, very particularly preferably from 100 to 800 ⁇ m, in particular from 120 to 600 ⁇ m.
  • the difference between the particle size parameters d 90 and dio represents a measure of the width of a grain size or a
  • Grain fraction The quotient of the width of a grain or a grain fraction and the respective
  • Particle size parameter d 50 corresponds to the relative width. It can be used, for example, to determine particle size distributions with very different mean particle sizes
  • the relative width of the grain is preferably the
  • Working grain 0.1 to 500, preferably 0.25 to 100, particularly preferably 0.5 to 50, in particular 0.75 to 10.
  • the determination of the particle sizes and particle size distribution can be done according to ISO 13320 (laser diffraction) and / or ISO 13322
  • Particle size parameters from particle size distributions can be done according to DIN ISO 9276-2.
  • Working grain has a mass-weighted surface area of 80 to 1800 cm 2 / g, preferably from 100 to 600 cm 2 / g, particularly preferably from 120 to 500 cm 2 / g, in particular from 150 to 350 cm 2 / g.
  • a 2-modal distribution density function has two maxima.
  • Fluidized bed can be avoided.
  • the distribution density function of the grain mixture are far apart.
  • the contact mass is, in particular, the mixture of grains that is in contact with the reaction gas.
  • the contact compound therefore preferably does not comprise any further components. It is preferably a grain mixture containing silicon, which is at most 5% by mass,
  • Si mg which usually has a purity of 98 to 99.9%.
  • a composition with 98% by mass of silicon metal for example, is typical, the remaining 2% by mass generally being composed for the most part of the following elements, which are selected from: Fe, Ca, A1, Ti, Cu, Mn, Cr , V, Ni, Mg, B, C, P and O.
  • the following elements selected from among: Co, W, Mo, As, Sb, Bi, S, Se, Te, Zr, Ge, Sn can also be contained , Pb, Zn, Cd, Sr, Ba, Y and CI.
  • the silicon-metal fraction is preferably greater than 75% by mass, preferably greater than 85% by mass, particularly preferably greater than 95% by mass.
  • the catalyst can be one or more elements from the group comprising Fe, Cr, Ni, Co, Mn, W, Mo, V, P, As, Sb, Bi, O, S, Se, Te, Ti, Zr , C, Ge, Sn, Pb, Cu, Zn, Cd, Mg, Ca, Sr,
  • the catalyst is preferably selected from the group with Fe, Al, Ca, Ni, Mn, Cu, Zn, Sn,
  • oxidic or metallic form as silicides or in other metallurgical phases, or as oxides or chlorides. Their proportion depends on the purity of the silicon used.
  • the catalyst can, for example, in metallic, alloyed and / or salt-like form of the working grain and / or
  • Contact mass are added. These can in particular be chlorides and / or oxides of the catalytically active elements. Preferred compounds are CuC1, CuC1 2 , CuO or mixtures thereof.
  • the working grain can also contain promoters, for example Zn and / or zinc chloride.
  • the elemental composition of the silicon used and the contact compound can be, for example, by means of
  • XRF X-ray fluorescence analysis
  • ICP-MS ICP-based analysis methods
  • ICP-OES ICP-OES
  • AAS atomic absorption spectrometry
  • the catalyst is based on silicon, preferably in a proportion of 0.1 to 20% by mass, particularly preferably 0.5 to 15% by mass, in particular 0.8 to 10% by mass, particularly preferably 1 to 5 Mass%, present.
  • the grain fractions with structural parameters S ⁇ 0 and S 3 0 are preferably used as a prefabricated grain mixture
  • the grain fractions with structural parameters S ⁇ 0 and S h 0 can also be fed to the fluidized bed reactor separately, in particular via separate feed lines and containers. Mixing then takes place when the fluidized bed is formed (in situ). Any further constituents of the contact compound which may be present can also be added separately or as a constituent of one of the two grain fractions.
  • the process is preferably carried out at a temperature of 400 to 700.degree. C., particularly preferably 450 to 650.degree.
  • the pressure in the fluidized bed reactor is preferably 0.5 to 5 MPa, particularly preferably 1 to 4 MPa, in particular 1.5 to 3.5 MPa.
  • the reaction gas preferably contains at least 10% by volume, particularly preferably at least 50% by volume, before it enters the reactor. -%, in particular at least 90% by volume, hydrogen and silicon tetrachloride.
  • the molar ratio is preferably hydrogen and
  • HCl and / or Cl 2 can be added to the reaction gas, in particular to enable an exothermic reaction process and to influence the equilibrium position of the reactions.
  • the reaction gas preferably contains 0.01 to 1 mol of HCl and / or 0.01 to 1 mol of C1 2 per mol of hydrogen present before it enters the reactor.
  • HCl can also be present as an impurity in recovered hydrogen.
  • the reaction gas can also contain a carrier gas which does not take part in the reaction, for example nitrogen or a noble gas such as argon.
  • the composition of the reaction gas is usually determined by means of Raman and infrared spectroscopy and gas chromatography before it is fed to the reactor. This can be done both via random samples and
  • the chlorosilanes of general formula 1 prepared by the process according to the invention are preferably at least one chlorosilane selected from the group
  • Other halosilanes can arise as by-products, for example monochlorosilane (H3SiCl), dichlorosilane (H2S1Cl2), silicon tetrachloride (STC, SiC1 4 ) and di- and oligosilanes.
  • impurities such as hydrocarbons,
  • Organochlorosilanes and metal chlorides can be by-products.
  • the crude product is then usually distilled.
  • the inventive method is preferably in one
  • the network includes in particular the following
  • FIG. 1 shows an example of a fluidized bed reactor 1 for carrying out the method according to the invention.
  • Reaction gas 2 is preferably blown into the contact mass from below and optionally from the side (for example tangential or orthogonal to the gas flow from below), whereby the particles of the contact mass are fluidized and form a fluidized bed 3.
  • the fluidized bed 3 is heated by means of a heating device (not shown) arranged outside the reactor. No heating is usually required during continuous operation.
  • a part of the particles is with the gas flow from the fluidized bed 3 into the free space 4 above the Fluidized bed 3 transported.
  • the free space 4 is characterized by a very low solid density, which decreases in the direction of the reactor outlet 5.
  • silicon was of the same type in terms of purity, quality and content of minor elements and
  • the grain fractions used in the working grains were produced by breaking lumpy Si mg (98.9% by mass Si) and subsequent grinding or by atomization techniques known to those skilled in the art to produce particulate Si mg (98.9% by mass Si). If necessary, classification was carried out by sieving / sifting. In this way, grain fractions with specific values for structural parameters S were produced in a targeted manner. By combining and mixing these
  • the operating temperature of the fluidized bed reactor was around 520 ° C. during the tests.
  • ms is the mass fraction of particles that have a

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Catalysts (AREA)

Abstract

L'invention concerne un procédé pour la production de chlorosilanes répondant à la formule générale 1 : HnSiCl4-n (1), dans laquelle n représente des valeurs de 1 à 4, dans un réacteur à lit fluidisé, dans lequel un gaz de réaction contenant du tétrachlorure de silicium et de l'hydrogène est mis en réaction avec une masse de contact particulaire, qui contient du silicium, à des températures de 350 à 800 °C, la granulométrie de travail, qui signifie la granulométrie ou le mélange de granulométries introduit dans le réacteur à lit fluidisé, contient des particules S contenant au moins 1 % en masse de silicium, lesquelles sont décrites par un paramètre de structure S, S présentant une valeur d'au moins 0 et étant calculé comme suit : formule 2 équation (1), dans laquelle φS représente un facteur de sphéricité pondéré en symétrie, ρSD la masse spécifique apparente [g/cm3], ρF la masse spécifique de solide particulaire moyenne [g/cm3].
EP19721256.6A 2019-04-29 2019-04-29 Procédé pour la production de trichlorosilane comprenant des particules de silicium à structure optimisée Pending EP3962861A1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/EP2019/060941 WO2020221421A1 (fr) 2019-04-29 2019-04-29 Procédé pour la production de trichlorosilane comprenant des particules de silicium à structure optimisée

Publications (1)

Publication Number Publication Date
EP3962861A1 true EP3962861A1 (fr) 2022-03-09

Family

ID=66379904

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19721256.6A Pending EP3962861A1 (fr) 2019-04-29 2019-04-29 Procédé pour la production de trichlorosilane comprenant des particules de silicium à structure optimisée

Country Status (8)

Country Link
US (2) US20220212938A1 (fr)
EP (1) EP3962861A1 (fr)
JP (1) JP7381605B2 (fr)
KR (1) KR102676116B1 (fr)
CN (1) CN113795462A (fr)
MY (1) MY206228A (fr)
TW (1) TWI724830B (fr)
WO (1) WO2020221421A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116272693B (zh) * 2023-01-31 2025-09-26 内蒙古鄂尔多斯多晶硅业有限公司 一种适用于冷氢化流化床的硅粉颗粒选取方法

Family Cites Families (17)

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NO166032C (no) * 1988-12-08 1991-05-22 Elkem As Fremgangsmaate ved fremstilling av triklormonosilan.
CN1153138A (zh) * 1995-09-21 1997-07-02 瓦克化学有限公司 制备三氯硅烷的方法
DE10045367A1 (de) * 2000-09-14 2002-03-28 Bayer Ag Verfahren zur Herstellung von Trichlorsilan
DE10062413A1 (de) * 2000-12-14 2002-07-04 Solarworld Ag Verfahren zur Herstellung von Trichlorsilan
DE102007021003A1 (de) * 2007-05-04 2008-11-06 Wacker Chemie Ag Verfahren zur kontinuierlichen Herstellung von polykristallinem hochreinen Siliciumgranulat
DE102008041974A1 (de) * 2008-09-10 2010-03-11 Evonik Degussa Gmbh Vorrichtung, deren Verwendung und ein Verfahren zur energieautarken Hydrierung von Chlorsilanen
DE102009037155B3 (de) * 2009-08-04 2010-11-04 Schmid Silicon Technology Gmbh Verfahren und Anlage zur Herstellung von Trichlorsilan
KR101672796B1 (ko) * 2009-11-10 2016-11-07 주식회사 케이씨씨 염소가스 혹은 염화수소를 이용하여 다결정실리콘 제조원료인 고순도의 삼염화실란을 제조하는 방법
JP5535679B2 (ja) * 2010-02-18 2014-07-02 株式会社トクヤマ トリクロロシランの製造方法
DE102011112662B4 (de) * 2011-05-08 2015-04-09 Centrotherm Photovoltaics Ag Verfahren zum Behandeln von metallurgischem Silizium
KR20140136985A (ko) * 2012-03-14 2014-12-01 센트로섬 포토볼타익스 유에스에이, 인크. 트리클로로실란의 제조
WO2014026588A1 (fr) * 2012-08-13 2014-02-20 江苏中能硅业科技发展有限公司 Procédé de préparation de germe cristallin à haute sphéricité et de silicium particulaire de lit fluidisé
WO2015089214A1 (fr) * 2013-12-10 2015-06-18 Summit Process Design, Inc. Procédé de production de trichlorosilane
KR101616043B1 (ko) * 2014-07-22 2016-04-27 한화케미칼 주식회사 삼염화실란의 제조방법
DE102015210762A1 (de) 2015-06-12 2016-12-15 Wacker Chemie Ag Verfahren zur Aufarbeitung von mit Kohlenstoffverbindungen verunreinigten Chlorsilanen oder Chlorsilangemischen
WO2018074269A1 (fr) * 2016-10-19 2018-04-26 株式会社トクヤマ Procédé de régulation de la concentration en contenu solide et procédé de production de trichlorosilane
EP3858788B1 (fr) 2017-10-05 2022-02-23 Wacker Chemie AG Procédé de préparation de chlorosilanes

Also Published As

Publication number Publication date
CN113795462A (zh) 2021-12-14
TW202039366A (zh) 2020-11-01
US20220212938A1 (en) 2022-07-07
JP2022533018A (ja) 2022-07-21
TWI724830B (zh) 2021-04-11
KR102676116B1 (ko) 2024-06-17
WO2020221421A1 (fr) 2020-11-05
JP7381605B2 (ja) 2023-11-15
MY206228A (en) 2024-12-05
KR20210138711A (ko) 2021-11-19
US20250230051A1 (en) 2025-07-17

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