WO2014000592A1 - Réacteur à lit fluidisé sans plateau perforé et procédé pour la préparation de trichlorure de bore - Google Patents

Réacteur à lit fluidisé sans plateau perforé et procédé pour la préparation de trichlorure de bore Download PDF

Info

Publication number
WO2014000592A1
WO2014000592A1 PCT/CN2013/077478 CN2013077478W WO2014000592A1 WO 2014000592 A1 WO2014000592 A1 WO 2014000592A1 CN 2013077478 W CN2013077478 W CN 2013077478W WO 2014000592 A1 WO2014000592 A1 WO 2014000592A1
Authority
WO
WIPO (PCT)
Prior art keywords
bed
carrier gas
sieve plate
fluidized bed
reaction
Prior art date
Application number
PCT/CN2013/077478
Other languages
English (en)
Chinese (zh)
Inventor
高远
朱刘
Original Assignee
广东先导稀材股份有限公司
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 广东先导稀材股份有限公司 filed Critical 广东先导稀材股份有限公司
Publication of WO2014000592A1 publication Critical patent/WO2014000592A1/fr

Links

Classifications

    • 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
    • B01J8/1818—Feeding of the fluidising gas
    • B01J8/1827—Feeding of the fluidising gas the fluidising gas being a reactant
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B35/00—Boron; Compounds thereof
    • C01B35/06—Boron halogen compounds
    • C01B35/061—Halides

Definitions

  • the present invention provides a fluidized bed without a sieve plate, comprising: a bed body; a carrier gas source for supplying a carrier gas from the lower portion of the bed body toward the upper portion of the bed body; a reaction gas supply device for supplying a reaction gas to the bed; a raw material supply device for supplying a powder raw material to the bed; a heating device for heating the bed; and a slag discharge port for discharging the reaction slag generated by the reaction in the bed; , connected to the bed, separating the substance reacted in the bed to obtain the final product.
  • the fluidized bed without the sieve plate further comprises: a reaction gas treatment device 9 for the reaction gas supply device 3
  • the reaction gas supplied to the bed 1 is subjected to dehydration drying and heating to increase the temperature.
  • the carrier gas of the carrier gas source 2 enters the direction of the carrier gas inlet 21 of the carrier gas guide 10 with respect to the carrier gas guide
  • the inner wall 103 at the position where the carrier gas inlet 21 is connected is inclined.
  • the method for preparing boron trichloride according to the second aspect of the present invention comprises the fluidized bed without the sieve plate according to the above aspect, wherein the preparation method of the boron trichloride comprises: passing the alkaline earth metal boride of the powder raw material
  • the raw material supply device 4 is filled in the bed 1 of the fluidized bed device without the sieve plate;
  • the carrier gas source 2 is turned on, and the carrier gas is introduced into the bed 1 of the fluidized bed device without the sieve plate, so that the powder raw material is
  • the bed 1 of the fluidized bed device without sieve plate is in a fluidized state;
  • the heating device 5 is turned on to heat the bed body 1, and after the temperature reaches a predetermined temperature, the reaction gas is supplied with anhydrous hydrogen chloride; after the reaction reaches a prescribed period of time , open and start the separation device 7 to obtain the desired boron trichloride.
  • the flow rate of the alkaline earth metal boride is 80 to 85 g/h, and the flow rate of anhydrous hydrogen chloride is 500 to 600 g/h.
  • the calcium boride is preferably calcium hexaboride.
  • the main substances in the reaction include: BC1 3 , carrier gas, hydrogen, BC1 3 , oxygen, nitrogen, Cl 2 , HC1 and the like, and calcium chloride slag and calcium boride.
  • carrier gas hydrogen
  • BC1 3 oxygen
  • nitrogen nitrogen
  • Cl 2 cyclopentadiene
  • HC1 cyclopentadiene
  • calcium chloride slag and calcium boride are preferably separated from other gases by a filter column composed of glass fibers to achieve gas-solid separation; in the gas separation device 72, preferably hot copper is used.
  • the main substances in the reaction are: BC1 3 , carrier gas, hydrogen, BC1 3 , oxygen, nitrogen, Cl 2 ,
  • the carrier gas The body is an inert gas.
  • the inert gas may be nitrogen, argon, helium or a mixed gas of two of them.
  • nitrogen is selected.
  • the flow rate is 0. 5m7h ⁇ 10 m7h.
  • the powdered calcium hexaboride having a particle diameter of 20 to 30 mesh is filled in the bed 1 of the fluidized bed without the sieve plate by the raw material supply device 4 at a flow rate of 80 g/h; the carrier gas source 2 is turned on, and the nitrogen gas is introduced into the absence of In the bed 1 of the fluidized bed of the sieve plate, the powdered calcium hexaboride is in a fluidized state in the bed 1 of the fluidized bed without the sieve plate; the heating device 5 is turned on to heat the bed 1 at a temperature After 550 ° C, 500 m / h flow rate into the bed 1 into the reaction gas treatment device 9 dehydration drying reaction of anhydrous hydrogen chloride, while continuously reducing the nitrogen flow to maintain the fluidized state of calcium boride, reaction lh; Thereafter, the separation device 7 is opened and started, and calcium chloride slag and calcium boride are separated by a filter column composed of glass fibers in the gas-solid separation device 71, and then oxygen and hydrogen
  • 100 ⁇ 120 mesh powder calcium hexaboride is filled into the bed 1 of the fluidized bed without sieve through the raw material supply device 4 at a flow rate of 85 g/h; the carrier gas source 2 is turned on, and the argon gas is introduced into the sieveless plate.
  • the powdered calcium hexaboride is in a fluidized state in the bed 1 of the fluidized bed without the sieve plate; the heating device 5 is turned on to heat the bed 1 at a temperature After 700 °C, the reaction gas of the dehydration and drying by the reaction gas treatment device 9 is introduced into the bed 1 at a flow rate of 600 g/h, and the flow rate of the argon gas is continuously lowered to maintain the fluidized state of the calcium boride. 5h; then opening and starting the separation device 7, separating the calcium chloride residue and the calcium boride by the filter column composed of the glass fiber in the gas-solid separation device 71, and then passing the oxygen through the hot carbon powder in the gas separation device 72.
  • the powdered magnesium boride of 180 ⁇ 200 mesh is filled into the bed 1 of the fluidized bed without the sieve plate through the raw material supply device 4 at a flow rate of 82 g/h; the carrier gas source 2 is opened, and the helium gas is introduced into the sieveless plate.
  • the powdered magnesium boride is in a fluidized state in the bed 1 of the fluidized bed without the sieve plate; the heating device 5 is turned on to heat the bed 1 after the temperature reaches 650 ° C.
  • the method for producing boron trichloride according to the present invention can obtain boron trichloride having a high purity.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Treating Waste Gases (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)

Abstract

L'invention porte sur un réacteur à lit fluidisé sans plateau perforé et sur un procédé pour la préparation de trichlorure de bore l'utilisant. Le procédé comprend : le remplissage du corps de réacteur (1) d'un réacteur à lit fluidisé sans plateau perforé d'une matière première en poudre, c'est-à-dire d'un borure de métal alcalinoterreux, par l'intermédiaire d'un dispositif (4) d'apport de matière première; l'ouverture d'une source (2) de gaz vecteur, l'introduction du gaz vecteur dans le corps de réacteur (1) du réacteur à lit fluidisé sans plateau perforé, afin que la matière première en poudre, c'est-à-dire le borure de métal alcalinoterreux, soit dans un état fluidisé dans le corps de réacteur (1) du réacteur à lit fluidisé sans plateau perforé; la mise en marche d'un dispositif de chauffage (5) pour chauffer le corps de réacteur (1), l'introduction d'un gaz réactionnel, c'est-à-dire de chlorure d'hydrogène anhydre, lorsque la température atteint la température spécifiée; et après que la réaction atteint la durée spécifiée, l'ouverture et le démarrage d'un dispositif de séparation (7), afin d'obtenir le trichlorure de bore nécessaire.
PCT/CN2013/077478 2012-06-28 2013-06-19 Réacteur à lit fluidisé sans plateau perforé et procédé pour la préparation de trichlorure de bore WO2014000592A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201210217421.0A CN103506056B (zh) 2012-06-28 2012-06-28 无筛板的流化床及三氯化硼的制备方法
CN201210217421.0 2012-06-28

Publications (1)

Publication Number Publication Date
WO2014000592A1 true WO2014000592A1 (fr) 2014-01-03

Family

ID=49782225

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2013/077478 WO2014000592A1 (fr) 2012-06-28 2013-06-19 Réacteur à lit fluidisé sans plateau perforé et procédé pour la préparation de trichlorure de bore

Country Status (2)

Country Link
CN (1) CN103506056B (fr)
WO (1) WO2014000592A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9669378B2 (en) 2014-03-18 2017-06-06 Matheson Tri-Gas, Inc. Reduction of SiCl4 in the presence of BCl3

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103950947B (zh) * 2014-05-20 2015-09-09 方治文 高纯三氯化硼-11的制备方法
CN106319216B (zh) * 2015-07-06 2018-01-23 广东先导稀材股份有限公司 气‑气反应装置
WO2020003925A1 (fr) * 2018-06-26 2020-01-02 昭和電工株式会社 Procédé de production de trichlorure de bore
CN114572992B (zh) * 2022-03-09 2023-06-23 福建福豆新材料有限公司 一种用于纯化三氯化硼的除氯化氢装置及三氯化硼的纯化系统
CN114570294B (zh) * 2022-04-21 2023-10-13 金宏气体股份有限公司 一种基于沸腾床反应器的三氟化硼连续生产装置及方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3839538A (en) * 1971-03-20 1974-10-01 Elektroschmelzwerk Kampten Gmb Process for the manufacture of boron halides
CN1155897A (zh) * 1995-06-07 1997-07-30 Gec阿尔松·斯坦工业公司 用于废物热处理的流化床反应器
CN1817437A (zh) * 2004-10-22 2006-08-16 阿尔斯通技术有限公司 调整循环式流化床反应系统固体循环量的方法和设备
CN201390803Y (zh) * 2008-12-02 2010-01-27 广州有色金属研究院 用于制备多晶硅颗粒的无筛板流化床反应装置
CN201431874Y (zh) * 2009-03-20 2010-03-31 仙桃市中星电子材料有限公司 螺旋式无筛板沸腾氯化炉
CN101912752A (zh) * 2010-08-20 2010-12-15 中国航天空气动力技术研究院 固体粒子播发器
CN102230732A (zh) * 2011-07-01 2011-11-02 广州有色金属研究院 沸腾氯化炉密闭式自动排渣装置

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3839538A (en) * 1971-03-20 1974-10-01 Elektroschmelzwerk Kampten Gmb Process for the manufacture of boron halides
CN1155897A (zh) * 1995-06-07 1997-07-30 Gec阿尔松·斯坦工业公司 用于废物热处理的流化床反应器
CN1817437A (zh) * 2004-10-22 2006-08-16 阿尔斯通技术有限公司 调整循环式流化床反应系统固体循环量的方法和设备
CN201390803Y (zh) * 2008-12-02 2010-01-27 广州有色金属研究院 用于制备多晶硅颗粒的无筛板流化床反应装置
CN201431874Y (zh) * 2009-03-20 2010-03-31 仙桃市中星电子材料有限公司 螺旋式无筛板沸腾氯化炉
CN101912752A (zh) * 2010-08-20 2010-12-15 中国航天空气动力技术研究院 固体粒子播发器
CN102230732A (zh) * 2011-07-01 2011-11-02 广州有色金属研究院 沸腾氯化炉密闭式自动排渣装置

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9669378B2 (en) 2014-03-18 2017-06-06 Matheson Tri-Gas, Inc. Reduction of SiCl4 in the presence of BCl3
US10010853B2 (en) 2014-03-18 2018-07-03 Matheson Tri-Gas, Inc. Reduction of SiCl4 in the presence of BCl3

Also Published As

Publication number Publication date
CN103506056B (zh) 2015-09-30
CN103506056A (zh) 2014-01-15

Similar Documents

Publication Publication Date Title
WO2014000592A1 (fr) Réacteur à lit fluidisé sans plateau perforé et procédé pour la préparation de trichlorure de bore
US7964172B2 (en) Method of manufacturing high-surface-area silicon
TWI778941B (zh) 以矽石製造高純度矽的裝置及方法
TWI386526B (zh) 高純度多結晶矽的製造方法及製造裝置
TWI466825B (zh) 製造超純矽之方法與裝置
JPH02233514A (ja) 多結晶シリコンの製造方法
EP2067751A1 (fr) Procédé et dispositif de fabrication de verre de silice
TWI555705B (zh) 在三氯化硼中減少四氯化矽之方法
TW201218254A (en) Apparatus and method for preparation of compounds or intermediates thereof from a solid material, and using such compounds and intermediates
CA2559846A1 (fr) Procedes de chloration sous vide cycliques faisant intervenir l'extraction de lithium
JPWO2013190945A1 (ja) 金属ケイ素及び多孔質炭素の製造方法
TW201221685A (en) Production of polycrystalline silicon in substantially closed-loop processes and systems
JP6123220B2 (ja) 多孔質炭素材料の製造方法
JP4692324B2 (ja) 高純度多結晶シリコンの製造装置
CN106219488A (zh) 一种制备盐酸并提纯石英砂的方法及装置
JP2007136392A (ja) アルカリ賦活の排ガスの処理方法
KR20140087326A (ko) 고순도 석영유리 분말 제조장치
JP5574295B2 (ja) 高純度シリコン微粉末の製造装置
RU2385291C1 (ru) Способ получения кристаллического кремния высокой чистоты (варианты)
CN115744919B (zh) 一种超高纯二氧化硅颗粒的制备方法
JP2008037747A (ja) ソーラーグレードのシリコン製造法
RU2554150C1 (ru) Способ и устройство карботермического получения кремния высокой чистоты
JP2008115066A (ja) シリコン製造装置
JP2013151379A (ja) 四塩化珪素の製造方法
JPS58172206A (ja) 金属窒化物の製造方法

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 13808708

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 13808708

Country of ref document: EP

Kind code of ref document: A1