WO2010116440A1 - Réacteur - Google Patents

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Publication number
WO2010116440A1
WO2010116440A1 PCT/JP2009/056447 JP2009056447W WO2010116440A1 WO 2010116440 A1 WO2010116440 A1 WO 2010116440A1 JP 2009056447 W JP2009056447 W JP 2009056447W WO 2010116440 A1 WO2010116440 A1 WO 2010116440A1
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WO
WIPO (PCT)
Prior art keywords
brick layer
main body
outer cylinder
brick
layer
Prior art date
Application number
PCT/JP2009/056447
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English (en)
Japanese (ja)
Inventor
靖史 松尾
晃一 竹村
和之 湯舟
誠 松倉
孝夫 竹内
裕介 和久田
Original Assignee
電気化学工業株式会社
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.)
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Application filed by 電気化学工業株式会社 filed Critical 電気化学工業株式会社
Priority to JP2011508083A priority Critical patent/JP5539967B2/ja
Priority to PCT/JP2009/056447 priority patent/WO2010116440A1/fr
Publication of WO2010116440A1 publication Critical patent/WO2010116440A1/fr

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    • 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
    • C01B33/10757—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of trichlorosilane
    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B01J19/0013—Controlling the temperature of the process
    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/02—Apparatus characterised by being constructed of material selected for its chemically-resistant properties
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00092—Tubes
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094—Jackets
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/0015—Controlling the temperature by thermal insulation means
    • B01J2219/00155—Controlling the temperature by thermal insulation means using insulating materials or refractories
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/02—Apparatus characterised by their chemically-resistant properties
    • B01J2219/025—Apparatus characterised by their chemically-resistant properties characterised by the construction materials of the reactor vessel proper
    • B01J2219/0272—Graphite

Definitions

  • the present invention relates to a reactor for performing a gas phase reaction under a high temperature condition.
  • the present invention relates to a reactor for trichlorosilane that converts tetrachlorosilane and hydrogen into trichlorosilane.
  • Trichlorosilane is expected to increase in demand as a raw material gas for high-purity silicon used in elements such as semiconductors and solar cells, and there has been a demand for efficient production of these.
  • trichlorosilane used as a raw material for producing high-purity silicon (Si: silicon) is produced by reacting tetrachlorosilane (SiCl4: silicon tetrachloride) with hydrogen and converting it. To do.
  • trichlorosilane is produced by a conversion reaction according to the following reaction formula (1).
  • SiCl4 + H2 ⁇ SiHCl3 + HCl (1) This reaction is performed by heating a raw material gas composed of gasified tetrachlorosilane and hydrogen to about 800 ° C. to about 1300 ° C. in a reaction furnace.
  • the trichlorosilane manufacturing apparatus is provided with a heat insulating structure for preventing heat transfer to the outside.
  • Patent Documents 1 and 2 a reaction vessel in which a supply gas of tetrachlorosilane and hydrogen is supplied to the inside and a reaction product gas of trichlorosilane and hydrogen chloride is generated by a conversion reaction, and the periphery of the reaction vessel
  • An apparatus for producing chlorosilane is disclosed.
  • the heat insulating material is formed of carbon and attached to the inner wall surface of the cylindrical wall, the upper surface of the bottom plate portion, and the lower surface of the top plate portion so as to be attached inside the storage container, and heat is transferred to the outside of the storage container. The movement is restrained.
  • the bottom of the reaction vessel is supported by a connecting pipe for gas supply and discharge.
  • the reaction container is supported by the support pillar member installed in the container center part.
  • a load due to the weight of the reaction vessel is locally applied to the tubular or columnar member and the bottom of the reaction vessel, which causes damage due to long-term use. It might be.
  • the present invention has been made in view of the above circumstances, and provides a reactor having high heat insulating properties, capable of producing stable trichlorosilane, and excellent in durability.
  • a substantially cylindrical outer cylinder container main body having a bottom plate, an outer cylinder container upper lid that hermetically seals the outer cylinder container main body, the outer cylinder container main body accommodated in the tetrachlorosilane,
  • a reaction vessel in which a gas containing hydrogen is supplied and a gas containing trichlorosilane and hydrogen chloride is generated, an upper lid heat insulating layer that covers the inner surface of the upper cover of the outer cylinder, and an inner surface of the outer cylinder body
  • a laminated structure in which a brick layer is laminated in the order of an outer brick layer with low thermal conductivity and an inner brick layer with high heat resistance from the inner surface of the outer cylinder container main body toward the center.
  • a reaction furnace is provided.
  • the outermost brick layer having low thermal conductivity means the outermost brick layer composed of bricks having lower thermal conductivity than the brick constituting the innermost brick layer.
  • a high heat-resistant innermost brick layer means the innermost brick layer comprised by the brick whose highest use temperature is higher than the brick which comprises an outermost brick layer.
  • the main body of the outer cylinder container is provided with a main body heat insulating layer and a brick layer, and the brick layer has a plurality of types of brick layers having different properties, i.e., the lowest thermal conductivity. Since it has the laminated structure laminated
  • the reactor according to the present invention has high heat insulation, can produce stable trichlorosilane, and is excellent in durability.
  • FIG. 1 is a schematic view of a reaction furnace according to the present invention. Sectional drawing of the main body heat insulation layer and brick layer (3 layer structure) provided inside the outer cylinder container main-body part which concerns on this invention. The front view of the stationary plate of the reaction container which concerns on this invention.
  • the reaction furnace 101 includes a substantially cylindrical outer cylinder container main body 102 having a bottom plate (outer cylinder container bottom 103) and an outer cylinder container main body 102 in an airtight manner.
  • a reaction in which a gas containing tetrachlorosilane and hydrogen is supplied to the inside, and a gas containing trichlorosilane and hydrogen chloride is generated by being accommodated in the outer cylinder container upper lid portion 104 and the outer cylinder container main body portion 102 that are sealed to each other.
  • 2 is a reactor having a laminated structure in which an outermost brick layer (203 in FIG. 2) with low thermal conductivity and an innermost brick layer (205 in FIG. 2) with high heat resistance are laminated in this order from the inner surface to the center. .
  • the reaction furnace 101 includes a main body heat insulating layer 107 that covers the inner surface of the outer cylindrical container main body 102, a gas introduction opening 110 for supplying gas into the reaction container 105, and a tricycle generated in the reaction container 105.
  • a reaction product gas extraction opening 111 for exhausting the reaction product gas containing chlorosilane and a heater 112 for heating the reaction vessel are provided.
  • the outer cylinder container main body 102 has a substantially cylindrical shape including a bottom plate (outer cylinder container bottom 103), and is made of metal such as aluminum, iron, and stainless steel. Although a heat load of 1100 ° C. to 1400 ° C. is applied to the innermost brick layer by the heater 112 for heating the reaction vessel 105, the main body heat insulating layer 107 and the brick layer provided on the inner side of the outer tube container main body 102. Accordingly, the surface temperature of the outer cylinder container main body 102 becomes about 70 to 90 ° C.
  • the upper opening end of the outer cylinder container main body 102 is provided with a fastening means for attaching an outer cylinder container upper lid 104 described later.
  • a fastening means will not be specifically limited if the inside of an outer cylinder container can be sealed airtightly.
  • a gas introduction opening 110 for supplying gas into the reaction vessel 105 is provided on the bottom plate of the outer cylinder vessel main body portion 102, and the reaction vessel 105 inner wall is provided on the side wall of the outer cylinder vessel main body portion 102.
  • a reaction product gas extraction opening 111 is provided for exhausting the reaction product gas containing trichlorosilane produced in (1).
  • a main body heat insulating layer 107 is provided inside the outer tube container main body 102 so as to cover it.
  • the main body heat insulating layer 107 is disposed so as not to transmit heat that could not be insulated by the brick layer 108 described later to the outside of the outer tube container main body portion 102. Therefore, the thermal load applied to the main body heat insulating layer 107 is It is small, about 800 ° C to 1200 ° C. Therefore, as a material constituting the main body heat insulating layer 107, the maximum use temperature may be low, but a material having more excellent heat insulating performance is preferable.
  • the main body heat insulating layer 107 is preferably composed of a plate-shaped heat insulating material.
  • a heat insulating material a heat insulating material mainly composed of alumina or silica can be cited, and the maximum use temperature is 1200 ° C. or higher. Some are preferably used.
  • a heat insulating board made of Khao wool (registered trademark) manufactured by Thermal Ceramics or Isowool (registered trademark) manufactured by Isolite Kogyo Co., Ltd.
  • a brick layer 108 formed by stacking a plurality of types of bricks having different properties is provided further inside the main body heat insulating layer 107.
  • the brick layer 108 has a laminated structure in which an outermost brick layer, an intermediate brick layer, and an innermost brick layer are laminated in this order toward the center of the outer container body 102.
  • the brick layer 108 preferably has a two-layer structure in which each of the outermost brick layer (203 in FIG. 2) and the innermost brick layer (205 in FIG. 2) is one type. Or as shown in FIG. 2, it is good also as a 3 layer structure made into 1 type about each layer of the outermost brick layer 203, the intermediate
  • the number of layers constituting the brick layer is not particularly limited, and is appropriately set depending on the size of the reaction furnace and the reaction temperature.
  • the shape of the brick may be a substantially rectangular parallelepiped, or may be formed so as to have a slight curvature in accordance with the shape of the outer cylinder container main body that is substantially cylindrical. Moreover, in order to laminate bricks, each member along the shape inside the side wall of the outer cylinder container main body 102 is used without using an adhesive or the like in order to avoid mixing the components in the adhesive into the reaction phase. Is preferably incorporated stably.
  • each brick constituting the brick layer 108 is more preferably one that has been baked at 1800 ° C. to remove the binder and organic matter in order to avoid contamination by foreign matter in the reaction phase.
  • Inner brick layer Since the innermost brick layer is disposed at a position closest to the reaction container among the heat insulating members of the outer cylinder container main body 102 and is exposed to a high temperature, a material having an excellent maximum use temperature is preferable.
  • the brick used for the innermost brick layer closest to the heater is subjected to a thermal load of about 1100 ° C to 1400 ° C, so the maximum operating temperature of the innermost brick layer is 1500 ° C or higher. Is preferred. Furthermore, it is preferable that the highest use temperature of the brick of an innermost brick layer is 1600 degreeC or more.
  • the innermost brick layer forms the inner wall surface of the outer cylinder container, it may come into contact with hydrogen, hydrogen chloride, or chlorosilanes leaked from the reaction container 105 and may be corroded by these substances. Therefore, it is preferably made of a material that does not react with these substances, has high erosion resistance to acidic and basic slugs, has high resistance to strong reducing gas such as H 2 gas, and has chemical resistance.
  • the brick having such characteristics is preferably made of Al 2 O 3 , SiO 2 , Fe 2 O 3 and having an Al 2 O 3 content of 99% or more.
  • Examples of such bricks include ISOLITE (registered trademark) BAL-99 manufactured by Isolite Industrial Co., Ltd., MB-G manufactured by AGC Ceramics Co., Ltd., and GM180H manufactured by Marukoshi Kogyo Co., Ltd.
  • the outermost brick layer is disposed between the innermost brick layer and the main body heat insulating layer 107, and insulates heat that has not been insulated by the innermost brick layer.
  • the maximum use temperature may be lower than the brick of the innermost brick layer, but it is preferable to use one having excellent heat insulation performance.
  • a brick it is preferable to use a low thermal conductivity brick having a thermal conductivity defined by JIS R 2616 of 0.7 W / m ⁇ K or less.
  • a low thermal conductivity brick having a thermal conductivity of 0.27 W / m ⁇ K or less.
  • the brick having such characteristics is preferably made of Al 2 O 3 , SiO 2 , Fe 2 O 3 and having a content of Fe 2 O 3 of 1% or less.
  • Examples of such low thermal conductivity bricks include ISOLITE (registered trademark) LBK-28 manufactured by Isolite Industry Co., Ltd. and GM-13 manufactured by Marukoshi Industry Co., Ltd.
  • An intermediate brick layer may be provided between the innermost brick layer and the outermost brick layer.
  • the intermediate brick layer is disposed between the innermost brick layer and the outermost brick layer, and insulates heat that is not insulated by the innermost brick layer.
  • the thermal load applied to the intermediate brick layer is about 1000 ° C to 1350 ° C.
  • the intermediate brick layer does not need to be resistant to these materials because it does not come into direct contact with hydrogen, hydrogen chloride, or chlorosilanes, but it uses bricks with better thermal insulation than the innermost brick layer. It is preferable.
  • Such a brick is preferably made of Al 2 O 3 , SiO 2 , Fe 2 O 3 and having an Al 2 O 3 content of 90% or more.
  • Examples of such bricks include ISOLITE (registered trademark) BAL-90 manufactured by Isolite Kogyo Co., Ltd. and GM-160 manufactured by Marukoshi Kogyo Co., Ltd.
  • the brick layer 108 is laminated at the bottom of the outer cylinder container main body 102 so as to surround the fixing plate 109 described later. If it can sufficiently withstand the weight of 105, the brick layer 108 can be laminated on the portion that contacts the fixing plate 109.
  • the outer cylinder container upper cover part 104 is a substantially disk-shaped member that hermetically seals the upper opening end of the outer cylinder container main body part 102 and is made of the same material as the outer cylinder container main body part 102.
  • the outer cylinder container upper cover part 104 is also provided with fastening means corresponding to the fastening means provided at the upper opening end of the outer cylinder container main body part 102.
  • An upper lid heat insulating layer 106 is provided on the inner side of the outer cylinder container upper lid portion 104 so as not to leak the heat in the outer cylinder container main body portion 102 to the outside.
  • the upper lid heat insulating layer 106 is attached to the inside of the outer cylinder container upper lid portion 104, it cannot be configured by incorporating bricks like the innermost brick layer. Therefore, it is preferable to use a material that has a high maximum use temperature, is excellent in corrosion resistance, and does not require incorporation, such as brick.
  • a heat insulating material include a heat insulating material made of alumina fiber, such as Denka Arsene (registered trademark) manufactured by Denki Kagaku Kogyo Co., Ltd., and Isowool (registered trademark) manufactured by Isolite Industrial Co., Ltd. Can be mentioned.
  • the heat insulation efficiency can be improved by attaching a heat insulating material constituting the upper cover heat insulating layer. By setting it as such a structure, the heat leak from the terminal part of the heater 112 can be suppressed.
  • the bottom surface of the reaction vessel 105 is preferably installed on the outer cylinder vessel bottom 103 by a fixed plate 109.
  • the fixing plate 109 is arranged on the bottom plate (outer cylinder container bottom 103) of the outer cylinder container main body 102, receives and supports the total weight of the reaction container 105 described later, and fixes it. Therefore, it is necessary to use a member having excellent strength so as to withstand the weight of the reaction vessel 105 as a member constituting the fixing plate 109, and for example, graphite can be used.
  • the fixing plate 109 corresponds to the gas introduction opening 110 provided in the outer cylinder container main body 102 so that the gas supply into the reaction container 105 is not hindered when arranged on the bottom plate of the outer cylinder container main body 102.
  • An opening is provided at a position to be used. The opening serves to fix the reaction vessel 105 by fitting a tubular projecting portion of a gas introduction opening 110 provided at the bottom of the reaction vessel 105 described later.
  • the fixed plate 109 has a plurality of holes penetrating in the thickness direction, that is, in the vertical direction when arranged between the bottom plate of the outer cylinder container main body 102 and the reaction vessel 105.
  • an air layer is formed in the through hole portion. Since air has a lower thermal conductivity than materials such as graphite used for the fixed plate 109, the formation of an air layer by providing such a through hole suppresses the release of heat through the fixed plate 109. Insulation performance can be improved. In addition, since the contact area between the fixed plate 109 and the reaction vessel can be reduced, heat transfer from the reaction vessel 105 to the fixed plate 109 can be prevented, and the heat insulation performance can be improved.
  • the number and shape of the holes provided in the fixing plate 109 are not particularly limited as long as sufficient strength can be secured to receive the total weight of the reaction vessel. Therefore, typically, as shown in FIG. 3, an opening for inserting the gas introduction opening 110 of the reaction vessel is provided at the center thereof, and a disk-like member having a plurality of through holes around the opening is provided. can do.
  • a pedestal made of expanded graphite is further provided between the fixed plate 109 and the outer cylinder container main body 102 to further suppress heat transfer from the lower portion of the fixed plate 109 to the outer cylinder container main body 102.
  • the reaction vessel 105 is a substantially cylindrical vessel for reacting tetrachlorosilane and hydrogen in a high temperature environment.
  • the reaction vessel 105 includes a gas introduction opening 110 for taking in tetrachlorosilane as a raw material and hydrogen gas, and a reaction product gas extraction opening 111 for deriving a reaction product gas containing trichlorosilane and hydrogen chloride.
  • the gas introduction opening 110 has a configuration in which the periphery of the opening extends vertically from the bottom to form a tubular protrusion, and is fitted into the opening provided in the center of the fixing plate. In this embodiment, as shown in FIG. 1, the gas introduction opening 110 is provided in the center of the bottom of the reaction furnace, and the reaction product gas extraction opening 111 is provided in the upper side wall of the reaction vessel 105. These positions are not limited to this.
  • a plurality of heaters 112 are installed at a predetermined interval between the reaction vessel 105 and the outer cylinder vessel main body 102.
  • the heater 112 is installed so as to be suspended from the outer cylinder container upper lid 104.
  • the heater installation method is not limited to the hanging type, and for example, the outer cylinder container main body with the electrode on the lower side. You may install so that it may stand up from the bottom of a part.
  • the inner side of the main body of the outer cylinder container includes a main body heat insulating layer and a brick layer, and the brick layer has a plurality of types of brick layers having different properties, that is, low thermal conductivity. Since it has the laminated structure laminated
  • the thermal conductivity of the brick of the outermost brick layer is 0.7 W / m ⁇ K or less, and further the thermal conductivity of the brick of the outermost brick layer is 0.27 W / m ⁇ K or less, the reactor The heat insulation performance can be improved.
  • the maximum use temperature of the innermost brick layer is 1500 ° C or higher, and the highest use temperature of the innermost brick layer brick is 1600 ° C or higher, it can be used for thermal loads reaching 1100 ° C to 1400 ° C. I can bear it. And the heat insulation and durability of a reaction furnace can be improved by using what was excellent in the corrosion resistance with respect to hydrogen, hydrogen chloride, and chlorosilanes for an innermost brick layer.
  • the heat insulation performance can be further improved.
  • the fixing plate which has a some hole penetrated to the up-down direction which is arrange
  • the area which a reaction container and an outer cylinder container main-body part contact can be reduced, and it can prevent that heat transfers to the exterior.
  • the reaction vessel is supported by a flat plate-like member, so that depending on the weight of the reaction vessel on the bottom of the reaction vessel or the member supporting the reaction vessel There is no local load.
  • reaction vessel is supported by depositing its entire weight on a fixed plate, it is not necessary to contact the upper cover of the outer tube vessel. Therefore, the area where the reaction container and the outer cylinder container come into contact can be reduced, and the heat of the reaction container can be prevented from escaping to the outside.
  • reaction vessel is supported only by the fixed plate, even if the reaction vessel expands due to heating, distortion and breakage due to thermal expansion are unlikely to occur in the outer cylinder vessel main body and the reaction vessel.
  • the fixing plate is made of graphite, even if the number of holes is increased in order to improve the heat insulation performance, the graphite is excellent in strength, so that it has sufficient strength to support the reaction vessel. be able to.
  • reaction furnace according to the present invention has been described above, the present invention is not limited to these.
  • Example 1 The reaction furnace as shown in FIG. 1 was produced using the outer cylinder container main body part which has the following heat insulation structures, and the reaction vessel fixing plate.
  • Outer cylinder container top cover Alumina fiber (manufactured by Denki Kagaku Kogyo Co., Ltd .: Arsen (registered trademark)) was filled inside the outer lid portion of the outer cylinder container as an upper lid heat insulating layer.
  • Outer cylinder body A heat insulation board (Iso wool (registered trademark) manufactured by Isolite Industry Co., Ltd.) was pasted as a main body heat insulation layer on the inner surface of the outer cylinder container main body, and the following heat-resistant bricks were stacked as a brick layer inside.
  • Inner brick layer BAL-99
  • Outer brick layer LBK-28 (Fixing plate)
  • a graphite disc-like plate material having an opening for fitting the tubular projection of the gas inlet of the reaction vessel at the center and a plurality of through holes around it is used. It was.
  • the diameter of the through hole was 5% of the diameter of the fixed plate, and the through hole was formed so as to occupy an area of 30% of the fixed plate.
  • the outer cylinder container main body and the outer cylinder container upper lid were made of iron, and the reaction vessel was formed by connecting a plurality of substantially cylindrical carbon cylinders made of isotropic graphite whose surface was treated with a silicon carbide coating. A thing was used.
  • the temperature of the surface part and outer peripheral surface part of the innermost brick layer of the reactor was measured.
  • the temperature of the surface portion of the innermost brick layer was 1100 ° C.
  • the temperature of the outer peripheral surface portion was 150 ° C.
  • the apparatus was disassembled and the inside of the outer cylinder container main body, the brick layer, the fixed plate, etc. were observed, and any member was found to be distorted or damaged. There wasn't.
  • Example 2 the brick layer has a three-layer structure as shown in FIG. At this time, BAL-90 was used for the intermediate brick layer. Other than that, the same experiment as in Example 1 was performed using a reactor manufactured in the same manner as in Example 1.
  • the temperature of the surface part and outer peripheral surface part of the innermost brick layer of the reactor was measured.
  • the temperature of the surface portion of the innermost brick layer was 1100 ° C.
  • the temperature of the outer peripheral surface portion was 80 ° C.
  • Example 3 In Example 3, a reactor similar to Example 2 was prepared except that a pedestal made of expanded graphite was disposed between the fixed plate and the outer cylinder container main body, and an experiment similar to Example 2 was performed. .
  • the temperatures of the bottom surface portion and the outer bottom surface portion of the innermost brick layer of the reactor were measured.
  • the temperature of the bottom surface portion of the innermost brick layer of the reactor was 1100 ° C.
  • the temperature of the outer bottom surface portion was 80 ° C.
  • Example 1 A single-layer brick layer was formed using only LBK-28. And the reactor similar to Example 1 was produced, and the experiment similar to Example 1 was conducted.
  • the temperature of the surface part and outer peripheral surface part of the innermost brick layer of the reactor was measured.
  • the temperature of the surface portion of the innermost brick layer was 1100 ° C.
  • the temperature of the outer peripheral surface portion was 250 ° C.
  • the apparatus was disassembled and the inside of the outer cylinder container main body, the brick layer, the fixed plate, etc. were observed, the brick layer was corroded.
  • the temperature of the outer peripheral surface of an outer cylinder container main-body part is clearly high compared with the case of Example 1, and the heat inside a reactor tends to leak outside.
  • the reaction furnace according to the present invention has high heat insulating properties, and thus has an effect of suppressing the manufacturing cost.
  • the reactor according to the present invention has high heat insulation, can produce stable trichlorosilane, and is excellent in durability.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Furnace Housings, Linings, Walls, And Ceilings (AREA)

Abstract

L'invention porte sur un réacteur ayant une isolation thermique élevée et une excellente durabilité, qui permet une production stable de trichlorosilane. Le réacteur comprend un corps principal généralement cylindrique de conteneur cylindrique externe ayant une plaque de fond ; un couvercle supérieur de conteneur cylindrique externe pour sceller de façon hermétique le corps principal de conteneur cylindrique externe ; une chambre de réaction pour produire un gaz contenant du trichlorosilane et du chlorure d'hydrogène, qui est contenu dans le corps principal de conteneur cylindrique externe et dans laquelle un gaz contenant du tétrachlorosilane et de l'hydrogène est introduit ; une couche d'isolation thermique de couvercle supérieur recouvrant la surface interne du couvercle supérieur de conteneur cylindrique externe, et une couche de briques disposée sur la surface interne du corps principal de conteneur cylindrique externe. La couche de briques a une structure multicouche dans laquelle une couche de briques externe faiblement conductrice de la chaleur et une couche de briques interne hautement résistante à la chaleur sont disposées dans cet ordre de la surface interne du corps principal de conteneur cylindrique externe vers le centre de celui-ci.
PCT/JP2009/056447 2009-03-30 2009-03-30 Réacteur WO2010116440A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP2011508083A JP5539967B2 (ja) 2009-03-30 2009-03-30 反応炉
PCT/JP2009/056447 WO2010116440A1 (fr) 2009-03-30 2009-03-30 Réacteur

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2009/056447 WO2010116440A1 (fr) 2009-03-30 2009-03-30 Réacteur

Publications (1)

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WO2010116440A1 true WO2010116440A1 (fr) 2010-10-14

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WO2012047658A1 (fr) * 2010-09-27 2012-04-12 Gtat Corporation Dispositif de chauffage et procédés associés
US9217609B2 (en) 2011-06-21 2015-12-22 Gtat Corporation Apparatus and methods for conversion of silicon tetrachloride to trichlorosilane
WO2016006576A1 (fr) * 2014-07-07 2016-01-14 株式会社Ihi Dispositif de traitement thermique
US9308510B2 (en) 2013-05-07 2016-04-12 Bruce Hazeltine Monolithic heat exchanger and apparatus and methods for hydrogenation of a halosilane

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CN114011348A (zh) * 2021-10-09 2022-02-08 周彤 一种控温式化工反应釜

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JPS62123011A (ja) * 1985-11-25 1987-06-04 Koujiyundo Silicon Kk トリクロルシランの製造方法およびその装置
JPS63112410A (ja) * 1986-10-31 1988-05-17 Nippon Steel Corp トリクロルシランの製造方法

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012047658A1 (fr) * 2010-09-27 2012-04-12 Gtat Corporation Dispositif de chauffage et procédés associés
US10315181B2 (en) 2010-09-27 2019-06-11 Gtat Corporation Heater and related methods therefor
US9217609B2 (en) 2011-06-21 2015-12-22 Gtat Corporation Apparatus and methods for conversion of silicon tetrachloride to trichlorosilane
US9308510B2 (en) 2013-05-07 2016-04-12 Bruce Hazeltine Monolithic heat exchanger and apparatus and methods for hydrogenation of a halosilane
WO2016006576A1 (fr) * 2014-07-07 2016-01-14 株式会社Ihi Dispositif de traitement thermique
JPWO2016006576A1 (ja) * 2014-07-07 2017-04-27 株式会社Ihi 熱処理装置
CN106662400A (zh) * 2014-07-07 2017-05-10 株式会社Ihi 热处理装置
CN106662400B (zh) * 2014-07-07 2019-09-13 株式会社Ihi 热处理装置

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