WO2010116500A1 - Tour de refroidissement de trichlorosilane et procédé de fabrication de trichlorosilane l'utilisant - Google Patents

Tour de refroidissement de trichlorosilane et procédé de fabrication de trichlorosilane l'utilisant Download PDF

Info

Publication number
WO2010116500A1
WO2010116500A1 PCT/JP2009/057208 JP2009057208W WO2010116500A1 WO 2010116500 A1 WO2010116500 A1 WO 2010116500A1 JP 2009057208 W JP2009057208 W JP 2009057208W WO 2010116500 A1 WO2010116500 A1 WO 2010116500A1
Authority
WO
WIPO (PCT)
Prior art keywords
trichlorosilane
reaction product
cooling
product gas
gas
Prior art date
Application number
PCT/JP2009/057208
Other languages
English (en)
Japanese (ja)
Inventor
潤 中本
一正 松音
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.)
Filing date
Publication date
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 PCT/JP2009/057208 priority Critical patent/WO2010116500A1/fr
Priority to JP2011508138A priority patent/JPWO2010116500A1/ja
Priority to TW099102352A priority patent/TW201036915A/zh
Publication of WO2010116500A1 publication Critical patent/WO2010116500A1/fr

Links

Images

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
    • 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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28C—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA COME INTO DIRECT CONTACT WITHOUT CHEMICAL INTERACTION
    • F28C3/00—Other direct-contact heat-exchange apparatus
    • F28C3/06—Other direct-contact heat-exchange apparatus the heat-exchange media being a liquid and a gas or vapour
    • F28C3/08—Other direct-contact heat-exchange apparatus the heat-exchange media being a liquid and a gas or vapour with change of state, e.g. absorption, evaporation, condensation

Definitions

  • the present invention relates to a trichlorosilane cooling tower used for producing trichlorosilane from tetrachlorosilane and hydrogen, and a method for producing trichlorosilane using the trichlorosilane cooling tower.
  • Trichlorosilane (SiHCl 3 ) is a special material gas used for manufacturing semiconductors, liquid crystal panels, solar cells, and the like. In recent years, demand has been steadily expanding, and growth is expected as a CVD material widely used in the electronics field.
  • Trichlorosilane is produced by bringing vaporized tetrachlorosilane (SiCl 4 ) and hydrogen (H 2 ) into contact in a reaction furnace to achieve the following thermal equilibrium state. SiCl 4 + H 2 ⁇ SiHCl 3 + HCl (1) This reaction is performed by heating a raw material gas composed of gasified tetrachlorosilane and hydrogen to 700 to 1400 ° C. in a reaction furnace.
  • Patent Document 1 in order to efficiently recover trichlorosilane, as shown in Patent Document 1, after reaching the thermal equilibrium state of the above formula (1), the reaction is performed so that once generated trichlorosilane does not return to tetrachlorosilane again. It is necessary to cool the product gas to a predetermined temperature as quickly as possible to freeze the equilibrium. In order to instantly freeze the equilibrium state, Patent Document 1 describes that the reaction product gas is rapidly cooled to 300 ° C. or less in less than 1 second.
  • high-boiling polymers such as Si 2 Cl 6 , Si 3 Cl 8 , and Si 2 H 2 Cl 4 are liable to be by-produced. Since these high-boiling-point polymers may adhere to the wall of the pipe in the plant and block the pipe and hinder continuous operation of the plant, it is preferable to suppress the generation thereof.
  • Patent Document 1 In the method described in Patent Document 1, a reaction product gas is led out from a high-temperature reactor to a cooling tower, where a coolant is directly sprayed on the reaction product gas, and reaction is performed using latent heat of vaporization when the coolant is vaporized. It has excellent cooling efficiency in that it takes heat away from the product gas.
  • Patent Document 1 does not specifically disclose a means for suppressing the formation of a high-boiling polymer that accompanies rapid cooling.
  • the produced trichlorosilane is mainly condensed in the quenching chamber and collected in a receiver provided below the quenching chamber. Therefore, a large amount of high boiling point polymers such as Si 2 Cl 6 , Si 3 Cl 8 , and Si 2 H 2 Cl 4 having a higher boiling point are mixed in the acceptor together with trichlorosilane, and from the recovered chlorosilane mixture, The load for the work of fractionating only the target trichlorosilane is increased.
  • the present invention has been made in view of the above circumstances, and a trichlorosilane cooling tower capable of suppressing by-product formation of a high boiling point polymer without reducing the recovery rate of trichlorosilane and a method for producing trichlorosilane using the same.
  • the purpose is to provide.
  • the trichlorosilane cooling tower of the present invention is A coolant is sprayed on a reaction product gas containing trichlorosilane obtained by reacting a raw material gas containing tetrachlorosilane and hydrogen at a temperature in the range of 700 to 1400 ° C., and cooled to a temperature range of 70 to 600 ° C.
  • the method for producing trichlorosilane of the present invention includes: A coolant is sprayed on a reaction product gas containing trichlorosilane obtained by reacting a raw material gas containing tetrachlorosilane and hydrogen at a temperature in the range of 700 to 1400 ° C., and cooled to a temperature range of 70 to 600 ° C. And a process of A step of bringing hydrogen chloride gas into contact with the reaction product gas after cooling; Have
  • reaction formula (2 ) To (4) can decompose the high-boiling point polymer and, at the same time, derive trichlorosilane from the high-boiling point polymer.
  • the amount of the high boiling point polymer contained in the reaction product gas after cooling is reduced without reducing the recovery rate of trichlorosilane. Can be reduced. Therefore, the productivity of trichlorosilane can be greatly improved, the operation efficiency of the plant can be increased, and continuous operation can be performed.
  • primary cooling refers to cooling intended to freeze the equilibrium reaction of the above formula (1) by instantaneously reducing the temperature of the reaction product gas to a temperature range of 70 to 600 ° C.
  • secondary cooling refers to auxiliary cooling for the purpose of further reducing the temperature of the reaction product gas after the primary cooling as necessary.
  • the temperature of the reaction product gas can be reduced by bringing the hydrogen chloride gas into contact with the reaction product gas after the primary cooling, the main purpose of bringing the hydrogen chloride gas into contact with the reaction product gas in the present invention is the high boiling point polymer.
  • cooling of the reaction product gas caused by contact with hydrogen chloride gas is not included in the concept of “secondary cooling”.
  • FIG. 1 schematically shows an apparatus for carrying out a trichlorosilane cooling tower of this embodiment and a method for producing trichlorosilane using the same.
  • the trichlorosilane cooling tower 100 of the present embodiment includes a substantially cylindrical metal container 101, a primary spray nozzle 102 and a secondary spray nozzle 103 that are means for spraying a cooling liquid into the metal container 101, and the primary spray.
  • Rapid cooling provided to accommodate the primary spray nozzle 102 inside the metal container 101 and the primary coolant supply pipe 104 and the secondary coolant supply pipe 105 that supply the coolant to the nozzle 102 and the secondary spray nozzle 103, respectively.
  • a hydrogen chloride gas supply pipe 114 for supplying hydrogen chloride gas to the injection nozzle 113 is provided.
  • the metal container 101 is not particularly limited as long as it is a material that does not react with the reaction product gas, and can typically be made of a metal such as stainless steel.
  • a reaction product gas introduction opening 108 for taking in the reaction product gas is provided on the side wall of the metal container 101.
  • a cooling tower gas component extraction pipe 109 for extracting a gas component of the cooled reaction product gas is connected to the top of the metal container 101, and the bottom of the metal container 101 was used for cooling.
  • a cooling tower liquid component extraction pipe 110 is connected to extract the cooling liquid and the condensed liquid component generated by cooling.
  • the quenching tube 106 is not particularly limited as long as it does not react with the reaction product gas, and can typically be composed of a metal such as stainless steel.
  • the quench pipe 106 is provided with an introduction opening 111 for taking in the reaction product gas at a position corresponding to the reaction product gas introduction opening 108 of the metal container 101. Further, the bottom of the quench pipe 106 is open on the entire surface, and a discharge opening 112 for discharging the cooled reaction product gas is formed.
  • a two-stage cooling liquid spraying means including a primary spray nozzle 102 and a secondary spray nozzle 103 is employed as a means for spraying the cooling liquid into the metal container 101.
  • the cooling liquid spraying means in multiple stages, the primary cooling by the primary spray nozzle 102 rapidly quenches the reaction product gas to a temperature sufficient to freeze the equilibrium, and the secondary cooling by the secondary spray nozzle 103 Cooling according to the purpose can be realized such that the reaction product gas is gently cooled exclusively to condense the high-boiling point polymer.
  • the coolant spraying means may consist only of primary cooling.
  • the primary spray nozzle 102 is installed from the canopy portion of the quench pipe 106 toward the inside of the quench pipe 106, and is connected to the primary coolant supply pipe 104.
  • the primary spray nozzle 102 sprays the cooling liquid toward the reaction product gas introduced from the introduction opening 111 of the quench pipe 106, so that the coolant and the reaction product gas are contained in a narrow space in the quench pipe 106. It is brought into contact efficiently and instantaneously cooled to 70 to 600 ° C., more preferably 500 to 600 ° C., where the equilibrium of the above formula (1) freezes.
  • the primary spray nozzle 102 various types of nozzles can be used, but a full conical nozzle capable of realizing an even flow distribution over the entire spray region is preferable.
  • the cooling liquid sprayed from the primary spray nozzle 102 can be sprayed in an average droplet particle diameter range of 2000 ⁇ m or less.
  • the average droplet particle size depends not only on the nozzle characteristics but also on the spraying conditions.
  • the spray amount is 0.1 to 0.3 l / min
  • the spray pressure is 0.1 to 0.2 MPa
  • a mixed liquid composed of tetrachlorosilane and trichlorosilane having a mixing ratio described later is used as the cooling liquid, those capable of realizing an average droplet diameter of 2000 ⁇ m or less are preferable.
  • the filling member 107 is arbitrarily installed above the primary spray nozzle 102.
  • the filling member 107 is provided with a gas passage so that the reaction product gas that is primarily cooled in the quench pipe 106 and pushed out from the discharge opening 112 of the quench pipe 106 is disturbed in its straight travel when rising inside the trichlorosilane cooling tower 100.
  • Any form can be used as long as it is formed.
  • it may be a form in which small blocks such as chips or blocks are packed irregularly, or a plurality of plate-like members provided with a large number of holes arranged at intervals.
  • the filling member 107 is not particularly limited as long as it does not react with the reaction product gas, and can typically be made of a metal such as stainless steel.
  • the secondary spray nozzle 103 is arbitrarily installed further above the primary spray nozzle 102 and the filling member 107 and is connected to the secondary coolant supply pipe 105.
  • the secondary spray nozzle 103 is ejected from the discharge opening 112 of the quench pipe 106, rises in the trichlorosilane cooling tower 100, and sprays the coolant toward the reaction product gas passing through the filling member 107.
  • the coolant sprayed from the secondary spray nozzle 103 also has a function of lowering the temperature inside the trichlorosilane cooling tower 100 and preventing the coolant from being vaporized before coming into contact with the reaction product gas.
  • the secondary spray nozzle 103 is not particularly limited, and various types of nozzles can be used. In particular, a full-cone nozzle that can achieve a uniform flow distribution over the entire spray region is preferred.
  • the average droplet diameter of the cooling liquid sprayed from the secondary spray nozzle 103 is not particularly limited, but is preferably in the range of 2000 ⁇ m or less, as in the case of the primary spray nozzle 102, because the cooling efficiency is excellent.
  • a mixed liquid composed of tetrachlorosilane and trichlorosilane is preferably used, and the content of tetrachlorosilane in the mixed liquid is preferably 80 to 100 mol%, more preferably 85 to 95 mol%.
  • the cooling liquid having such a specific composition the reaction can be frozen while the equilibrium of the above formula (1) is sufficiently moved to the right side, and trichlorosilane can be recovered with a high yield.
  • the temperature of the coolant is preferably adjusted to 50 ° C. or lower. If the temperature of the cooling liquid is adjusted to 50 ° C. or less, the temperature of the reaction product gas can be rapidly cooled in a short time, so that the state of being sufficiently moved to the right side in the above equation (1) is maintained. The equilibrium can be frozen.
  • the hydrogen chloride gas injection nozzle 113 is installed at an arbitrary position where hydrogen chloride gas can be injected toward the reaction product gas cooled by the primary spray nozzle 102 and / or the secondary spray nozzle 103. Connected to the supply pipe 114. Since the high boiling point polymer decomposition reaction of the above formulas (2) to (4) is promoted at an atmospheric temperature of 500 to 600 ° C., the hydrogen chloride gas injection nozzle 113 is a reaction immediately after the equilibrium is frozen by the primary spray nozzle 102. It is particularly preferable to provide a position where hydrogen chloride gas can be injected toward the product gas.
  • the hydrogen chloride gas injection nozzle 113 is provided in the vicinity of the discharge opening 112 of the quench pipe 106, whereby the hydrogen chloride gas is efficiently brought into contact with the reaction product gas after the primary cooling and injected.
  • the reaction product gas after the secondary cooling can be contacted.
  • the hydrogen chloride gas supplied to the hydrogen chloride gas injection nozzle 113 needs to have a temperature that does not increase the temperature of the reaction product gas after the primary cooling. Further, when low-temperature hydrogen chloride gas is used, not only the high boiling point polymer is decomposed, but also the effect of cooling the reaction product gas can be obtained. In the present embodiment, hydrogen chloride generated by the reaction of the above formula (1) is taken out and supplied directly to the hydrogen chloride gas injection nozzle 113 to be used as hydrogen chloride gas.
  • the reaction product gas generated by the above formula (1) is cooled by the condenser 300 described later from the cooling tower gas component extraction pipe 109 together with the generated trichlorosilane, unreacted tetrachlorosilane, hydrogen, etc. It is separated into chlorosilanes having a high boiling point and hydrogen chloride and hydrogen having a low boiling point. Since the hydrogen chloride obtained at this time is cooled to at least normal temperature or less in the condenser, it can be supplied to the hydrogen chloride gas injection nozzle 113 without further cooling.
  • a method for producing trichlorosilane using the above-described trichlorosilane cooling tower will be described with reference to FIG.
  • a raw material gas in which gasified tetrachlorosilane and hydrogen are mixed is supplied to the bottom of the reaction furnace 201 through a raw material gas supply pipe 200.
  • the reaction furnace 201 is made of graphite, and is heated by a heater 202 provided around it, so that the inside of the reaction furnace 201 can be maintained in a state exceeding 700 ° C. and 1400 ° C. or less. If the reaction temperature is 700 ° C. or higher, the equilibrium of the above formula (1) is sufficiently tilted to the right, and if it is 1400 ° C. or lower, it is preferable because the phenomenon that metal silicon precipitates and leads to blockage of the apparatus can be suppressed.
  • the reaction product gas that has been heated in the reaction furnace 201 and has reached the thermal equilibrium state shown in the above formula (1) moves to the upper side of the reaction furnace 201 and maintains a temperature of 700 ° C. or higher in the reaction gas extraction pipe.
  • 203 is introduced into the trichlorosilane cooling tower 100.
  • the reactor gas extraction pipe 203 passes through the side wall of the trichlorosilane cooling tower 100 and the side wall of the quench pipe 106 and reaches the inside of the quench pipe 106.
  • a coolant is sprayed from the primary spray nozzle 102 connected to the primary coolant supply pipe 104 to the reaction product gas introduced into the quenching pipe 106, and instantaneously reaches a range of 70 to 600 ° C. where the equilibrium is frozen. Cool rapidly.
  • the reaction product gas and the liquid droplets in the form of fine droplets are mixed in the narrow quenching tube 106 so that they are more reliably brought into contact with each other by utilizing the latent heat of vaporization when the cooling liquid evaporates. Heat can be taken from the produced gas instantly and efficiently.
  • the equilibrium state between the substances in the reaction product gas is frozen.
  • the reaction product gas primarily cooled in the quench pipe 106 is pushed out from the discharge opening 112 at the bottom of the quench pipe 106.
  • hydrogen chloride gas is injected from the hydrogen chloride gas injection nozzle 113 connected to the hydrogen chloride gas supply pipe 114, and the high boiling point polymer contained in the reaction product gas is decomposed.
  • the reaction product gas rises in the trichlorosilane cooling tower 100 together with the hydrogen chloride gas, and passes through the filling member 107.
  • the coolant is further sprayed from the secondary spray nozzle 103 connected to the secondary coolant supply pipe 105 to condense the high-boiling point polymer remaining in the reaction product gas, and the temperature of the reaction product gas is set to 30. Gently cool to ⁇ 60 ° C.
  • the gas component that is still in a gaseous state even after cooling to the range of 30 to 60 ° C. is extracted from the cooling tower gas component extraction pipe 109 and cooled by the condenser 300, where a large amount of chlorosilane in the gas is obtained.
  • the portion is condensed and collected in the storage tank 301.
  • the chlorosilane collected in the storage tank 301 is further sent to a distillation tower (not shown) and separated into trichlorosilane and unreacted tetrachlorosilane.
  • the hydrogen chloride taken out from the condenser 300 as an uncondensed portion remains in the form of a mixture with other low-boiling substances such as hydrogen, or after isolation and purification, the hydrogen chloride is passed through the hydrogen chloride gas supply pipe 114 as hydrogen chloride gas. And supplied to the hydrogen chloride gas injection nozzle 113.
  • a condensed liquid component such as a high boiling point polymer that condenses in the temperature range of 30 to 60 ° C. flows down to the bottom of the trichlorosilane cooling tower 100 together with the cooling liquid, and is extracted from the cooling tower liquid component extraction pipe 110. It is.
  • the cooling liquid used for cooling and the condensate condensed by cooling are collected in the circulating liquid tank 400 via the cooling tower liquid component extraction pipe 110. Further, a preparation liquid composed of tetrachlorosilane and / or trichlorosilane is supplied to the circulating liquid tank 400 through the preparation liquid supply pipe 401 in order to keep the concentration of tetrachlorosilane in the cooling liquid constant.
  • the cooling liquid prepared in the circulating liquid tank 400 is extracted by the pump 402, cooled by the heat exchanger 403, and supplied again to the trichlorosilane cooling tower 100 through the primary cooling liquid supply pipe 104 and the secondary cooling liquid supply pipe 105.
  • the hydrogen chloride gas is jetted upward from the bottom of the quench pipe, but if the hydrogen chloride gas can be brought into contact with the reaction product gas after the primary cooling, the recovery rate of trichlorosilane Since the amount of the high-boiling point polymer contained in the reaction product gas after cooling can be reduced without lowering the temperature, the position and direction of injecting the hydrogen chloride gas can be changed as appropriate. Further, the reaction product gas and hydrogen chloride gas may be brought into contact with the reaction product gas extracted from the trichlorosilane cooling tower.
  • Examples 1 and 2 In both Examples 1 and 2, the apparatus shown in FIG. 1 was used. In Examples 1 and 2, the primary spray nozzle 102 and the secondary spray nozzle 103 capable of spraying the coolant with different average droplet particle sizes were used.
  • the reaction furnace 201 has an inner diameter of 50 mm and a length of 800 mm, and is heated by the heater 202. The reaction furnace 201 was heated so that the central portion of the reaction furnace 201 was 1300 ° C.
  • the metal container 101 was provided with a quenching tube 106 having an inner diameter of 140 mm and a length of 1300 mm, and an inner diameter of 35 mm and a length of 420 mm and having a bottom opened.
  • a raw material gas composed of tetrachlorosilane and hydrogen previously heated to 600 ° C. is continuously supplied to the reaction furnace 201 through the raw material gas supply pipe 200 at a flow rate of 27 mol / hour, and the gas reacted in the reaction furnace 201 is further supplied to the reaction furnace.
  • the gas was supplied to the quenching pipe 106 installed inside the metal container 101 through the gas extraction pipe 203.
  • the raw material tetrachlorosilane was 33 mol% with respect to the total of tetrachlorosilane and hydrogen.
  • the heat exchanger 403 is cooled with cooling water at 20 ° C. 402 was driven, and the coolant in the circulating fluid tank 400 was sprayed continuously into the quench pipe 106 and the metal container 101 through the primary spray nozzle 102 and the secondary spray nozzle 103, respectively.
  • the coolant supplied through the primary spray nozzle 102 has a spray amount of 0.1 l / min and a spray pressure of 0.15 MPa, and passes through the secondary spray nozzle 103.
  • the supplied coolant was sprayed with a spray amount of 0.6 l / min and a spray pressure of 0.15 MPa.
  • the temperature of the cooling liquid was kept at 30 ° C. by passing through the heat exchanger 403.
  • the coolant extracted from the bottom of the metal vessel 101 was collected in the circulating fluid tank 400 and used continuously. If necessary, the cooling liquid was continuously supplemented with tetrachlorosilane through the preparation liquid supply pipe 401 to keep the tetrachlorosilane concentration constant.
  • the gas component taken out from the top of the trichlorosilane cooling tower 100 is divided into a condensate containing chlorosilanes and an uncondensed gas component containing hydrogen chloride and hydrogen in the condenser 300, and the non-condensed gas component is supplied with hydrogen chloride gas. It was supplied to the hydrogen chloride gas injection nozzle 113 through the pipe 114 and injected as hydrogen chloride gas into the trichlorosilane cooling tower 100 under the conditions of an injection amount of 20 l / min and an injection pressure of 0.1 MPa. The temperature of hydrogen chloride gas at the time of injection was 20 ° C. On the other hand, the condensate containing chlorosilanes was temporarily stored in the storage tank 301 and then led to a distillation column (not shown), where trichlorosilane was separated and recovered.
  • Comparative Example 1 In Comparative Example 1, the same apparatus as in Example 1 was used except that hydrogen chloride gas was not injected into the trichlorosilane cooling tower 100.
  • Comparative example 2 In Comparative Example 2, the same apparatus as in Example 2 was used except that hydrogen chloride gas was not injected into the trichlorosilane cooling tower 100.
  • Comparative Example 3 is the same as Example 1 except that an injection nozzle similar to the hydrogen chloride gas injection nozzle 113 is installed instead of the primary spray nozzle 102, and a hydrogen chloride gas supply pipe 114 is branched and connected thereto. A device was used. As a result, in Comparative Example 3, primary cooling of the reaction product gas in the quench pipe 106 was performed by mixing with hydrogen chloride gas.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Silicon Compounds (AREA)

Abstract

L'invention porte sur une tour de refroidissement de trichlorosilane qui permet de réduire la quantité de polymère à point d'ébullition élevé contenu dans un produit de réaction gazeux après refroidissement, sans réduire le taux de récupération de trichlorosilane. La tour présente un moyen de pulvérisation qui pulvérise un fluide de refroidissement dans le produit de réaction gazeux, qui contient du trichlorosilane obtenu par réaction d'une matière de départ gazeuse qui contient du tétrachlorosilane et de l'hydrogène à une température se situant dans la plage de 700 à 1 400°C, et refroidit le gaz à une plage de températures de 70 à 600°C, et un moyen d'injection pour amener le chlorure d'hydrogène gazeux en contact avec le produit de réaction gazeux après refroidissement.
PCT/JP2009/057208 2009-04-08 2009-04-08 Tour de refroidissement de trichlorosilane et procédé de fabrication de trichlorosilane l'utilisant WO2010116500A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
PCT/JP2009/057208 WO2010116500A1 (fr) 2009-04-08 2009-04-08 Tour de refroidissement de trichlorosilane et procédé de fabrication de trichlorosilane l'utilisant
JP2011508138A JPWO2010116500A1 (ja) 2009-04-08 2009-04-08 トリクロロシラン冷却塔およびそれを用いたトリクロロシラン製造方法
TW099102352A TW201036915A (en) 2009-04-08 2010-01-28 Cooling tower of trichlorosilane and producing method of trichlorosilane using the same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2009/057208 WO2010116500A1 (fr) 2009-04-08 2009-04-08 Tour de refroidissement de trichlorosilane et procédé de fabrication de trichlorosilane l'utilisant

Publications (1)

Publication Number Publication Date
WO2010116500A1 true WO2010116500A1 (fr) 2010-10-14

Family

ID=42935809

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2009/057208 WO2010116500A1 (fr) 2009-04-08 2009-04-08 Tour de refroidissement de trichlorosilane et procédé de fabrication de trichlorosilane l'utilisant

Country Status (3)

Country Link
JP (1) JPWO2010116500A1 (fr)
TW (1) TW201036915A (fr)
WO (1) WO2010116500A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018203579A (ja) * 2017-06-07 2018-12-27 三菱マテリアル株式会社 クロロシラン類の回収方法及びクロロシラン類回収装置

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102794070B (zh) * 2012-07-25 2014-12-10 新疆大全新能源有限公司 一种三氯氢硅合成气的处理方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS52133022A (en) * 1976-04-30 1977-11-08 Mitsubishi Metal Corp Production of high purity silicon
JPS5673617A (en) * 1979-11-17 1981-06-18 Osaka Titanium Seizo Kk Manufacture of trichlorosilane
JPS5738524B2 (fr) * 1972-02-26 1982-08-16
WO2008056550A1 (fr) * 2006-11-07 2008-05-15 Mitsubishi Materials Corporation Procédé de fabrication de trichlorosilane et appareil de production de trichlorosilane
JP2008156209A (ja) * 2006-11-30 2008-07-10 Mitsubishi Materials Corp トリクロロシランの製造方法およびトリクロロシランの製造装置
JP2009007240A (ja) * 2007-05-25 2009-01-15 Mitsubishi Materials Corp トリクロロシランの製造方法と製造装置および多結晶シリコンの製造方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5738524B2 (fr) * 1972-02-26 1982-08-16
JPS52133022A (en) * 1976-04-30 1977-11-08 Mitsubishi Metal Corp Production of high purity silicon
JPS5673617A (en) * 1979-11-17 1981-06-18 Osaka Titanium Seizo Kk Manufacture of trichlorosilane
WO2008056550A1 (fr) * 2006-11-07 2008-05-15 Mitsubishi Materials Corporation Procédé de fabrication de trichlorosilane et appareil de production de trichlorosilane
JP2008156209A (ja) * 2006-11-30 2008-07-10 Mitsubishi Materials Corp トリクロロシランの製造方法およびトリクロロシランの製造装置
JP2009007240A (ja) * 2007-05-25 2009-01-15 Mitsubishi Materials Corp トリクロロシランの製造方法と製造装置および多結晶シリコンの製造方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018203579A (ja) * 2017-06-07 2018-12-27 三菱マテリアル株式会社 クロロシラン類の回収方法及びクロロシラン類回収装置

Also Published As

Publication number Publication date
JPWO2010116500A1 (ja) 2012-10-11
TW201036915A (en) 2010-10-16

Similar Documents

Publication Publication Date Title
KR101602006B1 (ko) 헥사클로로디실란의 회수 방법 및 그 방법을 위한 플랜트
US8568682B2 (en) Apparatus and method for the condensed phase production of trisilylamine
JP5397580B2 (ja) トリクロロシランの製造方法と製造装置および多結晶シリコンの製造方法
CN101511732B (zh) 甲硅烷的连续式制造方法
KR101292545B1 (ko) 트리클로로실란의 정제 방법 및 정제 장치
JP5633160B2 (ja) トリクロロシランの製造装置
JP5329641B2 (ja) クロロシラン回収装置およびそれを用いたクロロシラン回収方法
JP5374576B2 (ja) トリクロロシラン冷却塔およびそれを用いたトリクロロシラン製造方法
WO2010116500A1 (fr) Tour de refroidissement de trichlorosilane et procédé de fabrication de trichlorosilane l'utilisant
KR20160034908A (ko) 이소시아네이트의 제조 방법
CN107074562B (zh) 五氯乙硅烷的制造方法以及采用该方法制造的五氯乙硅烷
JP6391389B2 (ja) オクタクロロトリシランの製造方法並びに該方法により製造されるオクタクロロトリシラン
TW201210940A (en) Process for separating monosilane from chlorosilanes-rich mixture
JP6391390B2 (ja) ヘキサクロロジシランの製造方法
JP6283482B2 (ja) トリクロロシラン製造方法
EP3536682A1 (fr) Méthode de production de n-vinylformamide
CN117339486A (zh) 固定床制备及提纯硅烷的节能型装置及方法

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: 09843010

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 2011508138

Country of ref document: JP

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 09843010

Country of ref document: EP

Kind code of ref document: A1