WO2012013123A1 - Procédé et système pour la préparation de silane à partir de trichlorosilane - Google Patents

Procédé et système pour la préparation de silane à partir de trichlorosilane Download PDF

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Publication number
WO2012013123A1
WO2012013123A1 PCT/CN2011/077336 CN2011077336W WO2012013123A1 WO 2012013123 A1 WO2012013123 A1 WO 2012013123A1 CN 2011077336 W CN2011077336 W CN 2011077336W WO 2012013123 A1 WO2012013123 A1 WO 2012013123A1
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catalyst bed
anion exchange
product mixture
dichlorosilane
hydrogen
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PCT/CN2011/077336
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English (en)
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Xianbo Ding
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BYD Co Ltd
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BYD Co Ltd
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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
    • C01B33/04—Hydrides of silicon
    • C01B33/043—Monosilane

Definitions

  • the present disclosure relates to a process of silicon purification, especially to a process and a system for preparing silane by the reduction of trichlorosilane.
  • Silane is widely used as a key raw material in various fields, such as electronics, semiconductors, and photovoltaic industry.
  • UCC Silane Process Union Carbide Corporation Silane Process
  • trichlorosilane is subjected to disproportionation in the presence of a catalyst to form dichlorosilane.
  • dichlorosilane is subjected to disproportionation in the presence of a catalyst to form silane.
  • Two reactions regarding the process are as follows:
  • the two reactions to form silane from trichlorosilane are both reversible disproportionation reactions and both have low conversion rate.
  • modified catalyst available from Mitsui Chemicals may result in a one-time conversion rate of from 8% to 10%.
  • various new and modified catalysts have been disclosed in many patent documents.
  • modified catalysts may result in the highest one-time conversion rate of about 12%.
  • modified catalysts are limited to experimental use for its instability, absorption to the final product silane, pollution, etc.
  • the present disclosure is directed to solve at least one of the problems existing in the prior art. Accordingly, a process for preparing silane with high conversion rate is provided. Further, a system for preparing silane from trichlorosilane is also provided.
  • a process for preparing silane from trichlorosilane comprising: reacting trichlorosilane with hydrogen in a first catalyst bed maintained at a temperature of from about 20 °C to about 100 °C to form a first product mixture comprising a dichlorosilane, and the first catalyst bed comprising a first anion exchange resin; separating the dichlorosilane from the first product mixture in a first distillation column; delivering the separated dichlorosilane from the first distillation column to a second catalyst bed maintained at a temperature of from about 20 °C to about 80 °C for a reaction with hydrogen to form a second product mixture comprising a silane, and the second catalyst bed comprising a second anion exchange resin; and separating the silane from the second product mixture in a second distillation column.
  • a system for preparing silane from trichlorosilane comprising: a first catalyst bed configured to allow reacting trichlorosilane with hydrogen at a temperature of from about 20 °C to about 100 °C to form a first product mixture comprising a dichlorosilane, wherein the first catalyst bed comprises a first anion exchange resin; a first distillation column connected to the first catalyst bed and configured to receive the first product mixture and separate the dichlorosilane from the first product mixture; a second catalyst bed connected to the first distillation column and configured to receive the seperated dichlorosilane and allow the separated dichlorosilane to react with hydrogen at a temperature of from about 20 °C to about 80 °C to form a second product mixture comprising a silane, wherein the second catalyst bed comprises a second anion exchange resin; and a second distillation column connected to the second catalyst bed and configured to receive the second product mixture and separate the silane from the second product mixture.
  • a highest conversion rate may be up to 18% or 20%. Further, the amount of the byproduct silicon tetrachloride is significantly reduced, which may greatly reduce energy consumption of the whole process. During the whole reactions of the process, the utilization rate of silicon is very high.
  • Fig. 1 is a partial flow chart of a process for preparing silane from trichlorosilane according to an embodiment of the present disclosure
  • Fig. 2 illustrates a system for preparing silane from trichlorosilane according to an embodiment of the present disclosure.
  • a process for preparing silane from trichlorosilane comprises: reacting trichlorosilane with hydrogen in a first catalyst bed maintained at a temperature of from about 20 °C to about 100 °C to form a first product mixture comprising a dichlorosilane, and the first catalyst bed comprising a first anion exchange resin; separating dichlorosilane from the first product mixture in a first distillation column; delivering the separated dichlorosilane from the first distillation column to a second catalyst bed maintained at a temperature of from about 20 °C to about 80 °C for reaction with hydrogen to form a second product mixture comprising silane, and the second catalyst bed comprising a second anion exchange resin; and separating silane from the second product mixture in a second distillation column.
  • the reactions may be carried out under anhydrous and anaerobic conditions.
  • moisture and oxygen are removed from reaction containers prior to the reactions.
  • the process further comprises purging the first and second catalyst beds with nitrogen for about 10 minutes to about 60 minutes and vacuumizing the first and second catalyst beds to reach a pressure below 100Pa prior to the reaction.
  • the process further comprises purging the first and second catalyst beds with nitrogen for about 10 minutes to about 60 minutes and vacuumizing the first and second catalyst beds to reach a pressure below 10Pa prior to the reaction.
  • the purging and vacuumizing steps may be performed five to ten times.
  • the trichlorosilane and hydrogen may be commercially available, or may be prepared by any technique known to those skilled in the art.
  • the trichlorosilane may have a purity of above 99.99 wt%
  • the hydrogen may have a purity of 99.999 wt% so as to form silane with high purity.
  • the molar ratio of the trichlorosilane to the hydrogen in the first catalyst bed is about 4: 1 to about 1 :6. In an alternative embodiment, the molar ratio of the trichlorosilane to the hydrogen in the first catalyst bed is about 2: 1 to about 1 :4 to obtain improved conversion rate.
  • the first catalyst bed may be maintained at a temperature of from about 20 °C to about 100 °C, particularly from about 60 °C to about 100 °C.
  • the trichlorosilane and hydrogen may be dehydrated prior to the reaction in the first and second catalyst beds. In a further embodiment, the trichlorosilane and hydrogen may be dehydrated in a dehydration column.
  • the trichlorosilane and hydrogen are passed from the bottom to the top of the first catalyst bed.
  • trichlorosilane and hydrogen When passing through the first catalyst bed, trichlorosilane and hydrogen will react with the first anion exchange resin, which may promote the reaction for converting trichlorosilane and hydrogen into dichlorosilane and hydrogen chloride.
  • the reaction of trichlorosilane and hydrogen in the first catalyst bed may form dichlorosilane and hydrogen chloride.
  • the reactions in the first catalyst bed are as follows:
  • the first anion exchange resin may be any one known to those skilled in the art. Catalytic active groups in the first anion exchange resin may react with chlorosilane (such as trichlorosilane), so that the intermediate product may be changed, and the activation energy of the reaction may be reduced, thus promoting the reaction of chlorosilane with hydrogen.
  • the first anion exchange resin may be a macroporous anion exchange resin, so as to facilitate chlorosilane and hydrogen to pass from the bottom to the top of the first catalyst bed without generating large pressure drop.
  • the first anion exchange resin may comprise tertiary ammonium salt group and/or quaternary ammonium salt group as the catalytic active groups.
  • the first anion exchange resin may have a particle size of about 0.2 millimeters to about 1 .0 millimeter, particularly 0.6 millimeters. In one embodiment, the first anion exchange resin may have a filling height of about 400 millimeters to about 1 ,000 millimeters.
  • trichlorosilane may react with hydrogen in the presence of the first anion exchange resin for about 2 seconds to about 5 seconds.
  • a pressure in the first catalyst bed may be maintained at about 1 bar to 12 bar during the reaction, particularly 4 bar to 10 bar.
  • the first product mixture may comprise dichlorosilane and hydrogen chloride formed by the main reaction, unreacted trichlorosilane and hydrogen, and silicon tetrachloride and other materials formed by the side reactions.
  • the first product mixture may be delivered into the first distillation column to separate the dichlorosilane from the first product mixture. Remaining fractions of the first product mixture may be recycled.
  • the process further comprises purging the second catalyst bed with nitrogen for about 10 minutes to about 60 minutes and vacuumizing the second catalyst bed to reach a pressure below 100Pa prior to the reaction. In a further alternative embodiment, the process further comprises purging the second catalyst bed with nitrogen for about 10 minutes to about 60 minutes and vacuumizing the second catalyst bed to reach a pressure below 10Pa prior to the reaction. In an alternative embodiment, the purging and vacuumizing steps may be performed five to ten times.
  • the molar ratio of the dichlorosilane to the hydrogen in the second catalyst bed is about 3: 1 to about 1 :5. In a further embodiment, the molar ratio of the dichlorosilane to the hydrogen in the second catalyst bed is about 1 :1 to about 1 :3 to obtain an improved conversion rate.
  • the second catalyst bed may be maintained at a temperature of from about 20 °C to about 80 °C. In a further embodiment, the second catalyst bed may be maintained at a temperature of from about 40 °C to about 80 °C.
  • the dichlorosilane separated in the first distillation column and hydrogen may be dehydrated prior to the reaction in the second catalyst bed. In a further embodiment, the dichlorosilane and hydrogen may be dehydrated in a dehydration column.
  • the dichlorosilane and hydrogen are passed from the bottom to the top of the second catalyst bed.
  • the reactions in the second catalyst bed may be as follows.
  • the second anion exchange resin may be any one known to those skilled in the art, and in one embodiment of the present disclosure, the first and second anion exchange resin may be the same.
  • Catalytic active groups in the second anion exchange resin may react with chlorosilane (such as dichlorosilane), so that the intermediate product may be changed, and the activation energy of the reaction may be reduced, thus promoting the reaction of chlorosilane with hydrogen.
  • the second anion exchange resin may be a macroporous anion exchange resin, so as to facilitate chlorosilane and hydrogen to pass from the bottom to the top of the second catalyst bed without generating large pressure drop.
  • the second anion exchange resin may comprise tertiary ammonium salt group and/or quaternary ammonium salt group as the catalytic active groups.
  • the second anion exchange resin may have a particle size of about 0.2 millimeters to about 1 .0 millimeter, particularly 0.6 millimeters. In one embodiment, the second anion exchange resin may have a filling height of about 400 millimeters to about 1 ,000 millimeters.
  • the first and second catalyst beds may have identical reaction principle and aim.
  • the first and second anion exchange resins may be identical or different, with identical or different particle sizes or filling heights.
  • dichlorosilane may react with hydrogen in the presence of the second anion exchange resin for about 2 seconds to about 5 seconds.
  • a pressure in the second catalyst bed may be maintained at about 1 bar to 10 bar during the reaction, particularly 4 bar to 8 bar, and further particularly 2 bar to 6 bar.
  • the second product mixture comprises silane and hydrogen chloride formed by the main reaction, unreacted dichlorosilane and hydrogen, and trichlorosilane and other materials formed by the side reactions.
  • the second product mixture may be delivered into the second distillation column to separate the silane from the second product mixture. Remaining fractions of the second product mixture may be recycled.
  • the first and second catalyst beds may be any one known in the art, which can be self-made or commercially available, provided that reactions therein are achieved sufficiently.
  • the first and second catalyst beds may be a single-stage bed or a two-stage bed, preferably a single-stage bed; and the first and catalyst beds may be made from ceramic or metal, with metal as preferable.
  • the catalysts used in the first and second catalyst beds may be independently any one known in the art, which can act the catalyst for the above recited reactions.
  • the catalysts used in the first and second catalyst beds may be amino-functionalized polystyrenes, amino-functionalized inorganic or organopolysiloxane catalysts.
  • a system for preparing silane from trichlorosilane comprises: a first catalyst bed 100, a first distillation column 200, a second catalyst bed 300, and and a second distillation column 400.
  • the first catalyst bed 100 comprises a first anion exchange resin
  • the first catalyst bed 100 is configured to allow reacting trichlorosilane with hydrogen at a temperature of from about 20 °C to about 100 °C to form a first product mixture comprising a dichlorosilane.
  • the first distillation column 200 is connected to the first catalyst bed 100 and is configured to receive the first product mixture and separate the dichlorosilane from the first product mixture.
  • the second catalyst bed comprises a second anion exchange resin connected to the first distillation column 200 and is configured to receive the seperated dichlorosilane and allow the separated dichlorosilane to react with hydrogen at a temperature of from about 20 °C to about 80 °C to form a second product mixture comprising a silane.
  • the second distillation column 400 is connected to the second catalyst bed 300 and is configured to receive the second product mixture and separate the silane from the second product mixture.
  • the first and second anion exchange resins each independently have a particle size of about 0.2 millimeters to about 1 .0 millimeter.
  • the first and second anion exchange resins each independently have a filling height of about 400 millimeters to about 1 ,000 millimeters. In some embodiments, the first and second anion exchange resins are each independently macroporous anion exchange resins containing tertiary ammonium salt group and/or quaternary ammonium salt group.
  • Fig. 1 shows a partial flow chart of a process for preparing silane from trichlorosilane according to an embodiment of the present disclosure.
  • a dehydration column A1 As shown in Fig. 1 , a dehydration column A1 , a catalyst bed A2, a chromatograph A3, valves K1 -9 are included in the flow chart.
  • Line V represents connection to a vacuum pump and line D represents connection to a distillation column.
  • valves K2, K3, and K7-9 are closed, and remaining valves are opened.
  • nitrogen is applied to purge the reaction system for about 10 minutes to about 60 minutes.
  • valves K8 and K9 are opened, and finally the reaction system is vacuumized to reach a pressure of about 1 Pa to about 100 Pa.
  • the above mentioned steps are performed about five to about ten times to remove the moisture and oxygen in the reaction system.
  • valves K1 , K8 and K9 are closed and valves K2, K3 and K5 are opened.
  • Trichlorosilane and hydrogen are injected into the dehydration column A1 , and then delivered to the catalyst bed A2 for reaction with hydrogen in the catalyst bed A2 to obtain a first product mixture comprising dichlorosilane.
  • the first product mixture is delivered to the distillation column through line D.
  • Valve K7 is opened when the reaction is stable. A part of the first product mixture is introduced into the chromatograph A3, and its composition is analyzed.
  • conversion rates of the reaction of trichlorosilane with hydrogen and the reaction of dichlorosilane with hydrogen may be significantly increased in the presence of the first and second anion exchange resins. It has been found by the inventors that the conventional UCC silane process by means of disproportionation reaction, which may have a very low conversion rate when the reaction comes to equilibrium. According to an embodiment of the present disclosure, detailed reactions of trichlorosilane in the presence of hydrogen are as follows:
  • EMBODIMENTS 1 to 5 describe the reaction between trichlorosilane and hydrogen
  • EMBODIMENTS 6 to 10 describe the reaction between dichlorosilane and hydrogen.
  • the reaction system was purged with nitrogen for 40 minutes, and then the reaction system was vacuumized to reach a pressure of about 90 Pa.
  • the purging and vacuuming steps were performed 10 times.
  • Trichlorosilane and hydrogen with a molar ratio of 1 :2 were mixed and delivered to the first catalyst bed via an air inlet on the bottom of the first catalyst bed with a flow rate of about 1 .5 L/min.
  • the first catalyst bed was filled with the first anion exchange resin with a filling height of 800 mm, and the first anion exchange resin was a macroporous anion exchange resin comprising tertiary ammonium salt group (Amberlyst A-21 ) and had an average particle size of 0.59 mm.
  • Trichlorosilane was reacted with hydrogen in the presence of the first anion exchange resin in the first catalyst bed to form a first product mixture.
  • the first catalyst bed is maintained at a temperature of 80 °C and a pressure of 10 bar.
  • the first product mixture was withdrawn from the top of the first catalyst bed and delivered to the first distillation column.
  • Dichlorosilane was separated from the first product mixture in the first distillation column, and remaining fractions were separated and recycled.
  • EMBODIMENT 2 is substantially the same as EMBODIMENT 1 except that: trichlorosilane and hydrogen with a molar ratio of 4: 1 were mixed.
  • EMBODIMENT 3 is substantially the same as EMBODIMENT 1 except that: trichlorosilane and hydrogen with a molar ratio of 1 :6 were mixed.
  • EMBODIMENT 4 is substantially the same as EMBODIMENT 1 except that: the first catalyst bed was filled with the first anion exchange resin with a filling height of 400 mm.
  • EMBODIMENT 5 is substantially the same as EMBODIMENT 1 except that: the first catalyst bed was filled with the first anion exchange resin with a filling height of 1000 mm.
  • the dichlorosilane from EMBODIMENTS 1 -5 and hydrogen with a molar ratio of 1 :3 were mixed and delivered to the second catalyst bed via an air inlet on the bottom of the second catalyst bed with a flow rate of about 1.5 L/min.
  • the second catalyst bed was filled with the second anion exchange resin with a filling height of 800 mm, and the second anion exchange resin was a macroporous anion exchange resin comprising quaternary ammonium salt group (Dowex MWA-1 ) and had an average particle size of 0.68 mm.
  • Dichlorosilane was reacted with hydrogen in the presence of the second anion exchange resin in the second catalyst bed to form a second product mixture.
  • the second catalyst bed is maintained at a temperature of 80 °C and a pressure of 6 bar.
  • the second product mixture was withdrawn from the top of the second catalyst bed and delivered to the second distillation column. Silane was separated from the second product mixture, and remaining fractions were separated and recycled.
  • EMBODIMENT 7 is substantially the same as EMBODIMENT 6 except that: dichlorosilane and hydrogen with a molar ratio of 3: 1 were mixed.
  • EMBODIMENT 8 is substantially the same as EMBODIMENT 6 except that: dichlorosilane and hydrogen with a molar ratio of 1 :5 were mixed.
  • EMBODIMENT 9 is substantially the same as EMBODIMENT 6 except that: the second catalyst bed was filled with the second anion exchange resin with a filling height of 400 mm.
  • EMBODIMENT 10 is substantially the same as EMBODIMENT 6 except that: the second catalyst bed was filled with the second anion exchange resin with a filling height of 1000 mm.
  • the reaction system was purged with nitrogen for 40 minutes, and then the reaction system was vacuumized to reach a pressure of about 90 Pa.
  • the purging and vacuuming steps were performed 10 times.
  • Trichlorosilane was delivered to the first catalyst bed via an air inlet on the bottom of the first catalyst bed with a flow rate of about 1 .5 L/min.
  • the first catalyst bed was filled with the first anion exchange resin with a filling height of 800 mm, and the first anion exchange resin was a macroporous anion exchange resin comprising tertiary ammonium salt group (Amberlyst A-21 ) and had an average particle size of 0.59 mm.
  • Trichlorosilane was reacted with hydrogen in the presence of the first anion exchange resin in the first catalyst bed to form a first product mixture.
  • the first catalyst bed is maintained at a temperature of 80 °C and a pressure of 5 bar.
  • the first product mixture was withdrawn from the top of the first catalyst bed and delivered to the first distillation column.
  • Dichlorosilane was separated from the first product mixture in the first distillation column, and remaining fractions were separated and recycled.
  • the dichlorosilane from COMPARATIVE EMBODIMENT 1 was delivered to the second catalyst bed via an air inlet on the bottom of the second catalyst bed with a flow rate of about 1 .5 L/min.
  • the second catalyst bed was filled with the second anion exchange resin with a filling height of 800 mm, and the second anion exchange resin was a macroporous anion exchange resin comprising quaternary ammonium salt group (Dowex MWA-1 ) and had an average particle size of 0.68 mm.
  • Dichlorosilane was reacted with hydrogen in the presence of the second anion exchange resin in the second catalyst bed to form a second product mixture.
  • the second catalyst bed is maintained at a temperature of 80 °C and a pressure of 5 bar.
  • the second product mixture was withdrawn from the top of the second catalyst bed and delivered to the second distillation column. Silane was separated from the second product mixture, and remaining fractions were separated and recycled.
  • the first and second product mixtures were collected and tested in the chromatograph (GC-2014). Testing results were shown in Table 1 and Table 2. Some byproducts formed by side reactions were not recorded in Table 1 and Table 2. The conversion rate ( ⁇ ) was calculated by the following formula:

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

L'invention concerne un procédé pour la préparation de silane à partir de trichlorosilane. Ce procédé comprend : la réaction de trichlorosilane avec de l'hydrogène dans un premier lit de catalyseur maintenu à une température d'environ 20°C à environ 100°C pour former un premier mélange de produits comprenant un dichlorosilane, le premier lit de catalyseur comprenant une première résine échangeuse d'anions ; la séparation du dichlorosilane du premier mélange de produits dans une première colonne de distillation ; le transfert du dichlorosilane séparé de la première colonne de distillation dans un deuxième lit de catalyseur maintenu à une température d'environ 20°C à environ 80°C pour une réaction avec l'hydrogène pour former un deuxième mélange de produits comprenant un silane, le deuxième lit de catalyseur comprenant une deuxième résine échangeuse d'anions ; et la séparation du silane du deuxième mélange de produits dans une deuxième colonne de distillation. En outre, un système pour la préparation de silane à partir de trichlorosilane est également décrit.
PCT/CN2011/077336 2010-07-29 2011-07-19 Procédé et système pour la préparation de silane à partir de trichlorosilane Ceased WO2012013123A1 (fr)

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CN 201010244420 CN102344145B (zh) 2010-07-29 2010-07-29 一种三氯氢硅制备硅烷的方法
CN201010244420.6 2010-07-29

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Cited By (2)

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CN103253676A (zh) * 2013-05-10 2013-08-21 河北工业大学 一种三氯氢硅的制备方法
US9352971B2 (en) 2013-06-14 2016-05-31 Rec Silicon Inc Method and apparatus for production of silane and hydrohalosilanes

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CN102951646A (zh) * 2012-11-22 2013-03-06 覃攀 硅烷的生产方法
CN103112860B (zh) * 2013-02-26 2015-09-02 天津大学 改良西门子法联产制备高纯硅烷的方法
CN117619375B (zh) * 2023-11-22 2025-12-12 浙江开化合成材料有限公司 歧化制备二氯氢硅的方法及所用的钼基负载型催化剂

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US4113845B1 (fr) * 1971-06-14 1984-01-24
US3968199A (en) * 1974-02-25 1976-07-06 Union Carbide Corporation Process for making silane
JPH01226712A (ja) * 1988-03-07 1989-09-11 Koujiyundo Silicon Kk ジクロルシランの製造方法
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103253676A (zh) * 2013-05-10 2013-08-21 河北工业大学 一种三氯氢硅的制备方法
CN103253676B (zh) * 2013-05-10 2015-04-08 河北工业大学 一种三氯氢硅的制备方法
US9352971B2 (en) 2013-06-14 2016-05-31 Rec Silicon Inc Method and apparatus for production of silane and hydrohalosilanes

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