WO2017193881A1 - Method for manufacturing disilane - Google Patents

Method for manufacturing disilane Download PDF

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WO2017193881A1
WO2017193881A1 PCT/CN2017/083418 CN2017083418W WO2017193881A1 WO 2017193881 A1 WO2017193881 A1 WO 2017193881A1 CN 2017083418 W CN2017083418 W CN 2017083418W WO 2017193881 A1 WO2017193881 A1 WO 2017193881A1
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disilane
catalyst
magnesium silicide
ammonium chloride
reaction
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PCT/CN2017/083418
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French (fr)
Chinese (zh)
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黄晓东
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浙江迅鼎半导体材料科技有限公司
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Publication of WO2017193881A1 publication Critical patent/WO2017193881A1/en

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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

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  • the invention belongs to the technical field of gas production, and particularly relates to a method for producing monosilane (SiH 4 ), disilane (Si 2 H 6 ), trisilane (Si 3 H 8 ), etc., and particularly to a method for producing disilane.
  • silicon is used to isolate the conductive layers in electronic precision components. Since components, such as chips, have repeatedly pursued precision, and the specification design has become more and more fine, from micron to nanometer, the silicon isolation layer has not been formed by mechanical cutting, but must be formed by vapor phase lamination, so silanes The use of the necessary materials.
  • Disilane is a promising precursor to silicon films. Compared with monosilane, it has the advantages of high deposition rate, low temperature requirement and high film uniformity. It is one of the most attractive specialty gases in the semiconductor industry.
  • the method has high production cost due to low yield, many by-products and expensive equipment.
  • the second method is the trichlorosilane purification method (commonly known as the UCC method).
  • the process of this method firstly reacts silicon powder with hydrogen chloride (commonly known as hydrochloric acid) to form trichlorosilane (Si+3HCl ⁇ HSiCl 3 +H 2 ).
  • trichlorosilane is reacted with hydrogen to form dichlorosilane and hydrogen chloride (HSiCl 3 + H 2 ⁇ H 2 SiCl 2 + HCl) by combining hydrogen with chlorine. Further, by reacting dichlorosilane with hydrogen, hydrogen and chlorine are combined to form monochlorosilane and hydrogen chloride (H 2 SiCl 2 + H 2 ⁇ H 3 SiCl + HCl). Then, the monochlorosilane is further reacted with hydrogen, that is, hydrogen and chlorine are combined to form silicon methane and hydrogen chloride (H 3 SiCl + H 2 ⁇ SiH 4 + HCl). This method can generate silicon methane. However, products such as silane, silane, and the like cannot be produced by this method.
  • a method for producing disilane which comprises reacting magnesium silicide with ammonium chloride as a raw material, and generating disilane gas in the presence of liquid ammonia and a catalyst, the reaction temperature is -10 ° C to 50 ° C, and the reaction pressure is 0.2-1 MPa.
  • the molar ratio of magnesium silicide to ammonium chloride is 1:2-5, and the catalyst is a complex of zinc.
  • reaction pressure is 0.25 to 0.55 MPa.
  • the molar ratio of the magnesium silicide to the ammonium chloride is 1:3.
  • reaction is carried out in a 3-10 M 3 reactor, preferably a 8.4 M 3 reactor.
  • the reactor is equipped with a magnetic stirrer to prevent material leakage.
  • the catalyst is one or more of C 54 H 45 P 3 ZnX 2 , C 68 H 56 Fe 2 P 4 ZnY 2 , C 52 H 48 P 4 ZnCl 2 , C 54 H 52 P 4 ZnCl 2 Where X is F, Cl, Br or I, and Y is Br or I.
  • the disilane gas is stored in a liquid phase in a storage tank by low-temperature decompression, and the storage tank is a jacket structure, and the inside of the jacket is a -30 ° C glycol cooling medium.
  • disilane is the main product of the production process, thereby solving the problem of by-products of large-scale production of disilane, greatly improving the production efficiency of producing high-purity disilane, low energy consumption, and low production cost.
  • the embodiment of the present invention adopts the following manufacturing method: reacting magnesium silicide with ammonium chloride as a raw material, and generating disilane gas in the presence of liquid ammonia and a catalyst, the reaction temperature is -10 ° C to 50 ° C, and the reaction pressure is 0.2- 1 MPa, the molar ratio of the magnesium silicide to the ammonium chloride is 1:2-5, and the catalyst is a complex of zinc.
  • Examples 1-10 of the present invention produced disilane in a yield having industrial applicability.
  • the synthesis reaction is carried out in the presence of liquid ammonia, which means that liquid ammonia is introduced into the reaction vessel at least during the feed, while allowing it to occur partially during the reaction or All vaporization.
  • Disilane is produced in accordance with the above method.
  • the reaction temperature is -10 ° C
  • the reaction pressure is 0.2 MPa
  • the molar ratio of the magnesium silicide to the ammonium chloride is 1:2
  • the catalyst is C 54 H 52 P 4 ZnCl 2
  • the reaction is at 3 M 3
  • the reaction kettle was carried out.
  • Example 1 was repeated except that the reaction temperature was 50 ° C, the reaction pressure was 1 MPa, the molar ratio of magnesium silicide to ammonium chloride was 1:5, and the catalyst was C 54 H 45 P 3 ZnX 2 .
  • the reaction was carried out in a 10 M 3 reactor equipped with a magnetic stirrer.
  • Example 1 was repeated except that the reaction temperature was 20 ° C, the reaction pressure was 0.6 MPa, the molar ratio of magnesium silicide to ammonium chloride was 1:3.5, and the catalyst was C 52 H 48 P 4 ZnCl 2 The reaction was carried out in a 6.5 M 3 reactor equipped with a magnetic stirrer.
  • Example 1 was repeated except that the reaction pressure was 0.25 MPa, the molar ratio of magnesium silicide to ammonium chloride was 1:3, and the catalyst was C 68 H 56 Fe 2 P 4 ZnY 2 . This was carried out in a 8.4 M 3 reactor equipped with a magnetic stirrer.
  • Example 4 was repeated except that the reaction pressure was 0.55 MPa and the catalyst was a mixture of C 54 H 45 P 3 ZnX 2 and C 68 H 56 Fe 2 P 4 ZnY 2 .
  • the disilane gas is stored in a liquid phase in a storage tank by low temperature decompression, and the storage tank is a jacket structure, and the inside of the jacket is a -30 ° C glycol cooling medium.
  • Example 5 was repeated except that the reaction pressure was 0.4 MPa and the catalyst was a mixture of C 54 H 45 P 3 ZnX 2 and C 52 H 48 P 4 ZnCl 2 , and the pressure in the tank jacket was 10Pa.
  • Example 2 was repeated except that the molar ratio of magnesium silicide to ammonium chloride was 1:3, the catalyst was C 68 H 56 Fe 2 P 4 ZnY 2 , and the reaction was at 8.4 M 3
  • the kettle was placed in a kettle equipped with a magnetic stirrer.
  • the disilane gas is stored in a liquid phase in a storage tank by low temperature decompression, and the storage tank is a jacket structure, and the inside of the jacket is a -30 ° C glycol cooling medium.
  • Example 3 was repeated, except that the magnesium silicide and ammonium chloride molar ratio of 1: 3, the catalyst is C 68 H 56 Fe 2 P 4 ZnY 2 and C 52 H 48 P 4 ZnCl 2 is The mixture was reacted in a 8.4 M 3 reactor equipped with a magnetic stirrer.
  • the disilane gas is stored in a liquid phase in a storage tank by low temperature decompression, and the storage tank is a jacket structure, and the inside of the jacket is a -30 ° C glycol cooling medium.
  • the pressure inside the tank jacket is 6 Pa.
  • Example 4 was repeated except that the reaction temperature was 20 ° C and the reaction pressure was 0.6 MPa, and the catalyst was a mixture of C 54 H 45 P 3 ZnX 2 and C 52 H 48 P 4 ZnCl 2 , the disilane
  • the gas is stored in a liquid phase in a storage tank by low temperature decompression, which is a jacketed structure with a -30 ° C glycol cooling medium in the jacket.
  • Example 5 was repeated except that the reaction temperature was -10 ° C, the reaction pressure was 0.3 MPa, the molar ratio of magnesium silicide to ammonium chloride was 1:4, and the catalyst was C 54 H 52 P 4 ZnCl. 2. The reaction was carried out in a 8.4 M 3 reactor with a pressure of 2 Pa in the jacket jacket.

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

Abstract

Provided is a method for manufacturing disilane. Magnesium silicide and ammonia chloride as raw materials are reacted in the presence of liquid ammonia and a catalyst so as to generate a disilane gas, wherein the reaction temperature is -10ºC to 50ºC, the reaction pressure is 0.2-1 MPa, the mole ratio of magnesium silicide to ammonia chloride is 1 : 2-5, and the catalyst is a zinc complex. In the method, disilane is a main product of the production process; thus the problem of byproducts in the large-scale production of disilane can be solved, the production efficiency of producing high-purity disilane is greatly improved, the energy consumption is low, and the production cost is reduced.

Description

一种乙硅烷的制造方法Method for producing disilane 技术领域Technical field
本发明属于气体生产技术领域，具体涉及生产甲硅烷(SiH4)、乙硅烷(Si2H6)、丙硅烷(Si3H8)等的方法，尤其适用乙硅烷的制造方法。The invention belongs to the technical field of gas production, and particularly relates to a method for producing monosilane (SiH 4 ), disilane (Si 2 H 6 ), trisilane (Si 3 H 8 ), etc., and particularly to a method for producing disilane.
背景技术Background technique
在微电子产品制造过程，硅用以隔离电子精密组件中各导电层。由于组件，例如芯片，一再追求精密度，规格设计越来越细，从微米级进步到纳米级，所以硅隔离层已经无法用机械方法切割形成，而必须用气相层积法形成，所以硅烷类的使用形成必须之材料。In the microelectronics manufacturing process, silicon is used to isolate the conductive layers in electronic precision components. Since components, such as chips, have repeatedly pursued precision, and the specification design has become more and more fine, from micron to nanometer, the silicon isolation layer has not been formed by mechanical cutting, but must be formed by vapor phase lamination, so silanes The use of the necessary materials.
乙硅烷是一种很有前途的硅膜先体。与甲硅烷相比，它具有沉积速度快、温度要求低、膜均匀度高等优越性，是半导体工业中颇有吸引力的特种气体之一。传统的硅烷制备方法至少有两种。一种是硅镁法，或称小松法，以硅粉及镁粉为初始材料，先合成硅化镁(Si+2Mg→Mg2Si)。再以硅化镁与氯化氨依用量比例反应，在液氨的环境下，生成硅甲烷气相及六氨氯化镁固相残渣。该方法因产率低、副产品多、设备昂贵导致生产成本过高。其中，用硅化镁与氯化铵在液氨中反应的生成物绝大部份是甲硅烷，少于2％的乙硅烷只能作为副产品回收以获取极为有限的回报。第二种方法是以三氯氢硅提纯法(俗称UCC法)。此方法之制程，首先以硅粉与氯化氢(俗称盐酸)反应生成三氯氢硅(Si+3HCl→HSiCl3+H2)。再以三氯氢硅与氢气反应，藉由氢气与氯元素结合而形成二氯氢硅及氯化氢(HSiCl3+H2→H2SiCl2+HCl)。依序再以二氯氢硅与氢气反应，藉由氢气与氯元素结合而形成单氯氢硅及氯化氢，(H2SiCl2+H2→H3SiCl+HCl)。然后，单氯氢硅再与氢气反应，也就是由氢气与氯元素结合而形成硅甲烷及氯化氢(H3SiCl+H2→SiH4+HCl)。此方法可以生成硅甲烷。然而，硅乙烷、硅丙烷等的产品则无法由该方法制得。 Disilane is a promising precursor to silicon films. Compared with monosilane, it has the advantages of high deposition rate, low temperature requirement and high film uniformity. It is one of the most attractive specialty gases in the semiconductor industry. There are at least two conventional silane preparation methods. One is the silicon magnesium method, or the Komatsu method, which uses silicon powder and magnesium powder as starting materials to synthesize magnesium silicide (Si+2Mg→Mg 2 Si). Further, the magnesium silicide and the ammonium chloride are reacted in a ratio of the amount, and in the liquid ammonia environment, a silicon methane gas phase and a hexaammonium chloride solid phase residue are formed. The method has high production cost due to low yield, many by-products and expensive equipment. Among them, most of the products obtained by reacting magnesium silicide with ammonium chloride in liquid ammonia are monosilane, and less than 2% of disilane can only be recovered as a by-product to obtain a very limited return. The second method is the trichlorosilane purification method (commonly known as the UCC method). The process of this method firstly reacts silicon powder with hydrogen chloride (commonly known as hydrochloric acid) to form trichlorosilane (Si+3HCl→HSiCl 3 +H 2 ). Further, trichlorosilane is reacted with hydrogen to form dichlorosilane and hydrogen chloride (HSiCl 3 + H 2 → H 2 SiCl 2 + HCl) by combining hydrogen with chlorine. Further, by reacting dichlorosilane with hydrogen, hydrogen and chlorine are combined to form monochlorosilane and hydrogen chloride (H 2 SiCl 2 + H 2 → H 3 SiCl + HCl). Then, the monochlorosilane is further reacted with hydrogen, that is, hydrogen and chlorine are combined to form silicon methane and hydrogen chloride (H 3 SiCl + H 2 → SiH 4 + HCl). This method can generate silicon methane. However, products such as silane, silane, and the like cannot be produced by this method.
换言之，无论半导体、液晶显示屏、太阳能电池、节能玻璃等行业，已经渐渐从硅甲烷的使用转向硅乙烷，而且对于环境保护的要求已经是所有人的共识，因此，一种新颖有效满足上述需求的制造方法必须应运而生。In other words, regardless of semiconductors, liquid crystal displays, solar cells, energy-saving glass and other industries, it has gradually shifted from the use of silicon methane to silicon ethane, and the requirements for environmental protection have been the consensus of all people. Therefore, a novel effectively meets the above requirements. The manufacturing method of demand must come into being.
发明内容Summary of the invention
为了解决上述问题，本发明通过以下技术方案实现。In order to solve the above problems, the present invention is achieved by the following technical solutions.
一种乙硅烷的制造方法，以硅化镁与氯化氨为原料进行反应，在液氨及催化剂存在下生成乙硅烷气体，反应温度为-10℃至50℃，反应压力为0.2-1MPa，所述硅化镁与氯化氨的摩尔比为1:2-5，所述催化剂为锌的配合物。A method for producing disilane, which comprises reacting magnesium silicide with ammonium chloride as a raw material, and generating disilane gas in the presence of liquid ammonia and a catalyst, the reaction temperature is -10 ° C to 50 ° C, and the reaction pressure is 0.2-1 MPa. The molar ratio of magnesium silicide to ammonium chloride is 1:2-5, and the catalyst is a complex of zinc.
进一步，所述反应压力为0.25-0.55MPa。Further, the reaction pressure is 0.25 to 0.55 MPa.
进一步，所述硅化镁与氯化氨的摩尔比为1:3。Further, the molar ratio of the magnesium silicide to the ammonium chloride is 1:3.
进一步，所述反应在3-10M3的反应釜内进行，优选8.4M3的反应釜。Further, the reaction is carried out in a 3-10 M 3 reactor, preferably a 8.4 M 3 reactor.
进一步，所述反应釜配置磁力搅拌器，以防止物料泄漏。Further, the reactor is equipped with a magnetic stirrer to prevent material leakage.
进一步，所述催化剂为C54H45P3ZnX2、C68H56Fe2P4ZnY2、C52H48P4ZnCl2、C54H52P4ZnCl2中的一种或几种；其中X为F、Cl、Br或I，Y为Br或I。Further, the catalyst is one or more of C 54 H 45 P 3 ZnX 2 , C 68 H 56 Fe 2 P 4 ZnY 2 , C 52 H 48 P 4 ZnCl 2 , C 54 H 52 P 4 ZnCl 2 Where X is F, Cl, Br or I, and Y is Br or I.
进一步，所述乙硅烷气体通过低温减压在储罐中以液相进行储存，所述储罐为夹套结构，夹套内为-30℃乙二醇冷却介质。Further, the disilane gas is stored in a liquid phase in a storage tank by low-temperature decompression, and the storage tank is a jacket structure, and the inside of the jacket is a -30 ° C glycol cooling medium.
本发明的乙硅烷制造方法中，乙硅烷是生产过程的主产品，因而可解决大规模生产乙硅烷的副产品问题，大大提高生产高纯乙硅烷的生产效率，耗能低，降低生产成本。In the method for producing disilane of the present invention, disilane is the main product of the production process, thereby solving the problem of by-products of large-scale production of disilane, greatly improving the production efficiency of producing high-purity disilane, low energy consumption, and low production cost.
具体实施方式detailed description
下面结合实施例对本发明进一步详细说明。 The present invention will be further described in detail below with reference to the embodiments.
本发明的实施例采用下述制造方法：以硅化镁与氯化氨为原料进行反应，在液氨及催化剂存在下生成乙硅烷气体，反应温度为-10℃至50℃，反应压力为0.2-1MPa，所述硅化镁与氯化氨的摩尔比为1:2-5，所述催化剂为锌的配合物。本发明的实施例1-10均以具有工业实用性的产率制得了乙硅烷。The embodiment of the present invention adopts the following manufacturing method: reacting magnesium silicide with ammonium chloride as a raw material, and generating disilane gas in the presence of liquid ammonia and a catalyst, the reaction temperature is -10 ° C to 50 ° C, and the reaction pressure is 0.2- 1 MPa, the molar ratio of the magnesium silicide to the ammonium chloride is 1:2-5, and the catalyst is a complex of zinc. Each of Examples 1-10 of the present invention produced disilane in a yield having industrial applicability.
在本发明、特别是以下实施例中，合成反应在液氨的存在下进行，这一反应体系是指至少在进料时将液氨投入反应容器中，而在反应过程中允许其发生部分或全部的汽化。In the present invention, particularly in the following examples, the synthesis reaction is carried out in the presence of liquid ammonia, which means that liquid ammonia is introduced into the reaction vessel at least during the feed, while allowing it to occur partially during the reaction or All vaporization.
实施例1Example 1
依照上述方法生产乙硅烷。其中，反应温度为-10℃，反应压力为0.2MPa，所述硅化镁与氯化氨的摩尔比为1:2，所述催化剂为C54H52P4ZnCl2，所述反应在3M3的反应釜内进行。Disilane is produced in accordance with the above method. Wherein, the reaction temperature is -10 ° C, the reaction pressure is 0.2 MPa, the molar ratio of the magnesium silicide to the ammonium chloride is 1:2, the catalyst is C 54 H 52 P 4 ZnCl 2 , and the reaction is at 3 M 3 The reaction kettle was carried out.
实施例2Example 2
重复实施例1，不同之处在于，反应温度为50℃，反应压力为1MPa，所述硅化镁与氯化氨的摩尔比为1:5，所述催化剂为C54H45P3ZnX2，所述反应在10M3的反应釜内进行，所述反应釜配置磁力搅拌器。Example 1 was repeated except that the reaction temperature was 50 ° C, the reaction pressure was 1 MPa, the molar ratio of magnesium silicide to ammonium chloride was 1:5, and the catalyst was C 54 H 45 P 3 ZnX 2 . The reaction was carried out in a 10 M 3 reactor equipped with a magnetic stirrer.
实施例3Example 3
重复实施例1，不同之处在于，反应温度为20℃，反应压力为0.6MPa，所述硅化镁与氯化氨的摩尔比为1:3.5，所述催化剂为C52H48P4ZnCl2，所述反应在6.5M3的反应釜内进行，所述反应釜配置磁力搅拌器。Example 1 was repeated except that the reaction temperature was 20 ° C, the reaction pressure was 0.6 MPa, the molar ratio of magnesium silicide to ammonium chloride was 1:3.5, and the catalyst was C 52 H 48 P 4 ZnCl 2 The reaction was carried out in a 6.5 M 3 reactor equipped with a magnetic stirrer.
实施例4Example 4
重复实施例1，不同之处在于，反应压力为0.25MPa，所述硅化镁与氯化氨的摩尔比为1:3，所述催化剂为C68H56Fe2P4ZnY2，所述反应在8.4M3的反应釜内进行，所述反应釜配置磁力搅拌器。Example 1 was repeated except that the reaction pressure was 0.25 MPa, the molar ratio of magnesium silicide to ammonium chloride was 1:3, and the catalyst was C 68 H 56 Fe 2 P 4 ZnY 2 . This was carried out in a 8.4 M 3 reactor equipped with a magnetic stirrer.
实施例5Example 5
重复实施例4，不同之处在于，反应压力为0.55MPa，所述催化剂为 C54H45P3ZnX2与C68H56Fe2P4ZnY2的混合物。所述乙硅烷气体通过低温减压在储罐中以液相进行储存，所述储罐为夹套结构，夹套内为-30℃乙二醇冷却介质。Example 4 was repeated except that the reaction pressure was 0.55 MPa and the catalyst was a mixture of C 54 H 45 P 3 ZnX 2 and C 68 H 56 Fe 2 P 4 ZnY 2 . The disilane gas is stored in a liquid phase in a storage tank by low temperature decompression, and the storage tank is a jacket structure, and the inside of the jacket is a -30 ° C glycol cooling medium.
实施例6Example 6
重复实施例5，不同之处在于，反应压力为0.4MPa，所述催化剂为C54H45P3ZnX2与C52H48P4ZnCl2的混合物，所述储罐夹套内的压力为10Pa。Example 5 was repeated except that the reaction pressure was 0.4 MPa and the catalyst was a mixture of C 54 H 45 P 3 ZnX 2 and C 52 H 48 P 4 ZnCl 2 , and the pressure in the tank jacket was 10Pa.
实施例7Example 7
重复实施例2，不同之处在于，所述硅化镁与氯化氨的摩尔比为1:3，所述催化剂为C68H56Fe2P4ZnY2，所述反应在8.4M3的反应釜内进行，所述反应釜配置磁力搅拌器。所述乙硅烷气体通过低温减压在储罐中以液相进行储存，所述储罐为夹套结构，夹套内为-30℃乙二醇冷却介质。Example 2 was repeated except that the molar ratio of magnesium silicide to ammonium chloride was 1:3, the catalyst was C 68 H 56 Fe 2 P 4 ZnY 2 , and the reaction was at 8.4 M 3 The kettle was placed in a kettle equipped with a magnetic stirrer. The disilane gas is stored in a liquid phase in a storage tank by low temperature decompression, and the storage tank is a jacket structure, and the inside of the jacket is a -30 ° C glycol cooling medium.
实施例8Example 8
重复实施例3，不同之处在于，所述硅化镁与氯化氨的摩尔比为1:3，所述催化剂为C68H56Fe2P4ZnY2与C52H48P4ZnCl2的混合物，所述反应在8.4M3的反应釜内进行，所述反应釜配置磁力搅拌器。所述乙硅烷气体通过低温减压在储罐中以液相进行储存，所述储罐为夹套结构，夹套内为-30℃乙二醇冷却介质。所述储罐夹套内的压力为6Pa。Example 3 was repeated, except that the magnesium silicide and ammonium chloride molar ratio of 1: 3, the catalyst is C 68 H 56 Fe 2 P 4 ZnY 2 and C 52 H 48 P 4 ZnCl 2 is The mixture was reacted in a 8.4 M 3 reactor equipped with a magnetic stirrer. The disilane gas is stored in a liquid phase in a storage tank by low temperature decompression, and the storage tank is a jacket structure, and the inside of the jacket is a -30 ° C glycol cooling medium. The pressure inside the tank jacket is 6 Pa.
实施例9Example 9
重复实施例4，不同之处在于，反应温度为20℃，反应压力为0.6MPa，所述催化剂为C54H45P3ZnX2与C52H48P4ZnCl2的混合物，所述乙硅烷气体通过低温减压在储罐中以液相进行储存，所述储罐为夹套结构，夹套内为-30℃乙二醇冷却介质。Example 4 was repeated except that the reaction temperature was 20 ° C and the reaction pressure was 0.6 MPa, and the catalyst was a mixture of C 54 H 45 P 3 ZnX 2 and C 52 H 48 P 4 ZnCl 2 , the disilane The gas is stored in a liquid phase in a storage tank by low temperature decompression, which is a jacketed structure with a -30 ° C glycol cooling medium in the jacket.
实施例10Example 10
重复实施例5，不同之处在于，反应温度为-10℃，反应压力为0.3MPa，所述硅化镁与氯化氨的摩尔比为1:4，所述催化剂为C54H52P4ZnCl2，所述反应在8.4M3的反应釜内进行，所述储罐夹套内的压力为2Pa。 Example 5 was repeated except that the reaction temperature was -10 ° C, the reaction pressure was 0.3 MPa, the molar ratio of magnesium silicide to ammonium chloride was 1:4, and the catalyst was C 54 H 52 P 4 ZnCl. 2. The reaction was carried out in a 8.4 M 3 reactor with a pressure of 2 Pa in the jacket jacket.
以上的详细说明用以揭示本发明之技术内容及特征，并辅以实施例说明，使本领域技术人员据此得以实施，然而上述说明并非用于限制本发明之权利范围，举凡简单之置换或等效技术之取代，仍应隶属本发明之范畴。 The above detailed description is to clarify the technical content and features of the present invention, and the description of the embodiments will be made by those skilled in the art, and the above description is not intended to limit the scope of the present invention. Substitution of equivalent techniques is still within the scope of the invention.

Claims (8)

  1. 一种乙硅烷的制造方法，其特征在于，以硅化镁与氯化氨为原料进行反应，在液氨及催化剂存在下生成乙硅烷气体，反应温度为-10℃至50℃，反应压力为0.2-1MPa，所述硅化镁与氯化氨的摩尔比为1:2-5，所述催化剂为锌的配合物。A method for producing disilane, which comprises reacting magnesium silicide with ammonium chloride as a raw material, and generating disilane gas in the presence of liquid ammonia and a catalyst, the reaction temperature is -10 ° C to 50 ° C, and the reaction pressure is 0.2. -1 MPa, the molar ratio of the magnesium silicide to the ammonium chloride is 1:2-5, and the catalyst is a complex of zinc.
  2. 根据权利要求1所述的方法，其特征在于，所述反应压力为0.25-0.55MPa。The method of claim 1 wherein said reaction pressure is from 0.25 to 0.55 MPa.
  3. 根据权利要求1所述的方法，其特征在于，所述硅化镁与氯化氨的摩尔比为1:3。The method of claim 1 wherein the molar ratio of magnesium silicide to ammonium chloride is 1:3.
  4. 根据权利要求1所述的方法，其特征在于，所述反应在3-10M3的反应釜内进行。The method of claim 1 wherein said reacting is carried out in a 3-10 M 3 reactor.
  5. 根据权利要求4所述的方法，其特征在于，所述反应在8.4M3的反应釜内进行。The method of claim 4 wherein said reacting is carried out in a 8.4 M 3 reactor.
  6. 根据权利要求4或5所述的方法，其特征在于，所述反应釜配置磁力搅拌器。A method according to claim 4 or 5, wherein the reactor is equipped with a magnetic stirrer.
  7. 根据权利要求1所述的方法，其特征在于，所述催化剂为C54H45P3ZnX2、C68H56Fe2P4ZnY2、C52H48P4ZnCl2、C54H52P4ZnCl2中的一种或几种；其中X为F、Cl、Br或I，Y为Br或I。The method according to claim 1, wherein the catalyst is C 54 H 45 P 3 ZnX 2 , C 68 H 56 Fe 2 P 4 ZnY 2 , C 52 H 48 P 4 ZnCl 2 , C 54 H 52 One or more of P 4 ZnCl 2 ; wherein X is F, Cl, Br or I, and Y is Br or I.
  8. 根据权利要求1所述的方法，其特征在于，所述乙硅烷气体通过低温减压在储罐中以液相进行储存，所述储罐为夹套结构，夹套内为-30℃乙二醇冷却介质。 The method according to claim 1, wherein the disilane gas is stored in a liquid phase in a storage tank by low temperature decompression, and the storage tank is a jacket structure, and the inside of the jacket is -30 ° C. Alcohol cooling medium.
PCT/CN2017/083418 2016-05-09 2017-05-08 Method for manufacturing disilane WO2017193881A1 (en)

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CN105800616B (en) * 2016-05-09 2017-03-22 浙江迅鼎半导体材料科技有限公司 Method for preparing disilane
CN106185949B (en) * 2016-08-02 2018-03-09 浙江迅鼎半导体材料科技有限公司 A kind of manufacture method of disilane
CN112661161A (en) * 2020-12-28 2021-04-16 烟台万华电子材料有限公司 Method for continuously producing high-order silane
CN113083166A (en) * 2021-03-16 2021-07-09 洛阳中硅高科技有限公司 Disilane preparation equipment and preparation method

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