CN114715901A - Device and method for preparing polychlorinated silane through catalytic synthesis - Google Patents

Device and method for preparing polychlorinated silane through catalytic synthesis Download PDF

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CN114715901A
CN114715901A CN202210310438.4A CN202210310438A CN114715901A CN 114715901 A CN114715901 A CN 114715901A CN 202210310438 A CN202210310438 A CN 202210310438A CN 114715901 A CN114715901 A CN 114715901A
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condenser
catalyst
catalytic
gas
column
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王乐强
郑锐
李强强
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Quanjiao Yagetai Electronic New Material Technology Co ltd
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Quanjiao Yagetai Electronic New Material Technology 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
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
    • B01D5/0033—Other features
    • B01D5/0036—Multiple-effect condensation; Fractional condensation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/0242—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid flow within the bed being predominantly vertical
    • B01J8/025—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid flow within the bed being predominantly vertical in a cylindrical shaped bed
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/0292—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds with stationary packing material in the bed, e.g. bricks, wire rings, baffles
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/584—Recycling of catalysts

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  • Organic Chemistry (AREA)
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  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention provides a device and a method for preparing polychlorinated silane by catalytic synthesis, wherein the device comprises a gas storage tank, the gas storage tank is connected with a catalytic column through a pipeline, filler is filled in the catalytic column, one side of the catalytic column is connected with a condenser through a circulating pipeline, a separation column is arranged on the lower side of the condenser, the lower side of the separation column is connected with a collecting tank through a gas pipe, and one side of the condenser is connected with a tail gas furnace through a pipeline. The monochlorosilane and the hydrogen chloride react in a catalytic column filled with a molecular sieve catalyst under the conditions of certain proportion, pressure, temperature and retention time to generate polychlorinated silane with a certain content, and the separation of products and the recovery of raw materials are carried out by a condenser, so that the production with high efficiency, energy conservation, long-term stability, safety and reliability is realized.

Description

Device and method for preparing polychlorinated silane through catalytic synthesis
Technical Field
The invention relates to the technical field of chlorosilane synthesis, in particular to a device and a method for preparing polychlorinated silane through catalytic synthesis.
Background
Chlorosilane, as an important epitaxial silicon source for the semiconductor industry, has significant application in the deposition of silicon dioxide and silicon nitride films for microelectronic devices. With the rapid development of the semiconductor industry, there is an increasing demand and use of chlorosilanes, especially low chlorosilanes.
The preparation method of the chlorosilane comprises the following steps:
disproportionation of monochlorosilane
Under the condition of a catalyst, trichlorosilane and dichlorosilane can be disproportionated to generate other chlorosilane respectively under the condition of the catalyst, wherein the type of the catalyst has great influence on the reaction yield and selectivity, and the amine and amide catalysts have higher yield on the catalytic generation of dichlorosilane. The selective disproportionation reaction for preparing chlorosilane requires chlorosilane as a raw material, and the reaction is a reversible reaction, which is not beneficial to the generation of monochlorosilane and has a certain limitation on the method.
The reaction formula is as follows: 2SiHCl3=SiH2Cl2+SiCl4
The reaction formula is as follows: 2SiH2Cl2=SiHCl3+SiH3Cl
Catalytic synthesis of di-and silane
Under the condition of selecting zeolite molecular sieve, silicon dioxide carrier containing AlCl3 and the like as catalysts, synthesizing chlorosilane from silane and methane chloride gas under a certain temperature condition.
The reaction formula is as follows: SiH4+HCl=SiH3Cl+H2
The reaction formula is as follows: SiH4+2HCl=SiH2Cl2+2H2
It is worth noting that under certain conditions, although appropriate chlorosilane can be produced, a certain thermal effect exists in the reaction process, partial products are decomposed to form particles to block the pore channels of the molecular sieve, the higher the temperature is, the more obvious the aging tendency of the catalyst is, generally, under the condition of the highest effective temperature, the catalytic efficiency is reduced to the initial 50% in 7 days, the catalytic activity is difficult to recover through high-temperature activation after aging, and the catalyst needs to be replaced more frequently, which is a great difficulty in industrialization.
Meanwhile, according to experimental results, the effect of synthesizing more polychlorinated silane by using silane and hydrogen chloride as raw materials is poor, the dichlorosilane conversion rate is low, the conversion rate of other polychlorinated silane is basically lower than 10%, wherein the more substitution, the lower the product conversion rate.
Third, synthetic method
Taking copper silicon powder, chloromethane and chlorine as raw materials to synthesize the chlorosilane at the temperature of 250-300 ℃. Among them, trichlorosilane has a high selectivity, and it is noted that this method is not suitable for the preparation of monochlorosilane, and the selectivity of dichlorosilane can be improved by introducing chlorine gas first to form SiCl.
The reaction formula is as follows: 2Si +5HCl = SiHCl3+SiH2Cl2+H2
Fourth, recovery method
In the polysilicon synthesis process, about 1 percent of dichlorosilane and part of unreacted trichlorosilane can be recovered by condensation rectification, and the preparation method is more dependent on the recovery of products.
In summary, the existing silicon polychloride has the disadvantages of low preparation efficiency and low product conversion rate, so the problem needs to be solved urgently.
Disclosure of Invention
The invention aims to provide a device and a method for preparing polychlorinated silane by catalytic synthesis, wherein monochlorosilane and hydrogen chloride react in a catalytic column filled with a molecular sieve catalyst under the conditions of certain proportion, pressure, temperature and retention time to generate polychlorinated silane with certain content, and a condenser is used for separating products and recovering raw materials, so that the problems of low preparation efficiency and low productivity of the center of the background technology are solved.
The invention provides a device for preparing polychlorinated silane by catalytic synthesis, which comprises a gas storage tank, wherein the gas storage tank is connected with a catalytic column through a pipeline, a filler is filled in the catalytic column, one side of the catalytic column is connected with a condenser through a circulating pipeline, a separation column is arranged at the lower side of the condenser, the lower side of the separation column is connected with a collecting tank through a gas pipe, and one side of the condenser is connected with a tail gas furnace through a pipeline.
The further improvement lies in that: the three gas storage tanks are respectively internally provided with argon, hydrogen chloride and monochlorosilane; the gas storage tank is provided with a flow control valve, and the flow control valve controls the gas output quantity of the gas through a control module.
The further improvement lies in that: condenser and holding vessel all are equipped with two, through the tube coupling between the condenser, condenser and holding vessel correspond and connect, and the condenser refrigerates through the refrigerator, and the holding vessel is raw materials holding vessel and finished product holding vessel respectively.
The further improvement is that: the filler comprises a catalyst and a metal wire mesh; the mixing volume ratio of the catalyst to the metal wire mesh is 1-2: 1-3.
The further improvement lies in that: the catalyst is a molecular sieve catalyst, and the silicon-aluminum ratio in the catalyst is 25: 100, the catalyst is spherical, the diameter of the catalyst is 2-10mm, and the aperture of the catalyst is 0.3-1 nm.
The further improvement lies in that: the condenser is connected with a detector through a pipeline, and the detector adopts gas chromatography for detection.
The invention also provides a method for preparing polychlorinated silane by catalytic synthesis, which comprises the following steps of 1, mixing and filling a catalyst and a wire mesh into a catalytic column, and performing activation pretreatment; step 2, introducing hydrogen chloride and monochlorosilane into the catalytic column, and carrying out catalytic reaction through a catalyst; step 3, introducing the reaction product into a condenser for separation and collection; and 4, treating the tail gas.
The further improvement lies in that: in the step 2, the volume ratio of the hydrogen chloride to the monochlorosilane is 1-2: 1-3; the reaction pressure is 1-3 bar; the reaction temperature is 30-80 ℃; the reaction time is 10-90 s.
The further improvement lies in that: and 3, condensing and separating the reaction product by two condensers in sequence, wherein the temperature of the first condenser is controlled to be-20 to-15 ℃, and the temperature of the second condenser is controlled to be-70 to-50 ℃.
The invention has the beneficial effects that: 1. the method adopts monochlorosilane and hydrogen chloride to generate the polychlorinated silane through catalytic reaction of the catalyst, is different from the existing chlorosilane preparation method, greatly improves the reaction conversion rate of the polychlorinated silane, and improves the yield of the polychlorinated silane product; in the catalytic synthesis reaction, the heat effect generated by synthesis is balanced, and the catalyst is relatively mild, so that the service life of the catalyst is prolonged, the catalyst is prevented from being replaced ordinarily, the use of resources is greatly reduced, and the production cost is reduced.
2. The reaction product is subjected to fractional condensation and separation through the plurality of condensers, the reaction product is gradually separated through the temperature difference between the condensers, and meanwhile, the raw material monochlorosilane can be separated, and the monochlorosilane is recycled, so that the utilization rate of the monochlorosilane is improved, the resource utilization rate is improved, and the production cost is reduced.
3. According to the invention, the catalyst and the metal wire mesh are filled into the catalytic column in proportion, and the catalyst adopts the spherical zeolite molecular sieve catalyst, so that the catalytic reaction efficiency is higher, the reaction production efficiency is improved, and the problem of pipeline blockage caused by the powder zeolite molecular sieve catalyst is also reduced.
4. According to the invention, the tail gas furnace is arranged, the reaction product is condensed and separated by the condenser, and the residual tail gas is conveyed into the tail gas furnace for incineration treatment, so that the tail gas is treated quickly, the tail gas emission pollution is reduced, and the production environment is effectively protected.
Drawings
FIG. 1 is a view showing the structure of the apparatus of the present invention.
Fig. 2 is a flow chart of the method of the present invention.
Wherein: 1-gas storage tank, 2-flow control valve, 3-catalytic column, 4-condenser, 5-collection tank, 6-tail gas furnace and 7-detector.
Detailed Description
For the purpose of enhancing understanding of the present invention, the present invention will be further described in detail with reference to the following examples, which are provided for illustration only and are not to be construed as limiting the scope of the present invention.
Example 1
As shown in fig. 1, the embodiment provides a device for preparing polychlorinated silane by catalytic synthesis, which includes three gas storage tanks, where the three gas storage tanks 1 are respectively filled with argon, hydrogen chloride, and monochlorosilane; the gas storage tank 1 is provided with a flow control valve 2, and the flow control valve 2 controls the gas output quantity of the gas through a control module. The gas holder 1 is connected with a catalytic column 3 through a pipeline, and gas in the gas holder 1 enters the catalytic column 3 along the pipeline to perform catalytic reaction. The catalytic column 3 is filled with filler, the filler is formed by mixing a catalyst and a wire mesh, and the mixing volume ratio of the catalyst to the wire mesh is 1-2: 1-3, the catalyst is a molecular sieve catalyst, and the silicon-aluminum ratio in the catalyst is 25: 100, the catalyst is spherical, the diameter size of the catalyst is 2-10mm, and the aperture of the catalyst is 0.3-1 nm; by passing
One side of the catalytic column 3 is connected with a condenser 4 through a circulating pipeline, the condenser 4 is connected with a detector 7 through a pipeline, and the detector 7 analyzes a reaction product through gas chromatography. Condenser 4 is equipped with two, through the tube coupling between condenser 4, there is the difference in temperature between condenser 4, 4 downside of condenser are equipped with the separation column, the separation column downside has holding vessel 5 through the trachea connection, holding vessel 5 is equipped with two, holding vessel 5 is raw materials holding vessel and finished product holding vessel respectively, condenser 4 corresponds with holding vessel 5 and connects, condensation separation in reaction product enters into condenser 4, the result of separation enters into classification respectively and collects in holding vessel 5 through the separation column separation. One side of the condenser 4 is connected with a tail gas furnace 6 through a pipeline, and the tail gas furnace 6 adopts an incinerator or liquid discharge treatment, so that the waste gas pollution is reduced.
As shown in fig. 2, this example also provides a method for preparing polychlorinated silane by catalytic synthesis, comprising the following steps;
step 1, mixing a catalyst and a wire mesh, filling the mixture into a catalytic column, and performing activation pretreatment; and 2, introducing hydrogen chloride and monochlorosilane into the catalytic column, wherein the volume ratio of the hydrogen chloride to the monochlorosilane is 1-2: 1-3, carrying out catalytic reaction by using a catalyst, wherein the reaction pressure is 1-3 bar; the reaction temperature is 30-80 ℃; the reaction time is 10-90 s;
step 3, introducing the reaction product into a condenser for separation and collection, condensing and separating the reaction product sequentially through two condensers, controlling the temperature of the first condenser to be within-20 to-15 ℃, controlling the temperature of the second condenser to be within-70 to-50 ℃, separating the reaction product sequentially through temperature difference, and performing classified collection through a raw material collection tank and a finished product collection tank;
and 4, discharging the residual gas into the incinerator, and treating tail gas to reduce tail gas pollution.
Example 2
The method comprises the following steps of building equipment, carrying out pressure maintaining and leakage detecting, and detecting the leakage: using a suction gun method to conduct helium detection at positive pressure of 10bar, wherein the leak rate is less than 2 x 10- 9Pa·m3And/s, and standby after qualification. 200g of zeolite molecular sieve catalyst H-ZSM-5, (catalyst Si: Al = 25: 280, catalyst particles are spherical, and the diameter =2-3mm) is placed in an oven at 110 ℃ for 24H, and the same volume of wire mesh filler is uniformly mixed with the catalyst particles and then filled into a catalytic column. And (3) carrying out pumping drying at the temperature of 350 ℃, and carrying out activation pretreatment on the catalyst. Controlling the volume ratio of the monochlorosilane to the hydrogen chloride mixed gas to be 1:1 by a mass flow meter, adjusting the reaction pressure to be 2bar, the reaction environment temperature to be 50 ℃, adjusting the reaction residence time to be 60s, and analyzing the gas phase product after the reaction by gas chromatography after the reaction is continuously operated for 2 hours, wherein the conversion rate of the monochlorosilane is 59.3%, the yield of dichlorosilane is 41.5%, the yield of trichlorosilane is 15.3%, and the yield of tetrachlorosilane is 2.5%. And when the reaction runs stably, controlling the temperature of a first condenser to be-20 to-15 ℃, liquefying and collecting polychlorinated silane (SiH 2Cl2, SiHCl3 and SiCl 4) in a finished product collecting tank by product airflow through the first condenser, and then rectifying to separate the three components. After passing through the first condenser, introducing monochlorosilane, hydrogen and hydrogen chloride gas in the residual gas into a second condenser, controlling the temperature of the second condenser to be-70 to-50 ℃, liquefying and collecting the monochlorosilane in a raw material collecting tank, and treating the residual gas through an incinerator; the recovered monochlorosilane is recycled.
Example 3
150g of zeolite molecular sieve catalyst H-ZSM-5 (wherein the catalyst Si: Al = 25: 200, the catalyst particles are spherical and have a diameter =2-3mm) was placed in an oven at 110 ℃ for 24 hours, and a wire mesh filler having a volume 2 times that of the molecular sieve catalyst was uniformly mixed therewith and packed into a catalytic column. And (3) carrying out pumping drying at the temperature of 350 ℃, and carrying out activation pretreatment on the catalyst. Controlling the feeding volume ratio of the monochlorosilane and hydrogen chloride mixed gas to be 1:1 through a flow control valve, adjusting the reaction pressure to be 2bar, the reaction environment temperature to be 80 ℃, adjusting the reaction residence time to be 90s, and analyzing the gas-phase product after the reaction through a gas chromatography of a detector after the reaction is continuously operated for 2 hours, wherein the conversion rate of the monochlorosilane is 64.6 percent, the yield of the dichlorosilane is 37.6 percent, the yield of the trichlorosilane is 23.7 percent, and the yield of the tetrachlorosilane is 3.3 percent. And when the reaction runs stably, controlling the temperature of a first condenser to be-20 to-15 ℃, liquefying and collecting polychlorinated silane (SiH 2Cl2, SiHCl3 and SiCl 4) in a finished product collecting tank by product airflow through the first condenser, and then rectifying to separate the three components. After passing through the first condenser, introducing monochlorosilane, hydrogen and hydrogen chloride gas in the residual gas into a second condenser, controlling the temperature of the second condenser to be-70 to-50 ℃, liquefying and collecting the monochlorosilane in a raw material collecting tank, and treating the residual gas through an incinerator; the recovered monochlorosilane is recycled.
Example 4
150g of zeolite molecular sieve catalyst H-ZSM-5 (wherein the catalyst Si: Al = 25: 100, the catalyst particles are spherical and have a diameter =2-3mm) was placed in an oven at 110 ℃ for 24 hours, and a wire mesh filler having a volume 2 times that of the molecular sieve was uniformly mixed therewith and packed into a catalytic column. And (3) carrying out pumping drying at the temperature of 350 ℃, and carrying out activation pretreatment on the catalyst. Controlling the volume ratio of the monochlorosilane to the hydrogen chloride mixed gas to be 1:1 by a mass flow meter, adjusting the reaction pressure to be 2bar, the reaction environment temperature to be 40 ℃, adjusting the reaction residence time to be 30s, and analyzing the gas phase product after the reaction by a gas chromatography detector after the reaction is continuously operated for 2 hours, wherein the conversion rate of the monochlorosilane is 57.9%, the yield of dichlorosilane is 46.4%, the yield of trichlorosilane is 10.3%, and the yield of tetrachlorosilane is 1.2%. And when the reaction runs stably, controlling the temperature of a first condenser to be-20 to-15 ℃, liquefying and collecting polychlorinated silane (SiH 2Cl2, SiHCl3 and SiCl 4) in a finished product collecting tank by product airflow through the first condenser, and then rectifying to separate the three components. After passing through the first condenser, introducing monochlorosilane, hydrogen and hydrogen chloride gas in the residual gas into a second condenser, controlling the temperature of the second condenser to be-70 to-50 ℃, liquefying and collecting the monochlorosilane in a raw material collecting tank, and treating the residual gas through an incinerator; the recovered monochlorosilane is recycled.
Example 5
200g of zeolite molecular sieve catalyst H-ZSM-5 (wherein the catalyst Si: Al = 80: 200, the processed particles are spherical, and the diameter =2-3mm) is placed in an oven at 110 ℃ for 24H, and a metal wire mesh filler with the volume 1 time that of the molecular sieve catalyst is uniformly mixed with the catalyst and then filled into a catalytic column. And (3) carrying out pumping drying at the temperature of 350 ℃, and carrying out activation pretreatment on the catalyst. Controlling the feeding volume ratio of the monochlorosilane and hydrogen chloride mixed gas to be 1:2 through a flow control valve, adjusting the reaction pressure to be 2bar, the reaction environment temperature to be 40 ℃, adjusting the reaction residence time to be 90s, and analyzing the gas phase product after the reaction through a gas chromatography of a detector after the reaction is continuously operated for 2 hours, wherein the conversion rate of the monochlorosilane is 73.4%, the yield of dichlorosilane is 53.2%, the yield of trichlorosilane is 15.5%, and the yield of tetrachlorosilane is 4.5%. And when the reaction runs stably, controlling the temperature of a first condenser to be-20 to-15 ℃, liquefying and collecting polychlorinated silane (SiH 2Cl2, SiHCl3 and SiCl 4) in a finished product collecting tank by product airflow through the first condenser, and then rectifying to separate the three components. After passing through the first condenser, introducing monochlorosilane, hydrogen and hydrogen chloride gas in the residual gas into a second condenser, controlling the temperature of the second condenser to be-70 to-50 ℃, liquefying and collecting the monochlorosilane in a raw material collecting tank, and treating the residual gas through an incinerator; the recovered monochlorosilane is recycled.

Claims (9)

1. The utility model provides a device of catalytic synthesis preparation polychlorinated silane, includes the gas holder, and the gas holder has catalytic column, its characterized in that through the tube coupling: the filler is filled in the catalysis column, a condenser is connected to one side of the catalysis column through a circulating pipeline, a separation column is arranged on the lower side of the condenser, a collecting tank is connected to the lower side of the separation column through a gas pipe, and a tail gas furnace is connected to one side of the condenser through a pipeline.
2. The apparatus for preparing polychlorinated silane through catalytic synthesis according to claim 1, wherein: the three gas storage tanks are respectively internally provided with argon, hydrogen chloride and monochlorosilane; the gas storage tank is provided with a flow control valve, and the flow control valve controls the gas output quantity of the gas through a control module.
3. The apparatus for the catalytic synthesis of polychlorosilane according to claim 1 wherein: condenser and holding vessel all are equipped with two, through the tube coupling between the condenser, condenser and holding vessel correspond and connect, and the holding vessel is raw materials holding vessel and finished product holding vessel respectively.
4. The apparatus for preparing polychlorinated silane through catalytic synthesis according to claim 1, wherein: the filler comprises a catalyst and a metal wire mesh; the mixing volume ratio of the catalyst to the metal wire mesh is 1-2: 1-3.
5. The apparatus for preparing polychlorinated silane through catalytic synthesis according to claim 4, wherein: the catalyst is a molecular sieve catalyst, and the silicon-aluminum ratio in the catalyst is 25-80: 100-280, the catalyst is spherical, the diameter of the catalyst is 2-10mm, and the aperture of the catalyst is 0.3-1 nm.
6. The apparatus for preparing polychlorinated silane through catalytic synthesis according to claim 1, wherein: the condenser is connected with a detector through a pipeline.
7. A method for preparing polychlorinated silane by catalytic synthesis using the device of any one of claims 1 to 6, wherein: the method comprises the following steps of 1, mixing a catalyst and a wire mesh, filling the mixture into a catalytic column, and performing activation pretreatment; step 2, introducing hydrogen chloride and monochlorosilane into the catalytic column, and carrying out catalytic reaction through a catalyst; step 3, introducing the reaction product into a condenser for separation and collection; and 4, treating the tail gas.
8. The process of claim 7 for the preparation of polychlorosilanes by catalytic synthesis, wherein: in the step 2, the volume ratio of the hydrogen chloride to the monochlorosilane is 1-2: 1-3; the reaction pressure is 1-3 bar; the reaction temperature is 30-80 ℃; the reaction time is 10-90 s.
9. The process of claim 7 for the preparation of polychlorosilanes by catalytic synthesis, wherein: and in the step 3, the reaction product is condensed and separated by two condensers in sequence, wherein the temperature of the first condenser is controlled to be within-20 to-15 ℃, and the temperature of the second condenser is controlled to be within-70 to-50 ℃.
CN202210310438.4A 2022-03-28 2022-03-28 Device and method for preparing polychlorinated silane through catalytic synthesis Pending CN114715901A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117208913A (en) * 2023-09-04 2023-12-12 全椒亚格泰电子新材料科技有限公司 Method and equipment for preparing polychlorosilane by catalytic synthesis

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117208913A (en) * 2023-09-04 2023-12-12 全椒亚格泰电子新材料科技有限公司 Method and equipment for preparing polychlorosilane by catalytic synthesis
CN117208913B (en) * 2023-09-04 2024-03-08 全椒亚格泰电子新材料科技有限公司 Method and equipment for preparing polychlorosilane by catalytic synthesis

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