KR101133658B1 - A Manufacturing Method and A Manufacturing Apparatus of TrichlorosilaneSiHCl3 using the Metal Catalyst - Google Patents

Abstract

The present invention relates to a method and apparatus for producing trichlorosilane by using metal silicon and silicon tetrachloride (STC) as a main raw material and adding hydrogen using a solid catalyst. The process conditions are relieved by recycling silicon tetrachloride and using a catalyst. And the purpose and effect of improving the recycling of resources and the efficiency of manufacturing.

The present invention minimizes waste generation by minimizing waste generation by recycling silicon tetrachlorine (STC), which is a by-product generated during the production of silane trichloride (TCS, SiHCl ₃ ) required for monocrystalline silicon, polycrystalline silicon and silane gas production. To prepare a trichlorosilane, more specifically, the size of the metal silicon particles used as a raw material is 50-400mesh, purity is 92% or more, silicon tetrachloride purity of 75% or more, hydrogen purity of 70% or more Inject hydrogen into the silicon tetrachloride tank, vaporize it with silicon tetrachloride and inject it into the reactor, maintain the temperature of the reactor at 150 ℃ ~ 800 ℃, and pass the reaction gas from the reactor through the distillation column to make the difference in boiling point. Separating into trichlorosilane and silicon tetrachloride by using, the separated trichlorosilane is transferred to the storage tank, and the recovered silicon tetrachloride is silicon tetrachloride tank It is configured to send for recycling.

 Silicon tetrachloride, silane trichloride, Pd catalyst, Pb catalyst, hydrogen, metal silicon

Description

A manufacturing method and a manufacturing apparatus of trichlorosilane (SiHCl3) using the metal catalyst}

In the present invention, in order to efficiently produce trichlorosilane (SiHCl ₃ ), which is widely used in gas purification and high purity silicon, the size of the metal grade silicon particles is 50-400mesh and the purity is 90% or more. The purity is more than 70%, the silicon tetrachloride (STC) is used for industrial purposes of 75% or more, the hydrogen flow is controlled by supplying about 70sccm by using MFC, silicon tetrachloride (STC, SiCl ₄ ) maintained at 50 ℃ heating Silicon tetrachloride and hydrogen are supplied to the reactor by bubbling hydrogen tetrachloride into the tank containing hydrogen, and silicon tetrachloride and hydrogen are loaded into the reactor, and the silicon silicon and metal catalysts (Pd and Pb) are mounted in the reactor, and tetrachloride injected into the reactor. Silicon and hydrogen react with metal silicon to produce trichlorosilane, which is heated using a heater to maintain the temperature of the reactor between 150 ° C and 800 ° C, and the reaction The fine powder metal silicon contained in the fluid discharged to the upper part is separated and recovered by a cyclone, and the distillation column separates the reaction product of trichlorosilane and silicon tetrachloride using the difference in boiling point, and the silicon tetrachloride collected in the lower reboiler is used as a raw material. It is fed back to the silicon tetrachloride tank for recycling, and the gas passing through the upper condenser contains TCS, STC, HCl and H ₂ , but the purity of trichlorosilane is more than 95% and designed to be stored in the liquid storage tank. The present invention relates to a method and apparatus for producing trichlorosilane using a metal catalyst.

As a conventional apparatus and method for producing trichlorosilane, a method of producing silicon-grade silicon by injecting hydrogen chloride using one of a fluidized bed reactor, a stirred bed reactor, and a fixed bed reactor has been mainly used.

In the case of producing silane gas and silicon, silicon tetrachloride (STC) is produced as a by-product, and the generated silicon tetrachloride generates silicon oxide and hydrogen chloride gas when it comes into contact with air or water. Since there is a problem that acts as an important constraint of the need for specific research and development of the apparatus for producing trichlorosilane by the addition of hydrogen to silicon tetrachloride.

In this case, when the catalyst is not used, the reaction does not occur in a section between 300 ° C. and 500 ° C., and in order to lower the reaction temperature, the European Patent Publication (0,658,359, A2) uses a catalyst composed of nickel, copper, and iron. The method has been proposed, and the technical content of the conversion of trichlorosilane of about 20% is disclosed in the vicinity of 300 ° C using a commonly known Cu catalyst. However, the conversion of trichlorosilane is relatively low and the technical configuration of recycling of silicon tetrachloride is Since it is not disclosed, the technical configuration for cost reduction due to the recycling of resources is not disclosed, and there is a problem that waste treatment must be performed separately.

The method of injecting hydrogen and silicon tetrachloride without using a catalyst is disclosed in the published PCT data (WO 2006/081980) to produce a trichlorosilane mixture at a temperature of 700 ° C to 1500 ° C. 10% to 20% is relatively low and the technical composition for recycling the fine powder metal silicon and silicon tetrachloride generated during the reaction is not disclosed, as well as the cost reduction and the waste treatment separately, Another problem is that Cu used as a catalyst volatilizes into CuCl ₂ to contaminate the product.

The problem to be solved by the present invention is a trichlorosilane production apparatus and method having a high conversion rate capable of continuously producing trichlorosilane by adding hydrogen under a metal catalyst (Pd or Pb) using metal silicon and silicon tetrachloride as a raw material To propose.

Another problem to be solved by the present invention is to increase the conversion rate of trichlorosilane by using a metal catalyst mounted in the reactor, to be manufactured under a low reaction temperature and low reaction pressure to reduce the installation cost of the device, production cost and maintenance To reduce costs.

Another problem to be solved by the present invention is to recover and recycle the fine powder metal silicon by using a cyclone during the production apparatus and process of trichlorosilane, and to separate the silicon tetrachloride and trichlorosilane using the boiling point difference in the distillation column to recycle silicon tetrachloride It is designed and manufactured to reduce the production cost, raw material cost and waste disposal cost significantly.

The problem solving means of the present invention is the size of silicon particles of the metal grade is 50-400mesh, purity is more than 90%, purity of hydrogen in order to efficiently produce trichlorosilane which is widely used in the preparation of gas purification and high purity silicon Is more than 70%, silicon tetrachloride purity is more than 75% is used for industrial purposes, the hydrogen flow is controlled to 70sccm using MFC, and silicon tetrachloride (STC) that is heated and maintained at about 50 ℃ by a heater device Hydrogen is injected into the tank and silicon tetrachloride is vaporized together with hydrogen and bubbled to the reactor, and the silicon silicon and metal catalysts (Pd and Pb) are mounted in the reactor, and silicon tetrachloride and hydrogen injected into the reactor are metal. Reaction with silicon produces trichlorosilane, which is heated using a heating apparatus to maintain the temperature of the reactor at a constant temperature between 150 ° C and 800 ° C. The metal silicon discharged to the upper part of the reactor separates and recovers the fine particles from the cyclone and is recycled to the reactor.In the distillation column, the reaction product is separated from the trichlorosilane and silicon tetrachloride using the difference in boiling point and the tetrachloride recovered in the lower reboiler. Silicon is fed back to the silicon tetrachloride tank for recycling as a raw material, and the gas passing through the condenser located above contains TCS, STC, HCl and H ₂ , but the trichlorosilane is stored in a liquid storage tank with 95% purity. It is to provide a method and apparatus for producing trichlorosilane using a catalyst designed to be manufactured.

Another solution of the present invention is to recover the fine powder metal silicon and silicon tetrachloride discharged through the reactor and to reduce the cost and production cost of the fine powder metal silicon is recovered as a cyclone and recycled to the reactor used as raw materials In addition, the silicon tetrachloride separated by using the difference in boiling point in the distillation column is to provide a method and apparatus for producing trichlorosilane designed to be recovered in the distillation column tank and fed back to the silicon tetrachloride tank for recycling.

The present invention is an apparatus and method for producing trichlorosilane, which is configured to continuously produce trichlorosilane by adding hydrogen under a metal catalyst (Pd or Pb) using metal silicon and silicon tetrachloride as raw materials to obtain a high conversion rate. It works.

Another effect of the present invention is to reduce the installation cost, production cost and maintenance cost by increasing the conversion rate of trichlorosilane and enabling the production under low reaction temperature and low reaction pressure by mounting a metal catalyst in the reactor.

Another effect of the present invention is that the fine powder metal silicon contained in the gas discharged through the reactor is recovered by the cyclone and recycled to the reactor as a raw material, and the silicon tetrachloride separated and recovered using the difference in boiling point in the distillation column It is fed back to the silicon tetrachloride tank and recycled to reduce waste disposal cost, raw material cost and production cost.

Hereinafter, the present invention will be described in detail. In the present invention, silicon tetrachloride, metal silicon, and hydrogen are used as raw materials, Pd-based catalysts and Pb-based catalysts are used as reaction catalysts, and Cu-based catalysts may also be used.

The apparatus for producing trichlorosilane using a metal catalyst according to the present invention is configured to continuously feed raw materials into a continuous filling reactor, and a cyclone is installed at the top of the reactor to separate and recover fine powder silicon.

A distillation column for separating the trichlorosilane and silicon tetrachloride contained in the reaction product passed through the cyclone using the difference in boiling point is installed at the stage next to the cyclone.

The fluid (gas) reacted with the metal silicon via the cylindrical reactor is configured to separate and recover the fine powder metal silicon from the cyclone and to feed back to the reactor for recycling. The fluid (gas) that has passed through the cyclone passes through a distillation column installed in the next stage, and the lower temperature of the distillation column is between 50 ° C and 58 ° C, and the upper temperature is maintained at a constant temperature between 30 ° C and 35 ° C. As it passes through the distillation column, silicon tetrachloride (boiling point: 57.6 ° C) and trichlorosilane (boiling point: 32 ° C) contained in the fluid are separated by the difference in boiling point. The silicon tetrachloride separated from the distillation column is recovered to a distillation column tank located at the bottom of the distillation column, and the recovered silicon tetrachloride is recycled to the silicon tetrachloride tank and used as a raw material.The trichlorosilane having a purity of 95% or more is formed at the top of the distillation column, so that the trichlorosilane storage tank is Liquefied in

Hereinafter, the configuration and operation of the embodiments of the present invention with reference to the accompanying drawings, the configuration and operation of the present invention shown and described in the drawings will be described by at least one embodiment, whereby the present invention described above The technical spirit and its core composition, the mixing ratio and action of the composition is not limited.

Look at the drawings to facilitate understanding of the present invention. 1 is an apparatus diagram for the production of trichlorosilane using a metal catalyst designed according to the present invention, Figure 2 is an enlarged view of the distillation column of the trichlorosilane production apparatus designed and manufactured according to the present invention. A specific embodiment according to the present invention will be described.

EXAMPLES

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS A preferred embodiment of the present invention will now be described with reference to the drawings. 1 is a device diagram for the production of trichlorosilane using a metal catalyst designed according to the present invention. The present invention relates to an apparatus and method for producing trichlorosilane with high conversion rate at a lower temperature and lower pressure than a conventional trichlorosilane production method by reacting a reactant using a metal catalyst. Powdered metal silicon is recovered by cyclone and recycled to the reactor, and silicon tetrachloride separated and recovered from the distillation column is recycled to the silicon tetrachloride tank, thereby reducing waste disposal costs and raw material costs, thereby reducing production costs. It is to provide a manufacturing apparatus and method.

More specifically, with reference to Figures 1 and 2 looks at with respect to the apparatus for producing trichlorosilane. The form of the reactor 9 for producing trichlorosilane according to the present invention is preferably cylindrical, and at the lower end of the cylindrical reactor 9, a catalyst layer 4 loaded with a metal catalyst such as Pd catalyst or Pb catalyst is located, Above the cylindrical reactor 9 is a metal silicon layer 5. The metal silicon layer 5 is supplied by a metal silicon feeder 1 designed and manufactured such that the metal silicon is continuously fed by a screw at a predetermined ratio as compared to the metal catalyst.

Outside the cylindrical reactor 9, a reactor heating device 2 is installed for reacting the reactants by maintaining the reaction temperature at a constant temperature between 150 ° C and 800 ° C.

The front end of the cylindrical reactor (9) is connected to the silicon tetrachloride tank (8), which is maintained at a temperature between 40 ° C and 100 ° C by pipes, by a heater device (16), and injected into the silicon tetrachloride tank (8). Hydrogen is configured to be continuously introduced in a predetermined amount by using a flow meter (7) installed on one side of the hydrogen supply line from the hydrogen supply source (7) is configured to be supplied to the reactor (9) by evaporating and bubbling with silicon tetrachloride. In this case, the reaction occurring in the reactor is shown in Scheme (1).

SiCl ₄ + H ₂ <-> SiHCl ₃ + HCl (1)

One side of the silicon tetrachloride tank 8 has a silicon tetrachloride level gauge 19 for measuring the level of silicon tetrachloride injected into the silicon tetrachloride tank 8, a temperature sensor 17 for measuring the internal temperature of the tank, and A pressure gauge 23 for measuring the pressure inside the tank is provided. Outside the silicon tetrachloride tank 8, a silicon tetrachloride tank heating device 16 is provided for heating the internal temperature of the silicon tetrachloride tank 8 at a constant temperature between 40 ° C and 100 ° C.

A hydrogen supply control valve 29 is installed between the hydrogen supply source 7 and the flowmeters 7 and MFC installed on one side of the hydrogen supply line, and silicon tetrachloride between the silicon tetrachloride tank 8 and the cylindrical reactor 9. A control valve 30 is installed to control the flow of the fluid generated by the reaction of hydrogen with hydrogen.

The silicon tetrachloride injected as a raw material into the silicon tetrachloride tank 8 has a purity of 75% or more, the size of the metal grade silicon particles is between 50-400 mesh, the purity is 90% or more, and the hydrogen purity is 70% or more. It is preferable to use it.

The internal temperature of the cylindrical reactor 9 is maintained at a constant temperature between 150 ° C. and 800 ° C. with a heating device 2 installed outside the cylindrical reactor 9, and more preferably, a reaction between 300 ° C. and 350 ° C. To make this happen. The internal pressure of the cylindrical reactor 9 is between 1 atm and 10 atm.

Since trichlorosilane is produced by an endothermic reaction, an electric heating device 2 is installed on the right side of the cylindrical reactor in order to supply the heat required for the endotherm, and thus the temperature is maintained at a temperature between 150 ° C and 800 ° C. It is configured to be.

The reaction inside the reactor consists of reaction formula (2) and reaction scheme (3).

Si + 3HCl <-> SiHCl₃ + H₂ (2)

Si + 2H₂ + 3SiCl₄ <-> 4SiHCl₃ (3)

The fluid that has passed through the cylindrical reactor 9 passes through a cyclone 48 installed on the cylindrical reactor 9, and collects and feeds back fine powder metal silicon contained in the fluid to be recycled back into the cylindrical reactor 9. It is designed and manufactured to reduce the cost by recycling the recycled metal silicon as a raw material.

In the upper part of the cylindrical reactor 9, a pressure gauge 24 is installed at the upper part of the reactor to measure the pressure in the reactor, and the recycling of the recovered metal silicon is controlled on the recycling line of the metal silicon installed at the lower side of the cyclone 48. To control valve 31 can be provided.

Silicon tetrachloride (STC) and trichlorosilane (TCS) are present at the same time in the gas from which fine powder metal silicon is separated and removed while passing through the cyclone 48, and the distillation column 10 for separating and recovering them using the boiling point difference is located at the bottom. Distillation column heating device 11 for heating to maintain a constant temperature between 50 ℃ to 58 ℃ is installed on one side of the bottom of the distillation column, for cooling to maintain a constant temperature between 30 ℃ to 35 ℃ The heat exchanger 13 is provided. Silicon tetrachloride separated and recovered using the boiling point difference in the distillation column (10) is transferred to the silicon tetrachloride storage tank (12), and is recycled and recycled to the silicon tetrachloride tank (12), and trichlorosilane (TCS) stores trichlorosilane. Condensation liquefaction and storage in the tank 15, wherein the purity of trichlorosilane is more than 95%.

The internal pressure of the distillation column 11 is made between 1 atm and 5 atm, and the internal temperature of the distillation column is made between 10 ° C and 100 ° C. Distillation tower tank level gauge 20 for measuring the level of silicon tetrachloride recovered in the distillation tower tank, and a distillation tower internal temperature sensor for measuring the internal temperature of the distillation tank 18 and an internal pressure gauge 26 for distillation column for measuring the internal pressure of the distillation column tank are provided.

The gas emitted through the cyclone 48 is injected into the lower portion of the distillation column along the pipe, and a control valve 32 for controlling the flow of gas is installed at one side of the pipe installed between the cyclone 48 and the distillation tower 11. In the upper part of the distillation column, a pressure gauge 25 for measuring the pressure inside the distillation column is installed.

In the distillation column tank, silicon tetrachloride having a high boiling point is collected at a lower portion due to the difference in boiling point as shown in FIG. 1, and the recovered silicon tetrachloride is supplied to the silicon tetrachloride storage tank 12 through a pipe to supply the pump 47. The control valves 43 and 44 for controlling the flow of a fluid are provided in the left and right sides of the pipe in which the feed pump 47 is installed. A baffle is installed in the distillation column tank to reduce the load of the heating device 11.

Inside the silicon tetrachloride storage tank 12, a level gauge 21 for measuring the level of silicon tetrachloride transferred from the distillation column and a pressure gauge 27 for measuring the pressure are provided, and the silicon tetrachloride storage tank 12 is provided. A baffle for stably supplying silicon tetrachloride to the silicon tetrachloride tank 8 by a supply pump 47 is installed inside.

A pipe is connected and installed between the silicon tetrachloride storage tank 12 and the silicon tetrachloride tank 8, and a supply pump 47 is installed on the pipe, and a control valve for controlling the flow of fluid in front and behind the supply pump 47. 36 and 37 are provided, and a control valve 45 capable of discharging silicon tetrachloride, if necessary, can be provided on one side of the silicon tetrachloride storage tank 12.

A cooling heat exchanger 13 is installed on the distillation column 10 to cool the gas from the distillation column to about 30 ° C. to 35 ° C., and one side of the heat exchanger 13 injects or blocks a refrigerant to the heat exchanger. Control valves 38 and 39 are provided. On the pipe of the upper part of the distillation column 10, a control valve 33 for controlling the flow of gas moving to the upper part of the distillation column is provided.

The gas that has passed through the cooling heat exchanger 13 installed above the distillation column 10 is transferred and stored through a pipe to a trichlorosilane storage tank 15 for storing trichlorosilane through a condenser, and the trichlorosilane storage tank 15 At the front of the heat exchanger, a cooling heat exchanger 14 for cooling the trichlorosilane is liquefied and stored. A control valve 40 or 41 for injecting or blocking a refrigerant into the heat exchanger is provided at one side of the heat exchanger 14. Is installed.

In order to control the fluid that has passed through the cooling condensation heat exchanger 14, control valves 34 and 35 are provided at the front and rear ends of the heat exchanger 14, respectively.

In the trichlorosilane storage tank 15, a level gauge 22 for measuring the level of liquefied trichlorosilane and a pressure gauge 28 for measuring the internal pressure of the trichlorosilane storage tank 15 are provided. The lower side of the trichlorosilane storage tank 15 may be provided with a control valve 42 for discharging trichlorosilane.

The cylindrical reactor (9) is a fixed bed reactor prepared by separating the catalyst layer (4) and the metal silicon layer (5) as shown in FIG. 1, a mixed reactor prepared by mixing and charging the catalyst and the metal silicon, and the catalyst and the metal silicon. It can be designed and manufactured by selecting one of the fluidized bed reactor to increase the conversion rate by increasing the reaction time by making to move inside the reactor.

FIG. 2 is an enlarged view of the distillation column 10 according to the present invention. The distillation column 10 of FIG. 2 includes a reboiler, a distillation column, and a condenser (condenser) on which the heater device 11 is mounted. In the reboiler, the heating device is heated to 50 ° C to 58 ° C. In the distillation column, the contact time of the fluid is increased to increase the purity of the trichlorosilane, and the condenser condenses the gas passing through the liquid to feed back as shown in The gas is configured to transfer to the trichlorosilane storage tank 15.

The various control valves and sensors described above can be additionally installed or removed as needed during design and manufacture, and the trichlorosilane is automatically or manually manufactured by interworking the plurality of control valves, supply pumps, heating devices and sensors with each other. The control unit using a microprocessor can be installed.

Pd catalysts include palladium salt of a concentration which is mounted in a cylindrical reactor (PdNO _3, PdCl ₂₎ alumina in solution, the zeolite, after selecting a tint of a silicon oxide, activated carbon and diatomaceous earth and dried impregnated with Na ₂ CO _3, K _It was neutralized with a solution such as ₂ CO ₃ , dried, calcined at 400 ° C., and reduced with hydrogen at 300 ° C. for 5 hours. Pb catalyst is composed of Pb, Ti, Sr, etc., and PbNO ₃ , TiCl 4, SrNO ₃ and the like in a proportion of the solution to select one of alumina, zeolite, silicon oxide, activated carbon and diatomaceous earth Impregnated, neutralized with a neutralizing agent, dried at about 100 ° C., calcined at 500 ° C., and reduced to hydrogen at 300 ° C. for 5 hours to be used as a catalyst. Cu catalyst was alumina, zeolite, and oxidation in a constant concentration of CuCl ₂ solution. One of silicon, activated carbon, and diatomaceous earth is selected, impregnated for a predetermined time, dried, neutralized with a neutralizing agent, dried, calcined, and reduced with hydrogen to use as a catalyst.

It looks at the manufacturing method for producing trichlorosilane. In the method for producing trichlorosilane according to the present invention, hydrogen is supplied through a pipe from a hydrogen supply source to a silicon tetrachloride tank, and hydrogen and silicon tetrachloride are bubbling from a silicon tetrachloride tank by supplying hydrogen through the pipe. Through the pipe and into the cylindrical reactor,
Hydrogen and silicon tetrachloride injected through the pipe from the silicon tetrachloride tank are heated and reacted with a heating device in a cylindrical reactor loaded with a metal catalyst and a metal silicon to generate trichlorosilane, and the cylindrical column is installed in the distillation column Silicon tetrachloride and trichlorosilane contained in the gas from the reactor is separated by using a difference in boiling point to obtain a trichlorosilane.

The manufacturing process of the trichlorosilane may further add a plurality of processes generated by the above-described manufacturing apparatus.

Example 1

In the apparatus for producing trichlorosilane using the catalyst according to the present invention, the cylindrical reactor has a diameter of 10 cm, a height of 2 m, and a cyclone having a diameter of 30 cm at the top thereof, and a diameter of 10 cm at the next stage of the cyclone. , 2m high distillation column is installed, the condenser is attached to the top of the distillation column, the lower part of the distillation column was configured to maintain 58 ℃ by heating with a heating device.

At the lower end of the cylindrical reactor 10 cm in diameter, 0.5 L of the Pd catalyst prepared by the method described above was loaded, and 3 L of metal silicon was loaded at the top.

A silicon tetrachloride tank of 2 L vessel was heated to 50 ° C. with an electric heater, and hydrogen was injected at 70 sccm to bubble.

The internal temperature of the reactor was maintained at 320 ° C by heating with an electric heating device installed on the outer wall of the cylindrical reactor.The gas chromatograph was connected to the 1/8 "tube through the cyclone for comparative analysis. The gas state was analyzed.

The conversion rate of the trichlorosilane (TCS) thus obtained was about 32%, and this gas was separated into a distillation column having a diameter of 10 cm and a height of 2 m, and the recovered gas was analyzed. The trichlorosilane (TCS) was analyzed. Purity) is 98%.

Example 2

The internal temperature of the reactor was maintained at 200 ° C. using an electric heating apparatus for maintaining the reaction temperature of the cylindrical reactor under the conditions of Example 1, wherein the trichlorosilane (TCS) conversion rate was 15%.

Example 3

In the condition of Example 1, the internal temperature of the reactor was maintained at 500 ° C. using an electric heating device for maintaining the reaction temperature of the cylindrical reactor, and the conversion rate of trichlorosilane (TCS) was 45%.

Comparative Example 4

When the internal temperature of the reactor was maintained at 320 ° C. under the conditions of Example 1, and the catalyst was not used, the conversion rate of trichlorosilane (TCS) was 0.

Example 4

When the Pb-based catalyst prepared in the same manner as in Example 1 and prepared by the method of preparing a metal catalyst was used, the conversion rate of trichlorosilane (TCS) was 25%.

Example 5

When the temperature was maintained at 200 ° C. in the reactor under the same conditions as in Example 4, the conversion rate of trichlorosilane (TCS) was 10%.

Example 6

When the temperature was maintained at 500 ° C. in the reactor under the same conditions as in Example 4, the conversion rate of trichlorosilane (TCS) was 35%.

As described above, as can be seen from Examples 1 to 6 and Comparative Example 4, when the catalyst using palladium is used, the conversion rate is superior to that of the lead (Pb-based) catalyst. It can be seen that the conversion rate is better when used than when not used.

The present invention relates to a method and apparatus for producing trichlorosilane by using metal element and silicon tetrachloride as a main material and adding hydrogen using a metal catalyst, and recycling silicon tetrachloride (STC) and using a catalyst. The industrial availability is very high because it can alleviate process conditions and improve the recycling of resources and manufacturing efficiency of trichlorosilane.

1 is a device diagram for the production of trichlorosilane designed according to the present invention

2 is an enlarged view showing a distillation column in a trichlorosilane production apparatus designed according to the present invention.

<Description of the symbols for the main parts of the drawings>

One; Metal silicon feeder 2; Reactor heating device

3; Reactor support 4; Catalyst bed

5; Metal silicon layer 6; Flow meter (FMC)

7; Hydrogen source 8; Silicon Tetrachloride Tank

9; Cylindrical reactor 10; Distillation tower

11; Distillation column heating apparatus 12; Silicon Tetrachloride Storage Tank

13; Heat exchanger 14 for distillation column cooling; Heat exchanger for trichlorosilane cooling

15; Silicon tetrachloride storage tank 16; Silicon tetrachloride tank heating device

17; Internal temperature sensor 18 of silicon tetrachloride tank; Temperature sensor inside the distillation column tank

19; Silicon tetrachloride tank level gauge 20; Distillation Column Tank Level Gauge

21; Silicon tetrachloride storage tank level gauge 22; Trichlorosilane Storage Tank Level Gauge

23; Silane tetrachloride tank pressure gauge 24; Pressure gauge inside reactor

25; Distillation column internal pressure gauge 26; Distillation Column Tank Pressure Gauge

27; Silicon tetrachloride storage tank pressure gauge 28; Trichlorosilane Storage Tank Pressure Gauge

29; Hydrogen supply control valve 30; Control valve

31; Control valve (recovered metal silicon) 32; Control valve (between reactor and distillation column)

33; Distillation column upper control valve

34; Trichlorosilane Storage Tank Heat Exchanger Upper Control Valve

35; Trichlorosilane Storage Tank Heat Exchanger Bottom Control Valve

36; Silicon tetrachloride storage tank supply pump control valve (shear)

37; Silicon tetrachloride storage tank supply pump control valve (rear)

38; Heat exchanger control valve (injection) for distillation column cooling

39; Heat exchanger control valve for distillation column cooling

40; Trichlorosilane Storage Tank Heat Exchanger Control Valve (Injection)

41; Trichlorosilane Storage Tank Heat Exchanger Control Valve (Exhaust)

42; Trichlorosilane storage tank lower control valve 43; Silicon tetrachloride supply control valve (shear)

44; Silicon tetrachloride supply control valve (rear) 45; Silicon tetrachloride storage tank lower control valve

46; Supply pump (to silicon tetrachloride storage tank)

47; Supply pump (to silicon tetrachloride tank side)

48; Cyclone

Claims (9)

In the manufacturing apparatus for manufacturing trichlorosilane, A hydrogen source for supplying hydrogen to the silicon tetrachloride tank; A silicon tetrachloride tank for receiving hydrogen from the hydrogen source through a pipe and bubbling it to be injected into a cylindrical reactor; A cylindrical reactor loaded with a Pd-based or Pb-based catalyst and metal silicon to react with the injected bubbling fluid through a pipe in the silicon tetrachloride tank to generate trichlorosilane; A heating device installed outside the cylindrical reactor for heating the cylindrical reactor; And The trichlorosilane production apparatus using a Pd-based or Pb-based catalyst consisting of a distillation column having a heating device at the bottom to separate the silicon tetrachloride and trichloride silane from the cylindrical reactor using a difference in boiling point. delete The method according to claim 1, The tin chloride of the Pd-based or Pb-based catalyst is prepared by impregnating one of alumina, zeolite, silicon oxide, activated carbon, and diatomaceous earth, and charged into a cylindrical reactor. . The method according to claim 1, The cyclone for separating and recovering fine powder metal silicon from the gas passed through the cylindrical reactor is installed at the upper portion of the cylindrical reactor, The separated and recovered powdered metal silicon is recycled to the place where the metal silicon charged in the cylindrical reactor is located. Silicon tetrachloride separated and recovered using the difference in boiling point in the distillation column is a trichlorosilane production apparatus using a Pd-based or Pb-based catalyst designed to be recycled to the silicon tetrachloride tank. The method according to claim 1, The cylindrical reactor is a fixed bed reactor prepared by separating the Pd-based or Pb-based catalyst layer and the metal silicon layer, A mixed reactor produced by mixing and charging a Pd-based or Pb-based catalyst with a metal silicon, and Preparation of trichloride silane using Pd-based or Pb-based catalyst prepared by selecting one of the fluidized bed reactors designed to increase the conversion time by increasing the reaction time by configuring the Pd-based or Pb-based catalyst and the metal silicon to move inside the cylindrical reactor Device. The method according to claim 1, The reaction temperature of the cylindrical reactor is made between 150 ℃ to 500 ℃, the internal pressure of the reactor is made between 1 atm and 10 atm, the internal air pressure of the distillation column is made between 1 atm and 5 atm, the inside of the distillation column Apparatus for producing trichlorosilane using a Pd-based or Pb-based catalyst, characterized in that the temperature is made between 10 ℃ to 100 ℃. The method according to claim 1, The distillation column comprises a reboiler for maintaining heating between 50 ℃ to 58 ℃ as a heater device, a distillation column for increasing the contact time of the fluid in order to increase the purity of trichlorosilane and a condenser for condensing the fluid. Trichloride silane production apparatus using a Pd-based or Pb-based catalyst. In the production method for producing trichlorosilane, Supplying hydrogen through a pipe from a hydrogen supply source to a silicon tetrachloride tank; Receiving hydrogen through a pipe from the hydrogen supply source and bubbling hydrogen and silicon tetrachloride in a silicon tetrachloride tank and injecting the hydrogen into a cylindrical reactor through the pipe; Generating hydrogen trichloride by heat-reacting hydrogen and silicon tetrachloride injected through a pipe in a silicon tetrachloride tank with a heating apparatus in a cylindrical reactor loaded with a Pd-based or Pb-based catalyst and metal silicon; And Trichloride silane using a Pd-based or Pb-based catalyst consisting of a process for obtaining trichlorosilane by separating silicon tetrachloride and trichlorosilane contained in the gas from the cylindrical reactor from the bottom of the distillation column equipped with a heating device at the bottom using a difference in boiling point. Manufacturing method. The method according to claim 8, Cyclone for separating and recovering fine powdered metal silicon is installed on the upper portion of the cylindrical reactor through the cylindrical reactor, and recycling the powdered metal silicon separated and recovered from the cyclone to the place where the metal silicon charged in the cylindrical reactor. fair; And Method for producing trichlorosilane using a Pd-based or Pb-based catalyst further comprising the step of recycling the silicon tetrachloride separated and recovered using the difference in boiling point in the distillation column to the silicon tetrachloride tank.

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