JP5343437B2 - Hydrogen chloride gas ejection member, reactor for producing trichlorosilane, and method for producing trichlorosilane - Google Patents

Description

  The present invention is used in a reaction apparatus for producing trichlorosilane used for producing trichlorosilane by reacting metal silicon powder with hydrogen chloride gas, and hydrogen chloride gas is contained in the metal silicon powder filled in the apparatus body. The present invention relates to a hydrogen chloride gas ejection member for ejecting hydrogen, a reaction apparatus for producing trichlorosilane provided with the hydrogen chloride gas ejection member, and a method for producing trichlorosilane using the hydrogen chloride gas ejection member.

Trichlorosilane (SiHCl ₃ ), which is used as a raw material for producing extremely high purity silicon of eleven or more, is made by reacting metal silicon powder (Si) with a purity of about 98% and hydrogen chloride gas (HCl). Manufactured by.
Thus, as a reaction apparatus for producing trichlorosilane for reacting metal silicon powder and hydrogen chloride gas to produce trichlorosilane, for example, as shown in Patent Document 1, an apparatus main body filled with metal silicon powder, A device provided with gas introduction means for introducing hydrogen chloride gas into the device body from the bottom of the device body has been proposed. Here, the gas introduction means is equipped with a hydrogen chloride gas ejection member having ejection holes for ejecting hydrogen chloride gas into the metal silicon powder.

A relatively small metal silicon powder having a particle size of 1000 μm or less is filled in the apparatus main body, hydrogen chloride gas is ejected from the bottom of the apparatus body through a hydrogen chloride gas ejection member at a high speed, and the metal silicon powder is flowed. Thereby, metal silicon powder and hydrogen chloride gas are sufficiently brought into contact, and trichlorosilane is obtained by these reactions.
JP 2002-220219 A

  By the way, the conventional hydrogen chloride gas ejection member is fixed to the bottom of the apparatus body such that the ejection hole opens upward of the apparatus body. Here, the metal silicon powder has a small particle size as described above, and there is a possibility that the metal silicon powder enters the ejection hole and becomes clogged. Therefore, it is necessary to replace or clean the hydrogen chloride gas ejection member. However, since the hydrogen chloride gas ejection member is fixed to the bottom of the apparatus main body, the hydrogen chloride gas ejection member can be easily removed. I couldn't.

  The present invention has been made in view of such circumstances, and is capable of suppressing clogging caused by metal silicon powder and capable of improving the production efficiency of trichlorosilane by widely dispersing hydrogen chloride gas. It is an object of the present invention to provide a hydrogen gas ejection member, a reactor for producing trichlorosilane provided with the hydrogen chloride gas ejection member, and a method for producing trichlorosilane using the hydrogen chloride gas ejection member.

In order to solve this problem, a hydrogen chloride gas jetting member according to the present invention is used for hydrogen chloride gas jetting used in a reactor for producing trichlorosilane that reacts metal chloride with hydrogen chloride gas to produce trichlorosilane. A shaft portion extending in the longitudinal direction and a head portion extending in a direction intersecting the longitudinal direction of the shaft portion, the shaft portion being directed in the longitudinal direction The head is provided with a plurality of ejection holes that communicate with the supply hole and extend in a direction intersecting the extending direction of the supply hole and open on the outer surface of the head. The screw portion is formed in the shaft portion, and a pressure equalizing pipe communicating with the supply hole is connected .

The hydrogen chloride gas ejection member having this configuration has a shaft portion extending in the longitudinal direction and a head portion extending in a direction intersecting the longitudinal direction of the shaft portion, and is provided on the shaft portion. Since the supply hole extends in the longitudinal direction of the shaft portion and the ejection hole extending in the direction intersecting the supply hole is provided in the head, the hydrogen chloride gas ejection member is provided in the above-described reactor for producing trichlorosilane. Is attached, it becomes difficult for the metal silicon powder to enter the ejection holes, and clogging of the ejection holes can be prevented.
Further, since a plurality of ejection holes are formed, hydrogen chloride gas can be ejected in a plurality of directions, and the reaction can be promoted by widely dispersing the hydrogen chloride gas in the metal silicon powder. .

Moreover, since the threaded portion before Kijiku portion is formed, it will be mounted detachably on the gas introduction means of the aforementioned producing trichlorosilane for reaction, even when it is degraded by using for a long time, easily Can be replaced. Further, even if the ejection hole is clogged, it can be removed and cleaned, so that maintenance is very easy. Moreover, it can be easily attached and detached by rotating the hydrogen chloride gas ejection member, and the maintenance can be further improved. In addition, it is preferable to make the head of the hydrogen chloride gas ejection member a shape that can lock a working tool such as a spanner.
Moreover, since the pressure equalizing pipe connected to the supply hole is connected, the pressure of the hydrogen chloride gas ejected from the ejection hole can be made uniform.

The hydrogen chloride gas ejection member of the present invention is characterized in that a plurality of the ejection holes are formed to extend radially from the supply holes.
In the hydrogen chloride gas ejection member having this configuration, the hydrogen chloride gas supplied through the supply holes is ejected radially from the plurality of ejection holes, and the hydrogen chloride gas is dispersed more widely in the metal silicon powder. Can do.

A reactor for producing trichlorosilane according to the present invention is a reactor for producing trichlorosilane, which produces trichlorosilane by reacting metal silicon powder with hydrogen chloride gas,
An apparatus main body to which the metal silicon powder is supplied; and a gas introducing means for introducing the hydrogen chloride gas into the apparatus main body from the bottom side of the apparatus main body, the gas introducing means comprising the hydrogen chloride gas The ejection member is detachably mounted through the bottom plate portion of the apparatus main body, and the head is disposed on the bottom plate portion.
In the reactor for producing trichlorosilane having this configuration, the hydrogen chloride gas ejection member can be prevented from being clogged, so that stable operation can be performed. Moreover, the production efficiency of trichlorosilane can be significantly improved by widely dispersing hydrogen chloride gas in the metal silicon powder.

The method for producing trichlorosilane according to the present invention is a method for producing trichlorosilane by reacting metal silicon powder and hydrogen chloride gas to produce trichlorosilane, the bottom plate portion of the apparatus body to which the silicon powder is supplied. in the wearing the hydrogen chloride gas jetting member, the head should be placed in the top of the bottom plate portion, while supplying the metal silicon powder in the lower portion of the apparatus main body, the hydrogen chrolide gas ejecting nozzle The hydrogen chloride gas is ejected from the ejection holes.

  ADVANTAGE OF THE INVENTION According to this invention, while being able to suppress clogging by metal silicon powder, the hydrogen chloride gas ejection member which can improve the production efficiency of trichlorosilane by widely dispersing hydrogen chloride gas, and this hydrogen chloride gas ejection A reactor for producing trichlorosilane provided with a member can be provided.

Embodiments of the present invention will be described below with reference to the accompanying drawings.
As shown in FIGS. 1 and 2, the hydrogen chloride gas ejection member 1 according to the present embodiment includes a shaft portion 2 having a substantially cylindrical shape, and a longitudinal direction of the shaft portion 2 at the upper end of the shaft portion 2 (FIG. 1). And a head 3 extending in a direction crossing the vertical direction).

In the present embodiment, the head portion 3 extends in a direction orthogonal to the longitudinal direction of the shaft portion 2, and has a regular hexagonal shape as viewed from above as shown in FIG. The upper surface 3A of the head 3 is a plane orthogonal to the longitudinal direction of the shaft portion 2, and the side surface 3B of the head 3 is configured to be orthogonal to the upper surface 3A and has a substantially regular hexagonal column shape.
Further, the shaft portion 2 is formed with a male screw on the outer peripheral surface thereof. As described above, the hydrogen chloride gas ejection member 1 has the same shape as a so-called hexagon bolt, and is configured such that a work tool such as a spanner can be engaged with the head 3.

The shaft portion 2 is provided with a supply hole 4 that opens in the lower end surface 2 </ b> B and extends along the longitudinal direction of the shaft portion 2. The supply hole 4 is not opened on the upper surface 3A of the head 3 and is a so-called blind hole.
The head 3 is formed with a plurality of ejection holes 5 communicating with the supply holes 4 and extending in a direction intersecting with the extending direction of the supply holes 4. In the present embodiment, as shown in FIGS. 1 and 2, the six ejection holes 5 are formed so as to be orthogonal to the extending direction of the supply holes 4. As shown in FIG. 2, these six ejection holes 5 are formed so as to extend radially from the supply hole 4 located at the center of the head 3, and are respectively opened on the side surfaces of the head 3 having a regular hexagonal column shape. doing. That is, the opening of the ejection hole 5 is oriented in a direction orthogonal to the longitudinal direction of the shaft portion 2.

Next, a reactor 10 for producing trichlorosilane in which the hydrogen chloride gas ejection member 1 according to this embodiment is used will be described.
As shown in FIG. 3, the reaction apparatus 10 for producing trichlorosilane includes an apparatus main body 11 having a barrel portion 12, a bottom plate portion 13, and a top plate portion 14 that form a substantially cylindrical shape. Here, as shown in FIGS. 3 and 4, the upper surface 13 </ b> A and the lower surface 13 </ b> B of the bottom plate portion 13 are arranged so as to be orthogonal to the axis of the cylinder formed by the body portion 12.

A silicon powder supply port 15 for supplying metal silicon powder into the apparatus main body 11 is formed in the lower part of the body 12 of the apparatus main body 11. A carrier gas introduction pipe 30 is connected to the silicon powder supply port, and metal silicon powder is supplied from the feed hopper 31 to the carrier gas introduction pipe 30, and the inside of the apparatus main body 11 is passed through the silicon powder supply port 15. To be supplied. The feed hopper 31 is connected with a cyclone 33 described later, and a silicon powder supply system 40 for supplying metal silicon powder from the outside.
Further, the top plate portion 14 of the apparatus main body 11 is provided with a gas outlet 17 for taking out the gas of trichlorosilane generated by the reaction to the outside.

A gas introduction means 20 for introducing hydrogen chloride gas into the apparatus main body 11 is provided below the apparatus main body 11.
The gas introduction means 20 includes a gas chamber 21 in which hydrogen chloride gas is stored, and a gas supply port 22 that supplies the hydrogen chloride gas into the gas chamber 21. Here, the gas chamber 21 is partitioned from the inside of the apparatus main body 11 by the bottom plate portion 13 of the apparatus main body 11.

And as shown in FIG. 4, the member 1 for hydrogen chloride gas ejection which is this embodiment is arrange | positioned at the baseplate part 13 of the apparatus main body 11. As shown in FIG. More specifically, a mounting hole 13C is provided in the bottom plate portion 13 of the apparatus main body 11, and the shaft portion 2 of the hydrogen chloride gas jetting member 1 is inserted into the mounting hole 13C, and the head of the hydrogen chloride gas jetting member 1 is inserted. 3 is disposed on the upper surface 13A of the bottom plate portion 13. A nut 25 is screwed into a male screw portion 2A formed on the shaft portion 2 from the lower surface 13B side of the bottom plate portion 13 and is fixed by sandwiching the bottom plate portion 13 between the nut 25 and the head portion 3. In addition, washers 26 are interposed between the head 3 and the upper surface 13A of the bottom plate portion 13 and between the nut 25 and the lower surface 13B of the bottom plate portion 13, respectively.
As a result, the shaft portion 2 of the hydrogen chloride gas ejection member 1 passes through the bottom plate portion 13 and is inserted into the gas chamber 21 and is detachably attached to the bottom plate portion 13. A pressure equalizing pipe 27 communicating with the supply hole 4 is connected to the shaft portion 2 of the hydrogen chloride gas ejection member 1.

  As described above, the hydrogen chloride gas ejection member 1 according to the present embodiment is fixed to the bottom plate portion 13 of the apparatus main body 11, and the shaft portion 2 faces downward from the bottom plate portion 13 (the trunk portion 12 of the apparatus main body 11). The upper surface 3A of the head 3 is disposed so as to be parallel to the upper surface 13A and the lower surface 13B of the bottom plate portion 13 of the apparatus main body 11. The lower end of the supply hole 4 of the shaft portion 2 is opened into the gas chamber 21, while the ejection hole 5 of the head portion 3 is orthogonal to the axis of the cylinder formed by the body portion 12 of the apparatus body 11. It arrange | positions so that it may open in a direction. The hydrogen chloride gas supplied from the gas supply port 22 into the gas chamber 21 is ejected from the ejection hole 5 into the apparatus main body 11 via the supply hole 4 of the hydrogen chloride gas ejection member 1. These gas supply port 22, gas chamber 21, and hydrogen chloride gas ejection member 1 constitute gas introduction means 20.

  In the present embodiment, as shown in FIG. 5, the plurality of hydrogen chloride ejection nozzles 1 are arranged in a staggered pattern over the entire upper surface 13 </ b> A of the bottom plate portion 13.

Next, the manufacturing method of trichlorosilane by the reactor 10 for manufacturing trichlorosilane configured as described above will be described.
The metal silicon powder is supplied from the silicon powder supply system 40 to the feed hopper 31 and is introduced from the feed hopper 31 through the valve 32 into the carrier gas introduction pipe 30, and the apparatus main body through the silicon powder supply port 15 by airflow transfer. 11 is supplied to the inside. At this time, hydrogen chloride gas is used as a carrier gas for air flow transfer. The carrier gas is introduced at a constant pressure.

  Further, hydrogen chloride gas is introduced into the apparatus main body 11 by the gas introduction means 20. The hydrogen chloride gas is ejected into the apparatus main body 11 through a plurality of hydrogen chloride gas ejection members 1 arranged on the bottom plate portion 13 of the apparatus main body 11. The hydrogen chloride gas ejected from the hydrogen chloride gas ejection member 1 is introduced into the metal silicon powder.

  Thus, hydrogen chloride gas is ejected to the metal silicon powder in the apparatus main body 11, whereby the metal silicon powder flows in the apparatus main body 11. When the metal silicon powder flows and comes into contact with the hydrogen chloride gas, the metal silicon powder and the hydrogen chloride gas react at a predetermined temperature to generate a trichlorosilane gas.

  The generated trichlorosilane gas is taken out from a gas outlet 17 provided in the top plate portion 14 of the apparatus main body 11 and supplied to a subsequent process. Further, the unreacted metal silicon powder in the apparatus main body 11 is discharged from the gas outlet 17 together with the trichlorosilane gas, recovered by the cyclone 33 in the subsequent process, and supplied to the feed hopper 31 to be introduced into the carrier gas introduction pipe. 30 is introduced into the apparatus main body 11 again. Metallic silicon powder that has not been recovered by the cyclone 33 is removed by a filter 34 in a subsequent process.

  The hydrogen chloride gas ejection member 1 according to this embodiment includes a shaft portion 2 having a substantially cylindrical shape, and a head portion 3 extending in a direction intersecting the longitudinal direction of the shaft portion 2 (vertical direction in FIG. 1). The shaft portion 2 is arranged so as to extend in the vertical direction of the apparatus main body 11, and the supply hole 4 provided in the shaft portion 2 is also arranged in the vertical direction of the apparatus main body 11 The cylinder 12 is arranged so as to face the axial direction of the cylinder formed by the portion 12. And since the opening part of the ejection hole 5 orthogonal to this supply hole 4 is opened by the side surface of the head 3, the opening part of the ejection hole 5 does not face the upper direction of the apparatus main body 11. FIG. Therefore, it becomes difficult for metal silicon powder to enter the ejection holes 5, and clogging of the ejection holes 5 can be prevented.

  Since the plurality of ejection holes 5 are formed so as to extend radially from the supply hole 4, hydrogen chloride gas can be ejected from a single hydrogen chloride gas ejection member 1 in a plurality of directions. Can be widely dispersed in the metal silicon powder to promote the reaction. Thereby, the reaction between the metal silicon powder and hydrogen chloride gas can be further promoted to improve the production efficiency of trichlorosilane.

  Further, since the hydrogen chloride gas ejection member 1 is detachably attached to the bottom plate portion 13 of the apparatus main body 11, it can be easily replaced even if it deteriorates after being used for a long time. Further, even if the ejection hole 5 is clogged, it can be cleaned in a state where it is removed from the bottom plate portion 13 of the apparatus main body 11, so that maintenance is very easy. Furthermore, since the head 3 of the hydrogen chloride gas ejection member 1 has a regular hexagonal column shape, the work tool such as a spanner can be locked and rotated to be easily attached and detached.

Moreover, since the hydrogen chloride gas ejection member 1 according to this embodiment has the same shape as a so-called hexagon bolt, the hydrogen chloride gas ejection member 1 is manufactured by drilling a general-purpose hexagon bolt. The manufacturing cost of the hydrogen chloride gas ejection member 1 can be reduced.
Furthermore, in this embodiment, since the pressure equalizing pipe 27 communicating with the supply hole 4 is connected to the shaft portion 2 of the hydrogen chloride gas ejection member 1, the pressure of the hydrogen chloride gas ejected from the ejection hole 5 is reduced. It can be made uniform.

The hydrogen chloride gas ejection member according to the embodiment of the present invention has been described above. However, the present invention is not limited to this, and can be appropriately changed without departing from the technical idea of the present invention.
For example, in the present embodiment, the description has been given of the case where the ejection hole is formed so as to be orthogonal to the extending direction of the supply hole. Therefore, it is only necessary to cross the supply hole so that the opening does not face above the apparatus main body.

  Moreover, although demonstrated as what formed the hexagon bolt shape and the six ejection holes, there is no limitation in the number of ejection holes. It is preferable to design appropriately considering the arrangement of the hydrogen chloride gas ejection member and the shape of the apparatus main body.

6 to 11 show modifications of the hydrogen chloride gas ejection member. In any of the modifications, the shape of the head is different from that of the embodiment, and the shaft portion is the same as that of the embodiment. In addition, the same code | symbol is attached | subjected also to the supply hole and ejection hole which are common in the thing of one Embodiment. The hydrogen chloride gas ejection member 51 shown in FIGS. 6 and 7 has a head 52 formed in a square shape in plan view, an upper surface 52A formed in a plane orthogonal to the length direction, and orthogonal to the supply hole 4. The four ejection holes 5 are opened on the side surfaces 52B of the head 52, respectively. The hydrogen chloride gas ejection member 53 shown in FIGS. 8 and 9 has a shape in which the head 54 is formed by cutting both sides of a circle in parallel in plan view, so that the upper surface 54A is in the length direction. Are formed in a plane perpendicular to the surface, but each side surface is formed with a pair of arcuate side surfaces 54B and planar side surfaces 54C. Further, the four ejection holes 5 orthogonal to the supply hole 4 are respectively opened on the arc-shaped side surface 54 </ b> B of the head 54. Further, the hydrogen chloride gas ejection member 55 shown in FIGS. 10 and 11 has a shape in which a head portion 56 is formed in a hemispherical shape and parts of both side portions thereof are cut out in parallel with each other. Therefore, the upper surface 56A of the head 56 is formed in a hemispherical surface, and a pair of planar side surfaces 56B are formed in parallel to the length direction. And the four ejection holes 5 which cross | intersect diagonally with respect to the supply hole 4 are opened to the hemispherical upper surface 56A diagonally upward.
Each of the hydrogen chloride gas ejection members has a planar portion at its head (each side surface 52B in FIGS. 6 and 7, planar side surface 54C in FIGS. 8 and 9, and planar side surface 56B in FIGS. 10 and 11). By attaching a tool such as a spanner and rotating the hydrogen chloride gas ejection member, it can be attached to and detached from the bottom plate portion.
In addition to these shapes, the shape of the head of the hydrogen chloride gas ejection member may be a triangle or the like in plan view, as long as a plane on which the tool can be locked is formed on the side surface.

It is a side view of the member for hydrogen chloride gas ejection which is an embodiment of the present invention. It is a top view of the member for hydrogen chloride gas ejection shown in FIG. It is a schematic explanatory drawing of the reaction apparatus for trichlorosilane manufacture in which the member for hydrogen chloride gas ejection shown in FIG. 1 is used. It is explanatory drawing which shows the state with which the hydrogen chloride gas ejection member shown in FIG. 1 was mounted | worn with the gas introduction means. It is explanatory drawing which shows the several member for hydrogen chloride gas ejection arranged in the baseplate part of an apparatus main body. It is a side view of the 1st modification of the member for hydrogen chloride gas ejection. It is a top view of the member for hydrogen chloride gas ejection shown in FIG. It is a side view of the 2nd modification of the member for hydrogen chloride gas ejection. It is a top view of the member for hydrogen chloride gas ejection shown in FIG. It is a side view of the 3rd modification of the member for hydrogen chloride gas ejection. It is a top view of the member for hydrogen chloride gas ejection shown in FIG.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Hydrogen chloride gas ejection member 2 Shaft part 2A Male thread part (engagement part)
3 Head 4 Supply hole 5 Ejection hole 10 Reactor 11 for producing trichlorosilane Device body 13 Bottom 20 Gas introduction means 51, 53, 55 Hydrogen chloride gas ejection member 52, 54, 56 Head

Claims (4)

A hydrogen chloride gas jetting member used in a reactor for producing trichlorosilane that reacts metal chloride powder with hydrogen chloride gas to produce trichlorosilane,
A shaft portion extending in the longitudinal direction and a head portion extending in a direction intersecting the longitudinal direction of the shaft portion;
The shaft portion is provided with a supply hole extending in the longitudinal direction, and the head portion communicates with the supply hole and extends in a direction intersecting the extending direction of the supply hole. A hydrogen chloride gas jetting member , wherein a plurality of jetting holes are formed on the outer surface of the part, a screw part is formed in the shaft part, and a pressure equalizing pipe communicating with the supply hole is connected . In the hydrogen chloride gas ejection member according to claim 1 ,
A member for ejecting hydrogen chloride gas, wherein the plurality of ejection holes are formed to extend radially from the supply holes. A reactor for producing trichlorosilane that reacts metal silicon powder with hydrogen chloride gas to produce trichlorosilane,
An apparatus main body to which the metal silicon powder is supplied, and gas introduction means for introducing the hydrogen chloride gas into the apparatus main body from the bottom side of the apparatus main body,
In this gas introducing means, the hydrogen chloride gas ejection member according to claim 1 or 2 is detachably mounted through the bottom plate portion of the apparatus main body, and the head is disposed on the bottom plate portion. A reactor for producing trichlorosilane, which is characterized in that A method for producing trichlorosilane by reacting metal silicon powder with hydrogen chloride gas to produce trichlorosilane,
The hydrogen chloride gas ejection member according to claim 1 or 2 is attached to a bottom plate portion of an apparatus main body to which the silicon powder is supplied, and the head is disposed on the bottom plate portion. A method for producing trichlorosilane, characterized in that hydrogen chloride gas is ejected from the ejection holes of the hydrogen chloride gas ejection member while supplying metallic silicon powder to the lower part of the apparatus body.

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