Apparatus and method for catalytic distillation

Abstract

A method and apparatus for catalytic distillation is disclosed. Embodiments may include a catalytic distiller including a pressure vessel; a reactive distillation device positioned in the pressure vessel including a distillation device and a fixed bed catalyst device positioned above the distillation device, wherein the fixed bed catalyst device includes a fixed bed catalyst component and a vapor riser; and flood prevention system to collect and direct a liquid from the fixed bed catalyst component through a fixed bed bypass pipe to the distillation device, wherein the fixed bed bypass pipe, which is connected to the pressure vessel, is positioned outside of the pressure vessel.

Description

APPARATUS AND METHOD FOR CATALYTIC DISTILLATION CROSSREFRENCE TO RELATED APPLICATIONSThe present application claims priority from US Patent Application No. 63 / 677,288, filed July 30, 2024, the entire contents of which is incorporated herein for all purposes by this reference.TECHNICAL FIELD

[0001] The various embodiments of the present invention relate to an apparatus and method for catalytic distillation. More specifically, the various embodiments of the present invention described in the present disclosure relate to a new method and apparatus to process trichlorosilane (TCS) to produce two co-products silane (SiH4) and silicon tetrachloride (STC).BACKGROUND

[0002] It is well known that silane (SiH4) is a very useful chemical for the production of electronic devices based on high purity crystalline silicon. Silane may be further processed to produce pure silicon or may be used in various processes to deposit silicon upon other materials such as carbon.

[0003] One example of many examples of the use of silane in the production of electronic devices is the production of Li-ion batteries as disclosed in US Patent 11,515,528. As discussed in US Patent Application Publication No. 2013 / 0156675 metallurgical grade silicon may be gasified by a reaction of hydrogen and silicon tetrachloride to form a mixture containing trichlorosilane (TCS), which is converted into a series of distillation separations and catalytic distribution reactions (reactive distillation zones) to produce silane, and which also produces silicon tetrachloride (STC) as a co-product.

[0004] However, during the processing of trichlorosilane (TCS) using prior art methods and apparatuses, there are operational problems with providing liquid chemical components to a fixed bed catalyst in a reaction zone. For example, US Patent 5,368,691 discloses a reactive distillation column for preforming both chemical reactions and separations by distillation of the mixtures obtained during the reaction. In this prior art, there is a problem in that the catalyst becomes compressed over time, which limits liquid flow through the catalyst. Liquid continues to accumulate on top of the reaction cells, which reduces flow of liquids and causes flooding of the column.

[0005] Accordingly, there is a need for a new apparatus and method to process trichlorosilane (TCS) to produce two co-products silane (SiH4) and silicon tetrachloride(STC), which includes efficiently delivering (supplying) liquid chemical components to a fixed bed catalyst device of a reactive distillation device positioned in columns to prevent flooding caused by the fixed bed catalyst device.SUMMARY

[0006] Various embodiments of the present disclosure provide a new apparatus and method for processing trichlorosilane (TCS) to produce two co-products silane (SiJU) and silicon tetrachloride (STC), which includes efficiently delivering (supplying) liquid chemical components to reactive distillation devices in columns to prevent flooding of the fixed bed catalyst devices of the reactive distillation devices.

[0007] According to one or more embodiments, there is provided a catalytic distiller which may comprise a pressure vessel; a reactive distillation device positioned in the pressure vessel including a distillation device and a fixed bed catalyst device positioned above the distillation device, wherein the fixed bed catalyst device includes a fixed bed catalyst component and a vapor riser; and a flood prevention system to collect and direct a liquid from the fixed bed catalyst component through fixed bed bypass pipe to the distillation device, wherein the fixed bed bypass pipe, which is connected to the pressure vessel, is positioned outside of the pressure vessel.

[0008] In one or more embodiments, the fixed bed catalyst device may further include an additional fixed bed catalyst component, the flood prevention system collects and directs the liquid from the additional fixed bed catalyst component through an additional fixed bed bypass pipe to the distillation device, and the additional fixed bed bypass pipe, which is connected to the pressure vessel, is positioned outside of the pressure vessel.

[0009] In one or more embodiments, the fixed bed catalyst component may include a fixed bed catalyst.

[0010] In one or more embodiments, the fixed bed catalyst may include catalyst particles having a diameter equal to or greater than about 0.8mm.

[0011] In one or more embodiments, the fixed bed catalyst component includes a fixed bed catalyst, and the additional fixed bed catalyst component includes an additional fixed bed catalyst.

[0012] In one or more embodiments, the fixed bed catalyst comprises catalyst particles having a diameter equal to or greater than about 0.8 mm, and the additional fixed bed catalyst comprises the catalyst particles having a diameter equal to or greater than about 0.8 mm.

[0013] In one or more embodiments, a catalytic distiller may further include a flush system, using a flushing liquid, to independently flush the fixed bed catalyst component and the additional fixed bed catalyst component.

[0014] In one or more embodiments, the catalytic distiller may further include a fixed bed catalyst sealing pan configured to collect liquid traversing the fixed bed catalyst, wherein the liquid enters a top of the fixed bed catalyst device and flows downward through the fixed bed catalyst device; a distillation device supply nozzle configured to deliver the collected liquid to the distillation device; and a fixed bed catalyst component pipe connected to the fixed bed catalyst sealing pan and the distillation device supply nozzle.

[0015] In one or more embodiments, the flood prevention system may include the fixed bed bypass pipe and may further include a bypass nozzle located above the fixed bed catalyst device and connected to the fixed bed bypass pipe; and a bypass return nozzle configured to deliver overflow liquid to the distillation device.BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Advantages and teachings of the present invention will become apparent to those skilled in the art with the benefit of the following detailed description of embodiments and upon reference to the accompanying drawings, in which:FIG. l is a diagram illustrating a catalytic distiller for processing trichlorosilane (TCS) to produce two co-products silane (SiH4) and silicon tetrachloride (STC);FIG. 2 is a diagram illustrating a reactive distillation device of a catalytic distiller according to an embodiment;FIG. 3 is a diagram illustrating a reactive distillation device of a catalytic distiller according to another embodiment;FIG. 4 is a diagram illustrating a reactive distillation device of a catalytic distiller according to another embodiment;FIG. 5 is a diagram illustrating a reactive distillation device of a catalytic distiller according to another embodiment; andFIG. 6 is a flowchart illustrating a method for flushing a fixed bed catalyst of a fixed bed catalyst device according to an embodiment.

[0017] While embodiments of the present disclosure may be susceptible to various modifications and alternative forms, specific embodiments thereof are shown by way of example in the drawings and will be described in the present disclosure in detail. The drawings may not be to scale. It should be understood, however, that the drawings anddetailed description thereto are not intended to limit the present invention to the particular form disclosed, but to the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the present invention as defined by the claims.DETAILED DESCRIPTION

[0018] Reference will now be made in detail to embodiments of the present disclosure, examples of which are illustrated in the accompanying drawings. It is noted that wherever practicable, similar or like reference numbers may be used in the drawings and may indicate similar or like elements.

[0019] The drawings depict embodiments of the present disclosure for purposes of illustration only. One skilled in the art would readily recognize from the following description that alternative embodiments exist without departing from the general principles of the disclosure.

[0020] Throughout the specification, the terms approach(es), technique(s), technology(ies), and method(s) are used interchangeably and have the same meaning.

[0021] Throughout the specification, the terms gas and vapor are used interchangeably.

[0022] Throughout the specification, the term gas may be one or more gases and the term vapor may be one or more vapors.

[0023] Throughout the specification the terms reactive distillation device, reactive distillation section, and reactive distillation zone may be used interchangeably.

[0024] Throughout the specification, the terms distillation section, distillation device, separation section, distillation zone, and mass transfer device may be used interchangeably.

[0025] Throughout the specification, the terms distillation trays or distillation packing may be referred to as distillation components.

[0026] Throughout the specification, the terms reaction section, reaction device, reaction zone, catalyst zone, fixed bed catalyst section, and fixed bed catalyst device may be used interchangeably.

[0027] Throughout the specification, the terms bed, catalyst bed, and fixed catalyst bed may be referred to interchangeably.

[0028] Throughout the specification, the terms vapor riser, gas riser, vapor channel, and gas channel may be used interchangeably.

[0029] The present disclosure relates to an apparatus and method for catalytic distillation. More specifically, the various embodiments of the present invention described in the present disclosure relate to a new method and apparatus to process trichlorosilane (TCS) to producetwo co-products silane (SiFL) and silicon tetrachloride (STC). Silane may be further processed to produce pure silicon or be used in various processes to deposit silicon upon other materials such as carbon. Silane and / or pure silicon are widely used to manufacture a wide variety of components including LCD displays, Li-ion batteries, semiconductor wafers, etc.

[0030] FIG. 1 is a diagram illustrating an apparatus for processing trichlorosilane (TCS) to produce two co-products silane (SiFL) and silicon tetrachloride (STC) according to an embodiment. The trichlorosilane (TCS) may be continuously supplied until the desired quantities of silane and / or silicon tetrachloride are produced (manufactured). The apparatus of Figure 1 may be referred to as a catalytic distiller 100. The catalytic distiller 100 includes a bottom distillation column 200 and a top distillation column 300, which are coupled through pipes.

[0031] The bottom distillation column 200 is configured to separate components generated in the reactive sections of the column. The bottom distillation column 200 includes a bottom pressure vessel 202, which may also be referred to as a bottom containment vessel. The temperature at the bottom of the bottom pressure vessel 202 may be about 130°C, and the temperature at the top of the bottom pressure vessel 202 may be about 45°CThe top distillation column 300 includes a top pressure vessel 302, which may also be referred to as a top containment vessel. The top pressure vessel 302 includes a top distillation device 304 positioned inside of the top pressure vessel 302. The temperature at the bottom of the top pressure vessel 302 may be about 45°C and the temperature at the top of the top pressure vessel 302 may be about -20°C to -80°C.

[0032] As indicated in Figure 1, trichlorosilane (TCS) is introduced as a liquid into the bottom distillation column 200 of the catalytic distiller 100 through a trichlorosilane (TCS) pipe 205. Co-products of reactions in the catalytic distiller 100 are silicon tetrachloride (STC) and silane (SiH4). Silane is output from the top of the top distillation column 300 as a silane gas (vapor). Silicon tetrachloride (STC) is output from the bottom of the bottom distillation column 200 as STC liquid through an STC reboiler system, which may include an STC input reboiler pipe 214, an STC output pipe 216, an STC reboiler 220, and an STC output reboiler pipe 222. The STC input reboiler pipe 214 provides STC to the STC reboiler 220, which heats the STC to recycle the STC for use in the bottom distillation column 200. The STC reboiler 220 heats the STC to convert (transform) the liquid STC to the STC gas. The STC output reboiler pipe 222 provides the gas STC to the bottom pressure vessel 202 (bottom containment vessel) of the bottom distillation column 200 as shown in Figure 1 for example.

[0033] The bottom distillation column 200 of the catalytic distiller 100 includes bottom distillation devices (bottom distillation sections), which are separation sections or mass transfer devices (bottom separation sections or bottom mass transfer devices). As discussed above, the top distillation column 300 also includes a top distillation device 304 (top distillation section), which is also a separation section or mass transfer device (top separation section or top mass transfer device). The top distillation device 304 is positioned in the top pressure vessel 302. The bottom distillation devices and the top distillation device 304 may have the same structure. For example, the distillation devices and the top distillation device 304 may include one or more distillation trays or distillation packing (separation packing). The distillation trays or distillation packing may be referred to as distillation components.

[0034] The bottom distillation column 100 further includes reaction sections, which may also be referred to as fixed bed catalyst sections, reaction devices, or fixed bed catalyst devices. A fixed bed catalyst device may include a single fixed bed catalyst component or two or more fixed bed catalyst components and a vapor (riser). In embodiments, a fixed bed catalyst component may include a container (vessel) with an open screen on the top and bottom of the container. The fixed bed catalyst component further includes a bed, which may be positioned within the container above the bottom screen of the container. Abed may also be referred to as a catalyst bed because the bed or catalyst bed comprises a catalyst. According to an embodiment of the present invention, the catalyst bed includes catalyst particles. For example, the catalyst particles may be composed of ion exchange resin for performing redistribution of chlorosilanes. The diameter of the catalyst particles may be equal to or greater than about 0.8mm. Preferably, the diameter of the catalyst particles may be in a range from about 0.8 mm to about 1.5mm. If the diameter of the catalyst particles is smaller than 0.7mm flow issues may occur. The bottom screen may be a Johnson screen, which supports a catalyst bed above the bottom of the fixed bed catalyst component. The fixed bed catalyst component further includes a sealing pan and a nozzle, which will be discussed in greater detail with respect to Figures 2-5. A fixed bed catalyst device introduces a catalyst to generate reactions that will eventually produce silane (SiFU). The vapor (gas) riser of the fixed bed catalyst device allows the vapor (gas) to rise through the catalyst bed without contacting the catalyst.

[0035] When the liquid trichlorosilane (TCS) reacts with catalysts of the fixed bed catalyst devices, five additional chemical components may be produced including: silane (SiFLj); trichlorosilane (TCS or SiChH); dichlorosilane (DCS or SiChFh); monochlorosilane (MCS or SiCliHs); and silicon tetrachloride STC (SiCh). These reactions that take place in the fixedbed catalyst devices are chlorosilane disproportionation reactions. The catalyst of the fixed bed catalyst devices increases the reaction kinetics so that the reactions lead to the production of silane.

[0036] When liquid including chemical components comes into contact with the catalyst, there is a chemical reaction involving the chemical components. Each distillation device separates the chemical components after the chemical reaction so that the heavier chemical components move in a downward direction toward the bottom of the bottom distillation column 200 and the lighter chemical components rise in an upward direction toward the top of the bottom distillation column 200. Silicon tetrachloride STC (SiCh) is heavier than trichlorosilane (TCS or SiChH), which is heavier than dichlorosilane (DCS or SiChEh), which is heavier than monochlorosilane (MCS or SiCliHi). Silane (SiEU) is the lightest of the five chemical components.

[0037] The bottom distillation devices include an STC distillation device 230, which is positioned below the TCS pipe 205. The STC distillation device 230 separates STC from other chemical components including trichlorosilane (TCS or SiChH); dichlorosilane (DCS or SiChH2); monochlorosilane (MCS or SiChH?). As discussed above, the separated liquid STC is output to the STC reboiler system, which may include the STC input reboiler pipe 214, the STC output pipe 216, the STC reboiler 220, and the STC output reboiler pipe 222.

[0038] The top of the bottom pressure vessel 202 outputs five chemical components as a gas (vapor) including: silane (SiH4); trichlorosilane (TCS or SiChH); dichlorosilane (DCS or SiChH2); monochlorosilane (MCS or SiChHs); and silicon tetrachloride STC (SiCh). The gas output at the top of the bottom pressure vessel 202 is a mixture of five chemical component gases with the quantity of STC in the gas (STC gas) being a small quantity in a range of <1%. The top of the bottom pressure vessel 202 outputs five chemical components as a gas into an intermediate condenser input pipe 312, which guides the gas to an intermediate condenser 314. The intermediate condenser 314 condenses most of the heavier trichlorosilane, dichlorosilane, and silicon tetrachloride into liquid form, and outputs this liquid to the bottom pressure vessel 202 for further processing by way of an intermediate condenser output pipe system. This liquid may be referred to as a bottom distillation column reflux. However, the intermediate condenser 314 does not fully condense the lighter gases of monochlorosilane and silane. The monochlorosilane and silane are output from the intermediate condenser 314 to a top pressure vessel 302 of the top distillation column 304 by way of the intermediate condenser output pipe system. The intermediate condenser output pipe system may include an intermediate condenser main output pipe 316, a first intermediatecondenser output pipe 318, and a second intermediate condenser output pipe 320. The intermediate condenser main output pipe 316 guides both the gas and liquid output from the intermediate condenser 314. The intermediate condenser main output pipe 316 is coupled to a first intermediate condenser output pipe 318 for guiding the gas to the top pressure vessel 302 and coupled to a second intermediate condenser output pipe 320 for guiding liquid reflux to the bottom column pressure vessel 202 as shown in Figure 1.

[0039] As discussed above, the top distillation column 300 includes a top column distillation device 304 in the top pressure vessel 302. The top column distillation device 304 separates monochlorosilane from silane. The top column distillation device 304 also separates any remaining trichlorosilane, dichlorosilane, and silicon tetrachloride. The top pressure vessel 302 outputs the monochlorosilane, di chlorosilane, trichlorosilane, and silicon tetrachloride in liquid form to the bottom pressure vessel 202 by way of a top pressure vessel output pipe 306 for further processing by the bottom distillation column 202. The top pressure vessel 302 also outputs silane gas (vapor) to a silane condenser 330. A silane condenser 330 is coupled to the top pressure vessel 302 by way of a condenser input pipe 335. The silane condenser 330 outputs silane by way of a silane output pipe 340, and outputs a silane reflux, which was silane condensed into a liquid by the condenser 330, through a silane reflux pipe 350 to the top pressure vessel 302. This silane reflux will be output through the top pressure vessel output pipe 306 for further processing by the bottom distillation column 200.

[0040] The reaction devices and the bottom distillation devices of the bottom distillation column 200 of the catalytic distiller 100 are now discussed in greater detail below. As discussed above, the bottom distillation column 200 of the catalytic distiller 100 includes bottom distillation devices (distillation sections), which are separation sections or mass transfer devices (bottom separation sections or bottom mass transfer devices) configured to separate chemical components. As discussed above, a rection device may also be referred to as a fixed bed catalyst device. A fixed bed catalyst device may include one or more fixed bed catalyst components and a vapor (riser). A vapor riser may also be referred to as a gas riser, a vapor channel, or a gas channel. The fixed bed catalyst device may introduce a catalyst to chemical components to increase the speed of reactions among chemical components.

[0041] In addition, as illustrated in Figure 1, vapor (gas) rises within the bottom pressure vessel 202 of the bottom distillation column 200 of the catalytic distiller 100 through vapor (gas) risers between the fixed bed catalyst devices, and the vapor (gas) rises within the bottom pressure vessel 202 of the bottom distillation column 200 through distillation devicesto separate chemical components. The separated liquid containing components falling downward through the bottom pressure vessel 202 and the vapor (gas) rising upward through the bottom pressure vessel 202 are contacted with a catalyst in the fixed bed catalyst devices to promote more chemical reactions so that chlorine so that silane (SiH4) is generated.

[0042] As shown in the bottom pressure vessel 202 of Figure 1, each reaction device (reaction section, fixed bed catalyst device, or fixed bed catalyst section) has a corresponding bottom distillation device (separation section) positioned below the reaction device. The combination of a bottom distillation device and a reaction device may be referred to as a reactive distillation device or reactive distillation section. In the embodiment shown in Figure 1, an upper reactive distillation device 400 includes an upper bottom distillation device 410 and an upper fixed bed catalyst device 420. A middle reactive distillation device 500 includes a middle bottom distillation device 510 and a middle fixed bed catalyst device 520. A lower reactive distillation device 700 includes a lower bottom distillation device 710 and a lower fixed bed catalyst device 720. In order to produce silane, at least two reactive distillation devices are required. However, three reactive distillation devices as shown in Figure 1 are preferable, because the energy consumption of three reactive distillation devices is lower than two reactive distillation devices. Alternatively, more than three distillation devices may be used to produce silane.

[0043] Although pairing one fixed bed catalyst device with one bottom distillation device is known in the prior art, there are operational problems with liquid chemical components being delivered (supplied) to a fixed bed catalyst device in the prior art, because the liquid components drop only inside a bottom pressure vessel in the prior art, which can cause flooding and limit reactions from taking place.

[0044] Accordingly, a new fixed bed catalyst device (new reaction section) for each reactive distillation device in the bottom distillation device having a new structure is needed to solve the problem of delivering (supplying) liquid chemical components to the fixed bed catalyst device to avoid flooding. By introducing flood prevention systems (flood prevention apparatuses, flood protection systems, or flood protection apparatuses) shown in Figures 2-5, flooding of the bottom distillation column can be prevented so that silane can be continuously produced by the catalytic distiller in Figure 1. In addition, Figure 6 shows a flush system, which provides the additional advantages of flushing fixed bed catalyst components independently while the catalytic distiller 100 is online producing silane, so that the fixed bed catalyst components that have been compressed can be decompressed and silane production by the catalytic distiller 100 continues without interruption.

[0045] In an embodiment shown in Figure 1, there are three reactive distillation devices including an upper reactive distillation device 400, a middle reactive distillation device 500, and a lower reactive distillation device 700. All reactive distillation devices may have the same or similar structure. When the liquid reacts with the lower fixed bed catalyst device 720 and chemical components are separated by the lower bottom distillation device 710, a gas (vapor) including TCS, DCS, MCS, and with a very small amount of silane will be separated and rise through the lower reactive distillation device 700, and the STC will be separated by the lower bottom distillation device 710 in a liquid form and fall toward the bottom of the bottom distillation column 200.

[0046] When liquid including TCS, DCS, MCS, and silane reacts with the middle fixed bed catalyst device 520 and chemical components are separated by the middle bottom distillation device 510, a gas (vapor) including MCS, DCS, TCS, and silane will be separated by the middle bottom distillation device 510 and rise through the middle reactive distillation device 500, and the STC and TCS will be separated by the middle bottom distillation device 510 in a liquid form and fall toward the bottom of the bottom distillation column 200. In addition, TCS and STC in liquid form will fall in the downward direction in the bottom distillation column 200.

[0047] When liquid including TCS, DCS, MCS, and silane reacts in the upper fixed bed catalyst device 420 and chemical components are separated by the upper bottom distillation device 410, a gas (vapor) including TCS, DCS, MCS, and silane will be separated by the upper bottom distillation device and rise through the upper reactive distillation device 400, and the STC, TCS, DCS, and will be separated by the upper bottom distillation device 410 in a liquid form and fall toward the bottom of the bottom distillation column 200.

[0048] FIG. 2 is a diagram illustrating a reactive distillation device according to an embodiment. More specifically, Figure 2 illustrates an embodiment of the middle reactive distillation device 500 in Figure 1. The middle reactive distillation device 500 includes a middle bottom distillation device 510 and a middle fixed bed catalyst device 520 (middle reaction device). The middle fixed bed catalyst device 520 may include a middle fixed bed catalyst component, and a vapor riser 570. A vapor riser 570 may also be referred to as a gas riser, a vapor channel, or a gas channel. The middle fixed bed catalyst device 520 may include additional middle fixed bed catalyst components having the same or similar structure.

[0049] The middle fixed bed catalyst component may include a fixed bed catalyst container 532 (first middle fixed bed catalyst vessel) with an open screen on the top and bottom of the fixed bed catalyst container 532. The open screen on the top of the fixed bedcatalyst container 532 may be referred to as a fixed bed catalyst top screen 534, and the open screen on the bottom of the fixed bed catalyst container 532 may be referred to as a fixed bed catalyst bottom screen 536. The fixed bed catalyst component may further include a fixed bed catalyst 538, which may be positioned within the fixed bed catalyst container 532 above the fixed bed catalyst bottom screen 536 of fixed bed catalyst container 532. The fixed bed catalyst bottom screen 536 may be a Johnson screen, which supports the fixed bed catalyst 538 above the bottom of the middle fixed bed catalyst component. The middle fixed bed catalyst component may further include a fixed bed catalyst sealing pan 540, a fixed bed catalyst container outlet nozzle 542, a fixed bed catalyst component pipe 544, and a distillation device supply nozzle 546.

[0050] In embodiments, the bypass nozzle 580, the bypass pipe 582, the and the bypass return nozzle 584 may form a flood prevention system (flood prevention apparatus, flood protection system, or flood protection apparatus). In embodiments, the upper reactive distillation device 400 and the lower reactive distillation device 700 may have the same structure as the middle reactive distillation device 500 shown in Figure 2. Accordingly, the upper reactive distillation device 400 and the lower reactive distillation device 700 may also include the flood prevention system.

[0051] FIG. 3 is a diagram illustrating a reactive distillation device according to an embodiment. More specifically, Figure 3 illustrates an embodiment of the middle reactive distillation device 500 in Figure 1. The middle reactive distillation device 500 includes a middle bottom distillation device 510 and a middle fixed bed catalyst device 520 (middle reaction device). The middle fixed bed catalyst device 520 includes a middle fixed bed catalyst component and a vapor riser 570. A vapor riser 570 may also be referred to as a gas riser, a vapor channel, or a gas channel. The middle fixed bed catalyst device 520 may include additional middle fixed bed catalyst components having the same or similar structure.

[0052] This figure is similar to Figure 2 but has a collection tray 590 above the catalyst bed. Liquid from the reflux or distillation section above is accumulated on the collection tray and directed to the fixed catalyst bed 538 via a collection tray outlet nozzle 592, catalyst bed feed pipe 548 and catalyst bed inlet nozzle 594. The middle fixed bed catalyst component may include a fixed bed catalyst container 532 (first middle fixed bed catalyst vessel) with an open screen on the top and bottom of the fixed bed catalyst container 532. The open screen on the top of the fixed bed catalyst container 532 may be referred to as a fixed bed catalyst top screen 534, and the open screen on the bottom of the fixed bed catalyst container 532 may be referred to as a fixed bed catalyst bottom screen 536. The fixed bed catalyst componentmay further include a fixed bed catalyst 538, which may be positioned within the fixed bed catalyst container 532 above the fixed bed catalyst bottom screen 536 of fixed bed catalyst container 532. The fixed bed catalyst bottom screen 536 may be a Johnson screen, which supports the fixed bed catalyst 538 above the bottom of the fixed bed catalyst component. The fixed bed catalyst component may further include a fixed bed catalyst sealing pan 540, a fixed bed catalyst container outlet nozzle 542, a fixed bed catalyst component pipe 544, and a distillation device supply nozzle 546.

[0053] In embodiments, the bypass nozzle 580, the bypass pipe 582, and the bypass return nozzle 584 may form a flood prevention system (flood prevention apparatus, flood protection system, or flood protection apparatus). In embodiments, the upper reactive distillation device 400 and the lower reactive distillation device 700 may have the same structure as the middle reactive distillation device 500 shown in Figure 2. Accordingly, the upper reactive distillation device 400 and the lower reactive distillation device 700 may also include the flood prevention system.

[0054] FIG. 4 is a diagram illustrating a middle reactive distillation device according to an embodiment. More specifically, Figure 4 illustrates an embodiment of the middle reactive distillation device 500 in Figure 1. The structures in Figure 4 are similar to the structures in Figure 3. In Figure 4 the catalyst bed inlet nozzle is located on the bottom of the catalyst bed and the fixed bed catalyst outlet nozzle 542 is located on the top of the catalyst bed. Accordingly, the embodiment shown in Figure 4 is a configuration where liquid flow through the catalyst bed is in the upward direction and provides a flood prevention system to prevent flooding of the distillation device above the fixed bed. In embodiments, the upper reactive distillation device 400 and the lower reactive distillation device 700 may have the same structure and the middle reactive distillation device 500 shown in Figure 4. Accordingly, flooding of the upper fixed bed catalyst device 420 of the upper reactive distillation device 400 and the flooding of the lower fixed bed catalyst device 720 of the lower reactive distillation device 700 are also prevented by the flood prevention system as shown in Figure 4. In addition, damage to the fixed bed catalysts of all fixed bed catalyst devices in the bottom pressure vessel 202 is prevented. Moreover, vapor (gas) continues to flow upward through the all bottom distillation devices 410, 510, and 710 and then through the vapor risers of all fixed bed catalyst devices 420, 520, and 720 in the bottom pressure vessel 202, so that the production of silane and STC can continue without interruption.

[0055] FIG. 5 illustrates a reactive distillation device according to another embodiment. More specifically, Figure 5 illustrates an embodiment of the middle reactive distillationdevice 520 of Figure 1. As shown in Figure 5, Figure 5 includes all of the structures of the embodiments in Figure 2 including the flood prevention system of the middle fixed bed catalyst device 520. The embodiment in Figure 5 further includes a flush system (flush apparatus) incorporated into the middle fixed bed catalyst device 520. The middle fixed bed catalyst device 520 including the flush system is configured to allow a back flush (back flush bath) so that the middle fixed bed catalyst device 520 can be flushed to eliminate compaction of the fixed bed catalyst 538. Once the pressure drop through the middle fixed bed catalyst 538 of the middle fixed bed catalyst device 520 has become too great, the middle fixed bed catalyst 538 can be backflushed with liquid chemical components (flush fluid) already in the bottom pressure vessel 202 such as TCS and / or chlorosilane to reduce compaction of the bed and bed pressure drop. The chemical components for the flushing operation may be supplied from the liquid TCS input into the bottom pressure vessel 202 or the liquid reflux of the bottom pressure vessel 202 in Figure 1. In Figure 5, a flushing valve 600 is opened to allow the liquid to move through the middle fixed bed catalyst feed container outlet nozzle 542. In addition, in order to perform the flush, the valve (not shown on sketch) on the middle distillation device supply nozzles is closed. This allows one or more flush chemical components to flow through the middle fixed bed catalyst container nozzles 542 about the bottom of the middle fixed bed catalyst 538. The flush chemical components up through the fixed bed catalyst 538 and of the middle fixed bed catalyst device 520, out the middle bypass nozzle 580 (location D) and then back into the second middle bypass supply nozzle 584 (locations Y and Y2) through the middle bypass pipe 582. This allows for regeneration of the middle fixed bed catalyst 538.

[0056] In embodiments, the upper reactive distillation device 400 and the bottom reactive distillation device 700 may have the same structure as the middle reactive distillation device 500 as shown in Figure 5. Accordingly, when the flushing operation is not being performed, flooding of the fixed bed catalysts of the bottom reactive distillation device 700, fixed bed catalysts of the bottom middle reactive distillation device 500, and the fixed bed catalysts of the upper reactive distillation device 700 is also prevented. Accordingly, damage to the fixed bed catalysts of the bottom reactive distillation device 700, fixed bed catalysts or the middle reactive distillation device 500, and the fixed bed catalysts of the upper reactive distillation devices 400 is also prevented by flushing the fixed bed catalysts of the bottom reactive distillation device the upper reactive distillation device. In addition, this structure permits independently flushing the fixed bed catalyst component and any additional fixed bed catalystcomponents in the middle reactive distillation device 500, the upper reactive distillation device 400, and the bottom reactive distillation device 700.

[0057] FIG. 6 is a flowchart illustrating a method for flushing a fixed bed catalyst of a fixed bed catalyst device according to an embodiment. In operation S10, a fixed bed catalyst container nozzle to a fixed bed catalyst device is open. In operation S20, a bypass nozzle positioned above a distillation device is open. In operation S30, a distillation device supply nozzle positioned above a distillation device is closed. Operations S10, S20, and S30 can be performed simultaneously or in any order before operation S40. In operation S40, the flushing valve is opened to allow a flushing liquid to flow through the fixed bed catalyst container nozzle toward the fixed bed catalyst. In operation S50, the fixed bed catalyst is flushed to maintain the fixed bed catalyst. In operation 560, the flushing valve is closed to stop the supply of the flushing liquid. In operation 570, the open distillation device nozzle is open and any remaining flushing liquid flows through the bypass nozzle or the distillation supply nozzle to the distillation device. Because each fixed bed catalyst device of each reactive distillation device is independent from the other fixed bed catalyst devices of the other reactive distillation devices, one or more of the fixed bed catalyst may be flushed at the same time or different times so that the production of two co-products silane (SiH4) and silicon tetrachloride (STC) is not interrupted.

[0058] While embodiments of this disclosure have been shown and described, further modifications and alternative embodiments of various aspects of the invention will be apparent to those skilled in the art in view of this description. Accordingly, this description is to be construed as illustrative only and is for the purpose of teaching those skilled in the art the general manner of carrying out the invention. It is to be understood that the forms of the invention shown and described herein are taken as examples of embodiments. Elements and materials may be substituted for those illustrated or described herein, parts and processes may be reversed, and certain features of the invention may be utilized independently, all as would be apparent to one skilled in the art having the benefit of this description of the invention. Changes may be made in the elements described herein without departing from the spirit and scope of the invention as described in the following claims.

Claims

CLAIMSWhat is claimed is:

1. A catalytic distiller comprising: a pressure vessel; a reactive distillation device positioned in the pressure vessel including a distillation device and a fixed bed catalyst device positioned above the distillation device, wherein the fixed bed catalyst device includes a fixed bed catalyst component and a vapor riser; and a flood prevention system to collect and direct a liquid from the fixed bed catalyst component through fixed bed bypass pipe to the distillation device, wherein the fixed bed bypass pipe, which is connected to the pressure vessel, is positioned outside of the pressure vessel.

2. The catalytic distiller of claim 1, wherein: the fixed bed catalyst device further includes an additional fixed bed catalyst component, the flood prevention system collects and directs the liquid from the additional fixed bed catalyst component through an additional fixed bed bypass pipe to the distillation device, and the additional fixed bed bypass pipe, which is connected to the pressure vessel, is positioned outside of the pressure vessel.

3. The catalytic distiller of claim 1, wherein the fixed bed catalyst component includes a fixed bed catalyst.

4. The catalytic distiller of claim 3, wherein the fixed bed catalyst comprises catalyst particles having a diameter equal to or greater than about 0.8 mm.

5. The catalytic distiller of claim 2, wherein the fixed bed catalyst component includes a fixed bed catalyst, and the additional fixed bed catalyst component includes an additional fixed bed catalyst.

6. The catalytic distiller of claim 5, wherein the wherein the fixed bed catalyst comprises catalyst particles having a diameter equal to or greater than about 0.8 mm, and the additional fixed bed catalyst comprises the catalyst particles having a diameter equal to or greater than about 0.8 mm.

7. The catalytic distiller of claim 2, further comprising a flush system, using a flushing liquid, to independently flush the fixed bed catalyst component and the additional fixed bed catalyst component.

8. The catalytic distiller of claim 4, further comprising: a fixed bed catalyst sealing pan configured to collect liquid traversing the fixed bed catalyst, wherein the liquid enters a top of the fixed bed catalyst device and flows downward through the fixed bed catalyst device; a distillation device supply nozzle configured to deliver the collected liquid to the distillation device; and a fixed bed catalyst component pipe connected to the fixed bed catalyst sealing pan and the distillation device supply nozzle.

9. The catalytic distiller of claim 1, wherein the flood prevention system comprises the fixed bed bypass pipe, and further comprises: a bypass nozzle located above the fixed bed catalyst device and connected to the fixed bed bypass pipe; and a bypass return nozzle configured to deliver overflow liquid to the distillation device.

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