JP5457627B2 - Reaction nozzle, gas-phase hydrolysis treatment apparatus, and gas-phase hydrolysis treatment method - Google Patents

Description

  The present invention relates to a reaction nozzle that ejects and reacts two types of fluids, a gas-phase hydrolysis treatment apparatus including the nozzle, and a gas-phase hydrolysis treatment method.

Silicone production equipment discharges a liquid of silicone containing tetramethoxysilane Si (OCH ₃ ) ₄ , hexamethyldisiloxane (CH ₃ ) ₃ SiOSi (CH ₃ ) _3, etc., and this is generally incinerated. It is. When incineration is performed, a liquid is sprayed from a nozzle in an incinerator, but there arises a problem that silica generated from the liquid adheres to the nozzle and closes the nozzle. Therefore, a center tube that ejects a liquid containing silicone, a second outer tube that ejects a flame-supporting / incombustible gas from the outside of the center tube, and a flame-supporting / incombustible property from the outside of the second outer tube. Using a concentric multiple tube structure including a gas supply channel, the liquid ejected from the central tube is spray-combusted by the combustion-supporting / incombustible gas from the second outer tube, and the generated flame There has been proposed a burner that prevents clogging by covering it with a combustion-supporting / non-combustible gas supplied from a flow path disposed in (see Patent Document 1).
Japanese Patent No. 3346266 (page 4, FIG. 2)

On the other hand, liquids containing various chlorosilanes including tetrachlorosilane SiCl ₄ are discharged from the semiconductor silicon manufacturing facility, and these liquids contain some organic substances. However, unlike a liquid containing silicone, which is an organosilicon compound, the combustion heat is low and self-combustion does not occur. Therefore, the above burner cannot be used, and water vapor is often supplied to cause hydrolysis. Also in this case, since silica is produced by hydrolyzing a silane compound-containing liquid such as tetrachlorosilane, it is required to prevent the silica from adhering to the nozzle. Accordingly, the present invention provides a nozzle that is less likely to be blocked by a solid component generated by the reaction while reacting two kinds of fluids, a gas phase hydrolysis treatment apparatus for treating a chlorosilane-containing liquid, and 2 It is an object of the present invention to provide a gas phase hydrolysis treatment method in which a fluid is ejected in a manner that is difficult to be blocked by a solid component generated by the reaction while reacting various types of fluid. The term “gas phase hydrolysis” as used herein means that the hydrolysis reaction proceeds in the gas phase, and is not limited to the reaction occurring after evaporation of the silane compound-containing liquid.

  In order to achieve the above object, the reaction nozzle according to the first aspect of the present invention includes, for example, a first nozzle 10 for ejecting a liquid first fluid, as shown in FIG. A second nozzle 20 that is concentrically arranged outside the first nozzle 10 and ejects a first gas that refines the first fluid; downstream from the first nozzle 10 and the second nozzle 20 And a third nozzle 30 that has an opening on the side and outside the flow of the first fluid and the first gas and ejects a second fluid that reacts with the first fluid.

  With this configuration, the first fluid ejected from the first nozzle is refined by the first gas ejected from the second nozzle, and the second fluid ejected from the third nozzle It becomes easy to react. Further, since the third nozzle has an opening on the downstream side of the first nozzle and the second nozzle and outside the flow of the first fluid and the first gas, The second fluid reacts at a position away from the openings of the first nozzle and the third nozzle, and the solid component resulting from the reaction is less likely to adhere to the nozzle. The term “fluid” simply refers to a gas, liquid, or a solid that has been finely divided to such an extent that it is ejected from a nozzle or accompanied by a liquid or gas, or a mixture thereof. "Refers to a liquid or a fluid mixture of liquid and solid.

  Further, the reaction nozzle as the second aspect of the present invention is concentric with the second nozzle 20 outside the second nozzle 20 in the reaction nozzle 1 as the first aspect, for example, as shown in FIG. And a fourth nozzle 40 that ejects a second gas that covers the fluid in which the first fluid and the second fluid have reacted. Here, the “fluid in which the first fluid and the second fluid have reacted” is a mixed fluid of the first fluid and the second fluid, and at least a part of the first fluid and the second fluid. A fluid that reacts with a part of the fluid.

  If comprised in this way, since the 2nd gas which covers the fluid which the 1st fluid and the 2nd fluid reacted from the 4th nozzle is ejected, the 1st fluid and the 2nd fluid reacted It is possible to prevent the fluid from circulating and flowing near the opening of the first nozzle or the second nozzle.

  Moreover, the reaction nozzle as the third aspect of the present invention includes, for example, a plurality of third nozzles 30 in a radial manner in the reaction nozzle 1 as the first or second aspect as shown in FIG. The second fluid is ejected from the nozzle 30 toward the first fluid refined by the first gas.

  If comprised in this way, since the 3rd nozzle is provided with two or more radially, it is easy to mix a 2nd fluid with a 1st fluid uniformly.

  A reaction nozzle according to a fourth aspect of the present invention is the reaction nozzle according to any one of the first to third aspects. The first fluid contains chlorosilane; the second fluid is water vapor; Silica fine particles are generated by the reaction between the second fluid and the second fluid.

  If comprised in this way, it will become a reaction nozzle with which a nozzle is hard to be obstruct | occluded with the silica fine particle produced | generated at the time of the hydrolysis of chlorosilane using water vapor | steam.

  In order to achieve the above object, a gas phase hydrolysis treatment apparatus according to a fifth aspect of the present invention comprises a gas phase hydrolysis treatment for treating a liquid containing chlorosilane and an organic compound, for example, as shown in FIG. An apparatus 6 comprising: a hydrolysis nozzle 60 comprising a reaction nozzle according to a fourth aspect for ejecting the liquid as a first fluid, and discharging a fluid obtained by reacting the first fluid and the second fluid; A combustion furnace 70 for burning the fluid discharged from the decomposition furnace 60; and a collection device 85 for collecting silica fine particles.

  If comprised in this way, since a hydrolysis furnace is equipped with said reaction nozzle, the silica fine particle produced | generated by the reaction of chlorosilane and water vapor | steam is hard to adhere to a reaction nozzle, and a nozzle is hard to be obstruct | occluded. Moreover, since the combustion furnace is provided and the fluid which the 1st fluid and the 2nd fluid reacted is burned, the combustible substance in the reacted fluid can be burned completely. Furthermore, since the collection apparatus which collects a solid component is provided, the gas discharged | emitted from a gaseous-phase hydrolysis processing apparatus can be cleaned.

  Further, the gas phase hydrolysis treatment apparatus as the sixth aspect of the present invention is the gas phase hydrolysis treatment apparatus according to the fifth aspect, wherein the temperature in the hydrolysis furnace 60 is controlled to 200 ° C. or more and 600 ° C. or less. The temperature in the combustion furnace 70 is controlled to 850 ° C. or higher and 1100 ° C. or lower.

  If comprised in this way, since the temperature in a hydrolysis furnace is temperature-controlled to 200 to 600 degreeC, the particle | grains of the solid component produced | generated by reaction will become large. Furthermore, since the fluid discharged from the hydrolysis furnace is burned at 850 ° C. or higher and 1100 ° C. or lower in the combustion furnace, the combustible material containing the solid oxide discharged from the hydrolysis furnace can be completely burned.

  In order to achieve the above object, in the gas phase hydrolysis treatment method according to the seventh aspect of the present invention, for example, as shown in FIG. 6, a gas phase hydrolysis treatment for treating a liquid containing chlorosilane and an organic compound. The method includes: ejecting the liquid (step S10), and finely subtracting the liquid by ejecting a first gas around the ejected liquid substantially in parallel with the ejected liquid (step S10). 12) A process of mixing water vapor with the refined liquid to hydrolyze chlorosilane at a temperature of 200 ° C. or higher and 600 ° C. or lower to produce silica fine particles (Step S14); And a step of burning the hydrolyzed fluid of chlorosilane at a temperature of 850 ° C. or higher and 1100 ° C. or lower (step S20); and a step of collecting silica fine particles (step S50). .

  If comprised in this way, the liquid containing chlorosilane and an organic compound will be ejected, and the said liquid will be refined | miniaturized by ejecting a 1st gas around the ejected liquid substantially parallel to the ejected liquid. Since water vapor is mixed with the resulting liquid to hydrolyze chlorosilane, a liquid containing chlorosilane and an organic compound can be ejected by a method that is less likely to be blocked by silica fine particles generated by hydrolysis. Further, since chlorosilane is hydrolyzed at 200 ° C. or more and 600 ° C. or less, the particles of solid components produced by the reaction become large. Further, since the hydrolyzed liquid is burned at 850 ° C. or higher and 1100 ° C. or lower, the combustible material containing the solid oxide discharged from the hydrolysis furnace can be burned completely. Furthermore, since silica with large particles generated by hydrolysis is collected, it is easy to collect and exhaust gas can be purified.

  According to the present invention, the reaction nozzle is disposed concentrically with the first nozzle on the outside of the first nozzle and the first nozzle that ejects the liquid first fluid, and refines the first fluid. A second nozzle that ejects the first gas; an opening on the downstream side of the first nozzle and the second nozzle and outside the flow of the first fluid and the first gas; And the third nozzle that ejects the second fluid that reacts with the first fluid, so that the first fluid ejected from the first nozzle is finer by the first gas ejected from the second nozzle. Easily react with the second fluid ejected from the third nozzle, and the first fluid and the second fluid are separated from the openings of the first nozzle and the third nozzle. The solid component resulting from the reaction is less likely to adhere to the nozzle. Accordingly, there is provided a reaction nozzle in which two kinds of fluids are reacted while a solid component generated by the reaction is difficult to adhere to the nozzle and is not easily blocked.

  According to the present invention, a gas-phase hydrolysis treatment apparatus for treating a liquid containing chlorosilane and an organic compound includes the above-described reaction nozzle that ejects a liquid containing chlorosilane and an organic compound as a first fluid. And a second fluid, a hydrolysis furnace that discharges the fluid, a combustion furnace that burns the fluid discharged from the hydrolysis furnace, and a collection device that collects silica fine particles. The silica fine particles produced by the reaction of the silica hardly adhere to the reaction nozzle, and the nozzle is not easily blocked. Accordingly, there is provided a gas phase hydrolysis treatment apparatus for treating a chlorosilane-containing liquid provided with a nozzle that is not easily blocked by a solid component generated by the reaction while reacting two kinds of fluids.

  According to the present invention, a gas phase hydrolysis treatment method for treating a liquid containing chlorosilane and an organic compound ejects a liquid containing chlorosilane and an organic compound, and the ejected liquid is substantially parallel to the ejected liquid. A step of generating a fine silica particle by spraying a first gas around the substrate to refine the liquid, mixing water vapor with the refined liquid, and hydrolyzing chlorosilane at a temperature of 200 ° C. to 600 ° C. , A fluid in which liquid and water vapor are mixed, and a fluid in which chlorosilane is hydrolyzed is combusted at a temperature of 850 ° C. or higher and 1100 ° C. or lower, and a step of collecting silica fine particles. A liquid containing chlorosilane and an organic compound can be ejected by a method that is difficult to be blocked by fine silica particles. Accordingly, there is provided a gas phase hydrolysis treatment method in which a fluid is ejected in a manner that is less likely to be blocked by a solid component generated by the reaction while reacting two kinds of fluid.

  Embodiments of the present invention will be described below with reference to the drawings. In each figure, the same or equivalent devices are denoted by the same reference numerals, and redundant description is omitted.

  First, the configuration of the reaction nozzle 1 will be described with reference to FIG. 1A and 1B are diagrams for explaining the configuration of the reaction nozzle 1. FIG. 1A is a front view of the reaction nozzle 1 viewed from the tip side, and FIG. The reaction nozzle 1 includes a first nozzle 10, a second nozzle 20, a third nozzle 30, and a fourth nozzle 40. The first nozzle 10, the second nozzle 20, and the fourth nozzle 40 are configured concentrically, with the first nozzle 10 on the inside and the second nozzle 20 on the outside. A fourth nozzle 40 is arranged. The tip 22 of the second nozzle 20 is retracted from the tip 12 of the first nozzle 10. The tip 42 of the fourth nozzle 40 is retracted from the tip 22 of the second nozzle 20. The opening of each nozzle 10, 20, 40 is arranged from the downstream side of the fluid flow in the order of the tip 12, the tip 22, and the tip 42, thereby preventing backflow of fluid to each nozzle 10, 20, 40. Can do.

  The first nozzle 10 is a straight pipe 14 in the vicinity of the tip 12, and the nozzle base (right side in FIG. 1B) is a straight pipe 16 that is thicker than the vicinity of the tip 12, and the outer surface therebetween. Has an inclined portion 18 which is inclined. The thin straight pipe 14 and the thick straight pipe 16 have different inner diameters and are narrow in the vicinity of the tip 12.

  The second nozzle 20 is formed in a shape in which the vicinity of the tip 22 is sunk. The inner diameter of the second nozzle 20 has a reduced diameter starting portion 24 where the first nozzle 10 starts to narrow at a position substantially corresponding to the inclined portion 18 inclined from the thick straight tube 16 to the thin straight tube 14, and the tip 22 It has the inclination 26 which becomes thin uniformly until it reaches. The tip 22 of the second nozzle 20 is disposed at a position corresponding to the thin straight pipe 14 of the first nozzle 10, that is, outside the thin straight pipe 14. Therefore, the flow path formed by the second nozzle 20 (between the inner surface of the second nozzle 20 and the outer surface of the first nozzle 10) is narrow in the vicinity of the tip 22.

  The tip of the fourth nozzle 40 is disposed at a position where the second nozzle 20 corresponds to the diameter reduction start portion 24 and has a shape that is constricted near the tip 42. The inner diameter of the fourth nozzle 40 starts to become narrower at a position substantially corresponding to the reduced diameter starting portion 28 where the outer diameter of the second nozzle 20 begins to shrink, or on the side of the thicker tube where it begins to shrink. Similarly, it has an inclination 44 that reaches the tip 42. The flow path formed by the fourth nozzle 40 (between the inner surface of the fourth nozzle 40 and the outer surface of the second nozzle 20) may be narrow in the vicinity of the tip 42, but is not necessarily narrow. Also good.

  The third nozzle 30 is composed of a small-diameter pipe disposed outside the fourth nozzle 40, but the number of pipes constituting the third nozzle 30 is not limited to four, and even with one, Two, three, five, six, etc. may be used. It is easier to mix the second fluid (described later) into the first fluid (described later) by providing a plurality of pipes. Further, in FIG. 1, the pipes of the third nozzle 30 are arranged at symmetrical positions with respect to the central axes of the first, second and fourth nozzles 10, 20, and 40, but are not symmetrical positions. It may be arranged. However, it is easier to mix the second fluid into the first fluid more uniformly when the pipes are arranged at symmetrical positions. The cross section of the pipe constituting the third nozzle 30 may be any shape such as an ellipse, a rectangle, and a hexagon, but typically has a circular cross section that has excellent strength and is widely used. The third nozzle 30 has a bent portion 34 that extends from the fourth nozzle 40 side and bends in the central axis direction at a position corresponding to the portion 46 in which the fourth nozzle 40 is recessed. In the third nozzle 30, a tip 32 is disposed at a position beyond the tip 12 of the first nozzle 10 and has an opening there. The tip 32 of the third nozzle 30 has an opening outside the flow of the first fluid ejected from the first nozzle 10 and the flow of the gas ejected from the second nozzle 20. The outside of the flow of the first fluid means that the first fluid is ejected from the opening of the tip 12 of the first nozzle 10, and therefore the outside of the surface arranged in parallel to the central axis from the opening of the tip 12. Become. Further, it is on the downstream side of the flow from the tip 12. Similarly, the outside of the flow of the gas ejected from the second nozzle 20 is the outside of the surface arranged in parallel to the central axis from the opening of the tip 22 of the second nozzle 20. Further, it is downstream of the flow from the tip 12 and the tip 22.

  The tip 32 of the third nozzle 30 is saddle-shaped with the central axis of the first, second, and fourth nozzles 10, 20, 40 extended from the center axis, that is, not toward the center of the flow but toward the eccentric direction. Is arranged. By disposing the tip 32 in a bowl shape in this way, the second fluid ejected from the third nozzle 30 is eccentrically mixed with the first fluid ejected from the first nozzle 10 and the like. As a result, it flows spirally. When the second fluid flows in a spiral shape, it becomes easier to mix with the first fluid. The tip 32 of the third nozzle 30 may be directed in the direction in which the central axes of the first, second, and fourth nozzles 10, 20, and 40 are extended, and in particular, the flow velocity or kinetic energy of the second fluid. Is large, it is preferable that the first fluid is ejected toward the center of the first fluid because the first fluid may penetrate through the first fluid.

  As shown in FIG. 2, the third nozzle 30 may be disposed in a flow path formed by the fourth nozzle 40. FIG. 2 is a diagram for explaining the configuration of the reaction nozzle 2 in which the third nozzle 30 is installed in the flow path formed by the fourth nozzle 40, and (a) is a front view of the reaction nozzle 2 viewed from the front end side. (B) is sectional drawing along the axis | shaft of the reaction nozzle 2. FIG. As shown in FIG. 2B, the third nozzle 30 is arranged inside the fourth nozzle 40 and outside the second nozzle 20. In that case, the third nozzle 30 is configured by a small-diameter pipe that can be installed in the flow path formed by the fourth nozzle 40. By disposing the third nozzle 30 in the fourth nozzle 40, the outer periphery of the fourth nozzle 40 can be made a uniform curved surface without the convex portion due to the third nozzle 30. However, by disposing the third nozzle 30 outside the fourth nozzle 40, the third nozzle 30 can be configured with a pipe that is thicker than the width of the flow path formed by the fourth nozzle 40. Become. Moreover, since the 3rd nozzle 30 can be arrange | positioned after forming the 1st, 2nd and 4th nozzle 10 * 20 * 40, manufacture of the reaction nozzle 1 becomes easy.

  Next, the operation of the reaction nozzle 1 will be described with reference to FIG. FIG. 3 is a schematic diagram for schematically explaining the movement of the fluid ejected from the reaction nozzle 1. From the first nozzle 10, the first fluid A (black circle in the figure), from the second nozzle 20, the first gas B (x in the figure), from the third nozzle 30, the second fluid The fluid C (white circle in the figure) is ejected from the fourth nozzle 40 by the second gas D (thick arrow in the figure). The first fluid A and the second fluid C react to generate a solid component (triangle in the figure) that is a reaction product.

  The first fluid A ejected from the first nozzle 10 maintains the same cross section as the opening of the first nozzle 10 in a region (region X in the drawing) immediately after being ejected. On the other hand, the first gas B ejected from the second nozzle 20 also maintains the same cross section as the opening of the second nozzle 20. Here, when the flow velocity of the first gas B ejected from the second nozzle 20 is increased, turbulent flow is caused, and the first fluid A flowing in the immediate vicinity is entrained by entraining the ambient gas around the flow. become. That is, the first gas B and the first fluid A start to be mixed. For example, if the first fluid A is a liquid and the first gas B is air, the liquid and air are mixed, and the first fluid A becomes fine particles. That is, the first fluid A is atomized into the first gas B (region Y in the figure). As a result, the first fluid A flows while being mixed with the first gas B. Even if the flow rate of the first gas B is not fast, the first fluid A and the first gas B may be mixed by flowing in contact with the first fluid A and the first gas B.

  The second fluid C ejected from the third nozzle 30 flows into the flow in which the first fluid A and the first gas B are mixed and flow (region Z in the figure). As described above, since the first fluid A is mixed with the first gas B and is, for example, fine particles, the first fluid A comes into contact with the second fluid C with a large surface area. Therefore, the reaction between the first fluid A and the second fluid C is promoted. Further, as described above, the third nozzle 30 is arranged in a bowl shape, and the second fluid C becomes spiral and mixes with the mixed flow of the first fluid A and the first gas B. , Mixing is easier and the reaction is promoted.

  When a solid component is generated by the reaction between the first fluid A and the second fluid C, if the reaction occurs at the nozzle outlet, the solid component adheres to the nozzle and causes problems such as blocking of the nozzle. However, as described above, the first fluid A ejected from the first nozzle 10 and the first gas B ejected from the second nozzle 20 flow independently in the region X near the nozzle, and the region Y To mix. And the 2nd fluid C spouted from the 3rd nozzle 30 which has the opening part 32 in the downstream from the opening parts 12 * 22 of the 1st nozzle 10 and the 2nd nozzle 20 is the 1st fluid A and the 1st The reaction occurs in the region Z away from the first nozzle 10, the second nozzle 20, and the third nozzle 30 because it flows into the region Z on the downstream side where the one gas B is mixed. That is, even if a solid component is generated by the reaction between the first fluid A and the second fluid C, it does not adhere to the first nozzle 10, the second nozzle 20, and the third nozzle 30. In particular, since the third nozzle 30 has an opening outside the flow of the first fluid A, the first fluid A does not reach the opening of the third nozzle 30, and the opening of the third nozzle 30. The first fluid A and the second fluid C do not react with each other. Furthermore, since the third nozzle 30 has an opening on the outside of the flow of the first gas B, the first gas B flows between the flow of the first fluid A and the opening of the third nozzle 30. Even if the flow is formed and the first fluid A is scattered for some reason, it is prevented from reaching the opening of the third nozzle 30, and the first fluid A and the first fluid A are prevented from reaching the opening of the third nozzle 30. The possibility of reacting with the second fluid C is further reduced. Therefore, the adverse effect of nozzle blockage does not occur. For example, when the first fluid A is a silane compound-containing liquid containing chlorosilane and the second fluid C is water vapor, the nozzle can be prevented from being clogged with silica resulting from the hydrolysis reaction. .

  Further, the second gas D is ejected from the fourth nozzle and flows along the outer surface near the tip 22 of the second nozzle 20, and the first gas B and the first fluid A / first The gas B and the second fluid C start to mix or flow so as to cover the part to be mixed. Therefore, it is possible to prevent the solid component that is a reaction product of the first fluid A and the second fluid C from adhering to the reaction nozzle 1, particularly the first nozzle 10 and the second nozzle 20. In the reaction nozzle 1, a part of the fluid (the first gas B is also mixed) after the first fluid A and the second fluid C have reacted becomes a circulating flow (thin arrow in the figure). , It may flow into the vicinity of the reaction nozzle 1. However, because of the second gas D flowing along the surface of the second nozzle 20, the weak circulation flow is accompanied by the flow of the second gas D and reaches the outer surface of the second nozzle 20. The first nozzle 10 and the second nozzle 20 are sealed from the fluid after the reaction. Therefore, the solid component is prevented from adhering to the surface of the second nozzle 20. The fourth nozzle 40 is the outermost surface, and even if a solid component adheres to the outer surface of the fourth nozzle 40, it is easy to remove. The opening of the fourth nozzle 40 has other nozzles 10. In general, it is formed larger than the opening 20/30, and the influence of the adhesion of some solid components is small, and there is often no problem.

  Next, referring to FIG. 4, a gas phase as a processing apparatus for a silane compound in a silane compound-containing liquid (hereinafter also simply referred to as “liquid”) provided with reaction nozzle 1 and containing chlorosilane and an organic compound. The hydrolysis treatment apparatus 6 will be described. FIG. 4 is a block diagram illustrating the configuration of a gas phase hydrolysis treatment apparatus 6 that hydrolyzes and burns a liquid containing a combustible material such as a silane compound and an organic compound. The gas-phase hydrolysis treatment apparatus 6 includes a reaction nozzle 1, hydrolyzes a liquid as a first fluid with water vapor as a second fluid, and discharges the fluid after the reaction. Combustion furnace 70 that completely burns the fluid discharged from the cracking furnace 60, that is, burns the combustible material in the fluid completely, and high-temperature gas discharged from the combustion furnace 70 (along with a solid component) A quenching tower 75 as a quenching device for cooling the water, a scrubber 80 as a neutralization device for neutralizing and removing acid gas contained in the gas discharged from the quenching tower 75, and a gas discharged from the scrubber 80. A removal device that collects and removes the solid components in the liquid, that is, a mist cotrel 85 as a collection device, and a suction device that sucks the gas and flows it in the above order while discharging it to the atmosphere from a stack (not shown) And a fan 90 as. As the combustion furnace 70, a swirl type combustion furnace, also called a jet furnace, is typically used.

  Here, the configuration of the hydrolysis furnace 60 will be described with reference to FIG. FIG. 5 is a schematic cross-sectional view illustrating the configuration of the hydrolysis furnace 60. The hydrolysis furnace 60 includes a cylindrical vertical container 62, a reaction nozzle 1 disposed in the vertical container 62, and a burner 65 into which fuel gas is introduced and burned. A hot gas nozzle 64 is connected to the center of the upstream end surface 52 of the vertical container 62. In FIG. 5, the hydrolysis furnace 60 is illustrated in the direction in which it is actually installed, and the upper side in the figure is the vertically upper side where it is actually installed, and is the upstream side. The reaction nozzle 1 is disposed on the shoulder portion of the end face 52. A gas outlet 66 is formed at the downstream side of the vertical container 62, that is, at the lower end. The high-temperature combustion gas generated by the burner 65 flows from the high-temperature gas nozzle 64 into the vertical container 62. The first fluid A, the first gas B, the second gas D, and the second fluid C (see FIG. 3) ejected from the reaction nozzle 1 are heated by the high-temperature combustion gas flowing from the high-temperature gas nozzle 64. However, it reacts in the vertical container 62 and is sent downstream through the gas outlet 66. A region Y (see FIG. 3) for mixing the first fluid A and the first gas B in front of the reaction nozzle 1, and a region where the first fluid A and the second fluid C react with each other. The vertical container 62 has a sufficient space below the reaction nozzle 1 so that Z (see FIG. 3) is appropriately formed. Further, the first fluid A, the first gas B, and the residence time sufficient for the reaction between the first fluid A and the second fluid C to be completed in the vertical container 62 are secured. The flow rate of the gas in which the second fluid C and the second gas D are mixed (which is accompanied by a solid as a reaction product. These are collectively referred to as “mixed gas” hereinafter) is determined. The mixed gas is sucked out by the fan 90 (see FIG. 4) and then sent out from the hydrolysis furnace 60 to the downstream side. As shown in FIG. 5, one hydrolysis furnace 60 may be provided with a plurality of reaction nozzles 1 or only one reaction nozzle 1. In any case, the reaction nozzle 1 is arranged near the upstream end of the vertical container 62 and near the hot gas nozzle 64.

Here, in the hydrolysis furnace 60, the first fluid is a liquid containing a silane compound containing chlorosilane and a combustible material such as an organic compound, the second fluid is water vapor, the first gas, and the second gas The gas is typically air. That is, a liquid containing a combustible material such as a silane compound and an organic compound that is the first fluid is ejected from the reaction nozzle 1, and the silane compound is reacted with water vapor that is the second fluid. The liquid is atomized by air, the silane compound in the atomized liquid reacts with water vapor, and silica SiO ₂ as a solid component is generated as fine particles by hydrolysis in the gas phase. Here, the “fine particles” are, for example, small particles having a particle size of 10 μm or less by an image analysis method using a scanning electron microscope of the collected particles, and are accompanied by a gas. Refers to particles.

  Here, it is preferable to control the reaction temperature of hydrolysis in the hydrolysis furnace 60 to 200 ° C. or more and 600 ° C. or less. When the hydrolysis reaction temperature is lower than 200 ° C., the generated silica fine particles adhere to the furnace wall of the hydrolysis furnace 60, and stable operation becomes difficult. On the other hand, when the temperature is higher than 600 ° C., the particle size of the silica fine particles generated by hydrolysis becomes small, and it becomes difficult to collect the silica fine particles by the mist cotrel 85 at the subsequent stage. In addition, when the reaction temperature of hydrolysis is 400 ° C. or more and 500 ° C. or less, it is more preferable because adhesion to the furnace wall can be reduced while keeping the size of the silica fine particles larger. In order to maintain the hydrolysis reaction temperature at a temperature of 200 ° C. or higher and 600 ° C. or lower, the fuel is burned by the burner 65 to be a heat source. Note that the heat source is not limited to the method of combusting with the burner 65, high-temperature superheated steam or high-temperature air may be introduced, the hydrolysis furnace 60 may be heated with an electric heater, or other known methods may be used. Good. In particular, when high-temperature superheated steam is introduced, it is preferable to supply steam for hydrolysis in addition to steam supplied from the third nozzle 30 (see FIG. 1). Since liquid, water vapor, and air are ejected from the reaction nozzle 1 to cause hydrolysis and combustion, silica is generated at a position separated from the reaction nozzle 1 and is prevented from adhering to the reaction nozzle 1.

Returning to FIG. 4, the description of the gas phase hydrolysis treatment device 6 will be continued. In order to burn the combustible material remaining in the hydrolysis furnace 60, a combustion furnace 70 is provided downstream of the hydrolysis furnace 60. The combustion furnace 70 is a device that introduces the fuel F and typically burns at 850 ° C. or higher and 1100 ° C. or lower. As the fuel, waste oil, heavy oil, or the like is used, and combustion air (not shown) is introduced so as to swirl within the container and burned. In the combustion at a temperature lower than 850 ° C., the combustible material cannot be combusted. Further, if the combustion is performed at a temperature higher than 1100 ° C., not only is the fuel F consumed excessively, it becomes uneconomical, but also the amount of chlorine gas Cl ₂ that is generated in equilibrium from hydrogen chloride HCl increases due to the high temperature, The subsequent scrubber 80 cannot be processed. That is, hydrogen chloride HCl generated by hydrolysis reacts with oxygen O _2, and the reaction of generating chlorine gas Cl ₂ and water H ₂ O becomes faster, so that the increased chlorine gas Cl ₂ cannot be treated. A combustion temperature of 900 ° C. or higher and 950 ° C. or lower is more preferable because fuel can be saved and the amount of chlorine gas Cl ₂ can be reduced while completely burning. In order to completely burn the combustibles in the liquid or to decompose harmful components, the capacity of the combustion furnace 70 and the fan 90 are set so that the residence time of the mixed gas in the combustion furnace 70 is, for example, 2 seconds or more. Suction speed or combustion air flow velocity and inflow direction (how to swirl) are designed.

  The mixed gas discharged from the combustion furnace 70 is guided to the quenching tower 75. The quenching tower 75 is a device that cools the high-temperature mixed gas by introducing the cooling water W and bringing the cooling water W into contact with the mixed gas while ejecting it from a nozzle (not shown) like a shower. The mixed gas combusted in the combustion furnace 70 is cooled to a temperature that does not cause inconvenience in the processing in the subsequent scrubber 80 and the mist cot rel 85, for example, 85 ° C. At this time, it is preferable to make the passage time in the temperature range of 400 to 200 ° C. as short as possible so as not to cause resynthesis of dioxins. Typically, the cooling water W introduced into the quenching tower 75 is collected at the bottom of the quenching tower 75 and is provided with a cooling water circulation passage for introducing it into the quenching tower 75 again.

The mixed gas cooled by the quenching tower 75 is introduced into the scrubber 80. The scrubber 80 is a device that neutralizes and removes acidic components such as hydrogen chloride HCl, chlorine Cl ₂ , and sulfur dioxide SO ₂ by bringing an alkaline substance such as magnesium hydroxide and caustic soda into contact with the mixed gas. is there. The scrubber 80 neutralizes acidic components in the mixed gas by bringing the slurry or aqueous solution of an alkaline substance into contact with the mixed gas while ejecting from a nozzle (not shown) like a shower.

  A mist cot rel (wet electrostatic precipitator) 85 applies a high voltage to a pair of parallel flat plates and collects fine dust on one flat plate using Coulomb force. In general, a wet dust collector can collect dust more efficiently than a dry dust collector such as a bag filter. The mixed gas from which the dust is removed by the mist cot rel 85 is sucked into the fan 90 and released from the stack (not shown) to the atmosphere.

  Here, with reference to FIG. 6, the processing method of the silane type compound containing liquid containing a chlorosilane and an organic compound is demonstrated collectively. FIG. 6 is a flowchart illustrating a method for treating a silane compound-containing liquid containing chlorosilane and an organic compound. First, a silane compound-containing liquid containing chlorosilane and an organic compound is ejected from the nozzle (step S10). At the same time, air is jetted in a direction parallel to the liquid to atomize the liquid (step S12). Here, the direction parallel to the liquid means that the liquid is not parallel in a strict sense but is ejected in the same direction as the liquid, for example, within 30 degrees or 15 degrees in angle. Next, water vapor is mixed with the liquid atomized with air (step S14). Then, the silane compound in the liquid is hydrolyzed by water vapor to produce silica fine particles. Here, it is preferable to keep the hydrolysis temperature at 200 ° C. or more and 600 ° C. or less. By hydrolyzing at 200 ° C. or more and 600 ° C. or less, the generated silica fine particles become large, and the silica fine particles do not adhere to surrounding devices and the like, and stable operation can be performed. And air is flowed so that the circumference | surroundings of the flow of the mixed gas by which the silane type compound in the liquid was hydrolyzed may be prevented, and mixed gas is prevented from flowing back to a nozzle direction (step S16). This is the process related to the hydrolysis of the liquid.

Next, the mixed gas is typically burned at 850 ° C. or higher and 1100 ° C. or lower, and the combustible material remaining in the mixed gas is completely burned (step S20). Combustion at 850 ° C or higher and 1100 ° C or lower completely burns the remaining combustible material, and does not increase the temperature excessively, so that fuel is not wasted and generation of chlorine gas Cl ₂ from hydrogen chloride HCl is suppressed. It is done. Subsequently, the mixed gas is rapidly cooled (step S30), the mixed gas is neutralized (step S40), and solid components including silica fine particles in the mixed gas are collected and removed (step S50). And the mixed gas from which the solid component was removed by the neutralization process is discharged | emitted (S60). Since hydrolysis is performed at a temperature of 200 ° C. or more and 600 ° C. or less, the silica fine particles to be produced are large and easy to collect and remove. Further, since combustion occurs chlorine gas Cl ₂ at 850 ° C. or higher 1100 ° C. or less are suppressed easily neutralization is.

  In the above description, the first fluid has been described as a silane compound-containing liquid and the second fluid as water vapor. However, the reaction nozzle 1 and the hydrolysis furnace 60 according to the present invention can be used for other purposes. it can. In particular, when the first fluid and the second fluid react to generate a solid component, the clogging of the nozzle by the solid component is prevented, so that the first fluid and the second fluid are preferably used.

  Using the experimental apparatus shown in FIG. 7, a silane compound-containing liquid and water vapor are ejected from the reaction nozzle 1 to hydrolyze the silane compound-containing liquid to the reaction nozzle 1 for silica fine particles as a reaction product. An experiment was conducted to examine the adhesion of the. FIG. 7 is a block diagram of the industrial waste incinerator 100. The industrial waste incinerator 100 corresponds to the rotary kiln 110 and the hydrolysis furnace, and corresponds to the rear chamber 120 and the combustion furnace for separating the burning husk following the rotary kiln 110. Swirling type secondary combustion furnace 130 that completely burns unburned materials, quench tower 140 that wet-cools high-temperature exhaust gas, scrubber 150 that absorbs and removes acidic gases such as hydrogen chloride, and mistcotrel that completely removes soot and dust ( Wet electrostatic precipitator) 160, induction fan 170 and chimney 180. The rear chamber 120 includes the reaction nozzle 1 shown in FIG. 1, and a silane compound-containing liquid is ejected from the reaction nozzle 1. The industrial waste incinerator 100 is an apparatus having a maximum incineration amount of 267 tons / day.

8 ton / hour of industrial waste IW is supplied to the rotary kiln 110 of the industrial waste incinerator 100 together with the auxiliary combustion oil AO1 and incinerated. In the rear chamber 120, the first nozzle 10 of the reaction nozzle 1 shown in FIG. To 220 kg / hr of silane compound-containing liquid SW, second nozzle 20 to 25 Nm ³ / hr of atomizing air AR1, third nozzle 30 to 70 kg / hr of steam ST, and fourth nozzle 40 to 30 Nm ³ / Hour sealing air AR2 was ejected. The amount of water vapor ST ejected is approximately twice the theoretical equivalent of the amount ejected of the silane compound-containing liquid SW. The composition of the silane compound-containing liquid SW is tetrachlorosilane 69 wt%, other chlorosilanes 30 wt%, and aromatic organic substances 1 wt%. Met.

  The above-described silane compound-containing liquid SW, atomizing air AR1, water vapor ST, and sealing air AR2 were ejected for a total of 20 hours using the reaction nozzle 1 shown in FIG. It was possible to use it without causing any problems. Further, when the reaction nozzle 1 was inspected after the experiment was completed, no silica fine particles were found attached. That is, it was confirmed that the reaction nozzle 1 was not easily blocked by the solid component generated by the reaction while reacting two kinds of fluids.

  Further, in order to confirm that the silane-based compound-containing liquid SW undergoes a hydrolysis reaction with the water vapor ST, and as a result, silica fine particles are generated, the supply amounts of the industrial waste IW and the auxiliary combustion oil AO1 are adjusted, The operation was performed while controlling the temperature of the rear chamber 120 at 660 to 800 ° C and 970 to 1150 ° C. Moreover, auxiliary combustion oil AO2 was supplied to the swirl type secondary combustion furnace 130, the temperature was maintained at 900 to 930 ° C, and combustibles were completely burned. As a result of observing the solid components collected by the mistcot rel 160, it was confirmed to be silica fine particles SP. That is, it was confirmed that the silane compound-containing liquid SW and the water vapor ST were hydrolyzed to generate silica fine particles.

  In addition, when the average particle diameter of the silica fine particles SP was measured, when the temperature of the rear chamber 120 was controlled to 660 to 800 ° C., it was 143 nm, and when the temperature of the rear chamber 120 was controlled to 970 to 1150 ° C. It was 96 nm. Here, the average particle diameter was measured by an image analysis method using a scanning electron microscope. Therefore, it was confirmed that the particle size of the silica fine particles SP generated as a result of the hydrolysis reaction is affected by the reaction temperature. In the industrial waste incinerator 100, it is difficult to lower the temperature of the rear chamber 120 to 600 ° C. or less, so the relationship between the hydrolysis temperature and the silica fine particle diameter was examined in detail in Example 2.

Using the test apparatus 200 shown in FIG. 8, the silica fine particle diameter and the by-product amount of chlorine gas Cl ₂ with respect to the hydrolysis temperature were examined. FIG. 8 is a block diagram illustrating the test apparatus 200. The test apparatus 200 includes a double tube nozzle 250 for flowing tetrachlorosilane into the inner tube and a heated steam / air mixture SA into the outer tube, and tetrachlorosilane and steam flowing out from the double tube nozzle 250. A quartz tube 252 through which the air mixture SA flows and an electrothermal vertical tubular furnace 254 for heating the quartz tube 252 are provided. Furthermore, a nozzle 260 that sucks a part of the mixed gas Mx flowing out from the outlet of the quartz tube 252; a water trap 262 that cools the mixed gas Mx while removing hydrogen chloride HCl from the mixed gas Mx sucked by the nozzle 260; Cylindrical filter paper dust collector 270 that collects soot from mixed gas My flowing out of water trap 262, and the concentration of chlorine gas Cl _{2 in} mixed gas Mz after collecting dust with cylindrical filter paper dust collector 270 A detection tube 280 for measurement and a vacuum pump 290 for sucking the mixed gas Mz from the nozzle 260 are provided. Furthermore, the test apparatus 200 includes a thermometer T that measures the temperature inside the quartz tube 252. The test apparatus 200 corresponds to the hydrolysis furnace 60 shown in FIG.

Steam / air mixing of tetrachlorosilane with a flow rate of 4.7 g / min for the inner tube of the double tube nozzle 250 and steam with a flow rate of 2 g / min for the outer tube and a normal flow rate of 4.2 dm ³ / min. Body SA was washed away. The amount of water was twice the theoretical equivalent. From the double-tube nozzle 250, tetrachlorosilane and steam / air mixture SA were passed through the quartz tube 252 and heated to cause a hydrolysis reaction. The inner diameter of the quartz tube 252 is 35 mm, the length is 1000 mm, and the length of the electrothermal vertical tubular furnace 254 is 420 mm. Here, the internal temperature of the quartz tube 252 is changed by the electrothermal vertical tubular furnace 254, and the internal temperature of the quartz tube 252 through which the tetrachlorosilane and the steam / air mixture SA flowing out of the double tube nozzle 250 flow is changed. The hydrolysis reaction temperature was measured. The tip of the double tube nozzle 250 that flows out the tetrachlorosilane and the steam / air mixture SA is located 150 mm from the upstream (double tube nozzle 250) side end of the electrothermal vertical tubular furnace 254. The internal temperature was measured at a position 210 mm from the upstream end of the electrothermal vertical tubular furnace 254 that is the highest temperature in the quartz tube 252. Then, the particle diameter of the silica fine particles collected by the cylindrical filter paper dust collector 270 was measured, and the concentration of the chlorine gas Cl ₂ was measured by the detector tube 280.

The measurement results of the particle diameter of silica fine particles and the concentration of chlorine gas Cl ₂ when the hydrolysis reaction temperature is changed to 200 ° C., 500 ° C., 800 ° C., 1000 ° C., and 1300 ° C. are collectively shown in FIG. In addition, the particle size of the silica fine particles is obtained by measuring the collected silica fine particles by an image analysis method using a scanning electron microscope, and showing the measured particle size range of the silica fine particles as a measurement result.
From the measurement results shown in FIG. 9, it can be seen that the lower the hydrolysis reaction temperature, the larger the particle size of the silica fine particles. That is, the lower the hydrolysis reaction temperature, the easier it is to collect the silica fine particles in the latter mist cotrel. In particular, when the temperature is 500 ° C. or less, the particle diameter of the silica fine particles is 300 nm or more, so that it is easy to collect.
It can also be seen that the lower the hydrolysis reaction temperature, the smaller the amount of chlorine gas by-produced. That is, lowering the hydrolysis reaction temperature reduces the burden on the subsequent scrubber.

It is a figure explaining the structure of a reaction nozzle, (a) is the front view which looked at the reaction nozzle from the front end side, (b) is sectional drawing along the axis | shaft of the reaction nozzle. It is a figure explaining the structure of the reaction nozzle which installed the 3rd nozzle in the flow path formed by the 4th nozzle, (a) is the front view which looked at the reaction nozzle from the front end side, (b) is the reaction nozzle It is sectional drawing along an axis. It is a schematic diagram which illustrates typically the motion of the fluid or gas ejected from the reaction nozzle. It is a block diagram explaining the structure of the gaseous-phase hydrolysis processing apparatus which hydrolyzes and burns the liquid containing combustible substances, such as a silane type compound and an organic compound. It is typical sectional drawing explaining the structure of a hydrolysis furnace. It is a flowchart explaining the processing method of the silane type compound containing liquid containing chlorosilane and an organic compound. It is a block diagram of the industrial waste incinerator which an applicant owns, and is an experimental device which investigated adhesion of the reaction product to the nozzle using the reaction nozzle concerning the present invention. It is a block diagram explaining the test apparatus which investigated the particle size of the silica particle with respect to a hydrolysis temperature, and the byproduct amount of chlorine gas. It is a figure which shows collectively the measurement result of the particle size of silica fine particle at the time of changing a hydrolysis reaction temperature with 200 degreeC, 500 degreeC, 800 degreeC, 1000 degreeC, and 1300 degreeC, and the density | concentration of chlorine gas.

Explanation of symbols

1, 2 Reaction nozzle 6 Gas phase hydrolysis treatment apparatus 10 First nozzle 12 First nozzle tip 14 Thin straight pipe 16 Thick straight pipe 18 Inclined portion 20 Second nozzle 22 Second nozzle tip 24 Diameter start portion 26 Inclination 28 Diameter reduction start portion 30 Third nozzle 32 Third nozzle tip 34 Bent portion 40 Fourth nozzle 42 Fourth nozzle tip 44 Inclination 46 Constricted portions 52, 54, 58 End face 56 Side 60 Hydrolysis furnace 62 Vertical vessel 64 High-temperature gas nozzle 65 Burner 66 Gas outlet 70 Combustion furnace 75 Quenching tower 80 Scrubber 85 Mist cotrel (collector)
90 Fan 100 Industrial waste incinerator 110 Rotary kiln 120 Rear chamber 130 Swirl secondary combustion furnace 140 Quench tower 150 Scrubber 160 Mist cot rel (wet electric dust collector)
170 Induction Fan 180 Chimney 200 Test Equipment
250 Double tube type nozzle 252 Quartz tube 254 Electric heating vertical tube furnace 260 Nozzle 262 Water trap 270 Cylindrical filter paper dust collector 280 Detector tube 290 Vacuum pump A First fluid B First gas C Second fluid D Second gas F Fuel Mx, My, Mz Mixed gas SA Steam / air mixture T Thermometer W Cooling water

Claims (7)

A first nozzle for ejecting a liquid first fluid;
A second nozzle that is arranged concentrically with the first nozzle outside the first nozzle and that ejects a first gas that refines the first fluid;
The second nozzle that has an opening on the downstream side of the first nozzle and the second nozzle and outside the flow of the first fluid and the first gas and reacts with the first fluid. A third nozzle for ejecting a fluid of ;
A fourth nozzle that is disposed concentrically with the second nozzle outside the second nozzle and that ejects a second gas that covers a fluid obtained by reacting the first fluid and the second fluid ; Comprising:
Reaction nozzle. A plurality of the third nozzles radially provided;
The second fluid is ejected from the third nozzle toward the first fluid refined by the first gas;
The reaction nozzle according to claim 1. A first nozzle for ejecting a liquid first fluid;
A second nozzle that is arranged concentrically with the first nozzle outside the first nozzle and that ejects a first gas that refines the first fluid;
The second nozzle that has an opening on the downstream side of the first nozzle and the second nozzle and outside the flow of the first fluid and the first gas and reacts with the first fluid. A third nozzle for ejecting a fluid of
The first fluid comprises chlorosilane;
The second fluid is water vapor;
Silica fine particles are generated by the reaction of the first fluid and the second fluid;
Reaction nozzle. The first fluid comprises chlorosilane;
The second fluid is water vapor;
Silica fine particles are generated by the reaction of the first fluid and the second fluid;
The reaction nozzle according to claim 1 or 2 . A gas phase hydrolysis treatment apparatus for treating a liquid containing chlorosilane and an organic compound:
A hydrolysis furnace comprising the reaction nozzle according to claim 3 or 4 for ejecting the liquid as the first fluid, and discharging a fluid obtained by reacting the first fluid and the second fluid;
A combustion furnace for burning the fluid discharged from the hydrolysis furnace;
A collection device for collecting the silica fine particles;
Gas phase hydrolysis treatment equipment. The temperature in the hydrolysis furnace is controlled to 200 ° C. or more and 600 ° C. or less;
The temperature in the combustion furnace is controlled to be 850 ° C. or higher and 1100 ° C. or lower;
The gas phase hydrolysis treatment apparatus according to claim 5. A gas phase hydrolysis treatment method for treating a liquid containing chlorosilane and an organic compound comprising:
Spouting the liquid,
The liquid is refined by ejecting a first gas around the ejected liquid substantially in parallel with the ejected liquid,
Mixing water vapor with the finely divided liquid and hydrolyzing the chlorosilane at a temperature of 200 ° C. or higher and 600 ° C. or lower to produce silica fine particles;
Combusting a fluid in which the liquid and the water vapor are mixed and the chlorosilane is hydrolyzed at a temperature of 850 ° C. or higher and 1100 ° C. or lower;
Collecting the silica fine particles;
Gas phase hydrolysis treatment method.

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