WO2016114036A1 - Continuous firing furnace - Google Patents

Continuous firing furnace Download PDF

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Publication number
WO2016114036A1
WO2016114036A1 PCT/JP2015/084254 JP2015084254W WO2016114036A1 WO 2016114036 A1 WO2016114036 A1 WO 2016114036A1 JP 2015084254 W JP2015084254 W JP 2015084254W WO 2016114036 A1 WO2016114036 A1 WO 2016114036A1
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WIPO (PCT)
Prior art keywords
firing furnace
continuous firing
honeycomb
gas
exhaust path
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PCT/JP2015/084254
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French (fr)
Japanese (ja)
Inventor
昌大 岩本
忠文 大橋
佳典 橋本
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イビデン株式会社
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Publication of WO2016114036A1 publication Critical patent/WO2016114036A1/en

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B9/00—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity
    • F27B9/04—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity adapted for treating the charge in vacuum or special atmosphere
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D17/00—Arrangements for using waste heat; Arrangements for using, or disposing of, waste gases

Definitions

  • the present invention relates to a continuous firing furnace.
  • particulates such as soot (hereinafter referred to as PM) and other harmful components contained in exhaust gas discharged from internal combustion engines such as buses and trucks and construction machinery and the like are harmful to the environment and the human body. It is a problem. Accordingly, various honeycomb structures made of porous SiC have been proposed as honeycomb filters for collecting PM in exhaust gas and purifying the exhaust gas. A honeycomb structure that functions as a honeycomb catalyst for purifying harmful gases in exhaust gas has also been proposed.
  • honeycomb structure When manufacturing such a honeycomb structure, first, SiC particles are kneaded with an organic binder or the like, and then formed into a predetermined shape using an extrusion molding die or the like to prepare a honeycomb formed body. Thereafter, the obtained honeycomb formed body is fired at 2000 to 2300 ° C. in a firing furnace to manufacture a honeycomb fired body made of recrystallized SiC. Thereafter, if necessary, the honeycomb fired body is bonded through an adhesive or cut into a predetermined shape using a diamond cutter or the like to manufacture a honeycomb structure.
  • a honeycomb fired body made of recrystallized SiC can be manufactured efficiently by firing the honeycomb formed body using a continuous firing furnace.
  • the firing treatment of the honeycomb formed body by the continuous firing furnace is performed in an inert gas atmosphere such as argon, and the temperature is gradually increased from room temperature and the firing treatment is performed at a maximum temperature of 2000 to 2300 ° C. There becomes a temperature region equal to or greater than 1400 ° C., SiO 2 and the oxidized silicon carbide particles surfaces, silicon monoxide gas attributed to SiO 2 (SiO gas) is generated that contains the silicon carbide as an impurity.
  • this SiO gas moves to a low temperature place in the continuous firing furnace, it solidifies as SiO 2 , accumulates on the inner wall of the muffle in the firing furnace, etc., and hinders the movement of the molded body placed on the conveying member. Inconveniences such as the conveyance member being stopped in conveyance and the molded body falling from the conveyance member occurred, which hindered continuous operation.
  • Patent Document 1 discloses a firing furnace in which silicon monoxide removing means for removing SiO contained in the gas in the muffle is provided in the exhaust path. Specifically, an exhaust pipe extending in the vertical direction is installed on the upper surface of the muffle, and a silicon monoxide removing material for removing silicon monoxide is provided therein.
  • an object of the present invention is to provide a continuous firing furnace capable of continuous operation over a long period of time and capable of producing recrystallized SiC efficiently and continuously.
  • a continuous firing furnace of the present invention is a continuous firing furnace for producing recrystallized SiC by continuously firing a compact containing SiC particles at 2000 to 2300 ° C.
  • An exhaust path for exhausting a gas containing SiO present in the furnace while maintaining a temperature of 1500 to 1900 ° C. is provided in the middle of the continuous firing furnace.
  • gas containing SiO is exhausted through the exhaust path. Since the gas passing through the exhaust path is maintained at a temperature of 1500 to 1900 ° C. by a heater or the like, Thus, the SiO gas hardly solidifies, and clogging does not occur in the exhaust path. In addition, since the gas inside the continuous firing furnace is constantly discharged through the exhaust path, the gas flows inside the continuous firing furnace toward the exhaust path, and the SiO gas is in a low temperature region in the firing furnace. It is difficult to move deposits due to SiO gas in the continuous firing furnace. As a result, it is possible to prevent inconveniences such as the conveyance member being stopped from conveyance or the molded body falling from the conveyance member, and recrystallized SiC can be manufactured continuously and efficiently.
  • the exhaust path is installed in a temperature range of 1500 to 1900 ° C. of the continuous firing furnace.
  • the SiO gas does not precipitate as a solid, and the continuous firing furnace passes through this exhaust path.
  • the gas flows toward a high temperature region, so that deposits due to SiO gas are less likely to deposit inside the continuous firing furnace, and the conveying member conveys It is possible to more effectively prevent the occurrence of inconveniences such as stoppage and falling of the molded body from the conveying member.
  • the exhaust path desirably includes a heater for heating the gas flowing through the exhaust path.
  • a heater for heating the gas flowing through the exhaust path is provided, so that the temperature range can be easily maintained. It is possible to prevent the deposit due to the SiO gas from being deposited in the exhaust path.
  • the heater is preferably made of carbon.
  • the inside of the continuous firing furnace is an inert gas atmosphere, it is difficult to deteriorate due to oxidation, and the inside of the exhaust path is relatively easily 1500. It can be maintained at ⁇ 1900 ° C., and deposition of deposits due to SiO gas can be prevented in the exhaust path.
  • a cyclone-type collection device is installed at the end of the exhaust path.
  • a cyclone-type collecting device is installed at the end of the exhaust path, so that precipitates and the like due to SiO gas can be efficiently recovered outside the exhaust path.
  • the continuous firing furnace is a method of manufacturing a honeycomb fired body by continuously firing a columnar honeycomb formed body including SiC particles and having a plurality of through holes arranged in parallel in the length direction. It is desirable to be a firing furnace.
  • the continuous firing furnace is used as a firing furnace for producing a honeycomb fired body by continuously firing columnar honeycomb formed bodies containing SiC particles and having a plurality of through holes arranged in parallel in the length direction.
  • a honeycomb fired body can be manufactured continuously and efficiently.
  • FIG. 1 (a) is a perspective view schematically showing a honeycomb formed body to be fired in the continuous firing furnace of the present invention
  • FIG. 1 (b) is a view of the honeycomb formed body shown in FIG. 1 (a). It is AA sectional view taken on the line.
  • FIG. 2 is a longitudinal sectional view schematically showing a case where the continuous firing furnace of the present invention is cut in the vertical longitudinal direction along the longitudinal direction.
  • FIG. 3 is a cross-sectional view schematically showing a case where the continuous firing furnace of the present invention is cut in a cross section perpendicular to the longitudinal direction.
  • FIG. 4 is an enlarged cross-sectional view showing an exhaust path portion in the continuous firing furnace shown in FIG. FIG.
  • FIG. 5 is a perspective view showing a honeycomb filter using a honeycomb fired body manufactured by the continuous firing furnace of the present invention.
  • 6 (a) is a perspective view of the honeycomb fired body constituting the honeycomb filter shown in FIG. 5, and
  • FIG. 6 (b) is a cross-sectional view taken along the line BB of the honeycomb fired body shown in FIG. 6 (a).
  • the continuous firing furnace of the present invention is a continuous firing furnace for producing recrystallized SiC by continuously firing a compact containing SiC particles at 2000 to 2300 ° C., and is in the middle of the continuous firing furnace.
  • An exhaust path for exhausting a gas containing SiO present in the furnace while maintaining a temperature of 1500 to 1900 ° C. is provided.
  • the manufacturing method of the molded object containing the said SiC particle is not specifically limited, What is obtained through the following (1) raw material preparation process for molded objects, (2) molded object preparation process, and (3) degreasing process It is desirable that Hereinafter, the manufacturing method of the molded object containing the SiC particle
  • Molded body raw material preparation step In this molded body raw material preparation step, a raw material composition containing a silicon carbide powder (SiC particles) and an organic additive containing at least an organic binder is mixed to obtain a raw material for a molded body. Prepare.
  • the particle size and the like of the silicon carbide powder are not particularly limited, but it is preferable to use two types of silicon carbide powders having different average particle sizes.
  • organic additive examples include an organic binder, a dispersion medium liquid, a plasticizer, and a lubricant.
  • organic binder examples include methyl cellulose, carboxymethyl cellulose, hydroxyethyl cellulose, polyethylene glycol, phenol resin, and epoxy resin. Of these, methylcellulose is preferred.
  • the dispersion medium liquid examples include alcohols such as methanol, organic solvents such as benzene, and water. It does not specifically limit as said plasticizer, For example, glycerol etc. are mentioned.
  • the lubricant is not particularly limited, and examples thereof include polyoxyalkylene compounds such as polyoxyethylene alkyl ether and polyoxypropylene alkyl ether. Specific examples of the lubricant include polyoxyethylene monobutyl ether and polyoxypropylene monobutyl ether.
  • the raw material for a molded body is prepared by mixing silicon carbide powder, an organic binder, and water as a dispersion medium liquid using a wet mixer. In that case, you may add the said plasticizer, the said lubricant, etc. as needed.
  • a honeycomb molded body a molded body containing SiC particles (hereinafter referred to as a honeycomb molded body) is manufactured by extruding the prepared raw material for a molded body.
  • the raw material for the obtained molded body is put into an extrusion molding machine, and extrusion molding is performed to produce a prismatic continuous body.
  • a raw honeycomb formed body in which cells are arranged side by side is manufactured.
  • the raw honeycomb formed body is dried by a dryer to obtain a dried honeycomb formed body.
  • a predetermined amount of a plug material paste is filled in any one end of the cells constituting the dried honeycomb molded body, and the through holes are plugged. Through such a process, a honeycomb formed body in which one end of the cell is plugged is manufactured.
  • FIG. 1 (a) is a perspective view schematically showing a honeycomb formed body to be fired in the continuous firing furnace of the present invention
  • FIG. 1 (b) is a view of the honeycomb formed body shown in FIG. 1 (a). It is AA sectional view taken on the line.
  • the manufactured honeycomb molded body 100 is provided with a large number of cells 110 having one end plugged with a sealing material 120 arranged in the longitudinal direction.
  • a wall 130 is formed between the cells 110.
  • the produced honeycomb formed body is heated to 300 to 650 ° C. in an oxygen-containing atmosphere to oxidatively decompose and completely remove the organic matter.
  • the produced plurality of honeycomb molded bodies are accommodated in a molded body placing jig having a predetermined shape, and the molded body placing jig in which the honeycomb molded body is accommodated is further placed on the conveying member,
  • a degreasing process is performed by carrying in a degreasing furnace.
  • a firing process is performed by carrying the conveying member on which the honeycomb formed body on which the degreasing process has been completed is placed as it is into a continuous firing furnace.
  • FIG. 2 is a longitudinal sectional view schematically showing a cut surface obtained by cutting the continuous firing furnace of the present invention in the vertical longitudinal direction along the longitudinal direction
  • FIG. 3 is a longitudinal view of the firing area of the continuous firing furnace of the present invention. It is sectional drawing which shows typically the cross section cut
  • FIG. 4 is an enlarged cross-sectional view showing an enlarged exhaust path portion in the continuous firing furnace shown in FIG.
  • the continuous firing furnace 10 includes a deaeration area 11, a preheating area 12, a temperature raising / firing area 13, a slow cooling area 14, a cooling area 15, a deaeration sequentially from the inlet direction.
  • Area 16 is provided.
  • the deaeration area 11 is provided in order to change the atmosphere inside and around the honeycomb formed body 100 after the degreasing process to be carried in, and after the honeycomb formed body 100 is placed on the transport member 29 and the like, Once the deaeration area 11 is evacuated and then an inert gas is introduced, the atmosphere inside and around the honeycomb formed body 100 is made an inert gas atmosphere.
  • the inert gas argon, nitrogen or the like is used.
  • the temperature of the honeycomb formed body 100 is gradually raised from room temperature to around 1000 ° C. using the heat of the temperature raising / firing area 13.
  • the temperature is further raised in the temperature raising / firing area 13 and the temperature is raised to 1900 ° C., followed by firing at 2000 to 2300 ° C.
  • This heating step in the temperature raising / firing area 13 corresponds to a firing step, and a honeycomb fired body made of recrystallized SiC (hereinafter referred to as a honeycomb fired body) is manufactured.
  • the fired honeycomb fired body is gradually cooled and further cooled to a temperature close to room temperature in the cooling area 15.
  • the inert gas is removed, air is introduced, and the honeycomb fired body is carried out, thereby completing a series of firing processes of the honeycomb formed body 100. .
  • the preheating area 12 for firing the honeycomb formed body 100, the temperature raising / firing area 13, the slow cooling area 14, and the cooling area 15 are honeycombs.
  • a cylindrical muffle 21 formed so as to secure a space for accommodating the molded body 100 is disposed, and in the temperature raising / firing area 13, heating heaters 22 are arranged above and below the muffle 21 at predetermined intervals. It is installed.
  • the continuous firing furnace 10 includes a heat insulating material 23 provided so as to include a muffle 21 and a heater 22 therein, and a furnace material 24 disposed outside the heat insulating material 23. It is isolated from the surrounding atmosphere by the furnace material 24.
  • the muffle 21 is configured such that the entire floor portion is supported by a support member (not shown), and the honeycomb formed body 100 disposed on the conveying member 29 can be moved.
  • the muffle 21 is provided in the entire area excluding the deaeration areas 11 and 16 and the cooling area 15.
  • Transport means such as a conveyor may be provided inside the muffle 21. In this case, the honeycomb molded body 100 can be automatically transported by placing the transport member 29 on the transport means.
  • a heat insulating material 23 is installed in the preheating area 12, the temperature raising / firing area 13, and the slow cooling area 14, and in the temperature raising / firing area 13, the heat insulating material 23 is provided further outside the heater 22 for heating. It is fixed by a fixing member as appropriate. And the furnace material 24 is provided in the outermost area over the whole area except the deaeration areas 11 and 16.
  • a gas containing SiO existing in the furnace is maintained at a temperature of 1500 to 1900 ° C.
  • An exhaust path 25 for exhausting is installed.
  • the exhaust path 25 includes a heater 26 for heating the gas flowing through the exhaust path 25.
  • the heater 26 is disposed so as to surround the internal pipe 25a.
  • the material of the heater 26 is not particularly limited, but the temperature in the ceramic internal pipe 25a through which the gas in the exhaust passage 25 circulates needs to be maintained at 1500 to 1900 ° C. From this point, a carbon heater is used. It is desirable to be.
  • the inner diameter of the internal pipe 25a is preferably 30 to 150 mm. If it is less than 30 mm, the exhaust amount may be insufficient, or SiO 2 may be deposited in the exhaust passage 25. If it is larger than 150 mm, the heat in the firing furnace escapes from the exhaust passage 25 and leads to energy loss. The exhaust flow rate becomes slow, the gas containing SiO gas is not exhausted sufficiently, and SiO 2 may be deposited in the firing furnace.
  • a heat insulating layer 27 is disposed on the outer periphery of the heater 26 to keep the heater 26 warm and prevent the temperature of the metal external pipe 25b disposed outside.
  • the material of the heat insulating layer 27 is not particularly limited, but is preferably made of porous carbon.
  • a cyclone type collecting device 28 is installed at the end of the exhaust path 25.
  • the structure of the collection device 28 is not particularly limited, but a cyclone type is desirable because it can collect even a small powder and can prevent the collection device 28 from being clogged.
  • the exhaust path 25 is provided with temperature measuring devices 17 a, 17 b, and 17 c at three locations, and a temperature measuring device 17 d is also provided in the collecting device 28, so that the exhaust gas close to the collecting device 28 is exhausted.
  • the path 25 is also provided with a thermometer 17c and constantly monitors the temperature of the exhaust path 25. A thermocouple, a radiation thermometer, etc. can be used as a thermometer.
  • the number of temperature measuring devices for monitoring the temperature is not limited to the above.
  • the honeycomb formed body 100 subjected to the degreasing treatment carried into the continuous firing furnace 10 is oxidized SiO 2 on the surface of silicon carbide particles, or SiO 2 contained as an impurity in silicon carbide.
  • Silicon monoxide gas (SiO gas) which is considered to be caused by the above, is generated. Since the inside of the continuous firing furnace 10 is always maintained at a pressure higher than the atmospheric pressure, the gas inside the continuous firing furnace 10 passes through the exhaust passage 25 disposed in the temperature raising / firing area 13 and is captured. It is discharged to the outside through the collecting device 28. Then, the solidified SiO 2 that has passed through the collection device 28 is collected by the collection device 28.
  • the amount of gas flowing through the exhaust path 25 is preferably 5 to 100 Nm 3 / hr, although it depends on the capacity of the firing furnace.
  • transduce inert gas such as argon.
  • the generated SiO gas also passes through the exhaust path 25, but the gas passing through the exhaust path 25 is kept at a temperature of 1500 to 1900 ° C. by a heater or the like.
  • the gas hardly solidifies, and clogging does not occur inside the exhaust passage 25.
  • the gas inside the continuous firing furnace 10 is steadily discharged through the exhaust passage 25, the gas flows inside the continuous firing furnace 10 toward the exhaust passage 25, and the SiO gas is continuously fired. It is difficult to move to a low temperature region in the furnace 10, and deposits due to SiO gas are difficult to deposit inside the continuous firing furnace 10. As a result, it is possible to prevent inconveniences such as the conveyance member 29 being stopped in conveyance and the honeycomb formed body 100 falling from the conveyance member 29.
  • a porous honeycomb fired body can be manufactured by passing through the continuous firing furnace and finishing the firing treatment of the honeycomb formed body.
  • the structure of the honeycomb fired body is basically the same as that of the honeycomb formed body 100 shown in FIG.
  • an adhesive paste layer is formed on the side surface of the honeycomb fired body to form an adhesive paste layer, and the adhesive paste layer is sequentially passed through the adhesive paste layer.
  • Another honeycomb fired body is laminated. This procedure is repeated to produce an aggregate of honeycomb fired bodies in which a predetermined number of honeycomb fired bodies are bonded via an adhesive paste layer.
  • an adhesive paste what consists of an inorganic binder, an organic binder, an inorganic fiber, and / or an inorganic particle can be used, for example.
  • this aggregate of honeycomb fired bodies is heated to dry and solidify the adhesive paste layer to form an adhesive layer.
  • the honeycomb fired body aggregate is cut into a ceramic block using a diamond cutter or the like, and the outer peripheral coating layer is formed by applying the outer peripheral coating material paste to the outer peripheral surface of the ceramic block and drying and solidifying the ceramic block.
  • the outer periphery coating material paste one having the same composition as the adhesive paste can be used.
  • FIG. 5 is a perspective view showing a honeycomb filter using a honeycomb fired body manufactured by the continuous firing furnace of the present invention.
  • 6 (a) is a perspective view of the honeycomb fired body constituting the honeycomb filter of the present invention shown in FIG. 5, and
  • FIG. 6 (b) is a B ⁇ of the honeycomb fired body shown in FIG. 6 (a). It is B line sectional drawing.
  • the honeycomb filter 40 of the present invention includes a plurality of porous honeycomb fired bodies 30 made of silicon carbide combined with an adhesive layer 41 to form a cylindrical ceramic block 45.
  • a coat layer 42 is formed around the ceramic block 45.
  • the shape of the ceramic block is a columnar shape.
  • the ceramic block is not limited to a columnar shape as long as it is a columnar shape. Any shape may be used.
  • a honeycomb fired body 30 shown in FIG. 6 is manufactured by degreasing and firing the honeycomb formed body 100 shown in FIGS. 1 (a) and 1 (b), and a large number of cells 31 are arranged in the longitudinal direction. Since one of the end portions of the cell 31 is plugged, the cell partition wall 33 that separates the cells 31 functions as a filter. That is, in the cells 31 formed in the honeycomb fired body 30, as shown in FIG. 6B, either the inlet side or the outlet side end of the exhaust gas is plugged with the sealing material 32, The exhaust gas flowing into the cell 31 always passes through the cell partition wall 33 separating the cells 31 and then flows out from the other cells 31.
  • the exhaust gas can be purified by collecting PM such as soot contained in the exhaust gas discharged from the internal combustion engine.
  • Example 1 Manufacture of honeycomb fired body First, as a raw material preparation process for a molded body, 52.0% by weight of coarse silicon carbide powder having an average particle diameter of 22 ⁇ m and fine silicon carbide powder having an average particle diameter of 0.5 ⁇ m 22. 2% by weight, and 3.9% by weight of organic binder (methylcellulose), 2.3% by weight of lubricant (Unilube manufactured by NOF Corporation), 1.0% by weight of glycerin, silica A raw material for a molded body (wet mixture) was obtained by adding 6.5% by weight of powder and 12.1% by weight of water and kneading.
  • organic binder methylcellulose
  • lubricant Unilube manufactured by NOF Corporation
  • a molded body manufacturing step extrusion molding was performed using the obtained raw material for molded body, and a raw honeycomb molded body containing SiC particles was obtained. Subsequently, the raw honeycomb formed body was dried using a microwave dryer, thereby manufacturing a dried body of the honeycomb formed body.
  • the plugging paste is filled in predetermined cells of the dried honeycomb molded body to seal the cells, and the plugged honeycomb molded body 100 shown in FIGS. 1A and 1B is obtained. It was.
  • the wet mixture was used as a sealing material paste. After sealing the cells, the dried honeycomb molded body filled with the plug paste was again dried using a dryer.
  • the plurality of honeycomb formed bodies obtained as described above are placed on a placing jig placed on the conveying member 29 and degreased at 400 ° C., and then continuously shown in FIGS. And it carried in to the continuous baking furnace 10 of the structure shown in FIG. 4, and baked on conditions of 2200 degreeC and 3 hours in argon atmosphere.
  • the gas is exhausted from the exhaust passage 25 provided in the continuous firing furnace 10 under the condition of 20 Nm 3 / hr, the cyclone is operated to introduce argon, and the solidified SiO 2 Was recovered.
  • the set temperature of the exhaust passage 25 is 1900 ° C., and the thermocouples 17a, 17b, The temperature was measured at 17c and 17d.
  • t1 1900 ° C.
  • t2 1895 ° C.
  • t3 1500 ° C.
  • t4 806 ° C.
  • the composition of the powder recovered by the cyclone was C: 30.00 mol%, O: 28.94 mol%, Si: 14.70 mol%, Ca: 14.13 mol%, Fe: 5.24 mol%, and other components: 6. It was 98 mol%, and in a continuous firing furnace without an exhaust path, the composition was almost the same as the composition of the solid deposited in the low temperature region.
  • the continuous firing furnace 10 was continuously operated for 8 hours. However, the exhaust passage 25 was not clogged at all, and almost no solidified SiO 2 was observed inside the continuous firing furnace 10. In addition, before performing Example 1, the continuous baking furnace 10 removed the solidified material of SiO 2 deposited in the furnace.
  • Example 1 Gas was exhausted from the exhaust path in the same manner as in Example 1 except that the heater was not provided in the exhaust path provided in the continuous firing furnace. As a result, 22.2 g of deposits were generated in the exhaust passage 25 when the continuous firing furnace 10 was continuously operated for 8 hours.
  • the composition of the powder recovered by the cyclone was C: 33.75 mol%, O: 30.55 mol%, Si: 10.12 mol%, Ca: 10.55 mol%, Fe: 5.91 mol%, and other components: It was 9.44 mol%, and the powder recovered in Example 1 and its composition were not so different.

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Abstract

The continuous firing furnace of the present invention is used for producing recrystallized SiC by continuously firing a molded article containing SiC particles at 2,000-2,300°C, wherein an exhaust pathway for exhausting gas that contains SiO present in the furnace while maintaining a temperature of 1,500-1,900°C is arranged in the center of the continuous firing furnace.

Description

連続焼成炉Continuous firing furnace
本発明は、連続焼成炉に関する。 The present invention relates to a continuous firing furnace.
バス、トラック等の車両や建設機械等の内燃機関から排出される排ガス中に含有されるスス等のパティキュレート（以下、ＰＭという）やその他の有害成分が環境や人体に害を及ぼすことが最近問題となっている。そこで、排ガス中のＰＭを捕集して排ガスを浄化するハニカムフィルタとして、多孔質ＳｉＣからなるハニカム構造体が種々提案されている。また、排ガス中の有害ガスを浄化するためのハニカム触媒として機能するハニカム構造体も提案されている。 Recently, particulates such as soot (hereinafter referred to as PM) and other harmful components contained in exhaust gas discharged from internal combustion engines such as buses and trucks and construction machinery and the like are harmful to the environment and the human body. It is a problem. Accordingly, various honeycomb structures made of porous SiC have been proposed as honeycomb filters for collecting PM in exhaust gas and purifying the exhaust gas. A honeycomb structure that functions as a honeycomb catalyst for purifying harmful gases in exhaust gas has also been proposed.
このようなハニカム構造体を製造する際には、まず、ＳｉＣ粒子を有機バインダ等と混練した後、押出成形用の金型等を用いて所定の形状に成形し、ハニカム成形体を作製する。この後、得られたハニカム成形体を焼成炉で２０００～２３００℃で焼成処理し、再結晶ＳｉＣからなるハニカム焼成体を製造する。
その後、必要により、このハニカム焼成体を、接着材を介して接着したり、ダイヤモンドカッター等を用いて所定の形状に切削加工することにより、ハニカム構造体を製造する。 When manufacturing such a honeycomb structure, first, SiC particles are kneaded with an organic binder or the like, and then formed into a predetermined shape using an extrusion molding die or the like to prepare a honeycomb formed body. Thereafter, the obtained honeycomb formed body is fired at 2000 to 2300 ° C. in a firing furnace to manufacture a honeycomb fired body made of recrystallized SiC.
Thereafter, if necessary, the honeycomb fired body is bonded through an adhesive or cut into a predetermined shape using a diamond cutter or the like to manufacture a honeycomb structure.
ハニカム成形体の焼成処理を、連続焼成炉を用いて行うことにより、効率よく再結晶ＳｉＣからなるハニカム焼成体を製造することができる。
連続焼成炉によるハニカム成形体の焼成処理は、アルゴン等の不活性ガス雰囲気中で行われ、室温から次第に温度を上げていき、最高温度２０００～２３００℃で焼成処理するが、連続焼成炉の温度が１４００℃以上の温度領域になると、炭化ケイ素粒子表面の酸化されたＳｉＯ２や、炭化ケイ素に不純物として含まれるＳｉＯ２に起因すると考えられる一酸化ケイ素ガス（ＳｉＯガス）が発生する。 A honeycomb fired body made of recrystallized SiC can be manufactured efficiently by firing the honeycomb formed body using a continuous firing furnace.
The firing treatment of the honeycomb formed body by the continuous firing furnace is performed in an inert gas atmosphere such as argon, and the temperature is gradually increased from room temperature and the firing treatment is performed at a maximum temperature of 2000 to 2300 ° C. There becomes a temperature region equal to or greater than 1400 ° C., SiO 2 and the oxidized silicon carbide particles surfaces, silicon monoxide gas attributed to SiO 2 (SiO gas) is generated that contains the silicon carbide as an impurity.
このＳｉＯガスは、連続焼成炉内の低温の場所に移動するとＳｉＯ２として固化し、焼成炉内のマッフルの内壁等に堆積し、搬送部材上に載置された成形体の移動を妨げるため、搬送部材が搬送停止となったり、上記成形体が搬送部材から転落する等の不都合が発生し、連続操業の妨げとなっていた。 When this SiO gas moves to a low temperature place in the continuous firing furnace, it solidifies as SiO 2 , accumulates on the inner wall of the muffle in the firing furnace, etc., and hinders the movement of the molded body placed on the conveying member. Inconveniences such as the conveyance member being stopped in conveyance and the molded body falling from the conveyance member occurred, which hindered continuous operation.
上記した不都合の発生を防止するため、特許文献１には、マッフル内の気体に含まれるＳｉＯを除去する一酸化ケイ素除去手段を排気経路に設けた焼成炉が開示されている。具体的には、マッフルの上面に上下方向に沿って伸びる排気筒が設置され、その内部に一酸化ケイ素を除去する一酸化ケイ素除去材が設けられていた。 In order to prevent the above-described inconvenience, Patent Document 1 discloses a firing furnace in which silicon monoxide removing means for removing SiO contained in the gas in the muffle is provided in the exhaust path. Specifically, an exhaust pipe extending in the vertical direction is installed on the upper surface of the muffle, and a silicon monoxide removing material for removing silicon monoxide is provided therein.
特開２００２－２４９３８５号公報JP 2002-249385 A
しかしながら、特許文献１に開示された焼成炉では、排気筒は、マッフルの最高温度領域には配置されているものの、排気筒の内部は、余り高い温度に維持されていないため、ガスが焼成炉内から排気筒の内部に入ると直ぐに冷却され、多量のＳｉＯ２が排気筒の内部に析出、堆積し、排気筒に短時間で詰まりが発生し、排気筒を設けない焼成炉と同じになってしまうという問題があった。 However, in the firing furnace disclosed in Patent Document 1, although the exhaust pipe is disposed in the maximum temperature region of the muffle, the inside of the exhaust pipe is not maintained at a very high temperature, so that the gas is fired in the firing furnace. As soon as it enters the inside of the exhaust pipe, it is cooled down, and a large amount of SiO 2 is deposited and deposited inside the exhaust pipe, resulting in clogging in the exhaust pipe in a short time, which is the same as a firing furnace without an exhaust pipe. There was a problem that.
本発明は、上記問題点に鑑みてなされたものであり、排気経路にＳｉＯガス等に起因する詰まりが発生せず、また、連続焼成炉の内部にもＳｉＯガスに起因する堆積物が存在しないため、長時間に渡って連続操業が可能で、効率よく、連続的に再結晶ＳｉＣを製造することが可能な連続焼成炉を提供することを目的とする。 The present invention has been made in view of the above problems, and clogging due to SiO gas or the like does not occur in the exhaust path, and deposits due to SiO gas do not exist inside the continuous firing furnace. Therefore, an object of the present invention is to provide a continuous firing furnace capable of continuous operation over a long period of time and capable of producing recrystallized SiC efficiently and continuously.
上記目的を達成するために、本発明の連続焼成炉は、ＳｉＣ粒子を含む成形体を２０００～２３００℃で連続的に焼成処理することにより再結晶ＳｉＣを製造するための連続焼成炉であって、上記連続焼成炉の途中に、炉内に存在するＳｉＯを含むガスを、１５００～１９００℃の温度を保ちながら排気する排気経路が設置されていることを特徴とする。 In order to achieve the above object, a continuous firing furnace of the present invention is a continuous firing furnace for producing recrystallized SiC by continuously firing a compact containing SiC particles at 2000 to 2300 ° C. An exhaust path for exhausting a gas containing SiO present in the furnace while maintaining a temperature of 1500 to 1900 ° C. is provided in the middle of the continuous firing furnace.
上記連続焼成炉では、排気経路でＳｉＯを含むガスの排気を行うが、上記排気経路の内部を通過するガスは、ヒータ等により１５００～１９００℃の温度に保たれているので、排気経路の内部でＳｉＯガスが殆ど固化することはなく、排気経路の内部に詰まりが発生することはない。また、定常的に連続焼成炉の内部のガスが排気経路を経て排出されるので、連続焼成炉の内部は、ガスが排気経路に向かって流れることとなり、ＳｉＯガスは、焼成炉内の低温領域に移動しにくく、連続焼成炉の内部にＳｉＯガスに起因する堆積物が堆積しにくい。その結果、搬送部材が搬送停止となったり、成形体が搬送部材から転落する等の不都合が発生するのを防止することができ、連続的かつ効率的に再結晶ＳｉＣを製造することができる。 In the continuous firing furnace, gas containing SiO is exhausted through the exhaust path. Since the gas passing through the exhaust path is maintained at a temperature of 1500 to 1900 ° C. by a heater or the like, Thus, the SiO gas hardly solidifies, and clogging does not occur in the exhaust path. In addition, since the gas inside the continuous firing furnace is constantly discharged through the exhaust path, the gas flows inside the continuous firing furnace toward the exhaust path, and the SiO gas is in a low temperature region in the firing furnace. It is difficult to move deposits due to SiO gas in the continuous firing furnace. As a result, it is possible to prevent inconveniences such as the conveyance member being stopped from conveyance or the molded body falling from the conveyance member, and recrystallized SiC can be manufactured continuously and efficiently.
本発明の連続焼成炉では、前記排気経路は、上記連続焼成炉の１５００～１９００℃の温度領域に設置されていることが望ましい。 In the continuous firing furnace of the present invention, it is desirable that the exhaust path is installed in a temperature range of 1500 to 1900 ° C. of the continuous firing furnace.
上記連続焼成炉で、排気経路は、連続焼成炉の１５００～１９００℃の温度領域に設置されていると、ＳｉＯガスが固体となって析出することはなく、この排気経路を介して連続焼成炉の内部を流通するガスを連続的に排気することにより、ガスは、高い温度領域に向かって流れるので、連続焼成炉の内部にＳｉＯガスに起因する堆積物がより堆積しにくく、搬送部材が搬送停止となったり、成形体が搬送部材から転落する等の不都合が発生するのをより効果的に防止することができる。 In the continuous firing furnace, when the exhaust path is installed in the temperature range of 1500 to 1900 ° C. of the continuous firing furnace, the SiO gas does not precipitate as a solid, and the continuous firing furnace passes through this exhaust path. By continuously exhausting the gas that circulates inside the gas, the gas flows toward a high temperature region, so that deposits due to SiO gas are less likely to deposit inside the continuous firing furnace, and the conveying member conveys It is possible to more effectively prevent the occurrence of inconveniences such as stoppage and falling of the molded body from the conveying member.
本発明の連続焼成炉では、排気経路は、該排気経路内を流通するガスを加熱するためのヒータを備えていることが望ましい。
上記連続焼成炉で、排気経路が、１５００～１９００℃の温度を保つために、該排気経路内を流通するガスを加熱するためのヒータを備えているので、容易に上記温度範囲に保つことができ、排気経路内にＳｉＯガスに起因する堆積物の堆積を防止することができる。 In the continuous firing furnace of the present invention, the exhaust path desirably includes a heater for heating the gas flowing through the exhaust path.
In the continuous firing furnace, since the exhaust path is maintained at a temperature of 1500 to 1900 ° C., a heater for heating the gas flowing through the exhaust path is provided, so that the temperature range can be easily maintained. It is possible to prevent the deposit due to the SiO gas from being deposited in the exhaust path.
本発明の連続焼成炉では、上記ヒータは、炭素製であることが望ましい。
上記連続焼成炉で、排気経路に設置されたヒータが炭素製であっても、連続焼成炉の内部は不活性ガス雰囲気であるので、酸化により劣化しにくく、比較的容易に排気経路内を１５００～１９００℃に維持することができ、排気経路内にＳｉＯガスに起因する堆積物の堆積を防止することができる。 In the continuous firing furnace of the present invention, the heater is preferably made of carbon.
In the continuous firing furnace, even if the heater installed in the exhaust path is made of carbon, since the inside of the continuous firing furnace is an inert gas atmosphere, it is difficult to deteriorate due to oxidation, and the inside of the exhaust path is relatively easily 1500. It can be maintained at ˜1900 ° C., and deposition of deposits due to SiO gas can be prevented in the exhaust path.
本発明の連続焼成炉では、上記排気経路の末端には、サイクロン型の捕集装置が設置されていることが望ましい。
上記連続焼成炉では、排気経路の末端に、サイクロン型の捕集装置が設置されることにより、ＳｉＯガスに起因する析出物等を、排気経路外で、効率よく回収することができる。 In the continuous firing furnace of the present invention, it is desirable that a cyclone-type collection device is installed at the end of the exhaust path.
In the continuous firing furnace, a cyclone-type collecting device is installed at the end of the exhaust path, so that precipitates and the like due to SiO gas can be efficiently recovered outside the exhaust path.
本発明の連続焼成炉では、上記連続焼成炉は、ＳｉＣ粒子を含み、長さ方向に複数の貫通孔が並設された柱状のハニカム成形体を連続的に焼成処理してハニカム焼成体を製造するための焼成炉であることが望ましい。 In the continuous firing furnace of the present invention, the continuous firing furnace is a method of manufacturing a honeycomb fired body by continuously firing a columnar honeycomb formed body including SiC particles and having a plurality of through holes arranged in parallel in the length direction. It is desirable to be a firing furnace.
上記連続焼成炉を、ＳｉＣ粒子を含み、長さ方向に複数の貫通孔が並設された柱状のハニカム成形体を連続的に焼成処理してハニカム焼成体を製造するための焼成炉として用いることにより、長期間に渡り、連続的に操業を行うことが可能となり、連続的かつ効率的にハニカム焼成体を製造することができる。 The continuous firing furnace is used as a firing furnace for producing a honeycomb fired body by continuously firing columnar honeycomb formed bodies containing SiC particles and having a plurality of through holes arranged in parallel in the length direction. Thus, it becomes possible to continuously operate over a long period of time, and a honeycomb fired body can be manufactured continuously and efficiently.
図１（ａ）は、本発明の連続焼成炉で焼成の対象となるハニカム成形体を模式的に示す斜視図であり、図１（ｂ）は、図１（ａ）に示すハニカム成形体のＡ－Ａ線断面図である。FIG. 1 (a) is a perspective view schematically showing a honeycomb formed body to be fired in the continuous firing furnace of the present invention, and FIG. 1 (b) is a view of the honeycomb formed body shown in FIG. 1 (a). It is AA sectional view taken on the line. 図２は、本発明の連続焼成炉を長手方向に沿って鉛直縦方向に切断した場合を模式的に示す縦断面図である。FIG. 2 is a longitudinal sectional view schematically showing a case where the continuous firing furnace of the present invention is cut in the vertical longitudinal direction along the longitudinal direction. 図３は、本発明の連続焼成炉を長手方向に垂直な断面で切断した場合を模式的に示す断面図である。FIG. 3 is a cross-sectional view schematically showing a case where the continuous firing furnace of the present invention is cut in a cross section perpendicular to the longitudinal direction. 図４は、図３に示した連続焼成炉における排気経路の部分を拡大して示した拡大断面図である。FIG. 4 is an enlarged cross-sectional view showing an exhaust path portion in the continuous firing furnace shown in FIG. 図５は、本発明の連続焼成炉で製造されるハニカム焼成体を用いたハニカムフィルタを示す斜視図である。FIG. 5 is a perspective view showing a honeycomb filter using a honeycomb fired body manufactured by the continuous firing furnace of the present invention. 図６（ａ）は、図５に示したハニカムフィルタを構成するハニカム焼成体の斜視図であり、図６（ｂ）は、図６（ａ）に示したハニカム焼成体のＢ－Ｂ線断面図である。6 (a) is a perspective view of the honeycomb fired body constituting the honeycomb filter shown in FIG. 5, and FIG. 6 (b) is a cross-sectional view taken along the line BB of the honeycomb fired body shown in FIG. 6 (a). FIG.
以下、本発明の連続焼成炉について具体的に説明する。しかしながら、本発明は、以下の記載に限定されるものではなく、本発明の要旨を変更しない範囲において適宜変更して適用することができる。 Hereinafter, the continuous firing furnace of the present invention will be specifically described. However, the present invention is not limited to the following description, and can be appropriately modified and applied without departing from the scope of the present invention.
本発明の連続焼成炉は、ＳｉＣ粒子を含む成形体を２０００～２３００℃で連続的に焼成処理することにより再結晶ＳｉＣを製造するための連続焼成炉であって、前記連続焼成炉の途中に、炉内に存在するＳｉＯを含むガスを、１５００～１９００℃の温度を保ちながら排気する排気経路が設置されていることを特徴とする。 The continuous firing furnace of the present invention is a continuous firing furnace for producing recrystallized SiC by continuously firing a compact containing SiC particles at 2000 to 2300 ° C., and is in the middle of the continuous firing furnace. An exhaust path for exhausting a gas containing SiO present in the furnace while maintaining a temperature of 1500 to 1900 ° C. is provided.
まず、最初に、本発明の連続焼成炉で焼成処理を行う対象となるＳｉＣ粒子を含む成形体について説明することにする。 First, a molded body containing SiC particles to be subjected to a firing process in the continuous firing furnace of the present invention will be described.
上記ＳｉＣ粒子を含む成形体の作製方法は特に限定されるものではないが、下記する（１）成形体用原料調製工程、（２）成形体作製工程及び（３）脱脂工程を経て得られるものであることが望ましい。以下、上記工程を含むＳｉＣ粒子を含む成形体の作製方法について説明していく。 Although the manufacturing method of the molded object containing the said SiC particle is not specifically limited, What is obtained through the following (1) raw material preparation process for molded objects, (2) molded object preparation process, and (3) degreasing process It is desirable that Hereinafter, the manufacturing method of the molded object containing the SiC particle | grains including the said process is demonstrated.
（１）成形体用原料調製工程
この成形体用原料調製工程では、炭化ケイ素粉末（ＳｉＣ粒子）、及び、少なくとも有機バインダを含む有機添加物を含む原料組成物を混合して成形体用原料を調製する。 (1) Molded body raw material preparation step In this molded body raw material preparation step, a raw material composition containing a silicon carbide powder (SiC particles) and an organic additive containing at least an organic binder is mixed to obtain a raw material for a molded body. Prepare.
炭化ケイ素粉末の粒径等は、特に限定されるものではないが、平均粒子径の異なる２種類の炭化ケイ素粉末を用いることが好ましい。 The particle size and the like of the silicon carbide powder are not particularly limited, but it is preferable to use two types of silicon carbide powders having different average particle sizes.
有機添加物としては、有機バインダが挙げられるほか、分散媒液、可塑剤、潤滑剤等が挙げられる。
上記有機バインダとしては、例えば、メチルセルロース、カルボキシメチルセルロース、ヒドロキシエチルセルロース、ポリエチレングリコール、フェノール樹脂、エポキシ樹脂等が挙げられる。これらのなかでは、メチルセルロースが好ましい。 Examples of the organic additive include an organic binder, a dispersion medium liquid, a plasticizer, and a lubricant.
Examples of the organic binder include methyl cellulose, carboxymethyl cellulose, hydroxyethyl cellulose, polyethylene glycol, phenol resin, and epoxy resin. Of these, methylcellulose is preferred.
上記分散媒液としては、例えば、メタノール等のアルコール、ベンゼン等の有機溶媒が挙げられるほか、水が挙げられる。上記可塑剤としては特に限定されず、例えば、グリセリン等が挙げられる。 Examples of the dispersion medium liquid include alcohols such as methanol, organic solvents such as benzene, and water. It does not specifically limit as said plasticizer, For example, glycerol etc. are mentioned.
上記潤滑剤としては特に限定されず、例えば、ポリオキシエチレンアルキルエーテル、ポリオキシプロピレンアルキルエーテル等のポリオキシアルキレン系化合物等が挙げられる。上記潤滑剤の具体例としては、例えば、ポリオキシエチレンモノブチルエーテル、ポリオキシプロピレンモノブチルエーテル等が挙げられる。 The lubricant is not particularly limited, and examples thereof include polyoxyalkylene compounds such as polyoxyethylene alkyl ether and polyoxypropylene alkyl ether. Specific examples of the lubricant include polyoxyethylene monobutyl ether and polyoxypropylene monobutyl ether.
上記成形体用原料を調製する際には、炭化ケイ素粉末、有機バインダ、及び、分散媒液である水を、湿式混合機を用いて混合することにより成形体用原料を調製する。その際、必要により、上記可塑剤や上記潤滑剤等を加えてもよい。 When preparing the raw material for a molded body, the raw material for a molded body is prepared by mixing silicon carbide powder, an organic binder, and water as a dispersion medium liquid using a wet mixer. In that case, you may add the said plasticizer, the said lubricant, etc. as needed.
（２）成形体作製工程
この成形体作製工程では、調製した成形体用原料を押出成形することによりＳｉＣ粒子を含む成形体（以下、ハニカム成形体という）を作製する。
この工程では、得られた成形体用原料を押出成形機に投入して、押出成形を行い、角柱形状の連続体を作製した後、所定の長さに切断することにより、長手方向に多数のセルが並設された生のハニカム成形体を作製する。この生のハニカム成形体を乾燥機により乾燥させ、ハニカム成形体の乾燥体とする。 (2) Molded body manufacturing process In this molded body manufacturing process, a molded body containing SiC particles (hereinafter referred to as a honeycomb molded body) is manufactured by extruding the prepared raw material for a molded body.
In this step, the raw material for the obtained molded body is put into an extrusion molding machine, and extrusion molding is performed to produce a prismatic continuous body. A raw honeycomb formed body in which cells are arranged side by side is manufactured. The raw honeycomb formed body is dried by a dryer to obtain a dried honeycomb formed body.
次いで、ハニカム成形体の乾燥体を構成するセルのいずれかの端部に、封止材ペーストを所定量充填し、貫通孔を目封止する。このような工程を経て、セルの一端部が目封止されたハニカム成形体を作製する。 Next, a predetermined amount of a plug material paste is filled in any one end of the cells constituting the dried honeycomb molded body, and the through holes are plugged. Through such a process, a honeycomb formed body in which one end of the cell is plugged is manufactured.
図１（ａ）は、本発明の連続焼成炉で焼成の対象となるハニカム成形体を模式的に示す斜視図であり、図１（ｂ）は、図１（ａ）に示すハニカム成形体のＡ－Ａ線断面図である。
図１（ａ）及び（ｂ）に示すように、作製されたハニカム成形体１００には、一端部が封止材１２０により目封止された多数のセル１１０が長手方向に並設されており、これらのセル１１０の間には壁部１３０が形成されている。 FIG. 1 (a) is a perspective view schematically showing a honeycomb formed body to be fired in the continuous firing furnace of the present invention, and FIG. 1 (b) is a view of the honeycomb formed body shown in FIG. 1 (a). It is AA sectional view taken on the line.
As shown in FIGS. 1A and 1B, the manufactured honeycomb molded body 100 is provided with a large number of cells 110 having one end plugged with a sealing material 120 arranged in the longitudinal direction. A wall 130 is formed between the cells 110.
（３）脱脂工程
次に、脱脂工程として、作製されたハニカム成形体を、酸素含有雰囲気中、３００～６５０℃に加熱することにより、有機物を酸化分解させて完全に除去する。
この脱脂処理では、作製された複数のハニカム成形体を所定形状の成形体載置用冶具に収容し、さらにハニカム成形体が収容された成形体載置用冶具を搬送部材上に載置し、脱脂炉に搬入することにより脱脂処理を行う。
通常は、この脱脂処理が終了したハニカム成形体が載置された上記搬送部材を、そのまま連続焼成炉に搬入することにより、焼成処理を行う。 (3) Degreasing Step Next, as the degreasing step, the produced honeycomb formed body is heated to 300 to 650 ° C. in an oxygen-containing atmosphere to oxidatively decompose and completely remove the organic matter.
In this degreasing process, the produced plurality of honeycomb molded bodies are accommodated in a molded body placing jig having a predetermined shape, and the molded body placing jig in which the honeycomb molded body is accommodated is further placed on the conveying member, A degreasing process is performed by carrying in a degreasing furnace.
Usually, a firing process is performed by carrying the conveying member on which the honeycomb formed body on which the degreasing process has been completed is placed as it is into a continuous firing furnace.
図２は、本発明の連続焼成炉を長手方向に沿って鉛直縦方向に切断した切断面を模式的に示す縦断面図であり、図３は、本発明の連続焼成炉の焼成エリアを長手方向に垂直な断面で切断した断面を模式的に示す断面図である。また、図４は、図３に示した連続焼成炉における排気経路の部分を拡大して示した拡大断面図である。 FIG. 2 is a longitudinal sectional view schematically showing a cut surface obtained by cutting the continuous firing furnace of the present invention in the vertical longitudinal direction along the longitudinal direction, and FIG. 3 is a longitudinal view of the firing area of the continuous firing furnace of the present invention. It is sectional drawing which shows typically the cross section cut | disconnected by the cross section perpendicular | vertical to a direction. FIG. 4 is an enlarged cross-sectional view showing an enlarged exhaust path portion in the continuous firing furnace shown in FIG.
図２に示すように、本発明に係る連続焼成炉１０には、入口方向から順次、脱気エリア１１、予熱エリア１２、昇温・焼成エリア１３、徐冷エリア１４、冷却エリア１５、脱気エリア１６が設けられている。 As shown in FIG. 2, the continuous firing furnace 10 according to the present invention includes a deaeration area 11, a preheating area 12, a temperature raising / firing area 13, a slow cooling area 14, a cooling area 15, a deaeration sequentially from the inlet direction. Area 16 is provided.
脱気エリア１１は、搬入する脱脂工程が終了したハニカム成形体１００の内部や周囲の雰囲気を変えるために設けられており、ハニカム成形体１００を搬送部材２９等に載置して搬入した後、一旦、脱気エリア１１を真空にし、続いて不活性ガスを導入することにより、ハニカム成形体１００の内部や周囲の雰囲気を不活性ガス雰囲気とする。不活性ガスとしては、アルゴン、窒素等が用いられる。 The deaeration area 11 is provided in order to change the atmosphere inside and around the honeycomb formed body 100 after the degreasing process to be carried in, and after the honeycomb formed body 100 is placed on the transport member 29 and the like, Once the deaeration area 11 is evacuated and then an inert gas is introduced, the atmosphere inside and around the honeycomb formed body 100 is made an inert gas atmosphere. As the inert gas, argon, nitrogen or the like is used.
予熱エリア１２では、昇温・焼成エリア１３の熱を利用してハニカム成形体１００の温度を、室温から１０００℃付近まで徐々に昇温させる。 In the preheating area 12, the temperature of the honeycomb formed body 100 is gradually raised from room temperature to around 1000 ° C. using the heat of the temperature raising / firing area 13.
次に、昇温・焼成エリア１３でさらに温度を上昇させ１９００℃まで昇温させた後、２０００～２３００℃で焼成を行なう。この昇温・焼成エリア１３内での加熱工程は、焼成工程に相当し、再結晶ＳｉＣからなるハニカム焼成体（以下、ハニカム焼成体という）が製造される。徐冷エリア１４では、焼成後のハニカム焼成体を徐々に冷却し、さらに冷却エリア１５で室温に近い温度まで冷却する。そして、脱気エリア１６にハニカム成形体１００を搬入した後、不活性ガスを抜いて空気を導入し、ハニカム焼成体を搬出することにより、ハニカム成形体１００の焼成処理の一連の流れが完了する。 Next, the temperature is further raised in the temperature raising / firing area 13 and the temperature is raised to 1900 ° C., followed by firing at 2000 to 2300 ° C. This heating step in the temperature raising / firing area 13 corresponds to a firing step, and a honeycomb fired body made of recrystallized SiC (hereinafter referred to as a honeycomb fired body) is manufactured. In the slow cooling area 14, the fired honeycomb fired body is gradually cooled and further cooled to a temperature close to room temperature in the cooling area 15. Then, after the honeycomb formed body 100 is carried into the deaeration area 16, the inert gas is removed, air is introduced, and the honeycomb fired body is carried out, thereby completing a series of firing processes of the honeycomb formed body 100. .
次に、上記連続焼成炉の構成の一例を説明する。
図２、図３及び図４に示したように、連続焼成炉１０において、ハニカム成形体１００の焼成を行う予熱エリア１２、昇温・焼成エリア１３、徐冷エリア１４及び冷却エリア１５は、ハニカム成形体１００を収容する空間を確保するように形成された筒状のマッフル２１が配置されており、昇温・焼成エリア１３では、マッフル２１の上方及び下方に所定間隔で加熱用ヒータ２２が配設されている。 Next, an example of the configuration of the continuous firing furnace will be described.
As shown in FIGS. 2, 3 and 4, in the continuous firing furnace 10, the preheating area 12 for firing the honeycomb formed body 100, the temperature raising / firing area 13, the slow cooling area 14, and the cooling area 15 are honeycombs. A cylindrical muffle 21 formed so as to secure a space for accommodating the molded body 100 is disposed, and in the temperature raising / firing area 13, heating heaters 22 are arranged above and below the muffle 21 at predetermined intervals. It is installed.
また、連続焼成炉１０は、マッフル２１と加熱用ヒータ２２とをその内部に含むように設けられた断熱材２３と、断熱材２３の外側に配設された炉材２４とを備えており、炉材２４により周囲の雰囲気と隔離されている。 The continuous firing furnace 10 includes a heat insulating material 23 provided so as to include a muffle 21 and a heater 22 therein, and a furnace material 24 disposed outside the heat insulating material 23. It is isolated from the surrounding atmosphere by the furnace material 24.
マッフル２１は、図示しない支持部材により床部分の全体が支持されており、搬送部材２９上に配置されたハニカム成形体１００を移動させることができるように構成されている。マッフル２１は、脱気エリア１１、１６および冷却エリア１５を除いた全域に設けられている。マッフル２１の内部にはコンベア等の輸送手段が設けられていてもよい。この場合、搬送部材２９を輸送手段に載置することにより、ハニカム成形体１００の自動輸送が可能となる。 The muffle 21 is configured such that the entire floor portion is supported by a support member (not shown), and the honeycomb formed body 100 disposed on the conveying member 29 can be moved. The muffle 21 is provided in the entire area excluding the deaeration areas 11 and 16 and the cooling area 15. Transport means such as a conveyor may be provided inside the muffle 21. In this case, the honeycomb molded body 100 can be automatically transported by placing the transport member 29 on the transport means.
予熱エリア１２、昇温・焼成エリア１３及び徐冷エリア１４には、断熱材２３が設置されており、昇温・焼成エリア１３では、断熱材２３は加熱用ヒータ２２のさらに外側に設けられており、適宜固定部材により固定されている。そして、一番外側には、脱気エリア１１、１６を除いた全域にわたって炉材２４が設けられている。 A heat insulating material 23 is installed in the preheating area 12, the temperature raising / firing area 13, and the slow cooling area 14, and in the temperature raising / firing area 13, the heat insulating material 23 is provided further outside the heater 22 for heating. It is fixed by a fixing member as appropriate. And the furnace material 24 is provided in the outermost area over the whole area except the deaeration areas 11 and 16.
また、図３及び図４に示すように、昇温・焼成エリア１３内の１５００～１９００℃の温度領域には、炉内に存在するＳｉＯを含むガスを、１５００～１９００℃の温度を保ちながら排気する排気経路２５が設置されている。 Further, as shown in FIGS. 3 and 4, in a temperature range of 1500 to 1900 ° C. in the temperature raising / firing area 13, a gas containing SiO existing in the furnace is maintained at a temperature of 1500 to 1900 ° C. An exhaust path 25 for exhausting is installed.
図４に示すように、この排気経路２５は、排気経路２５の内部を流通するガスを加熱するためのヒータ２６を備えている。ヒータ２６は、内部配管２５ａを取り囲むように配設されている。ヒータ２６の材料は特に限定されるものではないが、排気経路２５のガスが流通するセラミック製の内部配管２５ａ内の温度を１５００～１９００℃に保つ必要があり、この点から炭素製のヒータであることが望ましい。内部配管２５ａの内径は、３０～１５０ｍｍであることが望ましい。３０ｍｍ未満では、排気量が不充分になったり、排気経路２５内にＳｉＯ２が堆積することがあり、１５０ｍｍより大きいと焼成炉内の熱が排気経路２５から逃げエネルギーロスにつながってしまったり、排気流速が遅くなり、ＳｉＯガスを含むガスが充分に排気されず、焼成炉内にＳｉＯ２が堆積することがある。 As shown in FIG. 4, the exhaust path 25 includes a heater 26 for heating the gas flowing through the exhaust path 25. The heater 26 is disposed so as to surround the internal pipe 25a. The material of the heater 26 is not particularly limited, but the temperature in the ceramic internal pipe 25a through which the gas in the exhaust passage 25 circulates needs to be maintained at 1500 to 1900 ° C. From this point, a carbon heater is used. It is desirable to be. The inner diameter of the internal pipe 25a is preferably 30 to 150 mm. If it is less than 30 mm, the exhaust amount may be insufficient, or SiO 2 may be deposited in the exhaust passage 25. If it is larger than 150 mm, the heat in the firing furnace escapes from the exhaust passage 25 and leads to energy loss. The exhaust flow rate becomes slow, the gas containing SiO gas is not exhausted sufficiently, and SiO 2 may be deposited in the firing furnace.
また、ヒータ２６の外側の外周には、ヒータ２６を保温し、かつ、外側に配設された金属製の外部配管２５ｂの温度上昇を防止するための断熱層２７が配置されている。断熱層２７の材料は特に限定されるものではないが、多孔質の炭素製であることが望ましい。 A heat insulating layer 27 is disposed on the outer periphery of the heater 26 to keep the heater 26 warm and prevent the temperature of the metal external pipe 25b disposed outside. The material of the heat insulating layer 27 is not particularly limited, but is preferably made of porous carbon.
さらに、排気経路２５の末端には、サイクロン型の捕集装置２８が設置されている。捕集装置２８の構造は特に限定されるものではないが、小さな粉末でも捕集が可能であること、捕集装置２８が詰まるのを防止することが可能である点からサイクロン型が望ましい。
また、この排気経路２５には、３個所に測温器１７ａ、１７ｂ、１７ｃが設けられるとともに、捕集装置２８内にも、測温器１７ｄが設けられており、捕集装置２８に近い排気経路２５にも、測温器１７ｃが設けられており、常時、排気経路２５の温度を監視している。測温器としては、熱電対、放射温度計などが使用できる。温度を監視するための測温器の数は、上記に限定されるものではない。 Further, a cyclone type collecting device 28 is installed at the end of the exhaust path 25. The structure of the collection device 28 is not particularly limited, but a cyclone type is desirable because it can collect even a small powder and can prevent the collection device 28 from being clogged.
The exhaust path 25 is provided with temperature measuring devices 17 a, 17 b, and 17 c at three locations, and a temperature measuring device 17 d is also provided in the collecting device 28, so that the exhaust gas close to the collecting device 28 is exhausted. The path 25 is also provided with a thermometer 17c and constantly monitors the temperature of the exhaust path 25. A thermocouple, a radiation thermometer, etc. can be used as a thermometer. The number of temperature measuring devices for monitoring the temperature is not limited to the above.
連続焼成炉１０に搬入される脱脂処理されたハニカム成形体１００は、炉内の温度が１４００℃を超えると、炭化ケイ素粒子表面の酸化されたＳｉＯ２や、炭化ケイ素に不純物として含まれるＳｉＯ２に起因すると考えられる一酸化ケイ素ガス（ＳｉＯガス）が発生する。
連続焼成炉１０の内部は、常に大気圧よりも高い気圧に維持されているので、連続焼成炉１０の内部のガスは、昇温・焼成エリア１３に配置された排気経路２５を通過し、捕集装置２８を通って外部に放出される。そして、捕集装置２８を通過し、固化したＳｉＯ２は、捕集装置２８により捕集される。排気経路２５を通過するガスの流通量は、焼成炉の容量にもよるが、５～１００Ｎｍ３／ｈｒであることが望ましい。なお、捕集装置２８では、連続焼成炉１０より排出されるガスを冷却するために、アルゴン等の不活性ガスを導入することが望ましい。 When the temperature in the furnace exceeds 1400 ° C., the honeycomb formed body 100 subjected to the degreasing treatment carried into the continuous firing furnace 10 is oxidized SiO 2 on the surface of silicon carbide particles, or SiO 2 contained as an impurity in silicon carbide. Silicon monoxide gas (SiO gas), which is considered to be caused by the above, is generated.
Since the inside of the continuous firing furnace 10 is always maintained at a pressure higher than the atmospheric pressure, the gas inside the continuous firing furnace 10 passes through the exhaust passage 25 disposed in the temperature raising / firing area 13 and is captured. It is discharged to the outside through the collecting device 28. Then, the solidified SiO 2 that has passed through the collection device 28 is collected by the collection device 28. The amount of gas flowing through the exhaust path 25 is preferably 5 to 100 Nm 3 / hr, although it depends on the capacity of the firing furnace. In addition, in the collection apparatus 28, in order to cool the gas discharged | emitted from the continuous baking furnace 10, it is desirable to introduce | transduce inert gas, such as argon.
従って、発生したＳｉＯガスも、排気経路２５を通過するが、排気経路２５の内部を通過するガスは、ヒータ等により１５００～１９００℃の温度に保たれているので、排気経路２５の内部でＳｉＯガスが殆ど固化することはなく、排気経路２５の内部に詰まりが発生することはない。また、定常的に連続焼成炉１０の内部のガスが排気経路２５を経て排出されるので、連続焼成炉１０の内部は、ガスが排気経路２５に向かって流れることとなり、ＳｉＯガスは、連続焼成炉１０内の低温領域に移動しにくく、連続焼成炉１０の内部にＳｉＯガスに起因する堆積物が堆積しにくい。その結果、搬送部材２９が搬送停止となったり、ハニカム成形体１００が搬送部材２９から転落する等の不都合が発生するのを防止することができる。 Therefore, the generated SiO gas also passes through the exhaust path 25, but the gas passing through the exhaust path 25 is kept at a temperature of 1500 to 1900 ° C. by a heater or the like. The gas hardly solidifies, and clogging does not occur inside the exhaust passage 25. Further, since the gas inside the continuous firing furnace 10 is steadily discharged through the exhaust passage 25, the gas flows inside the continuous firing furnace 10 toward the exhaust passage 25, and the SiO gas is continuously fired. It is difficult to move to a low temperature region in the furnace 10, and deposits due to SiO gas are difficult to deposit inside the continuous firing furnace 10. As a result, it is possible to prevent inconveniences such as the conveyance member 29 being stopped in conveyance and the honeycomb formed body 100 falling from the conveyance member 29.
連続焼成炉を通過し、ハニカム成形体の焼成処理が終了することにより、多孔質のハニカム焼成体を製造することができる。ハニカム焼成体の構造は、基本的に、図１に示したハニカム成形体１００と同様である。 A porous honeycomb fired body can be manufactured by passing through the continuous firing furnace and finishing the firing treatment of the honeycomb formed body. The structure of the honeycomb fired body is basically the same as that of the honeycomb formed body 100 shown in FIG.
得られたハニカム焼成体を用いてハニカムフィルタを製造する際には、上記ハニカム焼成体の側面に、接着材ペーストを塗布して接着材ペースト層を形成し、この接着材ペースト層を介して順次他のハニカム焼成体を積層する。この手順を繰り返して所定数のハニカム焼成体が接着材ペースト層を介して接着されたハニカム焼成体の集合体を作製する。なお、接着材ペーストとしては、例えば、無機バインダと有機バインダと無機繊維及び／又は無機粒子とからなるものを使用することができる。 When manufacturing a honeycomb filter using the obtained honeycomb fired body, an adhesive paste layer is formed on the side surface of the honeycomb fired body to form an adhesive paste layer, and the adhesive paste layer is sequentially passed through the adhesive paste layer. Another honeycomb fired body is laminated. This procedure is repeated to produce an aggregate of honeycomb fired bodies in which a predetermined number of honeycomb fired bodies are bonded via an adhesive paste layer. In addition, as an adhesive paste, what consists of an inorganic binder, an organic binder, an inorganic fiber, and / or an inorganic particle can be used, for example.
次に、このハニカム焼成体の集合体を加熱して接着材ペースト層を乾燥、固化させて接着材層とする。その後、ダイヤモンドカッター等を用いてハニカム焼成体の集合体に切削加工を施してセラミックブロックとし、セラミックブロックの外周面に外周コート材ペーストを塗布して乾燥固化させることにより外周コート層を形成することにより、ハニカムフィルタを製造することができる。上記外周コート材ペーストとして、接着材ペーストと同様の組成のものを使用することができる。 Next, this aggregate of honeycomb fired bodies is heated to dry and solidify the adhesive paste layer to form an adhesive layer. Thereafter, the honeycomb fired body aggregate is cut into a ceramic block using a diamond cutter or the like, and the outer peripheral coating layer is formed by applying the outer peripheral coating material paste to the outer peripheral surface of the ceramic block and drying and solidifying the ceramic block. Thus, a honeycomb filter can be manufactured. As the outer periphery coating material paste, one having the same composition as the adhesive paste can be used.
図５は、本発明の連続焼成炉で製造されるハニカム焼成体を用いたハニカムフィルタを示す斜視図である。図６（ａ）は、図５に示した本発明のハニカムフィルタを構成するハニカム焼成体の斜視図であり、図６（ｂ）は、図６（ａ）に示したハニカム焼成体のＢ－Ｂ線断面図である。 FIG. 5 is a perspective view showing a honeycomb filter using a honeycomb fired body manufactured by the continuous firing furnace of the present invention. 6 (a) is a perspective view of the honeycomb fired body constituting the honeycomb filter of the present invention shown in FIG. 5, and FIG. 6 (b) is a B− of the honeycomb fired body shown in FIG. 6 (a). It is B line sectional drawing.
図５に示すように、本発明のハニカムフィルタ４０は、炭化ケイ素からなる多孔質のハニカム焼成体３０が、接着材層４１を介して複数個組み合わされて円柱状のセラミックブロック４５を構成し、このセラミックブロック４５の周囲にコート層４２が形成されている。 As shown in FIG. 5, the honeycomb filter 40 of the present invention includes a plurality of porous honeycomb fired bodies 30 made of silicon carbide combined with an adhesive layer 41 to form a cylindrical ceramic block 45. A coat layer 42 is formed around the ceramic block 45.
図５に示したハニカムフィルタ４０では、セラミックブロックの形状は円柱状であるが、本発明において、セラミックブロックは、柱状であれば円柱状に限定されることはなく、例えば、楕円柱状や角柱状等任意の形状のものであってもよい。 In the honeycomb filter 40 shown in FIG. 5, the shape of the ceramic block is a columnar shape. However, in the present invention, the ceramic block is not limited to a columnar shape as long as it is a columnar shape. Any shape may be used.
図６に示すハニカム焼成体３０は、図１（ａ）及び（ｂ）に示したハニカム成形体１００が脱脂、焼成されることにより製造されたものであり、長手方向に多数のセル３１が並設され、セル３１のいずれかの端部が目封止されているため、セル３１同士を隔てるセル隔壁３３がフィルタとして機能するようになっている。即ち、ハニカム焼成体３０に形成されたセル３１は、図６（ｂ）に示したように、排気ガスの入口側又は出口側の端部のいずれかが封止材３２により目封じされ、一のセル３１に流入した排気ガスは、必ずセル３１を隔てるセル隔壁３３を通過した後、他のセル３１から流出するようになっている。 A honeycomb fired body 30 shown in FIG. 6 is manufactured by degreasing and firing the honeycomb formed body 100 shown in FIGS. 1 (a) and 1 (b), and a large number of cells 31 are arranged in the longitudinal direction. Since one of the end portions of the cell 31 is plugged, the cell partition wall 33 that separates the cells 31 functions as a filter. That is, in the cells 31 formed in the honeycomb fired body 30, as shown in FIG. 6B, either the inlet side or the outlet side end of the exhaust gas is plugged with the sealing material 32, The exhaust gas flowing into the cell 31 always passes through the cell partition wall 33 separating the cells 31 and then flows out from the other cells 31.
このように構成されたハニカムフィルタでは、内燃機関から排出される排ガス中に含有されるスス等のＰＭを捕集することにより、排ガスを浄化することができる。 In the honeycomb filter configured as described above, the exhaust gas can be purified by collecting PM such as soot contained in the exhaust gas discharged from the internal combustion engine.
（実施例）
以下、本発明の実施形態をより具体的に開示した実施例を示す。なお、本発明はこれらの実施例のみに限定されるものではない。 (Example)
Examples that specifically disclose the embodiments of the present invention will be described below. In addition, this invention is not limited only to these Examples.
（実施例１）
（１）ハニカム焼成体の製造
まず、成形体用原料調製工程として、平均粒子径２２μｍを有する炭化ケイ素の粗粉末５２．０重量％と、平均粒子径０．５μｍの炭化ケイ素の微粉末２２．２重量％とを混合し、得られた混合物に対して、有機バインダ（メチルセルロース）３．９重量％、潤滑剤（日油社製　ユニルーブ）２．３重量％、グリセリン１．０重量％、シリカ粉末６．５重量％、及び、水１２．１重量％を加えて混練して成形体用原料（湿潤混合物）を得た。 (Example 1)
(1) Manufacture of honeycomb fired body First, as a raw material preparation process for a molded body, 52.0% by weight of coarse silicon carbide powder having an average particle diameter of 22 μm and fine silicon carbide powder having an average particle diameter of 0.5 μm 22. 2% by weight, and 3.9% by weight of organic binder (methylcellulose), 2.3% by weight of lubricant (Unilube manufactured by NOF Corporation), 1.0% by weight of glycerin, silica A raw material for a molded body (wet mixture) was obtained by adding 6.5% by weight of powder and 12.1% by weight of water and kneading.
この後、成形体作製工程として、得られた成形体用原料を用いて押出成形を行い、ＳｉＣ粒子を含む生のハニカム成形体を得た。次いで、マイクロ波乾燥機を用いて上記生のハニカム成形体を乾燥させることにより、ハニカム成形体の乾燥体を作製した。 Thereafter, as a molded body manufacturing step, extrusion molding was performed using the obtained raw material for molded body, and a raw honeycomb molded body containing SiC particles was obtained. Subsequently, the raw honeycomb formed body was dried using a microwave dryer, thereby manufacturing a dried body of the honeycomb formed body.
その後、ハニカム成形体の乾燥体の所定のセルに封止材ペーストを充填してセルの封止を行い、図１（ａ）及び（ｂ）に示す目封止されたハニカム成形体１００を得た。なお、上記湿潤混合物を封止材ペーストとして使用した。セルの封止を行った後、封止材ペーストを充填したハニカム成形体の乾燥体を再び乾燥機を用いて乾燥させた。 Thereafter, the plugging paste is filled in predetermined cells of the dried honeycomb molded body to seal the cells, and the plugged honeycomb molded body 100 shown in FIGS. 1A and 1B is obtained. It was. The wet mixture was used as a sealing material paste. After sealing the cells, the dried honeycomb molded body filled with the plug paste was again dried using a dryer.
上記のようにして得られた複数のハニカム成形体を、搬送部材２９上に設置された載置冶具上に載置し、４００℃で脱脂処理を行った後、連続的に図２、図３及び図４に示す構成の連続焼成炉１０に搬入して、アルゴン雰囲気中、２２００℃、３時間の条件で焼成処理を行った。 The plurality of honeycomb formed bodies obtained as described above are placed on a placing jig placed on the conveying member 29 and degreased at 400 ° C., and then continuously shown in FIGS. And it carried in to the continuous baking furnace 10 of the structure shown in FIG. 4, and baked on conditions of 2200 degreeC and 3 hours in argon atmosphere.
ハニカム成形体の焼成処理を行っている間、連続焼成炉１０に設けられた排気経路２５からガスを２０Ｎｍ３／ｈｒの条件で排気させ、サイクロンを稼働させてアルゴンを導入し、固化したＳｉＯ２を回収した。
排気経路２５の設定温度は、１９００℃とし、連続焼成炉出口（ｔ１）、排気経路中央（ｔ２）、排気経路出口（ｔ３）、サイクロン内（ｔ４）の４ヶ所において、熱電対１７ａ、１７ｂ、１７ｃ、１７ｄで温度を測定した。その結果、ｔ１＝１９００℃、ｔ２＝１８９５℃、ｔ３＝１５００℃、ｔ４＝８０６℃であった。 During the firing treatment of the honeycomb formed body, the gas is exhausted from the exhaust passage 25 provided in the continuous firing furnace 10 under the condition of 20 Nm 3 / hr, the cyclone is operated to introduce argon, and the solidified SiO 2 Was recovered.
The set temperature of the exhaust passage 25 is 1900 ° C., and the thermocouples 17a, 17b, The temperature was measured at 17c and 17d. As a result, t1 = 1900 ° C., t2 = 1895 ° C., t3 = 1500 ° C., t4 = 806 ° C.
サイクロンにより回収した粉末の組成は、Ｃ：３０．００ｍｏｌ％、Ｏ：２８．９４ｍｏｌ％、Ｓｉ：１４．７０ｍｏｌ％、Ｃａ：１４．１３ｍｏｌ％、Ｆｅ：５．２４ｍｏｌ％、その他の成分：６．９８ｍｏｌ％であり、排気経路を設けなかった連続焼成炉において、低温領域で析出した固体の組成とほぼ同様の組成であった。 The composition of the powder recovered by the cyclone was C: 30.00 mol%, O: 28.94 mol%, Si: 14.70 mol%, Ca: 14.13 mol%, Fe: 5.24 mol%, and other components: 6. It was 98 mol%, and in a continuous firing furnace without an exhaust path, the composition was almost the same as the composition of the solid deposited in the low temperature region.
上記条件で、連続焼成炉１０を８時間、連続稼働させたが、排気経路２５に詰まりは全く見られず、連続焼成炉１０の内部にＳｉＯ２の固化物も殆ど観察されなかった。なお、連続焼成炉１０は、実施例１を行う前に、炉内に析出したＳｉＯ２の固化物を除去しておいた。 Under the above conditions, the continuous firing furnace 10 was continuously operated for 8 hours. However, the exhaust passage 25 was not clogged at all, and almost no solidified SiO 2 was observed inside the continuous firing furnace 10. In addition, before performing Example 1, the continuous baking furnace 10 removed the solidified material of SiO 2 deposited in the furnace.
（比較例１）
連続焼成炉に設ける排気経路にヒータを設けなかったほかは、実施例１と同様にして、排気経路よりガスを排気させた。
その結果、連続焼成炉１０を８時間、連続稼働させた時点で、排気経路２５に２２．２ｇの堆積物が発生した。
なお、サイクロンにより回収した粉末の組成は、Ｃ：３３．７５ｍｏｌ％、Ｏ：３０．５５ｍｏｌ％、Ｓｉ：１０．１２ｍｏｌ％、Ｃａ：１０．５５ｍｏｌ％、Ｆｅ：５．９１ｍｏｌ％、その他の成分：９．４４ｍｏｌ％であり、実施例１で回収した粉末と、その組成は余り変わらなかった。 (Comparative Example 1)
Gas was exhausted from the exhaust path in the same manner as in Example 1 except that the heater was not provided in the exhaust path provided in the continuous firing furnace.
As a result, 22.2 g of deposits were generated in the exhaust passage 25 when the continuous firing furnace 10 was continuously operated for 8 hours.
The composition of the powder recovered by the cyclone was C: 33.75 mol%, O: 30.55 mol%, Si: 10.12 mol%, Ca: 10.55 mol%, Fe: 5.91 mol%, and other components: It was 9.44 mol%, and the powder recovered in Example 1 and its composition were not so different.
１０　連続焼成炉
１１、１６　脱気エリア
１２　予熱エリア
１３　昇温・焼成エリア
１４　徐冷エリア
１５　冷却エリア
１７（１７ａ、１７ｂ、１７ｃ、１７ｄ）　測温器（熱電対）
２１　マッフル
２２　加熱用ヒータ
２３　断熱材
２４　炉材
２５　排気経路
２５ａ　内部配管
２５ｂ　外部配管
２６　ヒータ　
２７　断熱層
２８　捕集装置
２９　搬送部材
３０　ハニカム焼成体
３１　セル
３２　封止材
３３　セル隔壁
４０　ハニカムフィルタ
４１　接着材層
４２　コート層
４５　セラミックブロック
１００　ハニカム成形体
１１０　セル
１２０　封止材
１３０　壁部 DESCRIPTION OF SYMBOLS 10 Continuous baking furnaces 11 and 16 Deaeration area 12 Preheating area 13 Temperature rising and baking area 14 Slow cooling area 15 Cooling area 17 (17a, 17b, 17c, 17d) Thermometer (thermocouple)
21 Muffle 22 Heating heater 23 Heat insulating material 24 Furnace material 25 Exhaust path 25a Internal piping 25b External piping 26 Heater
27 Heat insulating layer 28 Collection device 29 Transport member 30 Honeycomb fired body 31 Cell 32 Sealing material 33 Cell partition wall 40 Honeycomb filter 41 Adhesive layer 42 Coat layer 45 Ceramic block 100 Honeycomb compact 110 Cell 120 Sealing material 130 Wall

Claims (6)

  1. ＳｉＣ粒子を含む成形体を２０００～２３００℃で連続的に焼成処理することにより再結晶ＳｉＣを製造するための連続焼成炉であって、
    前記連続焼成炉の途中に、炉内に存在するＳｉＯを含むガスを、１５００～１９００℃の温度を保ちながら排気する排気経路が設置されていることを特徴とする連続焼成炉。     A continuous firing furnace for producing recrystallized SiC by continuously firing a compact containing SiC particles at 2000 to 2300 ° C.,
    A continuous firing furnace characterized in that an exhaust passage for exhausting a gas containing SiO present in the furnace while maintaining a temperature of 1500 to 1900 ° C. is provided in the middle of the continuous firing furnace.
  2. 前記排気経路は、前記連続焼成炉の１５００～１９００℃の温度領域に設置されている請求項１に記載の連続焼成炉。 The continuous firing furnace according to claim 1, wherein the exhaust path is installed in a temperature range of 1500 to 1900 ° C of the continuous firing furnace.
  3. 前記排気経路は、該排気経路内を流通するガスを加熱するためのヒータを備えている請求項１又は２に記載の連続焼成炉。 The continuous firing furnace according to claim 1 or 2, wherein the exhaust path includes a heater for heating a gas flowing through the exhaust path.
  4. 前記ヒータは、炭素製である請求項１～３のいずれかに記載の連続焼成炉。 The continuous firing furnace according to any one of claims 1 to 3, wherein the heater is made of carbon.
  5. 前記排気経路の末端には、サイクロン型の捕集装置が設置されている請求項１～４のいずれかに記載の連続焼成炉。 The continuous firing furnace according to any one of claims 1 to 4, wherein a cyclone-type collection device is installed at an end of the exhaust path.
  6. 前記連続焼成炉は、ＳｉＣ粒子を含み、長さ方向に複数の貫通孔が並設された柱状のハニカム成形体を連続的に焼成処理してハニカム焼成体を製造するための焼成炉である請求項１～５のいずれかに記載の連続焼成炉。 The continuous firing furnace is a firing furnace for producing a honeycomb fired body by continuously firing columnar honeycomb formed bodies containing SiC particles and having a plurality of through holes arranged in parallel in a length direction. Item 6. The continuous firing furnace according to any one of Items 1 to 5.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0925112A (en) * 1995-07-11 1997-01-28 Shin Etsu Chem Co Ltd Treatment of metal silicate and apparatus therefor
JP2001261442A (en) * 2000-03-17 2001-09-26 Ngk Insulators Ltd Production process of recrystallized silicon carbide
JP2002249385A (en) * 2001-02-22 2002-09-06 Ibiden Co Ltd Calcination furnace, method for removing silicon monoxide in calcination furnace and method for manufacturing silicon carbide filter
WO2007091451A1 (en) * 2006-02-10 2007-08-16 Ngk Insulators, Ltd. Method of discharging gas from continuous oven and gas discharge structure

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0925112A (en) * 1995-07-11 1997-01-28 Shin Etsu Chem Co Ltd Treatment of metal silicate and apparatus therefor
JP2001261442A (en) * 2000-03-17 2001-09-26 Ngk Insulators Ltd Production process of recrystallized silicon carbide
JP2002249385A (en) * 2001-02-22 2002-09-06 Ibiden Co Ltd Calcination furnace, method for removing silicon monoxide in calcination furnace and method for manufacturing silicon carbide filter
WO2007091451A1 (en) * 2006-02-10 2007-08-16 Ngk Insulators, Ltd. Method of discharging gas from continuous oven and gas discharge structure

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