Furnace wall carbon collection container and furnace wall carbon collection method

Abstract

To provide a furnace wall carbon collection container that can collect furnace wall carbon more in less time.SOLUTION: A furnace wall carbon collection container for collecting furnace wall carbon generated when coke is produced from coal, comprises: an airtight container comprising a coal burning part having a hollow columnar shape, which is made of bricks and is placed on the bottom, a furnace wall carbon adhesion part having a hollow columnar shape, which is placed on the coal burning part, and a lid part; and a columnar spacer part enclosed in the airtight container. The outer diameter of the coal burning part and the furnace wall carbon adhesion part is 20 mm or larger and 52 mm or smaller. The wall thickness of the coal burning part and the furnace wall carbon adhesion part is 1 mm or more and 5 mm or less. The height of the coal burning part is 30 mm or higher and 50 mm or lower. The height of the furnace wall carbon adhesion part is 30 mm or higher and 50 mm or lower. The gap between the outer wall of the spacer part and the inner wall of the coal burning part and the furnace wall carbon adhesion part is 1 mm or more and 5 mm or less. The height of the spacer part is 35 mm or higher and 55 mm or lower.SELECTED DRAWING: Figure 1

Description

[Technical field]

[0001] The present invention relates to a container for collecting furnace wall carbon and a method for collecting furnace wall carbon. [Background technology]

[0002] When coal is charged into a coke oven chamber and carbonized, the gas generated from the coal precipitates as carbon and adheres to the walls of the chamber. This carbon grows with repeated carbonization, but if the amount of carbon adhering to the walls of the coke oven chamber becomes excessive, the resistance to coke extrusion, as represented by the extrusion power, increases, causing clogging and damaging the walls.

[0003] Patent Document 1 discloses an apparatus for evaluating the amount of carbon adhesion to the walls of a coke oven carbonization chamber during coal carbonization, the apparatus having a sample section for placing a coal sample, a heating section for heating and carbonizing the sample, and a collection section for adhering and collecting carbon from the distilled sample, the heating section being composed of a first heating section for heating the sample section, a second heating section for heating the collection section, and an insulating section provided between the first heating section and the collection section, the apparatus raising the temperature of the first heating section from a non-heated state to the carbonization temperature while the second heating section is heated to the carbonization temperature, and the carbon adhesion evaluation apparatus (claim 1) discloses an apparatus for evaluating the amount of carbon adhesion to the walls of a coke oven carbonization chamber during coal carbonization from data on the amount of carbon that has been adhered and collected. Patent Document 1 also discloses a carbon adhesion amount evaluation method for heating a coal sample placed in a sample section, adhering and collecting carbon from the carbonized sample in a collection section, and evaluating the amount of carbon adhesion to the furnace wall of a coke oven carbonization chamber during coal carbonization from data on the amount of carbon adhered and collected, the carbon adhesion amount evaluation method including the steps of (a) placing a coal sample in the sample section, (b) heating the collection section to a carbonization temperature, (c) raising the temperature of the sample section from an unheated state to the carbonization temperature, and (d) measuring the amount of carbon adhered and collected in the collection section, and the carbon adhesion amount evaluation method (claim 4) discloses a carbon adhesion amount evaluation method for obtaining data on the carbon amount related to the sample in advance by steps (a) to (d), and determining coefficients of an estimation equation required for estimating the carbon adhesion amount. Furthermore, Patent Document 1 discloses that by raising the temperature of the sample from an unheated state to the carbonization temperature and evaluating the amount of carbon attached to the walls of the coke oven chamber during coal carbonization from the data on the amount of carbon attached and collected, it is possible to set up a highly accurate estimation formula specific to this device using a previously unavailable index (paragraph

[0013] ). [Prior art documents] [Patent documents]

[0004] [Patent Document 1] JP 2012-063213 A Summary of the Invention [Problem to be solved by the invention]

[0005] As mentioned above, carbon adhering to the walls of the coke oven chamber (hereinafter also referred to as "oven wall carbon") has a significant effect on the operation of the coke oven. Therefore, there is a demand to collect and evaluate only the oven wall carbon that is generated from coal during the coke conversion of coal.

[0006] The carbon adhesion amount evaluation device and carbon adhesion amount evaluation method described in Patent Document 1 can be used to collect oven wall carbon generated during coking of coal. In other words, it is possible to collect oven wall carbon generated during coking for each coal to be evaluated (coal sample). However, the carbon adhesion amount evaluation device and carbon adhesion amount evaluation method described in Patent Document 1 require a certain amount of time to collect oven wall carbon and have a low yield, leaving room for improvement.

[0007] The present invention has been made in consideration of the above-mentioned problems, and an object of the present invention is to provide a furnace wall carbon collection container and a furnace wall carbon collection method that enable a larger amount of furnace wall carbon to be collected in a shorter time. [Means for solving the problem]

[0008] The present inventors have conducted extensive research into a furnace wall carbon collection container and a furnace wall carbon collection method. As a result, they have found that by adopting the following configuration, it is possible to collect a larger amount of furnace wall carbon in a shorter time, and have completed the present invention.

[0009] That is, the present invention provides the following. [1] A vessel for collecting furnace wall carbon generated during the coking of coal, It is made up of bricks, A sealed container including a circular plate-shaped bottom, a hollow cylindrical coal burning unit disposed on the bottom, a hollow cylindrical furnace wall carbon deposition unit disposed on the coal burning unit and having the same inner and outer diameters as the coal burning unit, and a circular plate-shaped lid disposed on the furnace wall carbon deposition unit; A cylindrical spacer portion enclosed in the sealed container; Equipped with The outer diameter of the coal burning section and the furnace wall carbon adhesion section is 20 mm or more and 52 mm or less, The wall thickness of the coal burning section and the furnace wall carbon adhesion section is 1 mm or more and 5 mm or less, The height of the coal burning section is 30 mm or more and 50 mm or less, The height of the furnace wall carbon adhesion portion is 30 mm or more and 50 mm or less, The gap between the outer wall of the spacer portion and the inner walls of the coal burning portion and the furnace wall carbon deposition portion is 1 mm or more and 5 mm or less, A furnace wall carbon collecting container, characterized in that the height of the spacer portion is 35 mm or more and 55 mm or less.

[0010] Usually, the walls of a coke oven are made of bricks. According to the above-mentioned configuration, since the oven wall carbon collection container is made of bricks, it is possible to create an environment more similar to that of an actual oven (coke oven).

[0011] In addition, according to the above-mentioned configuration, the furnace wall carbon collecting container has a relatively small overall size as described above. Therefore, the coal can be carbonized in a short time. As a result, the furnace wall carbon can be collected in a short time.

[0012] In addition, according to the above configuration, the thickness of the coal burning section and the furnace wall carbon deposit section is 1 mm or more and 5 mm or less, which is relatively thin, and therefore the temperature outside is easily transferred to the inside during carbonization. As a result, it is possible to carbonize the coal in a short time.

[0013] In addition, according to the above configuration, since the height of the coal burning section is 30 mm or more and 50 mm or less, a relatively large amount of coal can be placed in the coal burning section. As a result, it is possible to collect a large amount of furnace wall carbon. In addition, since the height of the coal burning section is 30 mm or more and 50 mm or less, coke powder adheres to the coal burning section, and it is possible to suppress the adhesion of coke powder to the furnace wall carbon adhesion section.

[0014] In addition, according to the above-mentioned configuration, the height of the carbon adhering portion of the furnace wall is 30 mm or more and 50 mm or less, and the carbon of the furnace wall adheres to this portion. This is clear from the examples. As a result, it is possible to collect a large amount of carbon of the furnace wall.

[0015] Regarding furnace wall carbon, the inventors have found that primary pyrolysis gas generated when coal softens and melts (at about 350 to 500°C) comes into contact with the high-temperature furnace wall and is heated, causing secondary pyrolysis, which causes carbon to adhere to the furnace wall. As a result, they have found that in order to collect a large amount of furnace wall carbon, it is efficient to bring the primary pyrolysis gas into contact with a high-temperature object at the same time as it is generated. Therefore, the gap between the outer wall of the spacer section and the inner walls of the coal burning section and the carbon deposition section on the furnace wall is set to 1 mm or more and 5 mm or less. As a result, the primary pyrolysis gas of coal can be brought into contact with the high-temperature coal burning section and the carbon deposition section on the furnace wall simultaneously with the generation of the primary pyrolysis gas, and the carbon on the furnace wall can be efficiently collected.

[0016] Furthermore, according to the above-mentioned configuration, since the spacer portion is provided, it is possible to prevent the coal / coke from flying up. In addition, since the height of the spacer portion is 35 mm or more, the gap between the inner wall of the coal burning portion and the carbon deposition portion on the furnace wall can be set to 1 mm or more and 5 mm or less, so that the primary pyrolysis gas can be brought into contact with the high-temperature coal burning portion and the carbon deposition portion on the furnace wall, making it possible to efficiently collect carbon on the furnace wall.

[0017] As described above, the furnace wall carbon collecting container having the above-mentioned configuration makes it possible to collect a larger amount of furnace wall carbon in a shorter period of time.

[0018] Furthermore, the present invention provides the following:

[0019] [2] A method for collecting furnace wall carbon using the furnace wall carbon collection container according to [1], A step A of disposing coal between the bottom of the furnace wall carbon collecting container and the spacer portion; After the step A, a step B of loading the furnace wall carbon collection container with coal disposed therein into a heater adjusted to a temperature range of 700° C. or more and 1200° C. or less; After the step B, a step C of removing the furnace wall carbon collecting container from the heater and obtaining the furnace wall carbon adhered to the furnace wall carbon adhering portion; A method for collecting furnace wall carbon, comprising the steps of:

[0020] According to the above-mentioned configuration, the furnace wall carbon collection container is not heated from a low temperature (e.g., about 300°C) (i.e., semi-cold loading), but is loaded (hot loading) into a heater that has been adjusted in advance to a temperature range of 700°C to 1200°C, making it possible to collect the furnace wall carbon in a shorter time. Furthermore, according to the above-mentioned configuration, since the oven wall carbon collecting container is used, it becomes possible to collect a larger amount of oven wall carbon in a shorter period of time. Effect of the Invention

[0021] According to the present invention, it is possible to provide a furnace wall carbon collecting container and a furnace wall carbon collecting method that make it possible to collect a larger amount of furnace wall carbon in a shorter time. [Brief description of the drawings]

[0022] [Figure 1] FIG. 2 is a schematic diagram for explaining a furnace wall carbon collection container according to the embodiment. [Diagram 2] FIG. 2 is a schematic diagram for explaining a method for collecting furnace wall carbon according to the present embodiment. [Diagram 3] 1 is a graph showing the relationship between the time elapsed since a furnace wall carbon collection container was loaded into a quartz glass test tube (Example 1) or the time elapsed since the test tube was loaded into a furnace (Comparative Example 1) and the temperature of a coal sample (coal core temperature). [Figure 4] 1 is a graph showing the relationship between the number of carbonization (firing) cycles and the amount of carbon adhesion (accumulation). [Diagram 5] 1 is a graph showing the relationship between the number of carbonization (firing) cycles and the amount of carbon adhesion (cumulative) per area of ​​the carbon adhesion portion on the furnace wall. [Figure 6] FIG. 2 is a schematic diagram of an apparatus according to Comparative Example 1. [Figure 7] 1 shows X-ray diffraction spectra of carbons obtained in Example 1 and Comparative Example 1. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0023] The furnace wall carbon collecting container 10 according to this embodiment will be described below. Fig. 1 is a schematic diagram for explaining a furnace wall carbon collecting container according to the present embodiment. The furnace wall carbon collecting container 10 is a container for collecting furnace wall carbon generated when coal is coked. Specifically, the furnace wall carbon collecting container 10 can be suitably used in a furnace wall carbon collecting method described later.

[0024] The furnace wall carbon collecting container 10 is made of bricks. Since the furnace wall carbon collecting container 10 is made of bricks, it can have an environment similar to that of an actual furnace (coke oven). The bricks are not particularly limited as long as they do not melt or expand excessively even when exposed to about 1100°C, and examples thereof include silica bricks, magnetic containers, ceramic containers, etc. Silica bricks are often used for the furnace walls of coke ovens, and therefore silica bricks are particularly preferred. In other words, since it is said that the amount of carbon attached and the development of crystals differ depending on the type of brick (Journal of the Fuel Science Society, Vol. 54, No. 576 (1975) pp. 250-256), silica bricks actually used in coke ovens are preferred.

[0025] As shown in FIG. 1, the furnace wall carbon collecting vessel 10 includes a sealed vessel 20 and a cylindrical spacer portion 22 sealed within the sealed vessel 20.

[0026] The sealed container 20 is composed of a circular plate-shaped bottom 12, a hollow cylindrical coal burning section 14 arranged on the bottom 12, a hollow cylindrical furnace wall carbon deposition section 16 arranged on the coal burning section 14 and having the same inner and outer diameters as the coal burning section 14, and a circular plate-shaped lid section 18 arranged on the furnace wall carbon deposition section 16.

[0027] The coal burning section 14 and the furnace wall carbon adhesion section 16 are hollow cylindrical and have an outer diameter of 20 mm or more and 52 mm or less. The outer diameter is preferably 25 mm or more and 50 mm or less, and more preferably 30 mm or more and 50 mm or less. Since the outer diameters of the coal burning section 14 and the furnace wall carbon adhesion section 16 are 20 mm or more and 52 mm or less, and are relatively small in size, the coal can be carbonized in a short time. As a result, the furnace wall carbon can be collected in a short time.

[0028] The coal burning section 14 and the furnace wall carbon deposition section 16 have a wall thickness of 1 mm or more and 5 mm or less. The wall thickness is preferably 1 mm or more and 4 mm or less, and more preferably 1 mm or more and 3 mm or less. Since the wall thickness is 1 mm or more and 5 mm or less, and is relatively thin, it is easy to transfer the external temperature to the inside during carbonization. As a result, it is possible to carbonize the coal in a short time. The inner diameters of the coal burning section 14 and the furnace wall carbon deposition section 16 are calculated by subtracting the wall thickness from the outer diameter.

[0029] The height of the coal burning section 14 is 30 mm or more and 50 mm or less, preferably 30 mm or more and 48 mm or less, and more preferably 30 mm or more and 45 mm or less. Since the height of the coal burning section 14 is 30 mm or more and 50 mm or less, a relatively large amount of coal can be placed in the coal burning section 14. As a result, a large amount of furnace wall carbon can be collected. In addition, since the height of the coal burning section 14 is 30 mm or more and 50 mm or less, coke powder adheres to the coal burning section 14, and the adhesion of coke powder to the furnace wall carbon adhesion section 16 can be suppressed.

[0030] The height of the furnace wall carbon adhesion portion 16 is 30 mm or more and 50 mm or less, preferably 30 mm or more and 45 mm or less, and more preferably 30 mm or more and 40 mm or less. The height of the furnace wall carbon adhesion portion 16 is 30 mm or more and 50 mm or less, and furnace wall carbon adheres to this portion. This is clear from the examples. As a result, it is possible to collect a large amount of furnace wall carbon. The height of the coal burning section 14 and the height of the furnace wall carbon deposition section 16 may be the same or different.

[0031] The bottom 12 is in the shape of a circular plate. The outer diameter of the bottom 12 (outer diameter in a plan view) is not particularly limited as long as it is equal to the outer diameter of the coal burning section 14 and the furnace wall carbon deposition section 16 or larger than the outer diameter of the coal burning section 14, but can be, for example, 20 mm or more and 52 mm or less.

[0032] The thickness of the bottom 12 is not particularly limited, and may be, for example, 5 mm or more and 25 mm or less. However, in this embodiment, since it is preferable that heat is not easily transferred from the bottom 12 to the inside, it is preferable that the thickness is 10 mm or more. In order to make it difficult for heat to be transferred from the bottom 12, a heat insulating material 42 (see FIG. 2) may be provided between the bottom 12 and the heater 50. When the heat insulating material 42 is provided between the bottom 12 and the heater 50, when the furnace wall carbon collecting container 10 is hot-loaded into the quartz glass test tube 40 described later, the quartz glass test tube 40 can be prevented from being broken by the impact of loading. When the heat insulating material 42 is provided between the bottom 12 and the heater 40, the thickness of the bottom 12 may be thin (for example, 20 mm or more and 50 mm or less).

[0033] The cover portion 18 is in the shape of a circular plate. The outer diameter of the cover portion 18 (outer diameter in a plan view) is not particularly limited as long as it is equal to the outer diameter of the coal burning portion 14 and the furnace wall carbon deposition portion 16 or larger than the outer diameter of the coal burning portion 14. For example, it can be 20 mm or more and 52 mm or less.

[0034] The thickness of the lid portion 18 is not particularly limited, but may be, for example, 5 mm or more and 25 mm or less, etc. However, in this embodiment, since it is preferable that heat is not easily transferred from the lid portion 18, it is preferable that the thickness is 10 mm or more.

[0035] It is preferable that a small through hole (not shown) is provided in the lid portion 18. The size of the through hole is preferably an outer diameter of 1 mm or more and 5 mm or less, and more preferably 1 mm or more and 3 mm or less. The position of the through hole is not particularly limited, but it can be, for example, the center of a circle in a plan view. By providing the through hole, gas can be released from the through hole, and the internal pressure can be prevented from becoming excessively high.

[0036] The spacer portion 22 is cylindrical, and its outer diameter is not particularly limited as long as the gap between the outer wall of the spacer portion 22 and the inner walls of the coal burning portion 14 and the furnace wall carbon deposition portion 16 is in the range of 1 mm to 5 mm. The gap between the outer wall of the spacer portion 22 and the inner walls of the coal burning portion 14 and the furnace wall carbon deposition portion 16 is preferably 1 mm to 5 mm, and more preferably 1 mm to 3 mm. For example, if the inner walls (inner diameter) of the coal burning portion 14 and the furnace wall carbon deposition portion 16 are 43 mm, the outer diameter of the spacer portion 22 is 33 mm to 41 mm. Regarding furnace wall carbon, the inventors have found that primary pyrolysis gas generated when coal softens and melts (at about 350 to 500°C) comes into contact with the high-temperature furnace wall and is heated, causing secondary pyrolysis, which causes carbon to adhere to the furnace wall. As a result, they have found that in order to collect a large amount of furnace wall carbon, it is efficient to bring the primary pyrolysis gas into contact with a high-temperature object at the same time as it is generated. Therefore, the gap between the outer wall of the spacer section 22 and the inner walls of the coal burning section 12 and the furnace wall carbon deposition section 14 is set to 1 mm or more and 5 mm or less. As a result, the primary pyrolysis gas of coal can be brought into contact with the high-temperature coal burning section 12 and the furnace wall carbon deposition section 14 at the same time as the primary pyrolysis gas is generated, and the furnace wall carbon can be efficiently collected.

[0037] The height of the spacer portion 22 is 35 mm or more and 55 mm or less, preferably 35 mm or more and 45 mm or less, and more preferably 35 mm or more and 40 mm or less. The height of the furnace wall carbon adhesion portion 16 is 30 mm or more and 50 mm or less, and furnace wall carbon adheres to this portion. This is clear from the examples. As a result, it is possible to collect a large amount of furnace wall carbon.

[0038] As described above, the furnace wall carbon collecting container 10 makes it possible to collect a larger amount of furnace wall carbon in a shorter period of time.

[0039] Next, a method for collecting oven wall carbon according to this embodiment will be described. Fig. 2 is a schematic diagram for explaining the method for collecting oven wall carbon according to this embodiment.

[0040] The method for collecting furnace wall carbon according to this embodiment includes the following steps: A method for collecting furnace wall carbon using a furnace wall carbon collection container 10, comprising: A process A of arranging coal between the bottom 12 of the furnace wall carbon collecting container 10 and the spacer portion 22; After the step A, a step B is performed in which the furnace wall carbon collecting container 10 in which the coal is disposed is charged into a heater 50 whose temperature is adjusted to a range of 700° C. or more and 1200° C. or less; After the step B, the process includes a step C of removing the furnace wall carbon collecting container 10 from the heater 50 and obtaining the furnace wall carbon adhered to the furnace wall carbon adhering portion 16.

[0041] <Process A> In the method for collecting oven wall carbon according to this embodiment, first, coal 30 is placed between the bottom 12 and the spacer part 22 of the oven wall carbon collecting container 10. The coal 30 is the coal from which oven wall carbon is to be collected. That is, in the method for collecting oven wall carbon according to this embodiment, oven wall carbon generated from the coal 30 is collected. The coal 30 is appropriately selected depending on the purpose of collecting the oven wall carbon (for example, investigating the composition of the oven wall carbon generated from the coal, etc.).

[0042] <Process B> After the step A, the furnace wall carbon collecting container 10 with the coal 30 disposed therein is charged into a heater 50 adjusted to a temperature range of 700°C to 1200°C. The furnace wall carbon collecting container 10 may be directly charged into the heater 50, but it is preferable to preliminarily place a quartz glass test tube 40 having an inner diameter slightly larger than the outer diameter of the furnace wall carbon collecting container 10 in the heater 50, and then charge the furnace wall carbon collecting container 10 into the quartz glass test tube 40. When using the quartz glass test tube 40, it is preferable to place a heat insulating material 42 at the bottom of the quartz glass test tube 40. In order to collect a large amount of furnace wall carbon, it is efficient to bring the primary pyrolysis gas into contact with the high-temperature furnace wall carbon adhering portion 16 at the same time as the primary pyrolysis gas is generated, so that a large amount of primary pyrolysis gas is generated near the furnace wall carbon adhering portion 16, not at the bottom of the furnace wall carbon collecting container 10.

[0043] The material of the heat insulating material 42 is not particularly limited, but examples thereof include high-temperature heat insulating boards. The thickness of the heat insulating material 42 is not particularly limited, but for example, it can be 20 mm or more and 50 mm or less, or 20 mm or more and 40 mm or less. The heat insulating material 42 plays a major role as a buffer material that prevents the quartz glass test tube 40 from breaking due to the impact of loading when the furnace wall carbon collecting container 10 is hot loaded into the quartz glass test tube 40, so there is no particular limitation as long as it can withstand high temperatures. For example, Superwool, a product name manufactured by Shin-Nihon Thermal Ceramics Co., Ltd., can be used.

[0044] The heater 50 is not particularly limited as long as it can be adjusted to a temperature range of 700° C. or more and 1200° C. or less and can accommodate the furnace wall carbon collection vessel 10 and the quartz glass test tube 40 .

[0045] Thereafter, carbonization is carried out within a temperature range of 700°C to 1200°C. The carbonization temperature is preferably 1000°C to 1150°C, more preferably 1100°C to 1150°C. The carbonization time is preferably 3 minutes to 10 minutes, more preferably 3 minutes to 5 minutes, after the temperature of the coal 30 (coal core temperature) reaches a predetermined temperature (within the carbonization temperature). By setting the temperature range and carbonization time as described above, primary pyrolysis gas can be suitably generated from the coal 30, and furnace wall carbon can be suitably collected.

[0046] <Process C> After the step B, the furnace wall carbon collecting container 10 is removed from the heater 50, and the furnace wall carbon adhered to the furnace wall carbon adhering portion 16 is obtained.

[0047] The entire furnace wall carbon collecting container 10 or only the furnace wall carbon adhering portion 16 may be reused, and steps A to C may be repeated multiple times. This allows a larger amount of furnace wall carbon to be collected. When only the furnace wall carbon adhering portion 16 is reused, new materials may be used for the other components.

[0048] As described above, according to the method for collecting furnace wall carbon of this embodiment, the furnace wall carbon collecting container 10 is not heated from a low temperature (for example, about 300°C) (i.e., not semi-cold loading), but is loaded (hot loading) into the heater 50 that has been adjusted in advance to a temperature range of 900°C or more and 1200°C or less, making it possible to collect furnace wall carbon in a shorter time. Furthermore, according to the method for collecting oven wall carbon according to the present embodiment, since the oven wall carbon collecting container 10 is used, it becomes possible to collect a larger amount of oven wall carbon in a shorter period of time.

[0049] The furnace wall carbon collecting method according to this embodiment has been described above. EXAMPLES

[0050] The present invention will be described in detail below using examples. However, the present invention is not limited to the following examples as long as it does not depart from the gist of the present invention.

[0051] Example 1 <Preparing a container for collecting furnace wall carbon> First, a furnace wall carbon collecting container made of silica bricks was prepared. The dimensions of the furnace wall carbon collecting container prepared were as follows:

[0052] Bottom: circular plate, outer diameter 50 mm, height (thickness) 10 mm Coal burning section: Hollow cylinder, outer diameter 50 mm, inner diameter 43 mm, height 45 mm Furnace wall carbon adhesion part: Hollow cylindrical, outer diameter 50 mm, inner diameter 43 mm, height 30 mm Lid: Circular plate, outer diameter 50 mm, height (thickness) 10 mm, with a through hole of outer diameter 2.5 mm in the center when viewed from above Spacer part: Cylindrical, outer diameter 40 mm, height 40 mm

[0053] The furnace wall carbon collection container was manufactured as follows. First, a drill press [cutting jig: Maruto Diamond Core Bit] was used to carve out a silica brick (Yotai refractory brick 476AK / 476BK) into a hollow cylinder (outer diameter 50 mm, inner diameter 43 mm).Then, the carved out hollow cylinder was cut into pieces with a height of 30 mm (for the carbon-attached part of the furnace wall) and 45 mm (for the coal-burning part) using a cutting machine [Refine Tech Refine Cutter RCA-237]. In addition, from the waste material generated during the process, a bottom portion with an outer diameter of 50 mm and a thickness of 10 mm, a lid portion with an outer diameter of 50 mm and a thickness of 10 mm, and a cylindrical spacer portion with an outer diameter of 40 mm and a height of 40 mm were made. A through hole having an outer diameter of 2.5 mm was drilled in the center of the circular plate (center in plan view) of the lid using a concrete drill bit.

[0054] <Collection of furnace wall carbon> First, the weight of the bricks in the carbon-adhered part of the furnace wall was measured. Next, the coal-burning part was placed on the bottom so that the outer circumference of the bottom and the outer circumference of the coal-burning part were aligned, and the bottom and the coal-burning part were fixed with Cellophane Tape (registered trademark). Next, 38 g of a coal sample with a bulk density (BD) of 0.94 dry-g / cm was placed in the coal-burning part. 3 The coal was packed so that the height of the coal in the vessel was about 30 mm. The coal samples used had the following properties: (Characteristics of coal samples) ASH: 8.8% VM: 35.8% TS: 0.42% Gieseler IST: 398℃ Gieseler MFT: 436℃ Gieseler MFD:271ddpm Gieseler logMF:2.43logddpm Gieseler ST: 464℃ Ro: 0.74% TI: 16.9%

[0055] Next, the spacer part was placed on the coal sample. Next, the furnace wall carbon adhesion part was placed on the coal burning part so that the outer periphery of the coal burning part and the outer periphery of the furnace wall carbon adhesion part were aligned, and the coal burning part and the furnace wall carbon adhesion part were fixed with Cellophane Tape (registered trademark). Furthermore, the lid part was placed on the furnace wall carbon adhesion part so that the outer periphery of the furnace wall carbon adhesion part and the lid part were aligned, and the furnace wall carbon adhesion part and the lid part were fixed with Cellophane Tape (registered trademark).

[0056] A 40 mm thick heat insulating material (product name: Superwool, manufactured by Nippon Thermal Ceramics Co., Ltd.) was placed at the bottom of a quartz glass test tube with an inner diameter of 50 mm. This quartz glass test tube was placed in a test tube furnace (manufactured by Osaka Seiko Co., Ltd.) and heated to 1000°C and maintained at that temperature. The test tube furnace corresponds to the heater of the present invention.

[0057] Next, the furnace wall carbon collection container containing the coal sample was placed in a quartz glass test tube (hot loading) and carbonized for 20 minutes. After that, N was poured into the quartz glass test tube.2 While the gas was flowing in, the furnace wall carbon collection container was removed from the test tube furnace (heating furnace) and allowed to cool to 150° C. The cooling was performed by introducing N 2 The reaction was carried out under a gas flow. The cellophane tape (registered trademark) was used to secure each part (each component) of the furnace wall carbon collection container to each other before inserting it into the quartz glass test tube. It will be carbonized and peeled off when heated to 1000°C, but this will not affect the collection of furnace wall carbon.

[0058] After cooling to 150°C, the bricks at the carbon-adhered portion of the furnace wall were weighed, and the weight of the adhering carbon was calculated from the difference between the weight of the bricks at the carbon-adhered portion of the furnace wall before carbonization and the weight of the adhering carbon.

[0059] The carbonization test was carried out by inserting a thermocouple into the coal sample to monitor the temperature at the center of the coal sample. Figure 3 is a graph showing the relationship between the time elapsed after the furnace wall carbon collection container was inserted into the quartz glass test tube and the temperature of the coal sample (coal core temperature) (graph labeled "Example").

[0060] The same operation was repeated using the furnace wall carbon collection container used above (furnace wall carbon collection container with carbon still attached thereto). That is, 38 g of a coal sample was filled into the coal burning section, the bottom of which and the coal burning section were fixed with Cellophane Tape (registered trademark), a spacer section was placed on top of the coal sample, the furnace wall carbon adhesion section with carbon from the first distillation still attached was placed on top of the coal burning section, a lid section was placed on the furnace wall carbon adhesion section, the furnace wall carbon collection container containing the coal sample was loaded (hot loading) into a quartz glass test tube kept at 1000°C, distilled for 20 minutes, and allowed to cool to 150°C. In this example, dry distillation was carried out three times in total.

[0061] The total amount of carbon adhesion in the three carbonizations is shown in Table 1. Table 1 also shows the amount of carbon adhesion per area of ​​the carbon adhesion part on the furnace wall, and the amount of carbon adhesion per charged coal sample. Furthermore, Fig. 4 shows a graph of the relationship between the number of carbonizations (firing) and the amount of carbon adhesion (cumulative). Fig. 5 shows a graph of the relationship between the number of carbonizations (firing) and the amount of carbon adhesion (cumulative) per area of ​​the carbon adhesion part on the furnace wall.

[0062] [Table 1]

[0063] As shown in Table 1, in the embodiment, a total of 519.8 mg of furnace wall carbon was obtained in three carbonizations. The area of ​​the furnace wall carbon deposits was 43 mm inner diameter × 3.14 × 30 mm height = 40.506 cm 2 Therefore, the amount of carbon per unit area of ​​the carbon deposit on the furnace wall is 519.8 mg / 40.506 cm 2 =about 12.8mg / cm 2 In addition, the total amount of coal sample charged in the three carbonizations was 38g x 3 = 114g, so 519.8mg / 114g = approximately 4.6mg per gram of coal sample.

[0064] (result) In Example 1, a furnace wall carbon collecting container with a relatively small overall dimension was used as described above, and the furnace wall carbon collecting container was charged (hot charging) into a quartz glass test tube already heated to 1000°C, so the charcoal core temperature reached approximately 1000°C in a short time. Therefore, as can be seen from Figure 3, the carbonization was completed in about 20 minutes from the start, and one cycle of operation could be completed in about 60 minutes including the cooling time. In Comparative Example 1 described later, one cycle was about 200 minutes, so it can be said that the furnace wall carbon could be collected in a short time. Moreover, a larger amount of furnace wall carbon was collected compared to Comparative Example 1 described later. Specifically, in Example 1, 519.8 mg of carbon was collected in three dry distillations. This is a larger amount of carbon collected compared to 12.4 mg in Comparative Example 1.

[0065] Comparative Example 1 <Collection of furnace wall carbon> Using the same coal sample as in Example 1, furnace wall carbon was collected by the method described in Patent Document 1 (JP 2012-063213 A). Specifically, the furnace wall carbon was collected as follows. Using the apparatus shown in FIG. 6, 1.3 g of coal sample S crushed to 0.25 mm or less was placed in a test tube with an inner diameter of 15 mm that constitutes the sample section 1 and the collection section 2, and the sample was placed in a bulk density (BD) of approximately 0.73 g / cm. 3 The test tube was filled with silica brick fragments P and suspended from above. The test tube was loaded into a furnace with the lower heater Ha held at a set temperature of 300°C and the upper heater Hb held at a set temperature of 900°C. After the temperature of the silica brick fragments P in the upper stage reached the set temperature, the temperature of the lower stage (sample part 1) was raised to 850°C at a rate of 5°C / min and the specimen was taken out after 10 minutes of dry distillation. The specimen was allowed to cool naturally to room temperature in a nitrogen stream, the brick fragments P were taken out and their weight was measured. This operation was repeated five times and the weight change of the brick fragments P was recorded each time. The silica brick piece P is a rectangular plate having dimensions of 20 mm in length, 10 mm in width, and 1 mm in thickness.

[0066] The carbonization test was carried out by inserting a thermocouple into the coal sample to monitor the temperature at the center of the coal sample. Figure 3 is a graph showing the relationship between the time elapsed after the test tube was inserted into the furnace and the temperature of the coal sample (coal core temperature) (graph labeled Comparative Example).

[0067] The total amount of carbon adhesion for three of the five carbonizations is shown in Table 1. Table 1 also shows the amount of carbon adhesion per area of ​​the silica brick pieces P and the amount of carbon adhesion per charged coal sample. As in Example 1, for Comparative Example 1, Fig. 4 shows a graph of the relationship between the number of carbonizations (firing) and the amount of carbon adhesion (cumulative), Fig. 5 shows a graph of the relationship between the number of carbonizations (firing) and the amount of carbon adhesion (cumulative) per area of ​​the silica brick pieces P, and Fig. 6 shows a graph of the relationship between the number of carbonizations (firing) and the amount of carbon adhesion (cumulative) per charged coal sample.

[0068] (result) In Comparative Example 1, the temperature was increased from 300°C to 850°C at 5°C / min, i.e., semi-cold charging was performed, and it took about 200 minutes to complete one cycle of carbonization, as can be seen from Figure 3. In addition, the amount of carbon that could be collected after three carbonizations was 12.4 mg.

[0069] <Qualitative evaluation> X-ray diffraction spectra were obtained for the carbon obtained in Example 1 and the carbon obtained in Comparative Example 1 using an X-ray diffractometer (manufactured by PANalytical, product name: X'Pert PRO MRD). The measurement conditions were as follows. The obtained X-ray diffraction spectra are shown in FIG. 8. <Measurement conditions> Measurement equipment: X-ray diffraction equipment (PANalytical, product name: X'Pert PRO MRD) Source: CuKα source Tube voltage: 45kV Tube current: 40mA Scanning speed: 2θ=5~90°: 38° / min

[0070] The bottom spectrum in Fig. 7 is the spectrum of silica bricks. The second spectrum from the bottom in Fig. 7 is the spectrum of oven wall carbon collected from a coke oven (actual oven). The third spectrum from the bottom in Fig. 7 is the spectrum of soot. The fourth spectrum from the bottom in Fig. 7 is the spectrum of carbon from Comparative Example 1. The top spectrum in Fig. 7 is the spectrum of carbon from Example 1. In the spectrum of furnace wall carbon taken from a coke oven, a broad peak was seen at 2θ=20-24°, and another broad peak was seen at 2θ=25-30°. In the spectrum of soot, a broad peak was seen at 2θ=20-24°, but no broad peak was seen at 2θ=25-30°. From these findings, the broad peak at 2θ=20-24° can be understood to be a peak derived from soot, and the broad peak at 2θ=25-30° can be understood to be a peak derived from carbon. Here, in Example 1, no broad peak was observed at 2θ=20 to 24°, but a broad peak was observed at 2θ=25 to 30°. On the other hand, in Comparative Example 1, a broad peak was observed at 2θ=20 to 24°, and further, a broad peak was observed at 2θ=25 to 30°. From these results, it was found that Example 1 produced less soot and more carbon.

[0071] Here, according to the Fuel Association Journal Vol. 48 (1969) No. 510 p. 732, it is reported that the furnace wall carbon is layered and has a structure with striped cracks, while the ceiling carbon is foamy and soot-like. The inventors observed the carbon of Example 1 and Comparative Example 1 with a SEM (scanning electron microscope) and an optical microscope, and found that the carbon of Example 1 was layered and had a structure with striped cracks. On the other hand, the carbon of Comparative Example 1 was foamy. From this, it is considered that Example 1 contains little ceiling carbon and much furnace wall carbon. Therefore, according to the method for collecting furnace wall carbon of Example 1, only the furnace wall carbon can be selectively collected with high purity. In this way, the furnace wall carbon collected with high purity can be suitably used for purposes such as selecting the most suitable coal for the operation of an actual furnace. [Explanation of symbols]

[0072] 10. Furnace wall carbon collection container 12 Bottom 14 Coal Burning Section 16 Carbon deposits on furnace wall 18 Lid 20. Airtight containers 22 Spacer part 30 Coal 40 Quartz glass test tube 42 Insulation 50 Heater

Claims

1. A vessel for collecting furnace wall carbon generated during the coking of coal, It is made up of bricks, A sealed container including a circular plate-shaped bottom, a hollow cylindrical coal burning unit disposed on the bottom, a hollow cylindrical furnace wall carbon deposition unit disposed on the coal burning unit and having the same inner and outer diameters as the coal burning unit, and a circular plate-shaped lid disposed on the furnace wall carbon deposition unit; A cylindrical spacer portion enclosed in the sealed container; Equipped with The outer diameter of the coal burning section and the furnace wall carbon adhesion section is 20 mm or more and 52 mm or less, The wall thickness of the coal burning section and the furnace wall carbon deposition section is 1 mm or more and 5 mm or less, The height of the coal burning section is 30 mm or more and 50 mm or less, The height of the furnace wall carbon deposition portion is 30 mm or more and 50 mm or less, A gap between an outer wall of the spacer portion and an inner wall of the coal burning portion and the furnace wall carbon deposition portion is 1 mm or more and 5 mm or less, A furnace wall carbon collecting container, characterized in that the height of the spacer portion is 35 mm or more and 55 mm or less.

2. A method for collecting furnace wall carbon using the furnace wall carbon collection container according to claim 1, A step A of disposing coal between the bottom of the furnace wall carbon collecting container and the spacer portion; After the step A, a step B of loading the furnace wall carbon collection container with the coal placed therein into a heater adjusted to a temperature range of 700° C. or more and 1200° C. or less; After the step B, a step C of removing the furnace wall carbon collecting container from the heater and obtaining the furnace wall carbon adhered to the furnace wall carbon adhering portion; A method for collecting furnace wall carbon, comprising the steps of:

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