JP2010000426A - Solid housing container, reaction tank, and reaction apparatus - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a solid housing container in which the action initiated when a solid and a liquid are brought into contact with each other is stably controlled and to provide a reaction tank and a reaction apparatus. <P>SOLUTION: A basket 202 is housed in an outer container having a first circulation part 252 together with caustic soda. The basket 202 is provided with a bottom 216, an outer cylinder 210 and an inner cylinder 212. Caustic soda can pass through the outer cylinder 210, the inner cylinder 212 and a partition member 214. The partition member 214 is arranged at two or more places between the outer cylinder 210 and the inner cylinder 212 and inserted into the outer cylinder 210, the inner cylinder 212 and the bottom 216 and fixed there. The partition member 214 is formed by winding a 12-mesh wire net to have a cylindrical shape. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention relates to a solid container, a reaction tank, and a reaction apparatus, and more particularly, to a solid container, a reaction tank, and a reaction apparatus that can stably control an action that occurs when a solid and a liquid are brought into contact with each other.

  Patent document 1 discloses the processing method of aluminum dross residual ash. This method is characterized in that the aluminum dross residual ash is hydrothermally treated using a sodium hydroxide solution having a pH of 11.5 to 13.0 as a dispersion medium. Almidros residual ash is aluminum dross after metallic aluminum or aluminum alloy is recovered. Almidros is a substance generated in the aluminum melting step and contains aluminum oxide as a main component.

  Patent document 2 discloses the processing method of aluminum dross residual ash. This method is characterized by treating aluminum dross residual ash according to the following four steps. The first step is a step of adding calcium hydroxide or sodium hydroxide and water to the aluminum dross ash. The second step is a hydrothermal treatment of the mixture produced in the first step while maintaining the paste state with stirring and kneading at a solid content concentration of 400 g to 800 g / liter or 30 to 55 wt%. A 3rd process is a process of wash | cleaning the mixture which passed through the 2nd process with water or warm water. The fourth step is a step of obtaining an alumina composition by solid-liquid separation of the mixture washed in the third step.

  According to the invention disclosed in Patent Documents 1 and 2, harmful impurities can be efficiently removed from aluminum dross residual ash in terms of resources and facilities, and an industrially useful alumina composition can be obtained.

  Patent Document 3 discloses a method for treating aluminum dross. This method is characterized by treating aluminum dross according to the following two steps. The first step is a step in which a caustic or alkali aluminate solution is added to aluminum dross and reacted to form a liquid phase containing a soluble component and a solid phase. The second step is a step of separating the liquid phase and the solid phase.

According to the invention disclosed in Patent Document 3, the reduction of the amount of aluminum dross itself and the stability of the waste can be compatible, the equipment can be made compact, the reaction efficiency can be improved, and aluminum can be recovered from the aluminum dross.
Japanese Patent Laid-Open No. 11-207285 JP 11-319753 A JP 2000-178663 A

  However, the inventions disclosed in Patent Documents 1 to 3 have a problem that it is difficult to control the reaction that occurs when a caustic or alkali aluminate solution is added to aluminum dross. In addition to these substances, it is often not easy to stably control the action that occurs when a solid and a liquid are brought into contact with each other.

  The present invention has been made to solve the above-described problems, and its object is to provide a solid container, a reaction vessel, and a reaction that can stably control the action that occurs when a solid and a liquid are brought into contact with each other. To provide an apparatus.

  In order to achieve the above object, according to one aspect of the present invention, the solid container is accommodated together with the liquid in an outer container having a member for introducing the liquid to the bottom. The solid container includes a bottom portion, an outer cylinder connected to the bottom portion, through which liquid can pass, and an inner cylinder surrounded by the outer cylinder, connected to the bottom portion, and through which liquid can pass. The solid container further includes a plurality of partition members that are provided between the outer cylinder and the inner cylinder, allow liquid to pass therethrough, and partition the outer cylinder and the inner cylinder.

  The solid container is stored together with the liquid in the outer container. The liquid can pass through the outer cylinder, the inner cylinder, and the partition member of the solid container. Thereby, the liquid enters the accommodation space through the outer cylinder, the inner cylinder, and the partition member. Since the liquid is introduced into the bottom in the outer container, the liquid contacts the liquid in order from the solid in the bottom of the accommodation space. In order from the solid at the bottom, the liquid that has passed through the outer cylinder, the inner cylinder, and the partition member comes into contact with the liquid, so that it is possible to stabilize the action that occurs when the liquid contacts the solid. As a result, it is possible to stably control the action that occurs when the solid and the liquid are brought into contact with each other.

  The partition member described above preferably has a cylindrical portion. When the partition member has a cylindrical portion, the inside of the cylindrical portion can be a liquid passage. When the inside of the cylindrical portion becomes a liquid passage, the liquid can be easily supplied to the space partitioned by the outer cylinder, the inner cylinder, and the partition member. In addition, it is easier to provide the passage as compared with the case where a liquid passage is provided between the outer cylinder and the inner cylinder using a partition member having no cylindrical portion.

  When the other situation of this invention is followed, a reaction tank is provided with an outer container and the solid container accommodated with a liquid in an outer container. The outer container includes an introduction member that introduces liquid into the bottom. The solid container includes a bottom, an outer cylinder that is connected to the bottom and allows liquid to pass through, an inner cylinder that is surrounded by the outer cylinder and connected to the bottom, and that allows liquid to pass through, and an outer cylinder and an inner cylinder. Provided with a plurality of partition members that allow liquid to pass therethrough and partition between the outer cylinder and the inner cylinder.

  According to another aspect of the present invention, the reaction device includes an outer container, a solid container accommodated in the outer container, a supply device, a measurement device, and a control device. The supply device supplies liquid into the outer container. The measuring device measures the gas amount of at least a part of the gas discharged from the outer container, and transmits gas amount information indicating the measured gas amount. The control device receives the gas amount information and feedback-controls the liquid supply amount based on the gas amount indicated by the gas amount information. The outer container has an introduction member. The introduction member introduces the liquid supplied by the supply device to the bottom. The solid container includes a bottom portion, an outer cylinder, an inner cylinder, and a plurality of partition members. The outer cylinder is connected to the bottom part and allows liquid to pass through. The inner cylinder is surrounded by the outer cylinder and connected to the bottom. And the liquid can pass through the inner cylinder. The partition member is a member provided between the outer cylinder and the inner cylinder. The partition member separates the outer cylinder from the inner cylinder. And a liquid can pass through a partition member. The control device is configured to supply a liquid when a solid that reacts with the liquid to generate a gas is stored in the storage space partitioned by the outer cylinder, the inner cylinder, and the partition member, and the gas is discharged from the outer container. To control.

  The solid container, the reaction vessel, and the reaction apparatus according to the present invention can stably control the action that occurs when the solid and the liquid are brought into contact with each other.

  Hereinafter, embodiments of the present invention will be described with reference to the drawings. In the following description, the same parts are denoted by the same reference numerals. Their names and functions are also the same. Therefore, detailed description thereof will not be repeated.

<First Embodiment>
Hereinafter, the solid container, the reaction tank, and the reaction apparatus according to the first embodiment of the present invention will be described.

  FIG. 1 is a diagram showing a processing flow of aluminum dross according to the present embodiment. FIG. 2 is a diagram illustrating a configuration of a low-grade aluminum dross processing plant according to the present embodiment. FIG. 3 is a view showing a cross section and a plane of the basket 202. FIG. 4 is an enlarged cross-sectional view showing the structure of the outer cylinder 210 of the basket 202. FIG. 5 is a diagram illustrating a configuration of the control device 36. FIG. 6 is a view showing a structure of a pipe provided between the sedimentation tank 72 and the filter press 80. As shown in FIG. FIG. 7 is a diagram showing a work flow when processing low-grade aluminum dross in the reaction tank 20.

  With reference to FIG. 1, the process flow of the aluminum dross which concerns on this embodiment is demonstrated. Aluminum dross that has been scraped and solidified from the surface of the molten metal, that is, raw dross, is put into a squeezing machine called MRM (Metal Recovery Machine). MRM squeezes molten metal aluminum from raw dross. The squeezed molten metal aluminum is recovered and used as a raw material.

  The aluminum dross after the molten metal aluminum is squeezed out is sorted and classified. As a result, coarse aluminum dross is removed. The removed aluminum dross is treated for further recovery of aluminum or used as a deoxidizer. The degree of granularity of aluminum dross to be removed is determined by specific specifications of a low-grade aluminum dross processing plant, which will be described later. In this embodiment, aluminum dross exceeding 5 mm in diameter is removed.

The fine-grained aluminum dross 240 remaining after the sorting and classification is immersed in an aqueous solution of sodium hydroxide. As a result, chemical reactions of the following formulas (1) and (2) occur, and sodium aluminate, hydrogen gas, and ammonia are generated. By the way, unless otherwise specified, in the following description, “caustic soda” means an aqueous solution of sodium hydroxide.

Hydrogen gas and some ammonia are reused as fuel. The remaining ammonia is reused as ammonia water, that is, as safety water. Since sodium aluminate is contained in water and the residue of aluminum dross remains solid, sodium aluminate is separated from the residue of aluminum dross by filtration. The separated sodium aluminate is decomposed into caustic soda and aluminum hydroxide by a chemical reaction represented by the following formula (3), that is, a crystallization reaction.

  Aluminum hydroxide produced by the crystallization reaction is separated from caustic soda as solid fine particles. The separated aluminum hydroxide is reused as a flame retardant and a flocculant. The separated caustic soda is reused for the treatment of the fine aluminum dross 240 described above.

  After sodium aluminate is formed, the aluminum dross residue separated from the sodium aluminate is washed with water and partly reused as roadbed material. A part of the water used for cleaning is diverted as makeup water during the treatment of the aluminum dross 240, and the rest is discharged after being diluted.

  With reference to FIG. 2, the structure of the low quality aluminum dross processing plant which concerns on this embodiment is demonstrated. The low-grade aluminum dross processing plant according to the present embodiment is a plant for processing the fine-grained aluminum dross 240 described above. That is, the low-grade aluminum dross processing plant according to the present embodiment is in charge of processing of a portion surrounded by a broken line in FIG. The low-grade aluminum dross processing plant according to the present embodiment includes a hydrogenation reaction unit and a crystallization unit. The hydrogenation reaction part is a part that decomposes the fine-grained aluminum dross 240 into sodium aluminate, hydrogen gas, ammonia, and a residue of aluminum dross by the chemical reaction of the above-described formulas (1) and (2). A crystallization part is a part which produces | generates sodium hydroxide and aluminum hydroxide from sodium aluminate by the chemical reaction of (3) Formula mentioned above.

  The hydrogenation reaction unit includes a reaction tank 20, a condensation tank 22, a first water sealing tank 24, an ammonia absorption tower 26, a flow meter 28, a second water sealing tank 30, a burner 32, and a flame detector. 34, a control device 36, a first caustic soda pump 38, a caustic soda tank 40, a residue filtration / separation device 42, a filtrate separation liquid storage tank 44, and a hot water tank 48.

  The hydrogenation reaction unit further includes a cooling tower 100, a refrigerant pump 102, an ammonia water storage tank 120, a water supply pump 140, a nitrogen supply device 144, and an exhaust pump 142.

  The reaction tank 20 accommodates fine aluminum dross 240 and caustic soda. Inside the reaction tank 20, the chemical reaction of the above-described formulas (1) and (2) occurs. A water supply pump 140, a nitrogen supply device 144, and an exhaust pump 142 are connected to the reaction tank 20. The water supply pump 140 supplies water into the reaction tank 20. The nitrogen supply device 144 in this embodiment is a nitrogen cylinder and supplies nitrogen into the reaction tank 20. The exhaust pump 142 forcibly exhausts gas from the reaction tank 20. The condensing tank 22 removes water vapor from the gas by cooling the gas generated as a result of the chemical reaction of the equations (1) and (2). The refrigerant used for cooling the gas in the condensing tank 22 is supplied from the cooling tower 100. The refrigerant whose temperature has been increased by being used for cooling is sent to the cooling tower 100 by the refrigerant pump 102. The first water sealing tank 24 prevents the gas from flowing backward and the outside air from entering the gas passage. In the first water sealing tank 24, a part of the ammonia is removed from the gas discharged from the condensing tank 22. The ammonia absorption tower 26 removes ammonia from the gas that has passed through the first water sealing tank 24. The gas that has passed through the ammonia absorption tower 26 is mainly composed of hydrogen and contains several ppm to several tens of ppm of ammonia. The ammonia removed by the first water sealing tank 24 and the ammonia absorption tower 26 is stored as ammonia water in the ammonia water storage tank 120 and reused. The flow meter 28 measures the flow rate of the gas that has passed through the ammonia absorption tower 26, that is, the amount of gas that has passed through the pipe at a predetermined time. The second water-sealed tank 30 prevents gas from flowing backward from the burner 32 and backfire. The burner 32 burns the gas that has passed through the second water sealing tank 30. Thereby, as mentioned above, hydrogen gas and a part of ammonia are reused as fuel. The flame detector 34 detects the presence or absence of a flame. In the present embodiment, the flame detector 34 is also a device (convergence detection device) that detects whether or not the chemical reactions of the above-described equations (1) and (2) have converged. This is because the gas that has passed through the second water-sealed tank 30 is burned by the burner 32 and the gas that has passed through the second water-sealed tank 30 is generated by the chemical reaction of the formulas (1) and (2). . Since the flame detector 34 operates as a convergence detection device, only in this embodiment, “convergence” is synonymous with a decrease in the generation rate of hydrogen gas to such an extent that combustion in the burner 32 cannot be continued. . The control device 36 controls the first caustic soda pump 38 based on the gas flow rate measured by the flow meter 28 and the presence or absence of flame detected by the flame detector 34. The first caustic soda pump 38 supplies caustic soda to the reaction tank 20. The caustic soda tank 40 stores caustic soda supplied by the first caustic soda pump 38. The residue filtration / separation device 42 removes water-insoluble solids from the mixture of aluminum dross and aqueous sodium aluminate solution by filtration. This solid is a residue after the above-described reaction of aluminum dross. The residue filtration / separation device 42 also removes water-insoluble solids from the mixture of aluminum dross and aqueous sodium aluminate solution by sedimentation. The filtrate separation liquid storage tank 44 temporarily stores the sodium aluminate aqueous solution from which the aluminum dross residue has been removed. The filtrate separation liquid storage tank 44 has a heating means using warm water. The heating means in the present embodiment includes a hot water tank 48 and a hot water circulation pump 49. The hot water tank 48 is provided with a heater 550 and a thermometer 552, and assists in heating the sodium aluminate aqueous solution in the precipitation tank 52 and the filtrate separation liquid storage tank 44. The heater 550 heats the hot water circulating through the precipitation tank 52 and the filtrate separation liquid storage tank 44. The thermometer 552 is a tool for measuring the temperature of the circulating hot water.

  The crystallization unit includes an aqueous solution pump 50, a precipitation tank 52, a recovery tank 54, a centrifuge 56, a filtrate storage tank 58, and a filtrate pump 60.

  The aqueous solution pump 50 supplies the sodium aluminate aqueous solution stored in the filtrate separation liquid storage tank 44 to the precipitation tank 52. Since the sodium aluminate aqueous solution is once stored in the filtrate separation liquid storage tank 44, the supply of the sodium aluminate aqueous solution to the precipitation tank 52 by the aqueous solution pump 50 is maintained at a constant flow rate. The precipitation tank 52 temporarily stores a sodium aluminate aqueous solution. The sodium aluminate aqueous solution stored in the precipitation tank 52 is maintained at a constant temperature by the circulating hot water supplied from the hot water tank 48. As a result, the chemical reaction of the above-described formula (3) occurs, and sodium aluminate is decomposed into sodium hydroxide and aluminum hydroxide. The recovery tank 54 temporarily stores the supernatant in the precipitation tank 52, that is, the caustic soda regenerated by the above-described equation (3). The centrifuge 56 separates sodium hydroxide from the mixture of caustic soda and aluminum hydroxide. In this embodiment, when separating caustic soda and aluminum hydroxide, washing water is added for the purpose of removing caustic soda attached to the aluminum hydroxide. The aluminum hydroxide separated by the centrifuge 56 is stored in a flexible container (flexible container bag) or the like and reused as a raw material for aluminum as described above. The filtrate storage tank 58 temporarily stores the caustic soda separated by the centrifuge 56. The filtrate pump 60 supplies caustic soda stored in the filtrate storage tank 58 to the precipitation tank 52.

  The hydrogenation reaction unit further includes a second caustic soda pump 46. The second caustic soda pump 46 supplies the caustic soda (regeneration) stored in the recovery tank 54 to the caustic soda tank 40.

  The configuration of the reaction tank 20 will be described with reference to FIGS. 2, 3, and 4. The reaction tank 20 includes an outer container 200 and a basket 202. The outer container 200 contains caustic soda. A first circulation part 252 and a second circulation part 254 are provided at the bottom of the outer container 200. The first caustic soda pump 38 and the feed water pump 140 are connected to these. Caustic soda and water are introduced into the bottom of the outer container 200 from the first caustic soda pump 38 and the water supply pump 140 via the first circulation part 252 and the second circulation part 254. The basket 202 is accommodated in the outer container 200 together with caustic soda.

  The basket 202 includes an outer cylinder 210, an inner cylinder 212, a plurality of partition members 214, a bottom portion 216, and an insertion guide member 218 for smooth insertion into the reaction tank 20.

  The outer cylinder 210 is fixed with bolts and hinges so that it can be easily attached to and detached from the bottom 216, and has a structure through which caustic soda can pass. A specific structure of the outer cylinder 210 will be described later. The inner cylinder 212 is surrounded by the outer cylinder 210 and is held in close contact with the bottom 216 via a seal member (not shown). The inner cylinder 212 is configured by rounding a 12-mesh wire mesh into a cylindrical shape. Thereby, the inner cylinder 212 has a structure through which caustic soda can pass. The partition member 214 is provided at a plurality of locations between the outer cylinder 210 and the inner cylinder 212, and is inserted and fixed to the outer cylinder 210, the inner cylinder 212, and the bottom portion 216. The partition member 214 in the present embodiment is a 12-mesh wire net rolled into a cylindrical shape. Thereby, the caustic soda can pass through the partition member 214. Further, when hydrogen gas or ammonia gas is generated, the partition member 214 can also serve as a passage for them. In the present embodiment, the bottom portion 216 has a double structure of a stainless punching metal and a fine open wire mesh in order to prevent the fine aluminum dross 240 as a raw material from flowing out. This allows caustic soda to pass through the bottom 216. Of course, if the outflow of the fine aluminum dross 240 can be prevented, the configuration of the bottom portion 216 may not be such a double structure. The insertion guide member 218 is a member for connecting the outer cylinder 210 and the outer container 200 so as to provide a gap between the bottom of the outer container 200 and the bottom portion 216, and the outer cylinder 210 is attached to the outer container 200. It also serves as a guide when inserting.

  The outer cylinder 210 includes an outer layer 220 made of stainless punching metal and an inner layer 222 made of 12-mesh wire mesh. The outer layer 220 prevents deformation of the inner layer 222 and allows caustic soda to pass through the holes 230. The inner layer 222 is configured by a 12-mesh wire mesh, thereby preventing the fine aluminum dross 240 from flowing into the outer container 200.

  The configuration of the control device 36 will be described with reference to FIG. The control device 36 includes a computer 400, a keyboard 402, and a display 404. The computer 400 processes various information in order to control the first caustic soda pump 38. The keyboard 402 is an input device used by an administrator of a low-grade aluminum dross processing plant to input information. The display 404 is an output device that outputs information to a manager of a low-grade aluminum dross processing plant.

  The computer 400 includes a flow meter I / O (Input / Output) 410, a flame detector I / O 412, a RAM (Random Access Memory) 414, a ROM (Read Only Memory) 416, an HD device 418, and a CPU. (Central Processing Unit) 420, a pump I / O 422, an input I / O 424, and a display I / O 426. The flow meter I / O 410 is a device that communicates gas amount information and control information with the flow meter 28. The flame detector I / O 412 is a device that communicates information indicating whether or not a flame is detected with the flame detector 34. The RAM 414 temporarily stores information processed by the CPU 420. The ROM 416 stores firmware executed by the CPU 420. The HD device 418 stores software executed by the CPU 420. A program for controlling the first caustic soda pump 38 is also a kind of software. The CPU 420 processes various information by executing the above-described firmware and software, and controls the HD device 418 and the like. The pump I / O 422 is a device that communicates control information with the first caustic soda pump 38. The input I / O 424 is a device that communicates information with the keyboard 402. The display I / O 426 is a device that communicates information with the display 404.

  With reference to FIG. 2 again, the configuration of the residue filtration separation device 42 will be described. The residue filtration and separation device 42 includes a gate valve 70, a sedimentation tank 72, a first discharge valve 74, a slurry pump 76, a first ball valve 78, a filter press 80, a second discharge valve 82, A two-ball valve 84, a first aqueous solution pipe 88, and a second aqueous solution pipe 90 are provided.

  The gate valve 70 is provided in the middle of the pipe from the reaction tank 20 to the sedimentation separation tank 72, and partitions the reaction tank 20 and the residue filtration separation device 42. The sedimentation / separation tank 72 once stores the mixture discharged from the reaction tank 20. This mixture contains fine aluminum dross and sodium aluminate aqueous solution. Inside the settling tank 72, the mixture is separated into a liquid containing a lot of aluminum dross and a liquid containing a lot of sodium aluminate by utilizing the action of specific gravity separation. The liquid containing a large amount of sodium aluminate discharged from the sedimentation tank 72 passes through the first discharge valve 74 and the first aqueous solution pipe 88 and is supplied to the slurry pump 76. The slurry pump 76 supplies the liquid to the filter press 80 through the second aqueous solution pipe 90. The liquid discharged from the slurry pump 76 passes through the first ball valve 78 while being supplied to the filter press 80. The filter press 80 removes solid content from the liquid by the filtering action of the filter cloth. This solid content is the reaction residue of aluminum dross described above. The aqueous sodium aluminate solution from which the solid content has been removed is discharged to the filtrate separation liquid storage tank 44 and temporarily stored therein.

  The mud-like slurry containing a lot of aluminum dross discharged from the settling tank 72 is discharged from a dross discharge port provided at the bottom of the settling tank 72, passes through the second discharge valve 82, and is supplied to the slurry pump 76. Is done. The liquid discharged from the slurry pump 76 is discharged through the second ball valve 84. The discharged aluminum dross is washed with water as necessary, and after drying with a belt filter or the like, it is naturally dried and used as a soil stabilizer and roadbed material.

  The sedimentation tank 72 includes a supernatant liquid discharge port 502, a heater 504, and a thermometer 506. The supernatant liquid discharge port 502 is a discharge port for discharging the supernatant of the mixture discharged from the reaction tank 20. This supernatant is supplied to the slurry pump 76 as a liquid containing a large amount of sodium aluminate. The heater 504 heats the mixture in order to prevent precipitation of aluminum hydroxide due to crystallization of the mixture discharged from the reaction vessel 20. The thermometer 506 is a tool for measuring the liquid temperature of the mixture.

  In this embodiment, the manager of the low-grade aluminum dross processing plant operates the heater 504 and the heater 550, so that the liquid temperature of the mixture and the liquid temperature of the sodium aluminate aqueous solution are maintained at about 353K. Of course, the temperature management may be automatically performed by the control device 36. In that case, the control device 36 must have I / O for monitoring these temperatures and controlling the heaters 504 and 550, and the HD device 418 needs to store software for that purpose. .

  With reference to FIG. 6, the structure of the 1st aqueous solution pipe | tube 88 and the 2nd aqueous solution pipe | tube 90 is demonstrated. The first aqueous solution pipe 88 and the second aqueous solution pipe 90 include a pipe body 570 and a heat insulating material 572. The pipe body 570 is a metal pipe through which the above-mentioned mixture passes. The material is preferably carbon steel pipe. The heat insulating material 572 is a material that blocks heat so that the liquid temperature of the mixture passing through the inside of the tube main body 570 does not decrease. Although the specific material used as the heat insulating material 572 is not specifically limited, For example, rock wool may be sufficient. Since it has such a structure, a drop in the liquid temperature of the mixture is suppressed while passing through the first aqueous solution pipe 88 and the second aqueous solution pipe 90.

  With reference to FIG. 7, the process with respect to the fine aluminum dross 240 in the reaction tank 20 is demonstrated.

  In step S600, the basket 202 is accommodated in the outer container 200. The basket 202 accommodates fine aluminum dross 240. The fine-grained aluminum dross 240 is accommodated in an accommodation space surrounded by the outer cylinder 210, the inner cylinder 212, and the partition member 214. After the basket 202 is accommodated, a lid (not shown) of the outer container 200 is closed.

  In step S <b> 602, water is supplied from the water supply pump 140 via the second circulation unit 254 of the outer container 200. Thereby, the inside of the outer container 200 is filled with water sequentially from the bottom. The target value of the amount of water supply is such that when the mixture is discharged to the residue filtration / separation device 42, the concentration of caustic soda therein is about 16 to 18%. In order to achieve this goal, it is necessary to examine in advance the concentration of caustic soda in the second caustic soda pump 46.

  In step S604, the exhaust pump 142 forcibly exhausts the gas in the outer container 200. On the other hand, the nitrogen supply device 144 introduces nitrogen gas into the outer container 200. The reason for introducing nitrogen gas is to prevent an explosion accident in the reaction process of the equations (1) and (2). After the atmosphere gas in the outer container 200 is replaced with nitrogen gas until the oxygen concentration becomes 4% or less, which is the explosion limit of hydrogen, the process proceeds to the next step.

  In step S <b> 606, the first caustic soda pump 38 supplies caustic soda into the outer container 200 according to an instruction from the control device 36. Thereby, the chemical reaction of the above-mentioned formulas (1) and (2) occurs, and hydrogen, ammonia, and sodium aluminate are generated from the fine-grained aluminum dross 240. As described above, hydrogen and ammonia that could not be removed by the ammonia absorption tower 26 are burned by the burner 32.

ただし、ΔＦは流量計２８が測定したガスの流量とその目標値との差を示し、単位は立法メートル毎時である。Ｆは流量計２８が測定したガスの流量を示し、単位は立法メートル毎時である。ｆ_０は初期設定時の回転数で、単位はヘルツである。その他の係数は実際の運転結果に基づいて定められる係数である。 In supplying caustic soda, the control device 36 performs feedback control based on the gas flow rate measured by the flow meter 28. That is, the control device 36 generates a control signal and outputs it to the first caustic soda pump 38 so that the rotation speed of a motor (not shown) of the first caustic soda pump 38 follows the following equation (4).

However, ΔF indicates the difference between the gas flow rate measured by the flow meter 28 and its target value, and the unit is cubic meters per hour. F represents the gas flow rate measured by the flow meter 28, and the unit is cubic meters per hour. f ₀ is the rotation speed at the time of initial setting, and the unit is Hertz. Other coefficients are coefficients determined based on actual operation results.

  Since a specific algorithm for performing feedback control according to the equation (4) is well known, detailed description thereof will not be repeated here.

  Caustic soda is supplied from the first caustic soda pump 38 through the first flow part 252. As a result, caustic soda is also supplied from the bottom of the outer container 200. The caustic soda enters the space in which the fine aluminum dross 240 is accommodated through the outer cylinder 210, the inner cylinder 212, and the bottom 216. Fine aluminum dross 240 contacts the caustic soda in order from the bottom. Moreover, since the caustic soda enters from the outer cylinder 210, the inner cylinder 212, and the bottom 216 and the space in which the aluminum dross is accommodated is finely divided, if the height from the bottom 216 is the same, Almidros also contacts caustic soda almost simultaneously. As a result, aluminum dross comes into contact with the liquid only by an amount proportional to the amount of caustic soda supplied (liquid depth).

  In step S608, after the chemical reactions of the expressions (1) and (2) converge, the gas in the outer container 200 is forcibly exhausted by the exhaust pump 142. Whether or not the chemical reactions of the expressions (1) and (2) have converged is determined based on whether or not the flame detector 34 detects a flame. When the chemical reaction of the formulas (1) and (2) converges, there is no more gas as a fuel (strictly speaking, “the rate of gas generation is so low that combustion cannot be continued”), flame It can be judged that the chemical reaction has converged when no more is detected. When the gas in the outer container 200 is forcibly exhausted after the chemical reactions of the formulas (1) and (2) converge, the pressure equilibrium between the liquid phase and the gas phase collapses, thereby evaporating water from the liquid phase. Advances. At that time, since the heat of vaporization is taken, the liquid temperature inside the reaction tank 20 rapidly decreases. The liquid temperature inside the reaction tank 20 is as high as 95 ° C. or more due to the chemical reaction of the expressions (1) and (2), but the liquid temperature can be rapidly lowered by this treatment. The internal mixture can be safely removed in a short time.

  In step S610, the gate valve 70 is opened, and the mixture in the reaction tank 20 is discharged to the settling separation tank 72.

  Since the gas in the reaction tank 20 is replaced with water vapor by the above-described exhaust operation, in step S612, a lid (not shown) of the reaction tank 20 is opened, and the basket 202 can be safely taken out. The residue remaining in the basket 202 is used for applications such as roadbed materials after washing with water and natural drying.

  As described above, the low-grade aluminum dross processing plant according to the present embodiment can process the fine-grained aluminum dross 240 to generate hydrogen, ammonia, aluminum hydroxide, and roadbed material. Moreover, the low-grade aluminum dross processing plant according to the present embodiment can disassemble the fine-grained aluminum dross 240 little by little due to the structure of the basket 202, so that stable feedback control is possible.

  In addition, the residue filtration / separation apparatus 42 according to the present embodiment can remove the residue from the sodium aluminate aqueous solution stably and in a short time. This is because the settling tank 72 is provided with a heater 504, and the first aqueous solution pipe 88 and the second aqueous solution pipe 90 have a two-layer structure of a pipe body 570 and a heat insulating material 572. The main reason why the residue cannot be removed stably is that the filter cloth of the filter press 80 is clogged. This is because the sodium aluminate aqueous solution is lowered in temperature, so that the solubility of sodium aluminate is lowered, and the chemical reaction of the above-described formula (3) is promoted to produce a fine powder of aluminum hydroxide. by. The substance that clogs the filter cloth is a fine powder of aluminum hydroxide. By preventing the liquid temperature from decreasing, clogging is prevented in advance, so that the residue can be removed stably. Moreover, the load on the filter press 80 is reduced by providing the sedimentation separation tank 72 and removing the aluminum dross in advance. This also stabilizes the removal of the residue.

  Further, after the treatment of the fine aluminum dross 240 in the reaction tank 20, the liquid temperature is once lowered by the heat of vaporization of water vapor, so that the mixture after the reaction can be taken out safely. Since the liquid temperature can be lowered by diverting a pump for substituting the gas, a new cooling facility is unnecessary. For this reason, the cost is hardly increased. As a result, the liquid temperature can be lowered safely without complicating and increasing the size of the equipment.

<Second Embodiment>
Hereinafter, a solid container, a reaction tank, and a reaction apparatus according to a second embodiment of the present invention will be described.

  FIG. 8 is a diagram showing a configuration of a low-grade aluminum dross processing plant according to the present embodiment. FIG. 9 is a view showing a cross section of the gas generation reaction device 154.

  With reference to FIG. 8, the structure of the low quality aluminum dross processing plant which concerns on this embodiment is demonstrated. As in the first embodiment, the low-grade aluminum dross processing plant according to this embodiment is a plant for processing fine aluminum dross 240.

  The hydrogenation reaction unit according to the present embodiment includes a hopper 150, a piston pump 152, a reaction tank 20, a residue filtration and separation device 42, a feed water pump 140, a nitrogen supply device 144, and an exhaust pump 142. A gas generating reaction device 154, a pinch valve 160, a separation tank 162, a drum filter 164, a residue storage tank 166, and an ammonia treatment filter 170 are provided.

  The hopper 150 supplies fine aluminum dross 240 to the piston pump 152. The piston pump 152 pumps fine aluminum dross 240 to the gas generation reaction device 154. Water is added to the fine-grained aluminum dross 240 delivered from the piston pump 152 before entering the gas generation reactor 154. Thereby, the fine aluminum dross 240 becomes muddy. The gas generation reaction apparatus 154 continuously generates hydrogen gas, ammonia, and sodium aluminate from the fine-grained aluminum dross 240 by the chemical reaction of the expressions (1) and (2) described in the first embodiment. To do. The pinch valve 160 separates the gas generation reaction device 154 and the separation tank 162. The separation tank 162 temporarily stores the sodium aluminate aqueous solution and the aluminum dross residue. The drum filter 164 separates the liquid mixture stored in the separation tank 162 into an aqueous sodium aluminate solution and an aluminum dross residue, and discharges the residue. The residue storage tank 166 stores the residue separated by the drum filter 164. The ammonia treatment filter 170 removes ammonia that is generated by adding water to aluminum dross and leaks from the hopper 150.

  With reference to FIG. 9, the structure of the gas generation reaction apparatus 154 is demonstrated. The gas generating reaction apparatus 154 according to the present embodiment includes a cylindrical reactor main body 640 arranged in the vertical direction and a screw 641 arranged inside the reactor main body 640.

  The reactor main body 640 includes a raw material inlet 643, a caustic soda supply hole 644, and a pressure detection port 645 at the upper part of the peripheral wall 642, and the piston pump 152 described above is connected to the raw material inlet 643. The first caustic soda pump 38 is connected to the caustic soda supply hole 644 described above, and caustic soda is supplied. A pressure detection device 647 and a safety device 648 are attached to the gas escape passage 646 connected to the pressure detection port 645. A heater may be attached to the reactor main body 640 as necessary. This is to promote the reaction at the time of start-up.

  A flange 650 is attached to the upper outer surface of the reactor main body 640 described above. A mounting flange 652 through which the shaft portion 651 of the screw 641 passes is fixed to the flange 650 via a gasket 653. A gas outlet 654 is opened in the mounting flange 652 so as to face the reactor main body 640 described above. A gas such as hydrogen is discharged from the gas outlet 654.

  The shaft portion 651 is disposed along the vertical axis 655 in the reactor main body 640. A spiral blade 656 is fixed around the shaft portion 651. The spiral blade 656 forms a spiral reaction chamber 657 extending in the vertical direction in the reactor main body 640. The raw material inlet 643 and the gas outlet 654 communicate with the reaction chamber 657.

  A liquid outlet 660 communicating with the reaction chamber 657 is opened at the lower portion of the reactor main body 640. A pinch valve 160 is connected to the liquid outlet 660.

  In the low-grade aluminum dross processing plant according to this embodiment, the other devices are the same as those in the first embodiment. Its function is also the same. Therefore, detailed description thereof will not be repeated here.

  The operation of the low-grade aluminum dross processing plant of this embodiment based on the above structure will be described.

  An administrator of the low-grade aluminum dross processing plant inputs an activation command from the keyboard of the control device 36 and activates the piston pump 152 and the shaft portion 651 at the same time. Fine hopper aluminum dross 240 is put in the hopper 150 in advance, and the piston pump 152 delivers it into the reactor main body 640. A small amount of water is supplied along the way. This prevents hydrogen from leaking out of the reactor body 640.

  When the fine aluminum dross 240 is put into the reactor main body 640, the rotation of the shaft portion 651 and the supply of caustic soda are also started. Thereby, the chemical reaction of the above-mentioned formulas (1) and (2) occurs, and hydrogen gas or the like is generated. The generated hydrogen gas or the like is consumed by combustion in the burner 32. In the present embodiment, the pressure inside the gas generation reaction device 154 is controlled to about 3 KPa. This control is performed according to the height of the water seal of the water seal tank connected to the gas outlet 654.

  When aluminum dross and sodium aluminate aqueous solution accumulate to some extent at the bottom of the reactor main body 640, an open command is issued to the pinch valve 160 by the liquid level gauge 158 connected to the liquid level tank 156. Thereby, aluminum dross and sodium aluminate aqueous solution are discharged to the separation tank 162 through the liquid outlet 660. In the present embodiment, the liquid level in the reactor main body 640 is controlled by detecting the liquid level in the liquid level tank 156 and thereby opening and closing the pinch valve 160.

  The alumidos and the sodium aluminate aqueous solution are discharged to the separation tank 162 and then separated by the drum filter 164. Almidros is stored in the residue storage tank 166 as a residue. The sodium aluminate aqueous solution is once stored in the filtrate separation liquid storage tank 44 and then processed in the same manner as in the first embodiment.

  As described above, the low-grade aluminum dross processing plant according to the present embodiment can process the fine-grained aluminum dross 240 to generate hydrogen, ammonia, aluminum hydroxide, and roadbed material. In addition, the low-grade aluminum dross treatment plant according to the present embodiment can retain the fine-grained aluminum dross 240 in the reactor for a certain period of time because of the structure of the gas generation reaction device 154, and is stable and stable. Reliable feedback control is possible.

<Modification>
The embodiments disclosed herein are illustrative in all respects. The scope of the present invention is not limited based on the above-described embodiments, and various design changes may be made without departing from the spirit of the present invention.

  For example, in the first embodiment, the first circulation part 252 and the second circulation part 254 may be provided not on the bottom of the outer container 200 but on the upper part of the outer container 200. In that case, in order to guide water or caustic soda to the bottom of the outer container 200, it is desirable to provide a pipe or the like on the inner periphery of the outer container 200. Further, the insertion guide member 218 may be a member that connects either the bottom 216 or the inner cylinder 212 and the outer container 200 so as to provide a gap between the bottom of the outer container 200 and the bottom 216.

  Only one of the first aqueous solution pipe 88 and the second aqueous solution pipe 90 may include the tube body 570 and the heat insulating material 572, and the other may not include the heat insulating material 572. Although it is desirable that both the first aqueous solution pipe 88 and the second aqueous solution pipe 90 include the pipe main body 570 and the heat insulating material 572, for example, only the first aqueous solution pipe 88 includes the heat insulating material 572, and the second aqueous solution pipe 90 is a pipe. It may consist only of the main body 570. Furthermore, at least one of the first aqueous solution pipe 88 and the second aqueous solution pipe 90 may include a heater.

  The reaction tank 20 according to the first embodiment and the gas generation reaction device 154 according to the second embodiment may be used for a chemical reaction between other substances instead of the fine aluminum dross and caustic soda. In this case, if the gas generated by the chemical reaction is water-insoluble, almost all of the gas passes through the first water-sealed tank 24 and the ammonia absorption tower 26. In that case, the flow meter 28 measures the flow rate of all the generated gases.

  The determination in step S608, that is, the determination of whether or not the chemical reactions of the expressions (1) and (2) have converged may not be based on the method described above. For example, when the gas flow rate measured by the flow meter 28 falls below a threshold value, it may be determined that the chemical reactions of the equations (1) and (2) have converged. In this case, the flow meter 28 serves as a convergence detection device. Further, “convergence” in this case is synonymous with the fact that the gas flow rate (and hence the gas generation rate) is below the threshold value.

It is a figure which shows the processing flow of the aluminum dross which concerns on the 1st Embodiment of this invention. It is a figure showing composition of a low grade aluminum dross processing plant concerning a 1st embodiment of the present invention. It is a figure which shows the basket which concerns on the 1st Embodiment of this invention. It is an expanded sectional view which shows the structure of the outer cylinder of the basket which concerns on the 1st Embodiment of this invention. It is a figure which shows the structure of the control apparatus which concerns on the 1st Embodiment of this invention. It is a figure which shows the structure of the pipe | tube which concerns on the 1st Embodiment of this invention. It is a figure which shows the work flow which concerns on the 1st Embodiment of this invention. It is a figure which shows the structure of the low quality aluminum dross processing plant which concerns on the 2nd Embodiment of this invention. It is a figure which shows the structure of the gas generation reaction apparatus which concerns on the 2nd Embodiment of this invention.

Explanation of symbols

20 Reaction tank 22 Condensation tank 24 First water sealing tank 26 Ammonia absorption tower 28 Flow meter 30 Second water sealing tank 32 Burner 34 Flame detector 36 Control device 38 First caustic soda pump 40 Caustic soda tank 42 Residual filtration separation device 44 Filtration separation Liquid storage tank 48 Hot water tank 49 Hot water circulation pump 46 Second caustic soda pump 50 Aqueous solution pump 52 Deposition tank 54 Recovery tank 56 Centrifugal separator 58 Filtrate storage tank 60 Filtrate pump 70 Gate valve 72 Sedimentation separation tank 74 First discharge valve 76 Slurry pump 78 First ball valve 80 Filter press 82 Second discharge valve 84 Second ball valve 88 First aqueous solution tube 90 Second aqueous solution tube 100 Cooling tower 102 Refrigerant pump 120 Ammonia water storage tank 140 Water supply pump 142 Exhaust pump 144 Nitrogen supply device 150 Hopper 152 Piston pump 154 Generation reactor 156 Liquid level tank 158 Liquid level gauge 160 Pinch valve 162 Separation tank 164 Drum filter 166 Residue storage tank 170 Ammonia treatment filter 200 Outer container 202 Basket 210 Outer cylinder 212 Inner cylinder 214 Partition member 216 Bottom 218 Insertion guide member 220 Outer layer 222 Inner layer 230 Hole 240 Almidross 252 First flow part 254 Second flow part 400 Computer 402 Keyboard 404 Display 410 I / O for flow meter
412 I / O for flame detector
414 RAM
416 ROM
418 HD device 420 CPU
422 I / O for pump
424 I / O for input
426 I / O for display
502 Supernatant outlet 504, 550 Heater 506, 552 Thermometer 570 Tube body 572 Heat insulation material 640 Reactor body 641 Screw 642 Perimeter wall 643 Raw material inlet 644 Caustic soda supply hole 645 Pressure detection port 646 Gas escape passage 647 Pressure detection device 648 Safety device 650 Flange 651 Shaft 652 Mounting flange 653 Gasket 654 Gas outlet 655 Shaft 656 Spiral blade 657 Reaction chamber 660 Liquid outlet

Claims (4)

A solid container accommodated together with the liquid in an outer container having a member for introducing the liquid to the bottom,
The bottom,
An outer cylinder connected to the bottom and capable of passing the liquid;
An inner cylinder surrounded by the outer cylinder, connected to the bottom, and capable of passing the liquid;
A solid container, further comprising a plurality of partition members provided between the outer cylinder and the inner cylinder, through which the liquid can pass, and partitioning between the outer cylinder and the inner cylinder.   The solid container according to claim 1, wherein the partition member has a cylindrical portion. An outer container,
A reaction vessel comprising a solid container accommodated together with a liquid in the outer container,
The outer container includes an introduction member for introducing the liquid into the bottom,
The solid container is
The bottom,
An outer cylinder connected to the bottom and capable of passing the liquid;
An inner cylinder surrounded by the outer cylinder, connected to the bottom, and through which the liquid can pass;
A reaction tank comprising a plurality of partition members provided between the outer cylinder and the inner cylinder, through which the liquid can pass, and partitioning between the outer cylinder and the inner cylinder. An outer container,
A solid container accommodated in the outer container;
A supply device for supplying liquid into the outer container;
A measuring device for measuring a gas amount of at least a part of the gas discharged from the outer container and transmitting gas amount information indicating the measured gas amount;
A reaction device comprising a control device for controlling the supply amount of the liquid,
The outer container has an introduction member that introduces the liquid supplied by the supply device to the bottom,
The solid container is
The bottom,
An outer cylinder connected to the bottom and capable of passing the liquid;
An inner cylinder surrounded by the outer cylinder, connected to the bottom, and through which the liquid can pass;
A plurality of partition members provided between the outer cylinder and the inner cylinder, allowing the liquid to pass therethrough, and partitioning between the outer cylinder and the inner cylinder;
The controller is
Receiving means for receiving the gas amount information;
Information generating means for generating control information for the supply device based on the gas amount information;
Transmission means for transmitting the control information to the supply device,
The information generating means contains a solid that reacts with the liquid to generate gas in any of the accommodation spaces partitioned by the outer cylinder, the inner cylinder, and the partition member, and from the outer container A reaction device that generates the control information for controlling a supply amount of the liquid when gas is discharged.

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